CN103058848A - Method for separating organic acid by using pseudo-homogeneous weak-base anion exchange resin - Google Patents
Method for separating organic acid by using pseudo-homogeneous weak-base anion exchange resin Download PDFInfo
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- 150000007524 organic acids Chemical class 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000003957 anion exchange resin Substances 0.000 title claims abstract description 19
- 239000011347 resin Substances 0.000 claims abstract description 47
- 229920005989 resin Polymers 0.000 claims abstract description 47
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 238000003795 desorption Methods 0.000 claims abstract description 15
- 238000000855 fermentation Methods 0.000 claims abstract description 8
- 230000004151 fermentation Effects 0.000 claims abstract description 8
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 35
- 238000010521 absorption reaction Methods 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 230000009514 concussion Effects 0.000 claims description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 20
- 239000001384 succinic acid Substances 0.000 claims description 19
- 238000004132 cross linking Methods 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 6
- 238000010560 atom transfer radical polymerization reaction Methods 0.000 claims description 6
- 239000004005 microsphere Substances 0.000 claims description 6
- 239000004793 Polystyrene Substances 0.000 claims description 5
- 229920002223 polystyrene Polymers 0.000 claims description 5
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- 238000010526 radical polymerization reaction Methods 0.000 claims description 3
- 238000005576 amination reaction Methods 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 239000002699 waste material Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 3
- 101710141544 Allatotropin-related peptide Proteins 0.000 claims 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical group CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical group CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Chemical group COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims 1
- 238000011084 recovery Methods 0.000 claims 1
- 125000001302 tertiary amino group Chemical group 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract 5
- 238000010364 biochemical engineering Methods 0.000 abstract 1
- 239000003480 eluent Substances 0.000 abstract 1
- 239000012086 standard solution Substances 0.000 abstract 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 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 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000274 adsorptive effect Effects 0.000 description 2
- 159000000007 calcium salts Chemical class 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 239000002028 Biomass Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 240000003183 Manihot esculenta Species 0.000 description 1
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000012262 fermentative production Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000011253 protective coating Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method for separating organic acid by pseudo-homogeneous weak-base anion exchange resin belongs to the technical field of biochemical engineering. The exchange resin is represented by MKF-D30X. The method comprises the steps of statically adsorbing an organic acid standard solution or a fermentation clear liquid thereof by MKF-D30X resin, detecting the adsorbed solution by a High Performance Liquid Chromatography (HPLC) method, desorbing the adsorbed resin by using a hydrochloric acid desorption solution, and detecting the desorption solution by the HPLC method. When the concentration of the organic acid solution is 1-50 g.L-1The MKF-D30X resin has an adsorption capacity of 70-455 mg g-1. Using 0.4-1.5 mol.L-1Hydrochloric acid solution is used as eluent, and the desorption rate is 85-98%. The method has the advantages of high organic acid adsorption amount, high desorption rate and good reusability of the resin.
Description
(1) technical field
The present invention relates to a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid, be specifically related to a kind of MKF-D30X resin organic acid in Succinic Acid or oxysuccinic acid or citric acid or its fermented liquid is separated.
(2) background technology
Increasing the weight of of the problem of environmental pollution that the in recent years soaring oil crisis that causes of, price in short supply along with petroleum resources, and petrochemical complex causes, chemical synthesis is owing to raw material, pollution, economic problems are restricted.Microbe fermentation method utilizes microbial strains, produce organic acid take agriculture product corn, cassava, stalk etc. as basic raw material, and the biomass resource source is abundant, pollution is few, so the fermentative Production organic acid gains great popularity.
The organic acid separation method mainly contains calcium salt precipitation method, liquid-liquid solvent extraction method, membrane separation process etc.Calcium salt method extracts and can produce the calcium sulfate waste; Solvent extration needs to consume the organic solvent of a large amount of costlinesses in the process of extracting, the toxicity of residual solvent has detrimentally affect to quality product; The membrane separating method process cost is high, such as the consumption of ionic membrane and the power consumption in the electrodialysis, and can not process divalent cation.And the resin absorption partition method has adsorption selectivity height, simple to operate, the advantage such as energy consumption is low, resin can recycle, and oneself is widely used in the aspects such as organic acid, amino acid, purification of pharmaceuticals.
Organic acid can participate in the vital process of animals and plants metabolism, is the intermediate product of metabolism, has significant biological activity, can prevent and cure diseases, and can be used as the raw material of organic synthesis, industrial and agricultural production and medicine industry.For example, Succinic Acid or oxysuccinic acid or citric acid all are some important organic compound, can be used as the intermediate of Organic Chemicals and synthetic complex organic compound, be widely used in medicine, food, synthetic plastics, rubber, protective coating, dyestuff and other industry.
The resin of exploring a kind of high-adsorption-capacity is significant for the organic acid separation and purification, reports seldom that about the systematic Study of anionite-exchange resin Adsorption organic acid (the D301 resin, when Succinic Acid concentration was 20g/1, adsorptive capacity was 380/mgg at present
-1(Li Song, Yao Zhong, Liu Hui, etc. basic resin separates Succinic Acid property research [J]. food and fermentation industries, 2007,33 (7): 54-57); The NERCB04 resin, when Succinic Acid concentration was 31g/l, adsorptive capacity was 378.8/mgg
-1(Qiang Li, Wang-liang Li, Dan Wang.pH Neutralization while Succinic Acid Adsorption onto Anion-Exchange Resins.Appl Biochem Biotechnol.2010,160:438445)).The present invention carries out the organic acid Static Adsorption with a kind of plan homogeneous phase weak base anion-exchange resin (MKF-D30X) of high-adsorption-capacity.This resin is the weakly alkaline tertiary amine-type anionite-exchange resin that reamination obtains after the pectination grafting of carrying out glycidyl methacrylate and acrylamide on the crosslinked chloroacetylation polystyrene microsphere with atom transfer radical polymerization (ATRP) method, has the pectination flexible chain structure of certain-length and the large advantage of degree of freedom.
(3) summary of the invention
Ion exchange resin is used in each different industrial sector widely at present, and the novel ion exchange resin of development research has profound significance.MKF-D30X resin of the present invention; after carrying out the pectination grafting of glycidyl methacrylate with the ATRP method on the crosslinked chloroacetylation polystyrene microsphere; the weakly alkaline tertiary amine-type anionite-exchange resin that after amination, obtains, and it is applied to adsorb organic acid in the fermented liquid.Concrete synthesis step is as follows:
Carry out with Transfer Radical Polymerization or ATRP method on the crosslinked chloroacetylation polystyrene microsphere glycidyl methacrylate or and the acrylamide copolymerization or and the pectination grafting of acrylic ester copolymer after the weakly alkaline tertiary amine-type anionite-exchange resin that obtains of reamination.
The MKF-D30X resin has the flexible pectination chain structure of certain-length and the large advantage of degree of freedom, when Adsorption organic acid because its special structure (pectination side chain, flexibility, extensibility are good), functional group is to star-shaped diffusion all around and have larger degree of freedom, effectively contact and increased with organic acid, be better affinity, therefore easier Adsorption organic acid.
A kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid provided by the invention, undertaken by following operation steps:
(1) configuration 40mL, concentration is 1~50gL
-1, the organic acid standardized solution of pH about 7.2~2.1 or its fermented liquid are in Erlenmeyer flask.
(2) (a certain amount of dried resin is immersed in 10h in 95% ethanolic soln to take by weighing 0.2~3g MKF-D30X resin, pure water is washed till without ethanol and distinguishes the flavor of, soak 2h with 5%HCl (v/v), pure water is washed till pH neutrality, use again 2~4%NaOH (w/v) to soak 2h, pure water is washed till pH neutrality, and is stand-by) be added in the organic acid soln;
The MKF-D30X exchange capacity of resin is 2.2~4.1mmo1g
-1, degree of crosslinking 2~15%, particle diameter 20~220 orders.
(3) organic acid soln that step (2) is obtained places 20~60 ℃ of water bath with thermostatic control shaking table concussion absorption 1~3h, and raffinate detects through high performance liquid chromatography (HPLC) after the absorption;
(4) the MKF-D30X resin after will adsorbing moves in the Erlenmeyer flask with 10~40ml, 0.4~1.5mo1L
-1The desorb of hydrochloric acid elutriant;
(5) elutriant that step (4) is obtained places 45~80 ℃ of water bath with thermostatic control shaking table concussion desorb 1~4h, filters its stripping liquid and detects through HPLC.
(4) description of drawings
Accompanying drawing is a kind of infared spectrum of intending the homogeneous phase weak base anion-exchange resin among the present invention.
(5) embodiment
Following examples are used for explanation the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
Adsorption conditions: configuration 1gL
-1Succinic Acid standardized solution 40mL (pH about 3.2) in Erlenmeyer flask, takes by weighing 0.2g, and exchange capacity is 2.0mmo1g
-1, degree of crosslinking is 2%, particle diameter be 20 purpose MKF-D30X resins in the Succinic Acid standardized solution, be placed on concussion absorption 2h in 20 ℃ of water bath with thermostatic control shaking tables, the solution after the absorption detects through HPLC, the resin after the absorption moves in the Erlenmeyer flask and uses 10ml, 1.5molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 45 ℃ of water bath with thermostatic control shaking table concussion desorb 1h, and stripping liquid detects through HPLC.Loading capacity is 100mgg
-1, desorption rate reaches 85%.
Embodiment 2
Adsorption conditions: configuration 20gL
-1Succinic Acid standardized solution 40mL (pH about 2.7) in Erlenmeyer flask, takes by weighing 0.2g, and exchange capacity is 3.3mmolg
-1, degree of crosslinking is 7%, particle diameter be 100 purpose MKF-D30X resins in the Succinic Acid standardized solution, be placed on concussion absorption 3h in 25 ℃ of water bath with thermostatic control shaking tables, the solution after the absorption detects through HPLC, the resin after the absorption moves in the Erlenmeyer flask and uses 40ml, 1.0mo1L
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 60 ℃ of water bath with thermostatic control shaking table concussion desorb 3h, and stripping liquid detects through HPLC.Loading capacity is 421mgg
-1, desorption rate reaches 98%.
Embodiment 3
Adsorption conditions: configuration 50gL
-1Succinic Acid standardized solution 40mL (pH about 2.1) in Erlenmeyer flask, takes by weighing 0.2g, and exchange capacity is 4.1mmolg
-1, degree of crosslinking is 10%, particle diameter be 220 purpose MKF-D30X resins in Succinic Acid solution, be placed on concussion absorption 3h in 25 ℃ of water bath with thermostatic control shaking tables, solution detects through HPLC after the absorption, the resin after the absorption moves in the Erlenmeyer flask and uses 20ml, 0.4molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 45 ℃ of water bath with thermostatic control shaking table concussion desorb 4h, and stripping liquid detects through HPLC.Loading capacity is 455mgg
-1, desorption rate reaches 89%.
Embodiment 4
Adsorption conditions: configuration 20gL
-1Oxysuccinic acid standardized solution 40mL (pH about 2.7) in Erlenmeyer flask, takes by weighing 3g, and exchange capacity is 3.3mmolg
-1, degree of crosslinking is 15%, particle diameter be 50 purpose MKF-D30X resins in the Succinic Acid standardized solution, be placed on concussion absorption 1h in 60 ℃ of water bath with thermostatic control shaking tables, the solution after the absorption detects through HPLC, the resin after the absorption moves in the Erlenmeyer flask and uses 20ml, 0.6molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 60 ℃ of water bath with thermostatic control shaking table concussion desorb 2h, and stripping liquid detects through HPLC.Loading capacity is 120mgg
-1, desorption rate reaches 94%.
Embodiment 5
Adsorption conditions: configuration 20gL
-1Citric acid standardized solution 40mL (pH about 2.4) in Erlenmeyer flask, takes by weighing 2g, and exchange capacity is 3.5mmolg
-1, degree of crosslinking is 7%, particle diameter be 100 purpose MKF-D30X resins in the Succinic Acid standardized solution, be placed on concussion absorption 3h in 45 ℃ of water bath with thermostatic control shaking tables, the solution after the absorption detects through HPLC, the resin after the absorption moves in the Erlenmeyer flask and uses 30ml, 1.0molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 70 ℃ of water bath with thermostatic control shaking table concussion desorb 2h, and stripping liquid detects through HPLC.Loading capacity is 200mgg
-1, desorption rate reaches 98%.
Embodiment 6
Adsorption conditions: take by weighing 0.2g, exchange capacity is 2.2mmolg
-1, degree of crosslinking is 7%, particle diameter is 220 purpose MKF-D30X resins, adds 40mL, 1gL
-1(pH about 7.2) citric acid fermentation broth is placed on concussion absorption 2h in 20 ℃ of water bath with thermostatic control shaking tables in Erlenmeyer flask, solution detects through HPLC after the absorption, and the resin after the absorption moves in the Erlenmeyer flask and uses 20ml, 0.4molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 60 ℃ of water bath with thermostatic control shaking table concussion desorb 2h, and stripping liquid detects through HPLC.Loading capacity is 70mgg
-1, desorption rate reaches 92%.
Embodiment 7
Adsorption conditions: take by weighing 2.0g, exchange capacity is 3.5mmolg
-1, degree of crosslinking is 10%, particle diameter is 100 purpose MKF-D30X resins, adds 40mL, 30gL
-1(pH about 6.5) succinic acid fermentation liquor is placed on concussion absorption 1h in 45 ℃ of water bath with thermostatic control shaking tables in Erlenmeyer flask, solution detects through HPLC after the absorption, and the resin after the absorption moves in the Erlenmeyer flask and uses 10ml, 0.6molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 80 ℃ of water bath with thermostatic control shaking table concussion desorb 1h, and stripping liquid detects through HPLC.Loading capacity is 100mgg
-1, desorption rate reaches 90%.
Embodiment 8
Adsorption conditions: take by weighing 3.0g, exchange capacity is 4.1mmolg
-1, degree of crosslinking is 15%, particle diameter is 50 purpose MKF-D30X resins, adds 40mL, 50gL
-1(pH about 6.4) malic acid fermentation liquid is placed on concussion absorption 2h in 60 ℃ of water bath with thermostatic control shaking tables in Erlenmeyer flask, solution detects through HPLC after the absorption, and the resin after the absorption moves in the Erlenmeyer flask and uses 30ml, 1.5molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 45 ℃ of water bath with thermostatic control shaking table concussion desorb 4h, and stripping liquid detects through HPLC.Loading capacity is 80mgg
-1, desorption rate reaches 96%.
Embodiment 9
Adsorption conditions: take by weighing 0.2g, exchange capacity is 3.2mmolg
-1, degree of crosslinking is 2%, particle diameter is 20 purpose MKF-D30X resins, adds 40mL, 40gL
-1(pH about 6.5) succinic acid fermentation liquor is placed on concussion absorption 3h in 25 ℃ of water bath with thermostatic control shaking tables in Erlenmeyer flask, solution detects through HPLC after the absorption, and the resin after the absorption moves in the Erlenmeyer flask and uses 40ml, 1.0molL
-1The hydrochloric acid elutriant carries out desorb, and Erlenmeyer flask is placed 60 ℃ of water bath with thermostatic control shaking table concussion desorb 3h, and stripping liquid detects through HPLC.Loading capacity is 271mgg
-1, desorption rate reaches 98%.
Claims (8)
1. method of intending homogeneous phase weak base anion-exchange resin separating organic acid, it is characterized in that this plan homogeneous phase weak base anion-exchange resin or MKF-D30X resin are to be obtained by following preparation method: on crosslinked acetobrom or chloroacetylation polystyrene microsphere with Transfer Radical Polymerization or ATRP method carry out glycidyl methacrylate or and the acrylamide copolymerization or and the pectination grafting of acrylic ester copolymer, then the weakly alkaline tertiary amine-type anionite-exchange resin that obtains of reamination;
The method of its Adsorption organic acid can be carried out according to the following steps: taking by weighing plan homogeneous phase weak base anion-exchange resin or MKF-D30X resin is 1~50gL in 40mL, concentration
-1, pH about 7.2~2.1 the organic acid standardized solution or as in Succinic Acid or oxysuccinic acid or the citric acid fermentation broth, solution is placed 20~60 ℃ of water bath with thermostatic control shaking tables concussion absorption, 1~3h, the solution after its absorption detects through HPLC; Resin after the absorption moves to and adds 0.4~1.5molL in the Erlenmeyer flask
-1Hydrochloric acid, and this Erlenmeyer flask placed 45~80 ℃ of C water bath with thermostatic control shaking tables concussion desorb, 1~4h filters its stripping liquid and detects through HPLC.
2. a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid according to claim 1 is characterized in that described organic acid can be Succinic Acid or oxysuccinic acid or citric acid or organic acid fermented liquid or its fermented waste fluid or contain this organic acid recovery liquid.
3. a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid according to claim 1; it is characterized in that described crosslinked acetobrom or chloroacetylation polystyrene microsphere can be gel or macroporous microsphere; its degree of crosslinking can be 2~15%, and particle diameter is 20~220 orders.
4. a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid according to claim 1, it is characterized in that describedly after intending homogeneous phase weak base anion-exchange resin or MKF-D30X resin absorption, the loading capacity of organic acid or Succinic Acid or oxysuccinic acid or citric acid is 70~455mg-g
-1, desorption efficiency reaches 85%~98% after the desorb.
5. a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid according to claim 1 is characterized in that described organic acid concentration is 1~50gL
-1, pH is about 7.2~2.1, and amount of resin is 0.2~3g, and the concentration of hydrochloric acid elutriant is 0.4~1.5molL
-1
6. a kind of method of intending homogeneous phase weak base anion-exchange resin separating organic acid according to claim 1 is characterized in that described adsorption temp is 20~60 ℃, and desorption temperature is 45~80 ℃.
7. a kind of preparation method who intends the homogeneous phase weak base anion-exchange resin according to claim 1 is characterized in that the described pectination percentage of grafting that obtains take Transfer Radical Polymerization or ATRP method is as mass ratio 200%~2000%.
8. a kind of preparation method who intends the homogeneous phase weak base anion-exchange resin according to claim 1 is characterized in that described amination can finish by adding dimethylamine or diethylamine or pyridine, and its tertiary amine group exchange capacity is 2.0~4.1mmolg-1.
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CN112877481A (en) * | 2020-12-28 | 2021-06-01 | 河北省农林科学院遗传生理研究所(河北省农林科学院农产品质量安全研究中心) | Purification treatment method for soluble sugar in fruits and vegetables |
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