CN108179054A - The extracting method of pecan tree seed oil and its application in hair dye - Google Patents
The extracting method of pecan tree seed oil and its application in hair dye Download PDFInfo
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- CN108179054A CN108179054A CN201810029813.1A CN201810029813A CN108179054A CN 108179054 A CN108179054 A CN 108179054A CN 201810029813 A CN201810029813 A CN 201810029813A CN 108179054 A CN108179054 A CN 108179054A
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- pecan tree
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- extract
- seed oil
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- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- JZRWCGZRTZMZEH-UHFFFAOYSA-N Thiamine Natural products CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N JZRWCGZRTZMZEH-UHFFFAOYSA-N 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- 235000019498 Walnut oil Nutrition 0.000 description 1
- PXFGMBLSJYYANM-UHFFFAOYSA-N [O].NC1=CC=CC(=C1)N Chemical compound [O].NC1=CC=CC(=C1)N PXFGMBLSJYYANM-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 125000000738 acetamido group Chemical group [H]C([H])([H])C(=O)N([H])[*] 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 125000004442 acylamino group Chemical group 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 239000002158 endotoxin Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000001976 enzyme digestion Methods 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 210000003754 fetus Anatomy 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000001530 fumaric acid Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000000665 guar gum Substances 0.000 description 1
- 235000010417 guar gum Nutrition 0.000 description 1
- 229960002154 guar gum Drugs 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 231100000283 hepatitis Toxicity 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 230000003752 improving hair Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- 229920006008 lipopolysaccharide Polymers 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 239000001369 metatartaric acid Substances 0.000 description 1
- 235000011042 metatartaric acid Nutrition 0.000 description 1
- HWPKGOGLCKPRLZ-UHFFFAOYSA-M monosodium citrate Chemical group [Na+].OC(=O)CC(O)(C([O-])=O)CC(O)=O HWPKGOGLCKPRLZ-UHFFFAOYSA-M 0.000 description 1
- 235000018342 monosodium citrate Nutrition 0.000 description 1
- 239000002524 monosodium citrate Substances 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 229960005323 phenoxyethanol Drugs 0.000 description 1
- 235000011007 phosphoric acid Nutrition 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000001508 potassium citrate Substances 0.000 description 1
- 229960002635 potassium citrate Drugs 0.000 description 1
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 description 1
- 235000011082 potassium citrates Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000019192 riboflavin Nutrition 0.000 description 1
- 229960002477 riboflavin Drugs 0.000 description 1
- 239000002151 riboflavin Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 210000002460 smooth muscle Anatomy 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- 235000017454 sodium diacetate Nutrition 0.000 description 1
- 229910000031 sodium sesquicarbonate Inorganic materials 0.000 description 1
- 235000018341 sodium sesquicarbonate Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000004334 sorbic acid Substances 0.000 description 1
- 235000010199 sorbic acid Nutrition 0.000 description 1
- 229940075582 sorbic acid Drugs 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 235000019605 sweet taste sensations Nutrition 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000019157 thiamine Nutrition 0.000 description 1
- KYMBYSLLVAOCFI-UHFFFAOYSA-N thiamine Chemical compound CC1=C(CCO)SCN1CC1=CN=C(C)N=C1N KYMBYSLLVAOCFI-UHFFFAOYSA-N 0.000 description 1
- 229960003495 thiamine Drugs 0.000 description 1
- 239000011721 thiamine Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- WCTAGTRAWPDFQO-UHFFFAOYSA-K trisodium;hydrogen carbonate;carbonate Chemical compound [Na+].[Na+].[Na+].OC([O-])=O.[O-]C([O-])=O WCTAGTRAWPDFQO-UHFFFAOYSA-K 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000008170 walnut oil Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000000230 xanthan gum Substances 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
- 235000010493 xanthan gum Nutrition 0.000 description 1
- 229940082509 xanthan gum Drugs 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/025—Pretreatment by enzymes or microorganisms, living or dead
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q5/00—Preparations for care of the hair
- A61Q5/10—Preparations for permanently dyeing the hair
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/04—Refining fats or fatty oils by chemical reaction with acids
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/06—Refining fats or fatty oils by chemical reaction with bases
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/02—Refining fats or fatty oils by chemical reaction
- C11B3/08—Refining fats or fatty oils by chemical reaction with oxidising agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B7/00—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils
- C11B7/0083—Separation of mixtures of fats or fatty oils into their constituents, e.g. saturated oils from unsaturated oils with addition of auxiliary substances, e.g. cristallisation promotors, filter aids, melting point depressors
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/42—Colour properties
- A61K2800/43—Pigments; Dyes
- A61K2800/432—Direct dyes
- A61K2800/4324—Direct dyes in preparations for permanently dyeing the hair
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Abstract
The present invention provides the extracting method of pecan tree seed oil, includes the following steps:(1) pecan tree slurry is prepared;(2) pecan tree crude oil is prepared;(3) pecan tree seed oil crude product is prepared;(4) exquisite pecan tree seed oil crude product obtains pecan tree seed olein product;(5) purifying pecan tree seed olein product obtains high-purity pecan tree seed oil.
Description
Technical field
The present invention relates to grease extraction purification technical field, in particular it relates to the extraction of pecan tree seed oil
Method and its application in hair dye.
Background technology
Carya illinoensis shell is easily peelable, kernel-taking is easy, is suitable for being machined, and benevolence has strong alcohol fragrance,
Not puckery, savory tasty, quality is delicate, slightly sweet taste, contains abundant fat, protein, vitamin.Benevolence is to extract oil well
Raw material, kernel percent is more than 50%, and the main component of aliphatic acid is unrighted acid in oil, and wherein oleic acid accounts for 75.1%-
76.1%, linoleic acid accounts for 17.4-20%, average to be reached as high as per 100g kernels 78.1g containing grease, 15.4g containing protein
22.5%;Containing 18 kinds of amino acid in protein, wherein eight kinds are amino acid necessary to human body;Also containing P 32 9mg, calcium
108mg, iron 3.2mg, carbohydrate 10.7g, niacin 1.0mg, thiamine 0.32mg, carrotene 0.17mg, riboflavin
0.11mg.Walnut kernel can inhibit bronchial smooth muscle tissue spasm, it also has Dingchuan ease constipation, temperature compensation lung kidney, astringing to arrest bleeding, U.S.
Also the diseases such as hepatitis, indigestion, influenza fever, stomachache and women's leucorrhea increasing can be cured the effect of holding beauty treatment.Therefore, it is pregnant
Woman, which often eats walnut, can make the skeleton development of fetus good;Children and adolescents, which often eat walnut, contributes to growth and development, protection to regard
Power, enhancing memory;Young people, which often eats walnut, can make skin smooth, strong and handsome, the middle-aged and the old often eat walnut can protect the heart support lung,
Lengthen the life intelligence development.In addition, the unsaturated glycerides energy anti-disease, anti-aging such as Carya illinoensis Linoleic acid, palmitic acid is old, and prevent
Hair matter is crisp, dry, easily broken.
In recent years, international market gradually increases high unsaturated fatty acid, the oils demand of particularly high-quality high oleic acid,
Solvent extraction method and mechanical pressing method are the prevailing technologies of current prepairng vegetable oil fat.Solvent extraction method oil yield efficiency is high, Residual oil
Rate is low, but extraction be easy to cause dissolvent residual, not only breaks up grease flavor, exists simultaneously security risk;Though mechanical pressing method
The risk of dissolvent residual is so effectively avoided, retains grease original local flavor, but cake slag residual rate is high, protein denaturation is tight in grouts
Weight, oil plant are made a low multiple use;Aqueous enzymatic method is developed on the basis of water substitution, is a kind of more oil of Recent study
Fat extractive technique, principle are by the affinity difference of oil and non-oil component to water and the fat using enzyme hydrolysis embedding grease
The ingredients such as albumen and lipopolysaccharides recycle oil to detach the two with the difference of water proportion, and aqueous enzymatic method, which carries oil, has technical equipment letter
The advantages that list, safe operation, mild extraction conditions.
Therefore, in view of the above-mentioned problems, the present invention provides a kind of extracting method of pecan tree seed oil and its in hair dye
In application, the extracting method has many advantages, such as that technical equipment simple, safe operation, extraction conditions are mild, in addition obtains
Unsaturated glyceride purity is high in pecan tree seed oil.
Invention content
To solve the above-mentioned problems, first aspect present invention provides the extracting method of pecan tree seed oil, including following
Step:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 5-60min, cooling
To room temperature, grinding obtains pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50-55 DEG C, insulation reaction 110-150min, 90 DEG C are warming up to, keeps the temperature 10-20min, is cooled to 60-65 DEG C, filtering stands and divides
Layer collects oil reservoir, obtains pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -10~-5 DEG C,
Stirring and crystallizing filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:(4-7);
The weight ratio of hydrolase described in the step (2) and pecan tree slurry is (0.02-0.05):1, the hydrolase packet
Include papain, cellulase, pectase;Pecan tree crude oil is with the mass concentration described in the step (3)
The weight ratio of 15% sodium hydroxide solution is 1:3;Pecan tree seed oil crude product described in the step (4) and the ether
Weight ratio be 1:4;The weight ratio of pecan tree seed olein product described in the step (5) and the acetonitrile is 1:12.
In one embodiment, modified silica-gel described in the step (5) is the chitosan of silica gel, grafted amino group acid.
In one embodiment, the weight of silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
Than being 1:(0.01-0.05).
In one embodiment, the pecan tree seed oil is applied in hair dye.
In one embodiment, the hair dye include A agent and B agent, calculate by weight, the A agent include go from
Sub- water 20-30 parts, 5-12 parts of surfactant, 1-5 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of antiseptic, EDETATE SODIUM 1-5
Part, 5-15 parts of colorant, 10-30 parts of plant extracts, 1-3 parts of pecan tree seed oil, 0.1-3 parts of polyvalent alcohol, polyalcohol
0.5-3 parts, 0.1-2 parts of pH adjusting agent, 1-2 parts of essence;The B agent includes 10-20 parts of deionized water, 2-5 parts of polyalcohol, pH tune
Save 0.1-2 parts of agent, 1-5 parts of EDETATE SODIUM, 3-12 parts of hydrogen peroxide.
In one embodiment, the hair dye include A agent and B agent, calculate by weight, the A agent include go from
Sub- 25 parts of water, 7 parts of surfactant, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant,
24 parts of plant extracts, 2 parts of pecan tree seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;Institute
It states B agent and includes 18 parts of deionized water, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide.
In one embodiment, plant extracts described in the hair dye A agent includes ginseng root extract, fennel fruit
Extract, german chamomile flower extract, lupulus extract, sweet mary leaf extract, Jojoba extract.
In one embodiment, ginseng root extract and institute described in plant extracts described in the hair dye A agent
State fennel berry extract, the german chamomile flower extract, the lupulus extract, the sweet mary leaf extract, it is described flash
The weight ratio of bar extract is 1:(0.1-1):(0.5-2):(0.1-1):(0.3-1.5):(1-3).
In one embodiment, ginseng root extract and institute described in plant extracts described in the hair dye A agent
State fennel berry extract, the german chamomile flower extract, the lupulus extract, the sweet mary leaf extract, it is described flash
The weight ratio of bar extract is 1:0.2:0.7:0.6:1.2:2.
Another aspect of the present invention provides a kind of hair-dyeing method, is 1 by weight by A agent and B agent:1 mixes in a reservoir
Conjunction forms mixed liquor, and is stirred evenly, and mixed liquor is applied on hair, and placement 3~after sixty minutes, it is rinsed.
The above-mentioned of the application and other features, aspect and advantage is more readily understood with reference to following detailed description.
Specific embodiment
The detailed description for preferred implementation method of the invention below of participating in the election of and including embodiment this hair can be more easily understood
Bright content.Unless otherwise defined, all technologies used herein and scientific terminology have common with fields of the present invention
The normally understood identical meaning of technical staff.When there is a conflict, the definition in this specification shall prevail.
As used herein term " by ... prepare " it is synonymous with "comprising".Term "comprising" used herein, " comprising ",
" having ", " containing " or its any other deformation, it is intended that cover including for non-exclusionism.For example, the combination comprising listed elements
Object, step, method, product or device are not necessarily limited to those elements, but can include not expressly listed other elements or
Such composition, step, method, product or the intrinsic element of device.
Conjunction " Consists of " excludes any element do not pointed out, step or component.If in claim, this
Phrase will make claim be closed, it be made not include the material in addition to the material of those descriptions, but relative normal
Except rule impurity.When being rather than immediately following after theme in the clause that phrase " Consists of " appears in claim main body,
It is only limited to the element described in the clause;Other elements are not excluded except the claim as a whole.
Equivalent, concentration or other values or parameter are excellent with range, preferred scope or a series of upper limit preferred values and lower limit
During the Range Representation that choosing value limits, this, which should be understood as, specifically discloses by any range limit or preferred value and any range
All ranges that any pairing of lower limit or preferred value is formed, regardless of whether the range separately discloses.For example, when open
During range " 1 to 5 ", described range should be interpreted as including range " 1 to 4 ", " 1 to 3 ", " 1 to 2 ", " 1 to 2 and 4 to
5 ", " 1 to 3 and 5 " etc..When numberical range is described herein, unless otherwise stated, otherwise range intention includes its end
Value and all integers and score in the range.
Singulative includes plural number and object is discussed, unless the context clearly dictates otherwise." optional " or it is " arbitrary
It is a kind of " refer to that the item described thereafter or event may or may not occur, and the description include situation that event occurs and
The situation that event does not occur.
Approximate term in specification and claims is used for modifying quantity, represents specific the present invention is not limited to this
Quantity further includes the modified part of the acceptable change without lead to related basic function close to the quantity.Phase
It answers, modifies a numerical value with " about ", " about " etc., mean that the present invention is not limited to the exact numericals.In some examples, it is approximate
Term likely corresponds to the precision of the instrument of measured value.In present specification and claims, range limits can be with
It combines and/or exchanges, these ranges include all subranges contained therebetween if not stated otherwise.
In addition, indefinite article " one kind " before element of the present invention or component and "one" quantitative requirement to element or component
(i.e. occurrence number) unrestriction.Therefore "one" or " one kind " should be read as including one or at least one, and odd number
The element or component of form also include plural form, unless the apparent purport of the quantity refers to singulative.
" polymer " means through the polymerizable compound prepared by the monomer that polymerize identical or different type.Generic term
" polymer " includes term " homopolymer ", " copolymer ", " terpolymer " and " copolymer "." copolymer " means to pass through polymerization
Polymer prepared by least two different monomers.Generic term " copolymer " including term " copolymer " (its generally to refer to by
Polymer prepared by two kinds of different monomers) (it is generally referring to what is prepared by three kinds of different monomers with term " terpolymer "
Polymer).It is also comprising the polymer manufactured by polymerizeing more kinds of monomers." blend " means that two or more is poly-
Object is closed to be mixed jointly and the polymer of formation by physics or chemical method.
In order to solve the above-mentioned technical problem, first aspect present invention provides the extracting method of pecan tree seed oil, including
Following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 5-60min, cooling
To room temperature, grinding obtains pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50-55 DEG C, insulation reaction 110-150min, 90 DEG C are warming up to, keeps the temperature 10-20min, is cooled to 60-65 DEG C, filtering stands and divides
Layer collects oil reservoir, obtains pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -10~-5 DEG C,
Stirring and crystallizing filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:(4-7);
The weight ratio of hydrolase described in the step (2) and pecan tree slurry is (0.02-0.05):1, the hydrolase packet
Include papain, cellulase, pectase;Pecan tree crude oil is with the mass concentration described in the step (3)
The weight ratio of 15% sodium hydroxide solution is 1:3;Pecan tree crude oil described in the step (3) and the saturated common salt
Water, the ether weight ratio be 1:6:5;The weight of pecan tree seed oil crude product described in the step (4) and the ether
Amount is than being 1:4;The weight ratio of pecan tree seed olein product described in the step (5) and the acetonitrile is 1:12.
Preferably, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;Institute
The weight ratio for stating hydrolase described in step (2) and pecan tree slurry is 0.036:1.
In one embodiment, papain described in the hydrolase and the cellulase, the pectase
Weight ratio be 1:(0.1-1):(0.5-1.2);Preferably, papain described in the hydrolase and the cellulose
Enzyme, the pectase weight ratio be 1:0.6:0.9.
In one embodiment, modified silica-gel described in the step (5) is the chitosan of silica gel, grafted amino group acid.
In one embodiment, the amino acid is one or more in arginine, glutamic acid, histidine;Preferably,
The amino acid is arginine, glutamic acid.
In one embodiment, the molar ratio of arginine described in the amino acid and the glutamic acid is 1:0.7.
The preparation method of the modified silica-gel includes the following steps:
(1) first 100 part of 300 mesh silica white is placed in mixer, adds 0.5 part of dibenzoyl peroxide and 5 parts of Malaysias
Acid anhydrides, is heated to 80 DEG C, and shear-mixed 0.5h obtains maleic anhydride modified silica white;
(2) chitosan, the tetra-benzyl thiram disulfide (No. CAS of grafted amino group acid is added in into step (1):10591-
85-2), N tert butyl benzothiazole 2 sulfenamide (No. CAS:95-31-8), cumyl peroxide (No. CAS:80-43-
3), then above-mentioned gained blend is placed in mould in vulcanizing press by melting temperature control at 40 DEG C, mixing time 15min
It is molded, it grinds, sieving obtains 300 mesh modified silica-gels;The maleic anhydride modified silica white and the curing tetrabenzyl autumn
Lan Mu, the N tert butyl benzothiazole 2 sulfenamide, the cumyl peroxide weight ratio be 1:0.02:0.01:
0.02。
The preparation method of the chitosan of the grafted amino group acid includes the following steps:
Chitosan, deionized water are added in into reactor, stirs 10min, adds in amino acid, condensing agent 1- ethyls-(3- bis-
Dimethylaminopropyl) carbodiimide hydrochloride (EDC, CAS:25952-53-8), coupling agent n-hydroxysuccinimide (NHS,
No. CAS:6066-82-6), with the salt acid for adjusting pH value of 0.1mol/L to 4.2,40 DEG C, insulation reaction 15h are warming up to, reaction knot
System pH is adjusted to 8 with the sodium hydroxide solution of 0.5mol/L, after product is fully precipitated, is fitted into bag filter, Yu Zheng by Shu Hou
It dialyses five days in distilled water, during which replaces first water every 6h, freeze-drying obtains the chitosan of grafted amino group acid;It is described
Chitosan is 1 with the deionized water, the molar ratio of the amino acid:10:0.5, the chitosan and the condensing agent EDC,
The weight ratio of the coupling agent NHS is 1:0.3:0.25.
Chitosan is after grafted amino group acid in the present invention, due to containing great amount of hydroxy group, amino and part second in molecular structure
The electronegativity group such as acylamino-, it is in the molecule and intermolecular there are a large amount of hydrogen bonds, due to these hydrogen bonds and intermolecular Van der Waals force
Presence, the long interchain of chitosan forms the aggregation of Non-covalent binding, then is obtained by the reaction and changes with maleic anhydride modified silica white
Property silica gel, the electronegativity group such as hydroxyl, amino and part acetylamino, promotes U.S. mountain core in the modified silica-gel stationary phase
The purification of unsaturated glyceride linoleic acid, palmitic acid in peach seed oil.
In one embodiment, the weight of silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
Than being 1:(0.01-0.05);Preferably, the weight of silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
Than being 1:0.025.
Acid value highest during extract by solvents Carya kernel oil, this may be in whipping process is extracted grease contacted with oxygen
It is more, while long-time heating, the peroxide generated in grease is made to further decompose into the small-molecule substances such as acid, aldehyde, is caused
Acid value of oil and fat increases, peroxide value is smaller;Although mechanical pressing method generates more peroxide during embryo is dried, when drying embryo
Between it is short, peroxide does not decompose largely, this may be that squeezing method extraction oil peroxidation value is higher, the reason of acid value is relatively low;Water
Walnut oil acid value, unsaponifiable matter, the phosphorus acid content of Enzymatic Extraction are low, and grease raciness.A variety of hydrolases carry out in the present invention
Synergistic effect, appropriate hydrolysis enzyme amount, enzyme digestion reaction time not only ensure that reaction has higher recovery rate, but also will not cause
The waste of hydrolase, while save the reaction time, improve efficiency.
In one embodiment, the pecan tree seed oil is applied in hair dye.
In one embodiment, the hair dye include A agent and B agent, calculate by weight, the A agent include go from
Sub- water 20-30 parts, 5-12 parts of surfactant, 1-5 parts of thickener, 1-2 parts of antioxidant, 1-3 parts of antiseptic, EDETATE SODIUM 1-5
Part, 5-15 parts of colorant, 10-30 parts of plant extracts, 1-3 parts of pecan tree seed oil, 0.1-3 parts of polyvalent alcohol, polyalcohol
0.5-3 parts, 0.1-2 parts of pH adjusting agent, 1-2 parts of essence;The B agent includes 10-20 parts of deionized water, 2-5 parts of polyalcohol, pH tune
Save 0.1-2 parts of agent, 1-5 parts of EDETATE SODIUM, 3-12 parts of hydrogen peroxide.
In one embodiment, the hair dye include A agent and B agent, calculate by weight, the A agent include go from
Sub- 25 parts of water, 7 parts of surfactant, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant,
24 parts of plant extracts, 2 parts of pecan tree seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;Institute
It states B agent and includes 18 parts of deionized water, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide.
Heretofore described surfactant includes glycerin monostearate, NaLS, octylphenol polyethylene ethylene oxide
It is one or more in ether.
The thickener includes one or more in xanthan gum, gum arabic, hydroxymethyl cellulose, guar gum.
The antioxidant includes one or more in sodium sulfite, ascorbic acid, arabo-ascorbic acid.
The antiseptic include benzoic acid, sodium benzoate, potassium sorbate, dehydroactic acid sodium and sodium Diacetate in one kind or
It is a variety of.
The colorant includes p-PDA, ethoxy-p-PDA sulfate, resorcinol, 2,4- diaminobenzene oxygen
It is one or more in base ethyl alcohol, 2- amino -3- pyridones;Preferably, the colorant for p-PDA, resorcinol, 2,
4- diamino phenoxy ethyl alcohol.
In one embodiment, p-PDA described in the colorant and the resorcinol, 2, the 4- diaminos
The weight ratio of phenoxyl ethyl alcohol is 12:7:3.
The polyvalent alcohol includes one or more in polyethylene glycol, polypropylene glycol, polyglycereol;Preferably, it is described poly- more
First alcohol is polyethylene glycol.
Heretofore described polyethylene glycol is PEG-75 lanolin.
The polyalcohol includes one or more in propylene glycol, butanediol, isopropanol;Preferably, the polyalcohol is
Propylene glycol, butanediol.
In one embodiment, the propylene glycol and the weight ratio of the butanediol are 1:1.
The pH adjusting agent can be divided into acid regulator and alkaline conditioner again, wherein, acid regulator includes lemon
It is a kind of or more in acid, sorbic acid, lactic acid, tartaric acid, malic acid, metatartaric acid, phosphoric acid, acetic acid, hydrochloric acid, ethanedioic acid, fumaric acid
Kind;Alkaline conditioner includes sodium bicarbonate, disodium hydrogen phosphate, sodium carbonate, sodium citrate, potassium citrate, sodium sesquicarbonate (sesquialter
Sodium carbonate), it is sodium dihydrogen citrate, one or more in ammonium hydroxide.
The essence includes one or more in Rosa Damascana, Lavender, lemon.
In one embodiment, plant extracts described in the hair dye A agent includes ginseng root extract, fennel fruit
Extract, german chamomile flower extract, lupulus extract, sweet mary leaf extract, Jojoba extract.
Heretofore described ginseng root extract is purchased from Shaanxi Sen Fu natural products Co., Ltd;The fennel berry extract
It is purchased from Shaanxi Sen Fu natural products Co., Ltd product;The german chamomile flower extract is purchased from the limited public affairs of Shaanxi Kang Yue biotechnologies
Department;The lupulus extract is purchased from Shaanxi Sen Fu natural products Co., Ltd;The sweet mary leaf extract is purchased from Guangzhou Lay
Abundant bio tech ltd;The Jojoba extract is purchased from Xi'an Bioisystech Co., Ltd of Tianrui.
In one embodiment, ginseng root extract and institute described in plant extracts described in the hair dye A agent
State fennel berry extract, the german chamomile flower extract, the lupulus extract, the sweet mary leaf extract, it is described flash
The weight ratio of bar extract is 1:(0.1-1):(0.5-2):(0.1-1):(0.3-1.5):(1-3).
In one embodiment, ginseng root extract and institute described in plant extracts described in the hair dye A agent
State fennel berry extract, the german chamomile flower extract, the lupulus extract, the sweet mary leaf extract, it is described flash
The weight ratio of bar extract is 1:0.2:0.7:0.6:1.2:2.
The preparation method of the coloring agent A agent is as follows:
Ionized water is added in into reactor by weight, is warming up to 45 DEG C, adds in thickener, EDETATE SODIUM, colorant, plant
Object extract, pecan tree seed oil, polyvalent alcohol, polyalcohol stir 0.5h, add in surfactant, antioxidant, antibacterial
Agent, pH adjusting agent, essence stir 1h, obtain the coloring agent A agent.
The preparation method of the coloring agent B agent is as follows:
Ionized water, polyalcohol, EDETATE SODIUM, hydrogen peroxide are added in by weight into reactor, stirs 0.5h, adds in pH
Conditioning agent stirs 1h, obtains the coloring agent B agent.
Another aspect of the present invention provides a kind of hair-dyeing method, is 1 by weight by A agent and B agent:1 mixes in a reservoir
Conjunction forms mixed liquor, and is stirred evenly, and mixed liquor is applied on hair, and placement 3~after sixty minutes, it is rinsed.
The present invention is added in the coloring agent that thickener and other auxiliary agents are prepared into, is reached using natural herbs extract
By the effect of coloring hairs, the hair dye is without any side effects to human body, Carya illinoensis Linoleic acid, palmitic acid etc.
Unsaturated glyceride energy anti-disease, anti-aging is old, and prevents hair matter crisp, dry, easily broken, the addition of dyeing auxiliaries, can reach dyeing jail
Gu, the effect taking care of hair, improve hair quality and make hair glossy.
Embodiment 1
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.025;The amino acid is arginine, glutamic acid, arginine described in the amino acid and the paddy ammonia
The molar ratio of acid is 1:0.7;
The preparation method of the modified silica-gel includes the following steps:
(1) first 100 part of 300 mesh silica white is placed in mixer, adds 0.5 part of dibenzoyl peroxide and 5 parts of Malaysias
Acid anhydrides, is heated to 80 DEG C, and shear-mixed 0.5h obtains maleic anhydride modified silica white;
(2) chitosan, tetra-benzyl thiram disulfide, the N- tertiary butyl -2- benzene of grafted amino group acid are added in into step (1)
And thiazolesulfenamide, cumyl peroxide, melting temperature is controlled at 40 DEG C, mixing time 15min, then by above-mentioned institute
It obtains blend and is placed in compression molding in vulcanizing press, grind, sieving obtains 300 mesh modified silica-gels;It is described maleic anhydride modified
Silica white and the tetra-benzyl thiram disulfide, the N tert butyl benzothiazole 2 sulfenamide, the peroxidating two are different
The weight ratio of propyl benzene is 1:0.02:0.01:0.02.
The preparation method of the chitosan of the grafted amino group acid includes the following steps:
Chitosan, deionized water are added in into reactor, stirs 10min, adds in amino acid, condensing agent 1- ethyls-(3- bis-
Dimethylaminopropyl) carbodiimide hydrochloride, coupling agent n-hydroxysuccinimide, with the salt acid for adjusting pH value of 0.1mol/L extremely
4.2,40 DEG C, insulation reaction 15h are warming up to, after reaction, system pH is adjusted to 8 with the sodium hydroxide solution of 0.5mol/L,
It after product is fully precipitated, is fitted into bag filter, dialyses five days in distilled water, during which replace first water every 6h, it is cold
It is lyophilized dry, obtains the chitosan of grafted amino group acid;The chitosan is 1 with the deionized water, the molar ratio of the amino acid:
10:0.5, the chitosan and the condensing agent EDC, the weight ratio of the coupling agent NHS are 1:0.3:0.25.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Embodiment 2
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.01;The amino acid is arginine, glutamic acid, arginine described in the amino acid and the glutamic acid
Molar ratio be 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Embodiment 3
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.05;The amino acid is arginine, glutamic acid, arginine described in the amino acid and the glutamic acid
Molar ratio be 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Embodiment 4
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.1:1.2;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.025;The amino acid is arginine, glutamic acid, arginine described in the amino acid and the paddy ammonia
The molar ratio of acid is 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Embodiment 5
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:1:0.5;Pecan tree crude oil described in the step (3) and the sodium hydroxide solution that the mass concentration is 15%
Weight ratio be 1:3;The weight of pecan tree crude oil described in the step (3) and the saturated salt solution, the ether
Than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
(5) weight ratio of the olein of pecan tree seed described in product and the acetonitrile is 1:12;Modified silicon described in the step (5)
Glue is silica gel, the chitosan of grafted amino group acid, silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
Weight ratio is 1:0.025;The amino acid is arginine, glutamic acid, arginine described in the amino acid and the glutamic acid
Molar ratio be 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 1
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving passes through 300 mesh silica gel solid phases
Stainless steel pillar, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains the high-purity U.S.
Hickory nut seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 2
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.025;The amino acid is arginine;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 3
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, the chitosan of grafted amino group acid, the chitosan of silica gel described in the modified silica-gel and grafted amino group acid
Weight ratio be 1:0.025;The amino acid is glutamic acid;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 4
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
Enzyme, cellulase, pectase, the weight of papain described in the hydrolase and the cellulase, the pectase
Than being 1:0.6:0.9;Pecan tree crude oil described in the step (3) and the sodium hydroxide that the mass concentration is 15% are molten
The weight ratio of liquid is 1:3;Pecan tree crude oil described in the step (3) and the saturated salt solution, the weight of the ether
Amount is than being 1:6:5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;The step
Suddenly the weight ratio of pecan tree seed olein product described in (5) and the acetonitrile is 1:12;It is modified described in the step (5)
Silica gel is silica gel, chitosan, and the weight ratio of silica gel described in the modified silica-gel and the chitosan is 1:0.025;
The preparation method is the same as that of Example 1 for the modified silica-gel.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 5
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase is Papain
Enzyme;Pecan tree crude oil described in the step (3) and the weight ratio of sodium hydroxide solution that the mass concentration is 15%
It is 1:3;The weight ratio of pecan tree crude oil described in the step (3) and the saturated salt solution, the ether is 1:6:
5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;Institute in the step (5)
The weight ratio for stating pecan tree seed olein product and the acetonitrile is 1:12;Modified silica-gel described in the step (5) is silicon
The chitosan of glue, grafted amino group acid, the weight ratio of silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
It is 1:0.025;The amino acid is arginine, glutamic acid, mole of arginine described in the amino acid and the glutamic acid
Than being 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Comparative example 6
The extracting method of pecan tree seed oil, includes the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 30min, is cooled to
Room temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to
50 DEG C, insulation reaction 130min, 90 DEG C are warming up to, keeps the temperature 15min, is cooled to 60 DEG C, filtering, stratification is collected oil reservoir, obtained
To pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% second
After stirring evenly, pecan tree crude oil is added portionwise in alcohol, and insulation reaction 4h with 6mol/L salt acid for adjusting pH value to 3.5, is protected
Temperature reaction 3h, is cooled to room temperature, adds in saturated salt solution and ether, stir 0.5h, stratification, collected organic layer, and depressurize
Concentration, obtains pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -8 DEG C, stirring analysis
Crystalline substance filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving is fixed by 300 mesh modified silica-gels
The stainless steel pillar of phase, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains high-purity
Pecan tree seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:6;It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is 0.036:1;The hydrolase includes Papain
The weight ratio of enzyme, cellulase, papain described in the hydrolase and the cellulase, the pectase is 1:
0.6;Pecan tree crude oil described in the step (3) and the weight ratio of sodium hydroxide solution that the mass concentration is 15%
It is 1:3;The weight ratio of pecan tree crude oil described in the step (3) and the saturated salt solution, the ether is 1:6:
5;The weight ratio of pecan tree seed oil crude product described in the step (4) and the ether is 1:4;Institute in the step (5)
The weight ratio for stating pecan tree seed olein product and the acetonitrile is 1:12;Modified silica-gel described in the step (5) is silicon
The chitosan of glue, grafted amino group acid, the weight ratio of silica gel described in the modified silica-gel and the chitosan of grafted amino group acid
It is 1:0.025;The amino acid is arginine, glutamic acid, mole of arginine described in the amino acid and the glutamic acid
Than being 1:0.7;
The preparation method of the modified silica-gel, grafted amino group acid chitosan the preparation method is the same as that of Example 1.
The pecan tree seed oil is applied in hair dye;
The hair dye includes A agent and B agent, calculates by weight, and the A agent includes 25 parts of deionized water, surface-active
7 parts of agent, 3 parts of thickener, 1 part of antioxidant, 2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts are beautiful
2 parts of state's hickory nut seed oil, 2 parts of polyvalent alcohol, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes deionized water
18 parts, 4 parts of polyalcohol, 0.5 part of pH adjusting agent, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide;
Wherein, A agent:The surfactant be NaLS, the thickener be gum arabic, the antioxygen
Agent is arabo-ascorbic acid, and the antiseptic is potassium sorbate, and the colorant is p-PDA, resorcinol, 2,4- diamino
Phenoxetol, p-PDA described in the colorant and the resorcinol, 2, the 4- diamino phenoxies ethyl alcohol
Weight ratio is 12:7:3;The polyvalent alcohol is PEG-75 lanolin;The polyalcohol is propylene glycol, butanediol, described the third two
The weight ratio of alcohol and the butanediol is 1:1;The pH adjusting agent is ammonium hydroxide;The essence is Rosa Damascana;It is described
Plant extracts includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf and carries
Take object, Jojoba extract, the ginseng root extract and the fennel berry extract, the german chamomile flower extract, the beer
Hop extraction object, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2;
B agent:The polyalcohol is propylene glycol, and the pH adjusting agent is phosphoric acid.
Performance test:
1st, pecan tree seed oil composition measuring
GC-MS analysis conditions:RTX-WAX (30.0m × 0.25mm × 0.25 μm) chromatographic column;250 DEG C of injector temperature rises
Warm program:100 DEG C of column temperature is raised to 170 DEG C with 10 DEG C/min, after keeping 1min, is raised to 230 DEG C with 3 DEG C/min, keeps 12min,
Carrier gas helium, constant current mode, flow velocity 1ml/min, Splitless injecting samples;Electron impact ion source (EI), ion source temperature 200
DEG C, interface temperature is 250 DEG C, and the ionization voltage 70eV solvent mute times are 3min;Full scan pattern, scanning mould speed 1666;
Scanning ion range is 45-500.
2nd, the assessment of hair dye color durability
The hair of dyeing is immersed in shampoo solution, with oscillator with 200rpm speed oscillations 30 minutes, flowing water punching
It washes 1 minute, then electricity consumption blowing drying, then, L values is measured with colorimeter.According to the Numerical evaluation color of the discrepancy delta L of brightness value
Persistence, smaller Δ L values refer to preferable color durability.
3rd, the assessment of hair dye color absorption
A agent and B agent are mixed with 1: 1 ratio in hair dye, which is pressed to the dosage pair of twice hair weight
The human hair level dyeing of 12cm long.The hair contains about 30% white hair.After 30 minutes, flowing water is carried out to hair dyeing with shampoo
Cleaning 1 minute, then electricity consumption blowing drying.The color of dry hair is measured with colorimeter (Hunterlab Labscan XE).By colorimetric
The brightness value L * results that meter measures are compared.Higher L* values refer to light color, and relatively low L* values then refer to dark color.Therefore, it is smaller
L* values show preferable hair dyeing effect.
4th, oil yield is the oil yield of pecan tree seed oil crude product.
1 the performance test results of table
It is seen from the above data that the extracting method of pecan tree seed oil provided by the invention, has technical equipment
Simply, safe operation, the advantages that extraction conditions are mild, unsaturated glyceride purity in the pecan tree seed oil in addition obtained
It is high.
Above-mentioned example is merely illustrative, some features of feature for explaining the present invention.Appended claim
The range as wide as possible that requirement is contemplated that is intended to, and embodiments as presented herein is only according to all possible embodiment
Combination selection embodiment explanation.Therefore, the purpose of applicant is that appended claim is not illustrated the present invention
Feature exemplary selectional restriction, and the progress in science and technology will not formed due to the inaccuracy that language is expressed and not
The possible equivalent or son being presently considered are replaced, and these variations also should in the conceived case be interpreted by appended
Claim covers.
Claims (10)
1. the extracting method of pecan tree seed oil, which is characterized in that include the following steps:
(1) pecan tree powder is added in into reactor, deionized water is warming up to 100 DEG C, keeps the temperature 5-60min, is cooled to room
Temperature, grinding obtain pecan tree slurry;
(2) into step (1), pecan tree slurry adds in hydrolase, with 6mol/L salt acid for adjusting pH value to 5.5, is warming up to 50-
55 DEG C, insulation reaction 110-150min, 90 DEG C are warming up to, keeps the temperature 10-20min, is cooled to 60-65 DEG C, is filtered, stratification,
Oil reservoir is collected, obtains pecan tree crude oil;
(3) sodium hydroxide solution that mass concentration is 15% is added in reactor, is warming up to 75 DEG C, adds in 95% ethyl alcohol, stir
After mixing uniformly, pecan tree crude oil, insulation reaction 4h, with 6mol/L salt acid for adjusting pH value to 3.5, insulation reaction is added portionwise
3h is cooled to room temperature, adds in saturated salt solution and ether, stirs 0.5h, stratification, collected organic layer, and be concentrated under reduced pressure, obtains
To pecan tree seed oil crude product;
(4) it adds in pecan tree seed oil crude product, ether into reactor, after stirring and dissolving, is cooled to -10~-5 DEG C, stirring
Crystallization filters, and freeze-drying obtains pecan tree seed olein product;
(5) pecan tree seed olein product is added in into acetonitrile, stirring and dissolving, passes through 300 mesh modified silica-gel stationary phases
Stainless steel pillar, leacheate rinse, and collect efflux, and efflux removes solvent through drying, reduced pressure, obtains the high-purity U.S.
Hickory nut seed oil;
Wherein, the weight ratio of pecan tree powder described in the step (1) and the deionized water is 1:(4-7);It is described
The weight ratio of hydrolase described in step (2) and pecan tree slurry is (0.02-0.05):1, the hydrolase includes wood
Melon protease, cellulase, pectase;Pecan tree crude oil described in the step (3) is 15% with the mass concentration
Sodium hydroxide solution weight ratio be 1:3;The weight of pecan tree seed oil crude product described in the step (4) and the ether
Amount is than being 1:4;The weight ratio of pecan tree seed olein product described in the step (5) and the acetonitrile is 1:12.
2. the extracting method of pecan tree seed oil according to claim 1, which is characterized in that described in the step (5)
Modified silica-gel is silica gel, the chitosan of grafted amino group acid.
3. the extracting method of pecan tree seed oil according to claim 2, which is characterized in that described in the modified silica-gel
The weight ratio of silica gel and the chitosan of grafted amino group acid is 1:(0.01-0.05).
4. according to the extracting method of any one of the claim 1-3 pecan tree seed oil, which is characterized in that the U.S. mountain
Walnut seed oil is applied in hair dye.
5. the extracting method of pecan tree seed oil according to claim 4, which is characterized in that the hair dye includes A agent
It with B agent, calculates by weight, the A agent includes 20-30 parts of deionized water, 5-12 parts of surfactant, and 1-5 parts of thickener resists
1-2 parts of oxygen agent, 1-3 parts of antiseptic, 1-5 parts of EDETATE SODIUM, 5-15 parts of colorant, 10-30 parts of plant extracts, pecan tree
1-3 parts of seed oil, 0.1-3 parts of polyvalent alcohol, 0.5-3 parts of polyalcohol, 0.1-2 parts of pH adjusting agent, 1-2 parts of essence;The B agent includes
10-20 parts of deionized water, 2-5 parts of polyalcohol, 0.1-2 parts of pH adjusting agent, 1-5 parts of EDETATE SODIUM, 3-12 parts of hydrogen peroxide.
6. the extracting method of pecan tree seed oil according to claim 5, which is characterized in that the hair dye includes A agent
With B agent, calculate by weight, the A agent include 25 parts of deionized water, 7 parts of surfactant, 3 parts of thickener, 1 part of antioxidant,
2 parts of antiseptic, 2 parts of EDETATE SODIUM, 10 parts of colorant, 24 parts of plant extracts, 2 parts of pecan tree seed oil, polyvalent alcohol 2
Part, 2 parts of polyalcohol, 1 part of pH adjusting agent, 1 part of essence;The B agent includes 18 parts of deionized water, 4 parts of polyalcohol, pH adjusting agent
0.5 part, 2 parts of EDETATE SODIUM, 10 parts of hydrogen peroxide.
7. the extracting method of pecan tree seed oil according to claim 6, which is characterized in that institute in the hair dye A agent
It states plant extracts and includes ginseng root extract, fennel berry extract, german chamomile flower extract, lupulus extract, sweet mary leaf
Extract, Jojoba extract.
8. the extracting method of pecan tree seed oil according to claim 7, which is characterized in that institute in the hair dye A agent
State ginseng root extract described in plant extracts and the fennel berry extract, the german chamomile flower extract, the hops
Extract, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:(0.1-1):(0.5-2):(0.1-
1):(0.3-1.5):(1-3).
9. the extracting method of pecan tree seed oil according to claim 8, which is characterized in that institute in the hair dye A agent
State ginseng root extract described in plant extracts and the fennel berry extract, the german chamomile flower extract, the hops
Extract, the sweet mary leaf extract, the Jojoba extract weight ratio be 1:0.2:0.7:0.6:1.2:2.
10. a kind of hair-dyeing method, which is characterized in that using any one of the claim 5-9 hair dyes, by A agent and B
Agent is 1 by weight:1 is mixed to form mixed liquor, and stirred evenly in a reservoir, and mixed liquor is applied on hair, is put
Put 3~after sixty minutes, it is rinsed.
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