CN113307825A - Method for extracting calcium phytate from rice bran waste residues - Google Patents
Method for extracting calcium phytate from rice bran waste residues Download PDFInfo
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- CN113307825A CN113307825A CN202110564183.XA CN202110564183A CN113307825A CN 113307825 A CN113307825 A CN 113307825A CN 202110564183 A CN202110564183 A CN 202110564183A CN 113307825 A CN113307825 A CN 113307825A
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- 239000002699 waste material Substances 0.000 title claims abstract description 95
- 235000007164 Oryza sativa Nutrition 0.000 title claims abstract description 89
- 235000009566 rice Nutrition 0.000 title claims abstract description 89
- WPEXVRDUEAJUGY-UHFFFAOYSA-B hexacalcium;(2,3,4,5,6-pentaphosphonatooxycyclohexyl) phosphate Chemical compound [Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])(=O)OC1C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C(OP([O-])([O-])=O)C1OP([O-])([O-])=O WPEXVRDUEAJUGY-UHFFFAOYSA-B 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 34
- 240000007594 Oryza sativa Species 0.000 title 1
- 241000209094 Oryza Species 0.000 claims abstract description 88
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000843 powder Substances 0.000 claims abstract description 66
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 49
- 239000007790 solid phase Substances 0.000 claims abstract description 48
- 239000000706 filtrate Substances 0.000 claims abstract description 46
- 238000001914 filtration Methods 0.000 claims abstract description 33
- 238000002156 mixing Methods 0.000 claims abstract description 27
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000001110 calcium chloride Substances 0.000 claims abstract description 19
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 239000000243 solution Substances 0.000 claims description 52
- 239000007787 solid Substances 0.000 claims description 29
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 28
- 238000001035 drying Methods 0.000 claims description 17
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 15
- 235000019774 Rice Bran oil Nutrition 0.000 claims description 14
- 239000008165 rice bran oil Substances 0.000 claims description 14
- 238000007873 sieving Methods 0.000 claims description 14
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 8
- 239000002244 precipitate Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000012716 precipitator Substances 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 4
- 229910021538 borax Inorganic materials 0.000 claims description 4
- 239000000920 calcium hydroxide Substances 0.000 claims description 4
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000741 silica gel Substances 0.000 claims description 4
- 229910002027 silica gel Inorganic materials 0.000 claims description 4
- 239000004328 sodium tetraborate Substances 0.000 claims description 4
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 3
- 159000000007 calcium salts Chemical class 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims description 2
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002253 acid Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical class OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical group [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 4
- 238000007792 addition Methods 0.000 description 4
- 235000002949 phytic acid Nutrition 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229940068041 phytic acid Drugs 0.000 description 2
- 239000000467 phytic acid Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- SQUHHTBVTRBESD-UHFFFAOYSA-N Hexa-Ac-myo-Inositol Natural products CC(=O)OC1C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C(OC(C)=O)C1OC(C)=O SQUHHTBVTRBESD-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- IWEDUKDKQUXPLH-NFJZTGFVSA-L [Mg++].OP(O)(=O)O[C@H]1[C@@H](OP(O)(O)=O)C(OP(O)([O-])=O)[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)C1OP(O)([O-])=O Chemical compound [Mg++].OP(O)(=O)O[C@H]1[C@@H](OP(O)(O)=O)C(OP(O)([O-])=O)[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)C1OP(O)([O-])=O IWEDUKDKQUXPLH-NFJZTGFVSA-L 0.000 description 1
- 239000002154 agricultural waste Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- CDAISMWEOUEBRE-GPIVLXJGSA-N inositol Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@@H]1O CDAISMWEOUEBRE-GPIVLXJGSA-N 0.000 description 1
- 229960000367 inositol Drugs 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000010815 organic waste Substances 0.000 description 1
- 239000010908 plant waste Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/06—Phosphorus compounds without P—C bonds
- C07F9/08—Esters of oxyacids of phosphorus
- C07F9/09—Esters of phosphoric acids
- C07F9/117—Esters of phosphoric acids with cycloaliphatic alcohols
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a method for extracting calcium phytate from rice bran waste residues, which comprises the following steps: pulverizing rice bran waste residue to obtain rice bran powder, mixing defatted rice bran powder with solid phase reagent, grinding the mixture in a ball mill, taking out the ground powder, adding acetic acid aqueous solution to dissolve, extracting at room temperature, filtering to obtain filtrate, adding inorganic alkaline water to adjust pH value, adding calcium chloride, standing and collecting precipitated calcium phytate. The method adopts the mechanochemical technology to extract the calcium phytate from the rice bran waste residue, has the advantages of high product yield, environmental protection, less acid and alkali consumption, less solvent residue, simple technical process and short production period, fully utilizes the waste defatted rice bran, and is an extraction and separation route with wide industrial prospect.
Description
Technical Field
The invention relates to the field of deep processing of crop waste residues, in particular to a method for extracting calcium phytate from rice bran waste residues.
Background
China is a big country for rice production, and according to statistics, the annual output of rice in China in 2019 all the year around is about 2.1 hundred million tons, and simultaneously, rice bran is produced by about 2000 ten thousand tons. However, defatted rice bran waste residue has been ignored for a long time as an agricultural waste. The rice bran contains 10% of phytate compounds, and mainly contains salts such as calcium phytate and magnesium phytate. The phytic acid obtained after the salt removal of the phytate is a natural product with extremely strong chelation, is widely used in industrial production of food, electroplating, environmental protection and the like, and has huge demand. The phytic acid is further hydrolyzed to obtain inositol with anti-aging and anti-oxidation effects. The conventional method for obtaining calcium phytate from rice bran waste residue usually uses a large amount of acid and alkali, which violates the theme of green chemistry. The novel methods for extracting calcium phytate comprise enzyme-assisted extraction, ion exchange resin-assisted extraction, microwave-assisted extraction and ultrasonic-assisted extraction, but the methods are not widely applied in actual production. Mechanochemical techniques use mechanical energy to break the interactions between substances, creating new interfaces and creating a physicochemical reaction in a localized area. The plant material can be fully contacted with the solid reagent under the action of mechanical force to generate a series of reactions which are difficult to carry out in solution. In addition, the mechanochemical technology shortens the production period, reduces the production cost, is simple to operate and does not need a large amount of solvent.
In this study, mechanochemical-assisted extraction was used to extract calcium phytate from rice bran waste. At present, no report is found, and the method is a great breakthrough of the traditional method for extracting calcium phytate from rice bran waste residue.
Disclosure of Invention
The invention mainly solves the technical problem of providing the method for extracting the calcium phytate from the rice bran waste residue, which is environment-friendly, simple to operate, safe and reliable in production, short in period, low in cost, high in product yield and good in purity.
The research idea of the invention is as follows: according to the chemical structure and property of calcium phytate, the rice bran waste residue and a solid phase reagent are reacted by using a mechanochemical effect to generate water-soluble phytate, and the calcium phytate is obtained after dissolution, neutralization and addition of a precipitator.
The technical scheme adopted by the invention is shown in figure 2.
A method for extracting calcium phytate from rice bran waste residues specifically comprises the following steps:
a mechanochemical-assisted method for extracting calcium phytate is adopted, rice bran waste residues are used as raw materials, the rice bran waste residues are sieved after being crushed, powder of 100 meshes is collected, the sieved powder and a solid-phase reagent are uniformly mixed according to a mass ratio, wherein the content of the solid-phase reagent is 1-10 wt%, the mixture is fully ground in a planetary ball mill, the ground powder is taken out, an acetic acid aqueous solution is added for dissolving, the mixture is extracted for a certain time at room temperature, the filtrate is adjusted to a certain pH value by an inorganic alkali aqueous solution after being filtered, a soluble calcium salt precipitator is added for standing, calcium phytate precipitate is collected after centrifugation, the calcium phytate precipitate is weighed after drying, and the content of the calcium phytate precipitate is measured.
Further, the solid phase reagent is one or any combination of two or more of the following: sodium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate, calcium carbonate, potassium hydroxide, potassium carbonate, disodium hydrogen phosphate, borax and silica gel.
Furthermore, the rice bran waste residue is derived from the rice bran waste residue after the rice bran oil is extracted, and the rice bran waste residue can be dried or dried in the sun without special requirements.
Further, the material of the tank body and the grinding balls of the planetary ball mill for mechanochemical treatment is stainless steel, the volume of the grinding tank is 250mL, the diameter of the ball milling beads is 10mm, and the number of the ball milling beads is 30.
Further, in the ball milling process, the rotating speed of the ball mill is 100-800 rpm, preferably 400rpm, and the ball milling time is 10-40 min, preferably 30 min.
Further, the pH value of the acetic acid aqueous solution is 4.0-6.0, and the material-liquid ratio of the grinding powder to the acetic acid aqueous solution is 1: 10-1: 60g: mL.
Further, the extraction time is 10-60 min.
Further, the inorganic alkaline water solution required for neutralizing the extracting solution is obtained by dissolving one of potassium hydroxide, sodium hydroxide and calcium hydroxide in water, and the pH value of the neutralized extracting solution is 6.5-9.5.
Furthermore, in the process of refining calcium phytate by adopting a precipitation method, the mass ratio of the added amount of the calcium chloride precipitator to the rice bran waste residue is 1: 0.5-1: 3.0.
Further, the standing time of the precipitate is 2-6 h.
Still further, more specifically, the method for extracting calcium phytate from rice bran waste residue is carried out according to the following steps: crushing the rice bran waste residue, and sieving the crushed rice bran waste residue with a 100-mesh sieve to obtain rice bran waste residue powder; uniformly mixing the rice bran waste residue and a solid phase reagent according to a mass ratio, wherein the content of the solid phase reagent is 1-10 wt%, and putting the mixture into a planetary ball mill for grinding for 10-40 min at 100-800 rpm to obtain mixed micro powder; adding the mixed micro powder into an acetic acid solution with the pH value of 4.0-6.0 according to the material-liquid ratio of 1: 10-1: 60g: mL, extracting for 10-60 min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the filter residue once again, filtering repeatedly, and finally combining all filtrates; adjusting the pH of the total filtrate to 6.5-9.5 by using an inorganic alkaline aqueous solution, and adding 2.5-15.0 g of soluble calcium salt into the solution; standing for 2-6 h, and filtering the precipitated light yellow solid; and washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate.
Compared with the prior art, the invention has the beneficial effects that:
(1) the extraction process does not use a large amount of organic solvents, does not have organic waste liquid and is environment-friendly.
(2) Based on mechanochemistry, the superfine grinding of raw materials is realized under the action of high-energy mechanical force, the wall breaking rate is improved, the exposed effective substances are directly dissolved out (figure 1), and compared with the traditional extraction process, the extraction time is shortened, and the extraction rate of calcium phytate is improved.
In conclusion, the method for extracting the calcium phytate from the rice bran waste residue has the advantages of environmental friendliness, high extraction rate, low acid and alkali consumption, short production period, simplicity in operation and the like, and has a good industrial popularization prospect.
Drawings
FIG. 1 shows the raw material rice bran waste residue observed by scanning electron microscope (A) and the rice bran waste residue after grinding with sodium carbonate for 30 minutes (B);
FIG. 2 is a flow chart of the technical scheme adopted by the invention.
Detailed Description
The technical means of the present invention will be described below in terms of specific embodiments, but the scope of the present invention is not limited thereto.
In the examples, the determination method of calcium phytate content is as follows: weighing about 0.5g of calcium phytate, dissolving with dilute hydrochloric acid, diluting to 100mL, taking 25mL of filtrate, adding 25mL of FeCl into each of three parts3And (4) standard solution. Heating in boiling water for 20min, cooling to room temperature, and diluting to 100 mL. Adding 1:1 ammonia water to pH 10, precipitating, and filtering. Placing the precipitate in a crucible which has been dried to constant weightAnd (3) placing the mixture in a muffle furnace, burning the mixture for 1h at 900 ℃, cooling and heaving the mixture, and calculating the content of the calcium phytate.
Example 1
The solid phase reagent content in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium carbonate.
Taking 4500mg of rice bran waste residue powder and 500mg of sodium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind for 30min at 300 rpm. Adding 150mL of acetic acid solution with pH of 5.5 into the mixed micro powder, extracting for 60min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 6.5 by using 10% sodium hydroxide solution, and adding 7.5g of calcium chloride into the solution; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Pale yellow amorphous powder, IR (KBr)1664, 1135, 1130, 1001, 846, 683, 648cm–1；
Example 2
The solid phase reagent content in the feed is 5 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium carbonate.
Taking 4750mg of rice bran waste residue powder and 250mg of sodium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, adding into a ball mill, and grinding at 300rpm for 30 min. Extracting the mixed micro powder and 150mL of acetic acid solution with the pH value of 5.5 for 60min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 7.0 by using 10% sodium hydroxide solution, and adding 7.5g of calcium chloride into the solution; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 3
The solid phase reagent content in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is potassium carbonate.
Taking 4500mg of rice bran waste residue powder and 500mg of potassium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind for 30min at 300 rpm. Adding the mixed micro powder into 150mL of acetic acid solution with pH of 5.5, extracting for 60min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 6.5 with 10% sodium hydroxide solution, and adding 15.0g calcium chloride; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 4
The content of solid phase reagent in the feed is 1 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is borax.
Taking 4950mg of rice bran waste residue powder and 50mg of borax, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind for 30min at 400 rpm. Adding the mixed micro powder into 150mL of acetic acid solution with pH of 5.5, extracting for 60min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 7.5 by using 10% sodium hydroxide solution, and adding 6.0g of calcium chloride into the solution; after standing for 4h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 5
The solid phase reagent content in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium bicarbonate.
Taking 4500mg of rice bran waste residue powder and 500mg of sodium bicarbonate, mixing the rice bran waste residue powder and the solid phase reagent, adding the mixture into a ball mill, and grinding at 600rpm for 10 min. Adding the mixed micro powder into 100mL of acetic acid solution with pH of 5.5, extracting for 30min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 6.5 with 10% sodium hydroxide solution, and adding 5.0g calcium chloride; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 6
The content of a solid phase reagent in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is silica gel and sodium carbonate 1: 1.
Taking 4500mg of rice bran waste residue powder, 250mg of silica gel and 250mg of sodium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind at 800rpm for 10 min. Adding the mixed micro powder into 300mL of acetic acid solution with pH of 5.5, extracting for 30min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 6.5 with 10% sodium hydroxide solution, and adding 2.5g calcium chloride; after standing for 4h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 7
The solid phase reagent content in the feed is 5 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium bicarbonate.
Taking 4750mg of rice bran waste residue powder and 250mg of sodium bicarbonate, mixing the rice bran waste residue powder and a solid phase reagent, adding into a ball mill, and grinding at 300rpm for 30 min. Adding the mixed micro powder into 100mL of acetic acid solution with pH of 5.5, extracting for 30min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 8.0 by using 10% potassium hydroxide solution, and adding 10.0g of calcium chloride into the solution; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 8
The solid phase reagent content in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium carbonate.
Taking 4500mg of rice bran waste residue powder and 500mg of sodium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind for 40min at 250 rpm. Adding the mixed micro powder into 300mL of acetic acid solution with pH of 4.5, extracting for 50min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 8.0 by using 10% potassium hydroxide solution, and adding 10.0g of calcium chloride into the solution; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 9
The solid phase reagent content in the feed is 10 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium hydroxide.
Taking 4500mg of rice bran waste residue powder and 500mg of sodium hydroxide, mixing the rice bran waste residue powder and the solid phase reagent, adding the mixture into a ball mill, and grinding for 40min at 600 rpm. Extracting the mixed micro powder and 200mL of acetic acid solution with the pH value of 4.0 for 20min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 7.0 with 10% calcium hydroxide solution, and adding 2.5g calcium chloride; after standing for 4h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 10
The solid phase reagent content in the feed is 5 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium hydroxide.
Taking 4750mg of rice bran waste residue powder and 250mg of sodium hydroxide, mixing the rice bran waste residue powder and the solid phase reagent, adding into a ball mill, and grinding at 200rpm for 40 min. Extracting the mixed micro powder and 200mL of acetic acid solution with the pH value of 6.0 for 40min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 8.0 with 10% sodium carbonate solution, and adding 7.5g calcium chloride; after standing for 6h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 11
The solid phase reagent content in the feed is 1 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium hydroxide.
Taking 4950mg of rice bran waste residue powder and 50mg of sodium carbonate, mixing the rice bran waste residue powder and the solid phase reagent, and adding the mixture into a ball mill to grind at 800rpm for 10 min. Extracting the mixed micro powder and 150mL of acetic acid solution with the pH value of 5.5 for 20min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 8.0 by using 10% potassium hydroxide solution, and adding 12.5g of calcium chloride into the solution; after standing for 3h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
Example 12
The solid phase reagent content in the feed is 5 wt%, wherein the rice bran waste residue powder is dry waste residue obtained by extracting rice bran oil and sieving after crushing, and the solid phase reagent is sodium hydroxide.
Taking 4750mg of rice bran waste residue powder and 250mg of sodium hydroxide, mixing the rice bran waste residue powder and the solid phase reagent, adding into a ball mill, and grinding at 200rpm for 40 min. Adding the mixed micro powder into 200mL of acetic acid solution with pH of 5.0, extracting for 20min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the residue once again, filtering again, and mixing all filtrates. Adjusting the pH of the total filtrate to 9.0 by using 10% sodium hydroxide solution, and adding 12.5g of calcium chloride into the solution; after standing for 2h, the precipitated pale yellow solid was filtered. And washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate product.
The yield and content of calcium phytate in the specific examples are shown in the following table:
by comparison between the examples, it can be seen that the best yield of calcium phytate can be obtained by using 10% sodium carbonate as grinding aid. The rotating speed of the ball mill and the pH value of the acetic acid solution also have certain influence on the yield of the calcium phytate, and when the rotating speed is 200-300rpm and the pH value of the acetic acid solution is 4.5-5.5, the extraction rate of the calcium phytate is higher. The addition amount of calcium chloride has an influence on both the yield and purity of calcium phytate, and when the addition amount of calcium chloride reaches 5.0 to 10.0g, better yield and purity can be obtained, and the addition amount of calcium chloride of 7.5g can obtain the best yield and purity of calcium phytate.
Claims (10)
1. A method for extracting calcium phytate from rice bran waste residues is characterized in that the rice bran waste residues are used as raw materials, a mechanochemical auxiliary extraction method is adopted, the rice bran waste residues are crushed, sieved and collected into 100-mesh powder, the sieved powder and a solid phase reagent are uniformly mixed according to a mass ratio, wherein the content of the solid phase reagent is 1-10 wt%, the mixture is fully ground in a planetary ball mill, the ground powder is taken out, an acetic acid aqueous solution is added for dissolution and extraction at room temperature for a certain time, after filtration, filtrate is adjusted to a certain pH value by an inorganic alkali aqueous solution, calcium chloride is added as a precipitator and then stands to refine calcium phytate, calcium phytate precipitate is collected after centrifugation, the calcium phytate precipitate is dried, the quality of the calcium phytate is weighed, and the content of the calcium phytate is measured.
2. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the solid phase reagent is one or any combination of two or more of the following: sodium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate, calcium carbonate, potassium hydroxide, potassium carbonate, disodium hydrogen phosphate, borax and silica gel.
3. The method for extracting calcium phytate from rice bran waste residue according to claim 1, wherein the rice bran waste residue is derived from rice bran waste residue after rice bran oil extraction, and no special requirement exists in drying or sun drying.
4. The method for extracting calcium phytate from rice bran waste residue according to claim 1, wherein a planetary ball mill used for mechanochemical treatment is adopted, the material of the tank body and the grinding balls is stainless steel, the diameter of the ball milling beads is 10mm, the rotating speed of the ball mill in the ball milling process is 100-800 rpm, preferably 400rpm, and the ball milling time is 10-40 min, preferably 30 min.
5. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the pH of the acetic acid aqueous solution is 4.0-6.0, and the feed-liquid ratio of the grinding powder to the solution is 1: 10-1: 60g: mL.
6. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the extraction time is 10-60 min.
7. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the inorganic alkaline aqueous solution required for neutralization of the extract is one of potassium hydroxide, sodium hydroxide and calcium hydroxide dissolved in water, and the pH value of the neutralized extract is 6.5-9.5.
8. The method for extracting calcium phytate from rice bran waste residue according to claim 1, wherein in the process of refining calcium phytate by a precipitation method, the mass ratio of the added amount of the calcium chloride precipitator to the rice bran waste residue is 1: 0.5-1: 3.0.
9. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the standing time of the precipitate is 2-6 h.
10. The method for extracting calcium phytate from rice bran waste residue as claimed in claim 1, wherein the method comprises the following steps: crushing the rice bran waste residue, and sieving the crushed rice bran waste residue with a 100-mesh sieve to obtain rice bran waste residue powder; uniformly mixing the rice bran waste residue and a solid phase reagent according to a mass ratio, wherein the content of the solid phase reagent is 1-10 wt%, and putting the mixture into a planetary ball mill for grinding for 10-40 min at 100-800 rpm to obtain mixed micro powder; adding acetic acid solution with the pH value of 4.0-6.0 into the mixed micro powder according to the material-liquid ratio of 1.0: 10-1.0: 60g: mL, extracting for 10-60 min, filtering the extracting solution, and collecting filtrate and filter residue; extracting the filter residue once again, filtering repeatedly, and finally combining all filtrates; adjusting the pH of the total filtrate to 6.5-9.5 by using an inorganic alkaline aqueous solution, and adding 2.5-15.0 g of soluble calcium salt into the solution; standing for 2-6 h, and filtering the precipitated light yellow solid; and washing and drying the light yellow solid at 80 ℃ to obtain the calcium phytate.
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