CN115991636A - Method for extracting quebrachitol from ion flocculation rubber wastewater - Google Patents
Method for extracting quebrachitol from ion flocculation rubber wastewater Download PDFInfo
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- CN115991636A CN115991636A CN202211251309.9A CN202211251309A CN115991636A CN 115991636 A CN115991636 A CN 115991636A CN 202211251309 A CN202211251309 A CN 202211251309A CN 115991636 A CN115991636 A CN 115991636A
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- Prior art keywords
- quebrachitol
- inositol
- flocculation
- liquid
- flocculated
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- DSCFFEYYQKSRSV-FIZWYUIZSA-N (-)-Quebrachitol Chemical compound CO[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@H]1O DSCFFEYYQKSRSV-FIZWYUIZSA-N 0.000 title claims abstract description 99
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000005189 flocculation Methods 0.000 title claims abstract description 41
- 230000016615 flocculation Effects 0.000 title claims abstract description 38
- 229920001971 elastomer Polymers 0.000 title abstract description 30
- 239000002351 wastewater Substances 0.000 title abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 75
- CDAISMWEOUEBRE-UHFFFAOYSA-N scyllo-inosotol Natural products OC1C(O)C(O)C(O)C(O)C1O CDAISMWEOUEBRE-UHFFFAOYSA-N 0.000 claims abstract description 51
- 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 claims abstract description 50
- 229960000367 inositol Drugs 0.000 claims abstract description 50
- 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 claims abstract description 48
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims abstract description 8
- 229920006173 natural rubber latex Polymers 0.000 claims abstract description 6
- 125000002091 cationic group Chemical group 0.000 claims description 12
- 229910021645 metal ion Inorganic materials 0.000 claims description 3
- 238000000605 extraction Methods 0.000 abstract description 17
- 239000000203 mixture Substances 0.000 abstract description 15
- 239000002994 raw material Substances 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 6
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- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 4
- 238000002425 crystallisation Methods 0.000 description 32
- 230000008025 crystallization Effects 0.000 description 32
- 239000000047 product Substances 0.000 description 31
- 238000003756 stirring Methods 0.000 description 22
- 239000012535 impurity Substances 0.000 description 15
- 229920000126 latex Polymers 0.000 description 15
- 239000004816 latex Substances 0.000 description 15
- 238000001953 recrystallisation Methods 0.000 description 15
- 230000003311 flocculating effect Effects 0.000 description 14
- 244000043261 Hevea brasiliensis Species 0.000 description 10
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 10
- 229920003052 natural elastomer Polymers 0.000 description 10
- 229920001194 natural rubber Polymers 0.000 description 10
- 230000008569 process Effects 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- 239000012043 crude product Substances 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000012528 membrane Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000006260 foam Substances 0.000 description 6
- 230000001939 inductive effect Effects 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 241000699670 Mus sp. Species 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical class COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 2
- 238000001471 micro-filtration Methods 0.000 description 2
- 238000001728 nano-filtration Methods 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 208000030507 AIDS Diseases 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 208000015580 Increased body weight Diseases 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 244000183278 Nephelium litchi Species 0.000 description 1
- 235000017343 Quebracho blanco Nutrition 0.000 description 1
- 241000065615 Schinopsis balansae Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000005862 Whey Substances 0.000 description 1
- 102000007544 Whey Proteins Human genes 0.000 description 1
- 108010046377 Whey Proteins Proteins 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000011097 chromatography purification Methods 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- -1 cyclic alcohols Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000009509 drug development Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 150000004001 inositols Chemical class 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000010090 natural rubber production Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 150000003904 phospholipids Chemical class 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000018770 reduced food intake Nutrition 0.000 description 1
- 238000001223 reverse osmosis Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Classifications
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for extracting quebrachitol from ion flocculation rubber wastewater and quebrachitol. The method comprises the following steps: adding natural rubber latex into the ionic flocculation liquid for flocculation, separating to obtain flocculated residual liquid, cooling and filtering to obtain clear liquid; and adding inositol into the obtained clear liquid, and filtering and separating precipitated crystals to obtain the quebrachitol. The invention has simple extraction process, adopts the wastewater in the flocculation process as the raw material, has high extraction efficiency and stable product, and can realize large-scale production; the product is a mixture of quebrachitol and inositol, wherein the inositol is harmless to human body, and can be used as medicine and food raw materials together with quebrachitol without affecting the efficacy of quebrachitol; the inositol has low price, and is beneficial to controlling the cost.
Description
Technical Field
The invention relates to the technical field of compounds, in particular to a method for extracting quebrachitol from ion flocculation rubber wastewater and quebrachitol.
Background
Quebracho Pi Chun is L-2-methoxyl inositol, and is an inositol derivative with optical rotation property naturally existing in the nature. Quebrachitol is present in a variety of common economic plants including baster, litchi, etc., and has therefore been considered as a raw material for synthesizing chiral compounds and inositol derivatives. In particular, the effect of chiral compounds is more and more emphasized in the field of medical and chemical industry, chiral drugs occupy the half-wall Jiangshan of drug development in the field of medicine, and the cost of synthesizing chiral compounds is difficult to control although the purity of chiral compounds can be ensured, so that a plurality of special effect drugs with natural price are also generated. The quebrachitol is used as a raw material, and the synthesized chiral molecules play an important role in the treatment of cancers, AIDS and the like, and can also be used as a raw material of various important reaction auxiliary agents in the chemical field.
The natural rubber is an important economic and national defense construction strategic resource, so far natural rubber consumption in China is mainly imported, domestic yield is only 15% of consumption, and especially in important industries such as aviation, precision instruments, military industry and the like, imported natural rubber from southeast Asia is mainly used, and the whole domestic natural rubber cannot occupy a high-end market, so that the domestic natural rubber production enterprises have low universal profit, are easily influenced by extreme weather and international market fluctuation, and are unfavorable for the healthy development of the whole industry. And the byproduct of high economic value, quebrachitol, is extracted from the processing residual wastewater, so that the economic benefit of the whole industry can be improved, the traditional rubber industry is related to the medical care field, and the adverse situation of the domestic natural rubber industry is favorably broken.
The natural latex consists of water, rubber particles and non-rubber components, wherein the non-rubber components have complex components, besides two major types of proteins and phospholipids, various small molecular alcohols, ketones, ethers and other organic matters, and the small molecular organic matters are harmful to human bodies, so that the small molecular organic matters need to be removed as impurities in the extraction process of quebrachitol, and the method is the most important step in the whole extraction process.
The natural rubber biological source extraction work of quebrachitol starts in the recent decades in China, but comprehensive existing researches find that the research is concentrated on the removal of impurities in the whole system, the complete analysis of whey components is needed, and the process is complicated. Chinese patent No. 103058834A discloses a method for extracting quebrachitol from natural rubber-making wastewater, which comprises the steps of filtering and impurity removing the natural rubber-making wastewater containing quebrachitol, sequentially passing through a microfiltration membrane, an ultrafiltration membrane, a nanofiltration membrane or a reverse osmosis membrane to remove protein and other small molecular impurities, and then decoloring, concentrating and crystallizing to obtain the quebrachitol product. The above method wastes a lot of energy in the impurity removal step, and is relatively complicated in steps, namely chromatography and membrane filtration methods.
The prior art has the defects of complex process, low yield, high cost and inapplicability to the subsequent industrialized production by utilizing methods such as chromatography purification, filter membrane purification, concentration crystallization purification and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for extracting quebrachitol from ion flocculation rubber wastewater and the quebrachitol.
The method is different from the traditional natural rubber positive flocculation process, adopts an ionic flocculant to prepare natural rubber, adopts a crystallization-inducing method to extract quebrachitol, adds natural latex into ionic flocculation liquid to flocculate, separates the flocculation liquid to obtain clear liquid, and then filters the clear liquid to add inositol similar to the quebrachitol structure to break the dissolution balance of the quebrachitol, thereby inducing the quebrachitol to crystallize and co-precipitate and obtaining a inositol and quebrachitol mixed crystallization product.
The method has simple extraction process, adopts the wastewater in the solidification process as the raw material, has high extraction efficiency and stable product, can realize large-scale production, and is beneficial to improving the comprehensive utilization level of the rubber industry.
The extract product extracted by the method is a mixture of quebrachitol and inositol, wherein the inositol is harmless to human body, and can be applied to the field of medical care together with the quebrachitol without affecting the efficacy of the quebrachitol.
The quebrachitol is a methyl ether derivative of inositol, the two substances are cyclic alcohols, the dissolution mechanism in water is similar, six groups on the inositol are hydroxyl groups and can form hydrogen bonds with water, compared with the quebrachitol with one substituent being methyl ether, the quebrachitol has better solubility in water, so that the dissolution balance of the quebrachitol in water can be destroyed by adding the inositol, and the crystallization is induced. According to the invention, inositol is added to induce the crystallization and precipitation of quebrachitol, so that the dissolution balance of other small molecules in a system is not influenced, the purification step is simplified to the greatest extent, the purification is simpler and more convenient, the time and the labor are saved, and the industrial popularization in the future is facilitated.
One of the purposes of the invention is to provide a method for extracting quebrachitol from ion flocculation rubber wastewater, which comprises the following steps:
(1) Adding natural rubber latex into the ionic flocculation liquid for flocculation, separating to obtain flocculated residual liquid, cooling and filtering to obtain clear liquid;
(2) And adding inositol into the obtained clear liquid, and filtering and separating precipitated crystals to obtain the quebrachitol.
Preferably, the method comprises the steps of,
adding inositol into the obtained clear liquid, stirring for full dissolution, standing for crystallization, separating solid from liquid to obtain a crude crystallization product, and recrystallizing for further purification to obtain a crystallized product of quebrachitol and inositol; preferably, the number of recrystallisation is from 2 to 3.
The solid-liquid separation can be carried out by adopting a suction filtration method.
In a preferred embodiment of the present invention,
the mass concentration of the natural rubber latex is 3% -60%, preferably 5% -60%, more preferably 10% -60%.
In a preferred embodiment of the present invention,
and (3) cooling to 0-20 ℃.
In a preferred embodiment of the present invention,
the inositol is 5-30% of the clear liquid mass, preferably 10-30%.
In a preferred embodiment of the present invention,
the ionic flocculation liquid is a solution of a cationic flocculant; the cationic flocculant is at least one of metal ion flocculant and high molecular cationic flocculant; the metal ion flocculant is preferably at least one of sodium chloride, calcium chloride, potassium chloride, aluminum sulfate, sodium sulfate and zinc sulfate; preferably an aqueous solution of a cationic flocculant.
The mass ratio of the natural rubber latex to the ionic flocculation liquid is 1: (1-8).
In a preferred embodiment of the present invention,
the mass of the cationic flocculant accounts for 0.1-5% of the total mass of the solution of the cationic flocculant, and is preferably 1-5%;
the ionic flocculation liquid can be prepared by recycling flocculation clear liquid, and is added and prepared to the above concentration.
In a preferred embodiment of the present invention,
step (1),
the flocculation temperature is 50-80 ℃; the stirring speed during flocculation is 10-300 m/min; until the rubber is completely flocculated; adding latex into cationic flocculant, stirring, collecting rubber in the latex into solid, directly taking out the solid, filtering the rest flocculating residual liquid, and removing floating rubber and impurities to obtain flocculating clear liquid.
In a preferred embodiment of the present invention,
step (2),
the dissolution temperature is 10-50 ℃; the dissolution time is 10-20 min; stirring rotation speed is 20-60 r/min;
the crystallization temperature is 0-20 ℃;
the recrystallization is to dissolve the crude crystallization product and then recrystallize;
under the induction of inositol, the quebrachitol and inositol are separated out together to form crystals, the supernatant is filtered to obtain a crystal crude product, the crude product is recrystallized to further remove impurities and purify, and the product obtained after recrystallization is washed and dried to obtain the quebrachitol product comprising quebrachitol Pi Chunhe.
In a preferred embodiment of the present invention,
and the recrystallization is to dissolve the crude crystallization product into ethanol at room temperature until saturation, cool the temperature to-20 to-10 ℃ at 2-5 ℃ until crystallization precipitation, and separate solid and liquid to obtain the crystallization product of the quebrachitol and inositol.
The filtration may be carried out by a method commonly known in the art, such as a cloth filtration, a suction filtration, etc.
It is a further object of the present invention to provide a quebrachitol product extracted by the above method, comprising quebrachitol and inositol.
The extracted product is quebrachitol and inositol mixture, wherein inositol is harmless to human body, and can be used together with quebrachitol in medical care field without affecting the efficacy of quebrachitol.
In a preferred embodiment of the present invention,
the mass fraction of quebrachitol is 0.1-6%; preferably 0.4 to 6%;
the mass fraction of inositol is 94-99.9%; preferably 94 to 99.6%.
Compared with the prior art, the invention has the beneficial effects that:
the method is different from the traditional natural rubber positive flocculation process, adopts an ionic flocculant to prepare natural rubber, adopts a crystallization-inducing method to extract quebrachitol, adds natural latex into ionic flocculation liquid to flocculate, separates the flocculation liquid to obtain clear liquid, and then filters the clear liquid to add inositol similar to the quebrachitol structure to break the dissolution balance of the quebrachitol, thereby inducing the quebrachitol to crystallize and co-precipitate and obtaining a inositol and quebrachitol mixed product.
The method has simple extraction process, adopts the wastewater in the solidification process as the raw material, has high extraction efficiency and stable product, can realize large-scale production, and is beneficial to improving the comprehensive utilization level of the rubber industry.
The extract product extracted by the method is a mixture of quebrachitol and inositol, wherein the inositol is harmless to human body, and can be used as medicine and food raw materials together with the quebrachitol without affecting the efficacy of the quebrachitol.
The inositol used in the invention has low price, which is beneficial to controlling the cost.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The starting materials used in the examples were all conventional commercially available.
Example 1
1kg of natural latex with the solid content of 60% is taken, 1kg of NaCl aqueous solution with the mass fraction of 1% is added for flocculation, the flocculation temperature is 80 ℃, and the stirring speed during flocculation is 300m/min until the rubber in the latex is completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 20 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 10% of the mass of the flocculating clear liquid into the flocculating clear liquid at 10 ℃, stirring for 10min to fully dissolve, wherein the stirring speed is 20r/min;
cooling to 1 ℃, standing for 24 hours to induce the crystallization of the myoethanol and the quebrachitol to be separated out together, filtering to obtain a crude crystallization product, and then carrying out 2 times of recrystallization. And (3) dissolving the crude product of the crystallization to a saturated state by using an ethanol solvent at normal temperature during recrystallization, cooling to-20 ℃ at 5 ℃/min, maintaining for 2 hours, and filtering to separate the crystallization and the solvent, wherein the steps are repeated twice.
Naturally drying the crystallized product at normal temperature to obtain quebrachitol product
The quebrachitol accounts for 3.7% of the mass of the mixture, the inositol accounts for 96.3% of the mass of the mixture, and the extraction rate of the quebrachitol is 48%.
Example 2
1kg of natural latex with solid content of 60% is taken and added with 2kg of CaCl with mass fraction of 2% 2 The aqueous solution was flocculated at 50℃and the stirring rate during flocculation was 50m/min until the rubber in the latex was completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 20 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 15% of the mass of the flocculating clear liquid into the flocculating clear liquid at 20 ℃, stirring for 20min to fully dissolve, wherein the stirring speed is 60r/min;
the temperature in the crystallization process is controlled at 5 ℃, standing is carried out for 30 hours to induce the crystallization of the myoethanol and the quebrachitol to be co-precipitated, the crude product of the crystallization is obtained after filtration and then is recrystallized for 2 times, the recrystallization step is the same as that of the example 1, and the crystallized product is naturally dried at normal temperature to obtain the quebrachitol product
The obtained mixture contains quebrachitol 2.0%, inositol 98% and quebrachitol 40%.
Example 3
1kg of natural latex with 30% solid content is taken, 4kg of KCl aqueous solution with 2% mass fraction is added for flocculation, the flocculation temperature is 60 ℃, and the stirring speed during flocculation is 100m/min until the rubber in the latex is completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 15 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 20% of the mass of the flocculating clear liquid into the flocculating clear liquid at 30 ℃, stirring for 15min to fully dissolve, wherein the stirring speed is 50r/min;
the crystallization process temperature is controlled at 10 ℃, standing is carried out for 48 hours to induce the crystallization of the myoethanol and the quebrachitol to be co-precipitated, the crude product of the crystallization is obtained after filtration and drying, and then the recrystallization is carried out for 2 times, and the recrystallization step is the same as that of example 1
The obtained mixture contains quebrachitol 1.1% and inositol 98.9% by weight, and the extraction rate of quebrachitol is 42%.
Example 4
1kg of natural latex with 25% of solid content is taken and added with 4kg of Na with 5% of mass fraction 2 SO 4 The aqueous solution was flocculated at 80℃and the stirring rate during flocculation was 300m/min until the rubber in the latex was completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 15 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 25% of the mass of the flocculating clear liquid into the flocculating clear liquid at 40 ℃, stirring for 15min to fully dissolve, wherein the stirring speed is 50r/min;
the temperature in the crystallization process is controlled at 15 ℃, standing is carried out for 48 hours to induce the crystallization of the myoethanol and the quebrachitol to be separated out together, the crude product of the crystallization is obtained after filtration and drying, then the recrystallization is carried out for 2 times, the recrystallization step is the same as that of the example 1, and the crystallized product is naturally dried at normal temperature to obtain the quebrachitol product
The obtained mixture contains quebrachitol 0.8% and inositol 99.2% by weight, and the extraction rate of quebrachitol is 41%.
Example 5
Taking 1kg of natural product with 20% solid contentLatex, 6kg of 5% by mass of Al is added 2 (SO 4 ) 2 The aqueous solution was flocculated at 80℃and the stirring rate during flocculation was 300m/min until the rubber in the latex was completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 10 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 30% of the mass of the flocculating clear liquid into the flocculating clear liquid at 50 ℃, stirring for 20min to fully dissolve, wherein the stirring speed is 60r/min;
the temperature of the crystallization process is controlled at 20 ℃, the mixture is kept stand for 72 hours, the myoethanol and the quebrachitol are induced to be crystallized and separated out together, the crude product of the crystal is obtained after filtration and drying, and then is recrystallized for 2 times, the recrystallization step is the same as that of the example 1, and the crystallized product is naturally dried at normal temperature, thus obtaining the quebrachitol product
The obtained mixture contains quebrachitol 0.5% and inositol 99.5% by weight, and the extraction rate of quebrachitol is 40%.
Example 6
1kg of natural latex with the solid content of 10% is taken and added with 8kg of ZnSO with the mass fraction of 1% 4 The aqueous solution was flocculated at 80℃and the stirring rate during flocculation was 300m/min until the rubber in the latex was completely flocculated. The rubber component in the latex is flocculated out and then taken out to obtain flocculated residual liquid, the flocculated residual liquid is cooled to 1 ℃, and filtered and separated to remove floating foam and impurities in the residual liquid to obtain flocculated clear liquid;
adding inositol accounting for 30% of the mass of the flocculating clear liquid into the flocculating clear liquid at 50 ℃, stirring for 20min to fully dissolve, wherein the stirring speed is 60r/min;
the temperature in the crystallization process is controlled at 20 ℃, standing is carried out for 72 hours to induce the crystallization of the myoethanol and the quebrachitol to be separated out together, the crude product of the crystallization is obtained after filtration and drying, then the recrystallization is carried out for 2 times, the recrystallization step is the same as that of the example 1, and the crystallized product is naturally dried at normal temperature to obtain the quebrachitol product
The obtained mixture contains quebrachitol 0.4% and inositol 99.6% by weight, and the extraction rate of quebrachitol is 43%.
Comparative example 1
1kg of the latex in example 2 was taken and flocculation was carried out by adding dilute acetic acid until the rubber had completely precipitated. Adding activated carbon into the separated flocculated residual liquid for decoloring, then carrying out rotary evaporation under the condition of 65 ℃ and 0.09MPa, concentrating to 5% of the original volume, adding 10 times of ethanol, filtering out residual rubber separated out after adding the ethanol, and cooling the obtained residual liquid to-20 ℃ at a speed of 5 ℃ per hour until crystallization is separated out. The obtained crude crystal product has complex components and needs impurity removal treatment. Dissolving the crude product, sequentially passing through a microfiltration membrane and a nanofiltration membrane, and repeating the concentration step, adding methanol, and carrying out repeated recrystallization and purification. Finally, 0.9g of quebrachitol is obtained, and the extraction rate is 14%.
Comparative example 2
4 groups of db/db mice (type II diabetic mice) were set, 3 experimental groups and one blank group, respectively. The experimental groups were fed quebrachitol, inositol and quebrachitol/inositol mixtures (molar ratio 1:9) respectively, at doses of 50mg/kgbw, dissolved in 5ml of water, once daily, with pure water for the blank group and the four remaining groups were all identical. Mice fed quebrachitol and quebrachitol/inositol mixtures were found to have reduced food intake, increased body weight, increased fasting plasma insulin levels, while mice fed inositol and the blank group had no significant changes.
Examples 1 to 6 ion flocculate natural latex and extract quebrachitol from the flocculated supernatant after filtration and removal of impurities at 40 to 48%, whereas comparative example 1 extract quebrachitol from the gel wastewater after acid flocculation at 14%.
Examples 1 to 6 extract quebrachitol by using a crystallization-inducing method, flocculate natural latex by adding it into an ionic flocculation liquid, separate the flocculation liquid, filter the flocculation liquid to obtain a clear liquid, add inositol having a structure similar to quebrachitol to break its dissolution balance, thereby inducing the co-precipitation of quebrachitol crystals and obtaining a inositol-quebrachitol mixed product. The method has simple extraction process, adopts the wastewater in the solidification process as the raw material, has high extraction efficiency and stable product, can realize large-scale production, and is beneficial to improving the comprehensive utilization level of the rubber industry; the extract product is quebrachitol and inositol mixture, wherein inositol is harmless to human body, and can be used together with quebrachitol as medicine and food raw material without affecting the efficacy of quebrachitol.
Claims (8)
1. A method of extracting quebrachitol, the method comprising:
(1) Adding natural rubber latex into the ionic flocculation liquid for flocculation, separating to obtain flocculated residual liquid, cooling and filtering to obtain clear liquid;
(2) And adding inositol into the obtained clear liquid, and filtering and separating precipitated crystals to obtain the quebrachitol.
2. The method for extracting quebrachitol according to claim 1, wherein:
the mass concentration of the natural rubber latex is 3-60%.
3. The method for extracting quebrachitol according to claim 1, wherein:
and (3) cooling to 0-20 ℃.
4. The method for extracting quebrachitol according to claim 1, wherein:
the mass of the inositol is 5-30% of the mass of the clear liquid.
5. The method for extracting quebrachitol according to claim 1, wherein:
the ionic flocculation liquid is a solution of a cationic flocculant.
6. The method for extracting quebrachitol according to claim 5, wherein:
the cationic flocculant is at least one of a metal ion flocculant and a high molecular cationic flocculant.
7. The method for extracting quebrachitol according to claim 5, wherein:
the mass of the cationic flocculant accounts for 0.1-5% of the total mass of the solution of the cationic flocculant.
8. Quebrachitol extracted by the method of any one of claims 1-7.
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| GB216982A (en) * | 1923-03-28 | 1924-06-12 | Giuseppe Bruni | A process for the production of phosphoric derivatives of inositol |
| CN103058834A (en) * | 2013-01-09 | 2013-04-24 | 云南省热带作物科学研究所 | Method for extracting quebracho bark alcohol from rubber-processing wastewater of natural rubber |
| CN110204430A (en) * | 2019-06-20 | 2019-09-06 | 海南中橡科技有限公司 | A kind of method of purification of quebracho alcohol crystals crude product |
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| GB216982A (en) * | 1923-03-28 | 1924-06-12 | Giuseppe Bruni | A process for the production of phosphoric derivatives of inositol |
| CN103058834A (en) * | 2013-01-09 | 2013-04-24 | 云南省热带作物科学研究所 | Method for extracting quebracho bark alcohol from rubber-processing wastewater of natural rubber |
| CN110204430A (en) * | 2019-06-20 | 2019-09-06 | 海南中橡科技有限公司 | A kind of method of purification of quebracho alcohol crystals crude product |
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