CN106520364A - Production process of semen coicis oil through subcritical low-temperature extraction - Google Patents
Production process of semen coicis oil through subcritical low-temperature extraction Download PDFInfo
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- 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
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F1/00—Fertilisers made from animal corpses, or parts thereof
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F5/00—Fertilisers from distillery wastes, molasses, vinasses, sugar plant or similar wastes or residues, e.g. from waste originating from industrial processing of raw material of agricultural origin or derived products thereof
-
- 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
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- 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
- C11B3/12—Refining fats or fatty oils by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/40—Bio-organic fraction processing; Production of fertilisers from the organic fraction of waste or refuse
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
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- Fats And Perfumes (AREA)
Abstract
The invention relates to a production process of semen coicis oil through subcritical low-temperature extraction. The production process comprises specific steps as follows: (1) subcritical low-temperature extraction: butane is adopted as an extracting agent; (2) preparation of crude oil; (3) dewatering of the crude oil; (4) steaming out of fatty acid through molecular distillation; (5) refining of the semen coicis oil; (6) fatty acid ethyl esterification; (7) refining of fatty acid ethyl ester; (8) treatment of semen coicis residues. The natural quality of a product is sufficiently guaranteed at the low temperature under the low pressure, the oil yield is high, and the production cost is low. Besides, the semen coicis residues produced in the production process can be used as base fertilizer, the base fertilizer can supply sufficient nutrients to the peony and also has the early weeding efficacy. The production process meets the environmental protection requirement, and the resource utilization rate is increased.
Description
Technical field
The present invention relates to a kind of production technology of subcritical low-temperature extraction Semen Coicis oil, belongs to Semen Coicis oil technology of preparing neck
Domain.
Background technology
Semen Coiciss are the annual sturdy vegetation of grass family, are distributed widely in Hubei Qichun, Hunan, Hebei, Jiangsu, Fujian, mountain
More than ten provinces and regions such as east, Henan, the ripe dry seed of Semen Coiciss is Semen Coiciss, has functions that diuretic spleen invigorating, and the traditional Chinese medical science is often by which
For diseases such as damp-retention due to hypofunction of the spleen.Modern pharmacology research finds that Semen Coiciss have anti-inflammatory and antalgic, anticoagulation, antitumor, enhancing body
The functions such as immunity, regulating and controlling blood sugar blood lipid metabolism, are the traditional integration of edible and medicinal herbs health food of China, particularly effect of Semen Coiciss
Composition Semen Coicis oil, not only can be made into various pharmaceutical formulations such as injection, capsule, oral agents, and is also widely used for each
Plant in the formula of health promoting product.The application space of Semen Coiciss has been expanded in the extraction of Semen Coicis oil significantly, increased the attached of Semen Coiciss
It is value added.Adopt milling process and 6# solvent extraction methods more traditional extraction technique, develop CO again at present2Supercritical extraction,
CN102994221A discloses a kind of method that Semen Coicis oil is extracted from Semen Coiciss, and the method includes following steps：A. powder
It is broken；B. supercritical CO2Extraction；C. filter deacidification；D. separate.Although organic solvent, nontoxic nothing are not used in the method overall process
Zest, nonflammable non-explosive, production operation is safer；But CO2Supercritical extraction pressure is extra-high, and apparatus expensive is unsuitable large-scale
Change scale, production cost is high.
In these methods, milling process oil yield is low, and 6# solvent extraction methods can introduce normal hexane residual, and normal hexane has nerve
Toxicity, CO2Supercritical extraction, energy consumption are too high, and equipment investment is expensive, and production cost is too high.
The content of the invention
For the problems referred to above, the invention provides a kind of production technology of subcritical abstraction low temperature Semen Coicis oil and production dress
Put, the present invention extracts the Semen Coicis oil in Semen Coiciss using subcritical butane, as Semen Coiciss crude oil acid value is generally greater than 20KOH
Mg/g, directly routinely refine, refining loss height, neutral oil yield are low, and the present invention is removed after fatty acid again using Physical Separation Technology
Refine.The technique adopts low-temp low-pressure, fully ensures that the natural quality of product, and oil yield is high, low production cost.The skill of the present invention
Art scheme is as follows：
A kind of production technology of subcritical low-temperature extraction Semen Coicis oil, comprises the following steps that：
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, Semen Coicis powder is put into the extractor of two series connection
In one of tank, to extractor evacuation, it is stirred after adding extractant butane, the quality volume of Semen Coicis powder and butane
Than for 1:2-3 (g/mL), rotating speed are 60r/min, and extraction temperature is 35-55 DEG C, pressure 0.25-0.40MPa, and extraction time is
40-50min, extraction times are 3 times, obtain the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
Preferably, 60 mesh sieves are crossed after crush Semen Coiciss, Semen Coicis powder is obtained, Semen Coicis powder is put into into the extraction of two series connection
Take in one of tank of tank, to extractor evacuation, be stirred after adding extractant butane, the matter of Semen Coicis powder and butane
Amount volume ratio g/mL is 1:2.5, rotating speed is 60r/min, and extraction temperature is 45 DEG C, and pressure 0.35MPa, extraction time are 45min,
Extraction times are 3 times, obtain the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil.
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with the heart of a lotus seed
The solvent of Semen Coicis oil is entered, and evaporator pressure rise, the solvent in tank to be extracted dissolved with crude oil fully flow into evaporator, closes extraction
The valve between tank and evaporator is taken, evaporator is warming up to into 40-55 DEG C again then, open precipitation valve, by compressor pressure
Contracting, condenser condense recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then beat
Vacuum pump evacuation is opened until the manometric registration of evaporator is -1, that is, is fully drawn out remaining solvent therein, is obtained Semen Coiciss
Crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Using molecular distillation apparatus (manufacturer：Xi'an Niu Saite chemical industry equipments Science and Technology Ltd., model：NCF-6S)
Molecular distillation is carried out to the crude oil after eliminating water, vapo(u)rizing temperature is 190-200 DEG C, vacuum is 2-10Pa, and knifing rotating speed is 300-
500 revs/min, dispensing speed is 100-120 ml/mins, distillates light components receiving port and obtains free fatty, and restructuring is separated
Mouth obtains the Semen Coiciss crude oil of deacidification valency；
Preferably, molecular distillation is carried out to the crude oil after eliminating water using molecular distillation apparatus, vapo(u)rizing temperature is 195 DEG C, true
Reciprocal of duty cycle is 5Pa, and knifing rotating speed is 400 revs/min, and dispensing speed is 110 ml/mins.
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is
2.0-3.0, it is 20%-30% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 100-120 DEG C, reaction end
Acid value is 1-3KOHmg/g, obtains crude product fatty-acid ethyl ester；
Preferably, the pH for adjusting reactant liquor with sulphuric acid is 2.5, and it is 25% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt,
Reaction temperature is 110 DEG C, and reaction end acid value is 2KOHmg/g.
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation, vacuum again using molecular distillation system
For 1-8Pa, vapo(u)rizing temperature is 160-180 DEG C, and dispensing speed is 200-300ml/min, and knifing rotating speed is 200-400r/min, is received
The faint yellow steaming thing of collection is corps acetoacetic ester；
Preferably, vacuum is 4.5Pa, and vapo(u)rizing temperature is 170 DEG C, and dispensing speed is 250ml/min, and knifing rotating speed is
300r/min。
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
A kind of Paeonia suffruticosa base fertilizer containing Semen Coiciss ground-slag end, including the following component counted by weight：
Semen Coiciss ground-slag end 25-40 parts, chicken manure 40-50 parts, Testa oryzae 5-10 parts, Testa Tritici 10-15 parts, shrimp powder 10-15 part,
EM strain 3-5 parts, eupolyphaga powder 5-10 parts.
Further, above-mentioned base fertilizer, by the following component counted by weight：
35 parts of Semen Coiciss ground-slag end, 45 parts of chicken manure, 7 parts of Testa oryzae, 13 parts of Testa Tritici, 13 parts of shrimp powder, 4 parts of EM strains, eupolyphaga
8 parts of powder.
The method for preparing above-mentioned base fertilizer, by Semen Coiciss ground-slag end, chicken manure, Testa oryzae, Testa Tritici, shrimp powder, EM strains and eupolyphaga
After powder stirs, under the conditions of 33 DEG C, fermentation is obtained final product for 5 days.
The application process of base fertilizer of the present invention, apply fertilizer 800-1100kg by per mu, and leveling is ploughed deeply after uniformly spreading fertilizer over the fields.Preferably,
Apply fertilizer 900kg by per mu.
The present invention has advantages below compared with prior art：
The present invention extracts the Semen Coicis oil in Semen Coiciss using subcritical butane, as Semen Coiciss crude oil acid value is generally greater than
20KOH mg/g, directly routinely refine, refining loss height, neutral oil yield are low, and the present invention removes fat using Physical Separation Technology
Refine again after acid.The technique adopts low-temp low-pressure, fully ensures that the natural quality of product, and oil yield is high, low production cost.Together
When, the Semen Coiciss slag produced in production process can be used as base fertilizer, and the base fertilizer of the present invention both can provide abundance to Paeonia suffruticosa
Nutrient, and there is early stage weeding, the present invention meets environmental requirement, improves resource utilization.
Specific embodiment
Further describe the present invention with reference to specific embodiment, advantages of the present invention and feature will be with description and
It is apparent.But embodiment is only exemplary, does not constitute any restriction to the scope of the present invention.Those skilled in the art should
It should be appreciated that, the details of technical solution of the present invention and form can be repaiied without departing from the spirit and scope of the invention
Change or replace, but these modifications and replacement are each fallen within protection scope of the present invention.
A kind of production technology of subcritical low-temperature extraction Semen Coicis oil of embodiment 1
Comprise the following steps that：
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, Semen Coicis powder is put into the extractor of two series connection
In one of tank, to extractor evacuation, it is stirred after adding extractant butane, the quality volume of Semen Coicis powder and butane
It is 1 than g/mL:2.5, rotating speed is 60r/min, and extraction temperature is 45 DEG C, and pressure 0.35MPa, extraction time are 45min, extraction time
Number is 3 times, obtains the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with the heart of a lotus seed
The solvent of Semen Coicis oil is entered, and evaporator pressure rise, the solvent in tank to be extracted dissolved with crude oil fully flow into evaporator, closes extraction
The valve between tank and evaporator is taken, evaporator is warming up to into 40-55 DEG C again then, open precipitation valve, by compressor pressure
Contracting, condenser condense recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then beat
Vacuum pump evacuation is opened until the manometric registration of evaporator is -1, that is, is fully drawn out remaining solvent therein, is obtained Semen Coiciss
Crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Using molecular distillation apparatus (manufacturer：Xi'an Niu Saite chemical industry equipments Science and Technology Ltd., model：NCF-6S)
Molecular distillation is carried out to the crude oil after eliminating water, vapo(u)rizing temperature is 195 DEG C, vacuum is 5Pa, and knifing rotating speed is 400 revs/min, is put
Material speed is 110 ml/mins, distillates light components receiving port and obtains free fatty, and restructuring sub-export obtains deacidification valency
Semen Coiciss crude oil；
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is
2.5, it is 25% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 110 DEG C, and reaction end acid value is 2KOHmg/
G, obtains crude product fatty-acid ethyl ester；
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation, vacuum again using molecular distillation system
For 4.5Pa, vapo(u)rizing temperature is 170 DEG C, and dispensing speed is 250ml/min, and knifing rotating speed is 300r/min, the faint yellow steaming of collection
Go out thing and be corps acetoacetic ester；
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
The purity of the Semen Coicis oil obtained by the present embodiment is that yield is 14.95%.
A kind of production technology of subcritical low-temperature extraction Semen Coicis oil of embodiment 2
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, Semen Coicis powder is put into the extractor of two series connection
In one of tank, to extractor evacuation, it is stirred after adding extractant butane, the quality volume of Semen Coicis powder and butane
Than for 1:2 (g/mL), rotating speed are 60r/min, and extraction temperature is 37 DEG C, and pressure 0.30MPa, extraction time are 40min, extraction time
Number is 3 times, obtains the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with the heart of a lotus seed
The solvent of Semen Coicis oil is entered, and evaporator pressure rise, the solvent in tank to be extracted dissolved with crude oil fully flow into evaporator, closes extraction
The valve between tank and evaporator is taken, evaporator is warming up to into 40-55 DEG C again then, open precipitation valve, by compressor pressure
Contracting, condenser condense recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then beat
Vacuum pump evacuation is opened until the manometric registration of evaporator is -1, that is, is fully drawn out remaining solvent therein, is obtained Semen Coiciss
Crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Using molecular distillation apparatus (manufacturer：Xi'an Niu Saite chemical industry equipments Science and Technology Ltd., model：NCF-6S)
Molecular distillation is carried out to the crude oil after eliminating water, vapo(u)rizing temperature is 190 DEG C, vacuum is 3Pa, and knifing rotating speed is 310 revs/min, is put
Material speed is 100 ml/mins, distillates light components receiving port and obtains free fatty, and restructuring sub-export obtains deacidification valency
Semen Coiciss crude oil；
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is
2.0, it is 20% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 100 DEG C, and reaction end acid value is
1.5KOHmg/g, obtains crude product fatty-acid ethyl ester；
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation, vacuum again using molecular distillation system
For 2Pa, vapo(u)rizing temperature is 160 DEG C, and dispensing speed is 210ml/min, and knifing rotating speed is 250r/min, and the faint yellow of collection steams
Thing is corps acetoacetic ester；
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
The purity of the Semen Coicis oil obtained by the present embodiment is that yield is 14.56%.
A kind of production technology of subcritical low-temperature extraction Semen Coicis oil of embodiment 3
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, Semen Coicis powder is put into the extractor of two series connection
In one of tank, to extractor evacuation, it is stirred after adding extractant butane, the quality volume of Semen Coicis powder and butane
Than for 1:3 (g/mL), rotating speed are 60r/min, and extraction temperature is 50 DEG C, and pressure 0.40MPa, extraction time are 48min, extraction time
Number is 3 times, obtains the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with the heart of a lotus seed
The solvent of Semen Coicis oil is entered, and evaporator pressure rise, the solvent in tank to be extracted dissolved with crude oil fully flow into evaporator, closes extraction
The valve between tank and evaporator is taken, evaporator is warming up to into 40-55 DEG C again then, open precipitation valve, by compressor pressure
Contracting, condenser condense recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then beat
Vacuum pump evacuation is opened until the manometric registration of evaporator is -1, that is, is fully drawn out remaining solvent therein, is obtained Semen Coiciss
Crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Using molecular distillation apparatus (manufacturer：Xi'an Niu Saite chemical industry equipments Science and Technology Ltd., model：NCF-6S)
Molecular distillation is carried out to the crude oil after eliminating water, vapo(u)rizing temperature is 200 DEG C, vacuum is 8Pa, and knifing rotating speed is 450 revs/min, is put
Material speed is 120 ml/mins, distillates light components receiving port and obtains free fatty, and restructuring sub-export obtains deacidification valency
Semen Coiciss crude oil；
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is
3.0, it is 28% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 120 DEG C, and reaction end acid value is 3KOHmg/
G, obtains crude product fatty-acid ethyl ester；
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation, vacuum again using molecular distillation system
For 7Pa, vapo(u)rizing temperature is 180 DEG C, and dispensing speed is 280ml/min, and knifing rotating speed is 400r/min, and the faint yellow of collection steams
Thing is corps acetoacetic ester；
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
The purity of the Semen Coicis oil obtained by the present embodiment is that yield is 14.21%.
A kind of Paeonia suffruticosa base fertilizer containing Semen Coiciss ground-slag end of embodiment 4
Including the following component counted by weight：
35 parts of Semen Coiciss ground-slag end, 45 parts of chicken manure, 7 parts of Testa oryzae, 13 parts of Testa Tritici, 13 parts of shrimp powder, 4 parts of EM strains, eupolyphaga
8 parts of powder.
The method for preparing above-mentioned base fertilizer, by Semen Coiciss ground-slag end, chicken manure, Testa oryzae, Testa Tritici, shrimp powder, EM strains and eupolyphaga
After powder stirs, under the conditions of 33 DEG C, fermentation is obtained final product for 5 days.
The herbicidal effect of test example base fertilizer of the present invention and the detection in terms of soil fertility improvement
The application process of base fertilizer, apply fertilizer 900kg by per mu, and leveling is ploughed deeply after uniformly spreading fertilizer over the fields.
It is as shown in table 1 to the preventive effect of grassy weed：
Test group：The base fertilizer that the embodiment of the present invention 4 is obtained；
Matched group 1：Semen Coiciss ground-slag end is replaced with the soil of plantation Paeonia suffruticosa in the base fertilizer that the embodiment of the present invention 4 is obtained；
Matched group 2：Barnyard manure of the Paeonia suffruticosa plantation with conventional base fertilizer-corruption heat, adds the Semen Coiciss ground-slag end of present invention acquisition, the heart of a lotus seed
Semen Coicis ground-slag end is 3 with the barnyard manure weight ratio of rotten heat:7；
Matched group 3：Blank；
Table 1
Note："-" represents, promotes the growth of grassy weed.
Additionally, base fertilizer of the present invention obtains improvement by a relatively large margin to soil fertility, the content of organic matter increases, beneficial in soil
Microflora increase etc..
Claims (10)
1. a kind of production technology of subcritical low-temperature extraction Semen Coicis oil, it is characterised in that comprise the following steps that：
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, the extractor that Semen Coicis powder is put into two series connection is wherein
In one tank, to extractor evacuation, it is stirred after adding extractant butane, the mass volume ratio g/ of Semen Coicis powder and butane
ML is 1:2-3, rotating speed are 60r/min, and extraction temperature is 35-55 DEG C, and pressure 0.25-0.40MPa, extraction time are 40-
50min, extraction times are 3 times, obtain the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with Semen Coiciss
The solvent of oil is entered, evaporator pressure rise, and the solvent in tank to be extracted dissolved with crude oil fully flows into evaporator, closes extractor
Then evaporator is warming up to 40-55 DEG C by valve and evaporator between again, opens precipitation valve, by compressor compresses, cold
Condenser condenses recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then opens true
Empty pumping vacuum is -1 until the manometric registration of evaporator, that is, be fully drawn out remaining solvent therein, obtain Semen Coiciss crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Molecular distillation is carried out to the crude oil after eliminating water using molecular distillation apparatus, vapo(u)rizing temperature is 190-200 DEG C, vacuum is 2-
10Pa, knifing rotating speed are 300-500 rev/min, and dispensing speed is 100-120 ml/mins, distillates light components receiving port and obtains
Free fatty, sub-export of recombinating obtain the Semen Coiciss crude oil of deacidification valency；
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is 2.0-
3.0, it is 20%-30% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 100-120 DEG C, reaction end acid value
For 1-3KOHmg/g, crude product fatty-acid ethyl ester is obtained；
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation again using molecular distillation system, vacuum is 1-
8Pa, vapo(u)rizing temperature are 160-180 DEG C, and dispensing speed is 200-300ml/min, and knifing rotating speed is 200-400r/min, collection
Faint yellow steaming thing is corps acetoacetic ester；
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
2. production technology according to claim 1, it is characterised in that 60 are crossed after in the step (1) crush Semen Coiciss
Mesh sieve, obtains Semen Coicis powder, in one of tank of the extractor that Semen Coicis powder is put into two series connection, extractor is taken out very
Sky, is stirred after adding extractant butane, and Semen Coicis powder is 1 with the mass volume ratio g/mL of butane:2.5, rotating speed is 60r/
Min, extraction temperature are 45 DEG C, pressure 0.35MPa, and extraction time is 45min, and extraction times are 3 times, are obtained dissolved with Semen Coiciss hair
The solvent and Semen Coiciss slag of oil.
3. production technology according to claim 1, it is characterised in that molecular distillation apparatus pair are utilized in the step (4)
Crude oil after eliminating water carries out molecular distillation, and vapo(u)rizing temperature is 195 DEG C, vacuum is 5Pa, and knifing rotating speed is 400 revs/min, blowing
Speed is 110 ml/mins.
4. production technology according to claim 1, it is characterised in that adjust reactant liquor with sulphuric acid in the step (6)
PH is 2.5, and it is 25% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 110 DEG C, and reaction end acid value is
2KOHmg/g。
5. production technology according to claim 1, it is characterised in that vacuum is 4.5Pa in the step (7), distillation
Temperature is 170 DEG C, and dispensing speed is 250ml/min, and knifing rotating speed is 300r/min.
6. a kind of Paeonia suffruticosa base fertilizer containing Semen Coiciss ground-slag end, it is characterised in that Paeonia suffruticosa base fertilizer includes following counting by weight
Component：
Semen Coiciss ground-slag end 25-40 parts, chicken manure 40-50 parts, Testa oryzae 5-10 parts, Testa Tritici 10-15 parts, shrimp powder 10-15 part, EM bacterium
Plant 3-5 parts, eupolyphaga powder 5-10 parts；
The preparation method of the Semen Coicis powder is as follows：
(1) subcritical low-temperature extraction
60 mesh sieves are crossed after Semen Coiciss are crushed, Semen Coicis powder is obtained, the extractor that Semen Coicis powder is put into two series connection is wherein
In one tank, to extractor evacuation, it is stirred after adding extractant butane, the mass volume ratio g/ of Semen Coicis powder and butane
ML is 1:2-3, rotating speed are 60r/min, and extraction temperature is 35-55 DEG C, and pressure 0.25-0.40MPa, extraction time are 40-
50min, extraction times are 3 times, obtain the solvent and Semen Coiciss slag dissolved with Semen Coiciss crude oil；
(2) preparation of crude oil
Solvent in step (1) dissolved with Semen Coiciss crude oil is put in advance evacuated evaporator, with dissolved with Semen Coiciss
The solvent of oil is entered, evaporator pressure rise, and the solvent in tank to be extracted dissolved with crude oil fully flows into evaporator, closes extractor
Then evaporator is warming up to 40-55 DEG C by valve and evaporator between again, opens precipitation valve, by compressor compresses, cold
Condenser condenses recycling design to solvent tank, the still a small amount of solvent of remaining of the crude oil in evaporator after recycling design, then opens true
Empty pumping vacuum is -1 until the manometric registration of evaporator, that is, be fully drawn out remaining solvent therein, obtain Semen Coiciss crude oil；
(3) crude oil eliminating water
The Semen Coiciss crude oil that step (2) is obtained is carried out into eliminating water using rotary evaporator, temperature is 100 DEG C, vacuum for-
0.095MPa, rotary evaporation 60 minutes；
(4) molecular distillation steams fatty acid
Molecular distillation is carried out to the crude oil after eliminating water using molecular distillation apparatus, vapo(u)rizing temperature is 190-200 DEG C, vacuum is 2-
10Pa, knifing rotating speed are 300-500 rev/min, and dispensing speed is 100-120 ml/mins, distillates light components receiving port and obtains
Free fatty, sub-export of recombinating obtain the Semen Coiciss crude oil of deacidification valency；
(5) refine Semen Coicis oil
The Semen Coiciss crude oil that will be obtained in step (4), carries out alkali refining, decolouring, deodorize and gets product Semen Coicis oil；
(6) fatty-acid ethyl ester
The fatty acid obtained in step (4) is carried out with dehydrated alcohol ethyl esterified, the pH with sulphuric acid regulation reactant liquor is 2.0-
3.0, it is 20%-30% that dehydrated alcohol accounts for the percentage ratio of fatty acid wt, and reaction temperature is 100-120 DEG C, reaction end acid value
For 1-3KOHmg/g, crude product fatty-acid ethyl ester is obtained；
(7) corps acetoacetic ester
The crude product fatty-acid ethyl ester obtained in step (6) is carried out into molecular distillation again using molecular distillation system, vacuum is 1-
8Pa, vapo(u)rizing temperature are 160-180 DEG C, and dispensing speed is 200-300ml/min, and knifing rotating speed is 200-400r/min, collection
Faint yellow steaming thing is corps acetoacetic ester；
(8) process of Semen Coiciss slag
Semen Coiciss slag is carried out air-drying, crushed 80 mesh sieves, Semen Coiciss ground-slag end is obtained.
7. Paeonia suffruticosa base fertilizer according to claim 6, it is characterised in that the Paeonia suffruticosa base fertilizer is counted by weight by following
Component：
35 parts of Semen Coiciss ground-slag end, 45 parts of chicken manure, 7 parts of Testa oryzae, 13 parts of Testa Tritici, 13 parts of shrimp powder, 4 parts of EM strains, eupolyphaga powder 8
Part.
8. the preparation method of Paeonia suffruticosa base fertilizer as claimed in claim 1 or 2, by Semen Coiciss ground-slag end, chicken manure, Testa oryzae, Testa Tritici, dried small shrimps
After powder, EM strains and eupolyphaga powder stir, under the conditions of 33 DEG C, fermentation is obtained final product for 5 days.
9. the application process of Paeonia suffruticosa base fertilizer as claimed in claim 1 or 2, apply fertilizer 800-1100kg by per mu, deep after uniformly spreading fertilizer over the fields
Turn over leveling.
10. using method according to claim 9, it is characterised in that apply fertilizer 900kg by per mu.
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Cited By (4)
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| CN107129865A (en) * | 2017-05-24 | 2017-09-05 | 中国农业大学 | A kind of method that pumpkin phylloquinone is extracted based on subcritical fluids and molecular distillation |
| CN110194807A (en) * | 2019-04-30 | 2019-09-03 | 福州帅宝生物科技有限公司 | A kind of extracting method of semen coicis water-soluble actives |
| CN113082173A (en) * | 2021-03-24 | 2021-07-09 | 贵州宏创农业产业开发有限公司 | Coix seed extract and application thereof in preparation of medicament for treating septicemia |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987316A (en) * | 2017-04-17 | 2017-07-28 | 中国林业科学研究院林产化学工业研究所 | A kind of preparation method of the red sandalwood essential oil with bacteriostatic activity |
| CN107129865A (en) * | 2017-05-24 | 2017-09-05 | 中国农业大学 | A kind of method that pumpkin phylloquinone is extracted based on subcritical fluids and molecular distillation |
| CN107129865B (en) * | 2017-05-24 | 2020-11-20 | 中国农业大学 | Method for extracting cucurbitacin based on subcritical fluid and molecular distillation |
| CN110194807A (en) * | 2019-04-30 | 2019-09-03 | 福州帅宝生物科技有限公司 | A kind of extracting method of semen coicis water-soluble actives |
| CN110194807B (en) * | 2019-04-30 | 2020-12-25 | 福州帅宝生物科技有限公司 | Method for extracting water-soluble active substance of coix seeds |
| CN113082173A (en) * | 2021-03-24 | 2021-07-09 | 贵州宏创农业产业开发有限公司 | Coix seed extract and application thereof in preparation of medicament for treating septicemia |
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