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CN-122011251-A - Macroporous weak base anion exchange resin and preparation method and application thereof

CN122011251ACN 122011251 ACN122011251 ACN 122011251ACN-122011251-A

Abstract

The invention relates to the technical field of resin preparation, in particular to a macroporous weak base anion exchange resin, and a preparation method and application thereof. The crosslinked styrene-divinylbenzene microsphere matrix obtained by regulating and controlling the preparation process of the crosslinked styrene, the divinylbenzene, the pore-forming agent and the crosslinking agent has the advantages of high mechanical strength, controllable specific surface area, adjustable pore diameter and the like. The total exchange capacity of the macroporous weak base anion exchange resin reaches more than 4.8mmol/g, the resin sphere rate in the fatigue strength of 100 cycles is more than 90 percent, the resin sphere rate in the fatigue strength of 300 cycles is more than 70 percent, and the first cycle treatment volume (BV) in the xylose decoloring process is more than 80 times, so that the purposes of improving the quality of the resin, reducing the environmental pollution and improving the energy efficiency ratio can be achieved.

Inventors

  • SUN JIANCHAO
  • LOU ZHENG
  • CHEN WANGBIN
  • ZHU JIAYING

Assignees

  • 荆门争光新材料科技有限公司

Dates

Publication Date
20260512
Application Date
20260202

Claims (10)

  1. 1. The preparation method of the macroporous weak base anion exchange resin is characterized by comprising the following steps: 1) Mixing styrene, divinylbenzene, a cross-linking agent, benzoyl peroxide and a pore-forming agent to obtain an oil phase; The cross-linking agent comprises one or more of triallyl isocyanurate, trimethylolpropane acrylate, vinyl acetate, ethylene glycol dimethacrylate and glycidyl methacrylate; 2) Mixing water, gelatin, disodium hydrogen phosphate, trisodium hydrogen phosphate, sodium lignin sulfonate and sodium chloride to obtain a water phase; 3) Mixing the oil phase in the step 1), the water phase in the step 2) and the methylene blue, and then carrying out heat treatment, and carrying out solid-liquid separation to obtain crosslinked polystyrene-divinylbenzene white balls; 4) Mixing the crosslinked polystyrene-divinylbenzene white balls obtained in the step 3) with chloromethyl ether solution, and swelling to obtain swelled white balls; 5) Mixing anhydrous ferric chloride and chloromethyl ether, then mixing the mixture with the swelling white ball and sulfuric acid solution in the step 4), and carrying out heat preservation treatment to obtain a chlorine ball; 6) Mixing the chlorine ball obtained in the step 5), sodium hydroxide solution and dimethylamine solution, and then stirring for reaction to obtain the macroporous weak base anion exchange resin.
  2. 2. The preparation method of claim 1, wherein the mass ratio of the styrene, the divinylbenzene, the crosslinking agent, the benzoyl peroxide and the porogen in the step 1) is 256:38:6:4.2:159-168; The porogen comprises isobutanol.
  3. 3. The preparation method according to claim 1, wherein the mass ratio of water, gelatin, disodium hydrogen phosphate, trisodium hydrogen phosphate, sodium lignin sulfonate and sodium chloride in the step 2) is 600:4.2:10:2.5:0.5:120.
  4. 4. The method of claim 1, wherein the mass ratio of the methine blue of step 3) to the water of step 2) is 0.6:600; The heat treatment conditions comprise 75 ℃ heat preservation treatment for 2 hours, 85 ℃ heat preservation treatment for 1 hour and 95 ℃ heat preservation treatment for 4 hours; the particle size of the crosslinked polystyrene-divinylbenzene white balls is 0.355-0.9 mm.
  5. 5. The preparation method of claim 1, wherein the volume ratio of the mass of the crosslinked polystyrene-divinylbenzene white balls to the chloromethyl ether solution in the step 4) is 100g to 400ml, and the mass percentage of the chloromethyl ether in the chloromethyl ether solution is 50%; The swelling time was 2h.
  6. 6. The method according to claim 1, wherein the ratio of the mass of anhydrous ferric chloride to the volume of chloromethyl ether in step 5) is 15g:200ml; The volume ratio of the chloromethyl ether to the sulfuric acid solution is 4:1, and the mass percentage of the sulfuric acid solution is 98%; the heat preservation treatment conditions comprise 48 hours of temperature and 12 hours of time.
  7. 7. The method of claim 1, wherein the mass of the chlorine spheres, the volume of sodium hydroxide solution, and the volume ratio of dimethylamine solution in step 6) is 200g:200ml:250ml; the stirring reaction conditions comprise the rotating speed of 150r/min, and the reaction is carried out for 5 hours at 60 ℃ and then for 5 hours at 70 ℃.
  8. 8. The preparation method according to claim 1, wherein the macroporous weak base anion exchange resin in step 6) is subjected to purification treatment, and the purification treatment method comprises the following steps of washing, acid treatment and alkali treatment of the macroporous weak base anion exchange resin in sequence; the reagent used in the acid treatment is hydrochloric acid solution with the concentration of 2mol/L, and the acid treatment conditions comprise that the hydrochloric acid solution is added into macroporous weak base anion exchange resin and is treated for 20min in a flask at the stirring speed of 150 r/min; The reagent used for the alkali treatment is sodium hydroxide solution of 2mol/L, and the sodium hydroxide solution is added into macroporous weak base anion exchange resin and is treated for 20min in a flask at a stirring speed of 150 r/min.
  9. 9. A macroporous weak base anion exchange resin prepared by the method of any one of claims 1 to 8.
  10. 10. The use of the macroporous weakly basic anion exchange resin of claim 9 for xylose decolorization.

Description

Macroporous weak base anion exchange resin and preparation method and application thereof Technical Field The invention relates to the technical field of resin preparation, in particular to a macroporous weak base anion exchange resin, and a preparation method and application thereof. Background In the current global scope, the market demands of health foods and health products are continuously rising, xylose is used as a non-caloric sweetener, has sweetness and flavor similar to those of glucose, and can improve the flavor and taste of desserts, but because the metabolism of the xylose in the body is irrelevant to insulin, the xylose can replace glucose to produce various low-caloric foods. The xylo-oligosaccharide is taken as an active substance with excellent physiological functions, has remarkable bifidobacterium proliferation capability, can improve organism immunity, does not cause blood sugar rise, has low heat quantity, can meet the food requirements of special people such as patients with diabetes, hyperlipidemia, obesity and the like, has caries resistance, is very suitable for being taken as a sweet additive of children foods, can promote the absorption of mineral elements such as calcium and the like, is an ideal raw material for developing infant, pregnant women and old foods, and has the functions of reducing serum cholesterol content, reducing blood pressure, generating nutrient substances, enhancing organism immunity, resisting tumors and the like, thereby bringing great attention to the application of the xylo-oligosaccharide in food, chemical industry, medicine and other departments. The main preparation methods of the xylo-oligosaccharide include an acid hydrolysis method, an enzyme hydrolysis method, a microwave treatment method, an ultrasonic preparation method and the like, but the raw materials of corncob, bagasse and the like contain a large amount of natural pigment substances in the production process. Therefore, how to efficiently and inexpensively desalt and decolorize the wastewater has been a problem. At present, the main methods adopted for removing pigment and inorganic salt ions include activated carbon adsorption, ion exchange resin adsorption, membrane separation decoloration and the like so as to improve the purity and quality of the product. The activated carbon has the advantages of convenient use, simple equipment and strong adsorption capacity, but has poor specificity, certain polysaccharide can be adsorbed while decoloring, hydrogen peroxide has oxidizing property and can destroy the biological activity of the sugar, and the membrane separation method has low removal rate of low-molecular-weight colored matters and inorganic matters. The macroporous ion exchange resin has the advantages of large adsorption capacity, strong regeneration capacity, strong stability, low cost and simple operation, and pigment molecules in xylose are in an ionization state and are negatively charged and can exchange with anion resin, so that the macroporous ion exchange resin is commonly applied to the xylose purification process. However, the research shows that after the conventional macroporous weak base anion resin is used for a period of time, the resin is broken due to insufficient strength, so that the work exchange capacity of the resin is obviously reduced, and the decoloring performance is obviously reduced. The performance of the resin cannot be recovered by conventional regeneration methods. Therefore, development of a high-performance macroporous weak base anion resin with high adsorption capacity and good mechanical strength is needed. Disclosure of Invention In order to solve the problems, the invention provides a macroporous weak base anion exchange resin, a preparation method and application thereof, wherein white balls with high mechanical strength, controllable specific surface area and adjustable aperture are obtained by regulating and controlling the preparation process of the cross-linked ethylene, the divinylbenzene and the pore-forming agent, and the purpose of decoloring sugar solution of xylose is realized by the macroporous weak base anion exchange resin synthesized by chloromethylation reaction and amination reaction of the white balls on the basis. Because the modified macroporous weak base anion resin has a controllable pore structure and good mechanical strength, has large exchange capacity and good wear resistance in the process of decoloring sugar liquid, and has long service life, the problem that the decoloring effect of the conventional macroporous weak base anion resin is obviously reduced after the modified macroporous weak base anion resin is used for a period of time is effectively improved. In order to achieve the above object, the present invention provides the following technical solutions: The invention provides a preparation method of macroporous weak base anion exchange resin, which comprises the following steps: 1) Mixing styrene, divinylben