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Manufacturing method of alcohol soluble sulfonic acid type cation exchange resin

A technology of cation exchange and manufacturing method, which is applied in the field of functional resin materials and its manufacturing, can solve the problems of inefficiency, high manufacturing cost of sulfonated products, unsuccinct treatment process, etc., and achieve uniform composition and structure, effective homogeneous Sulfonation reaction, effect of improving product appearance

Active Publication Date: 2018-05-25
雷引林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

That is to say, the manufacturing cost of the whole sulfonated product remains high due to the unsophisticated and inefficient solvent post-treatment process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First according to Chinese invention patent application (application number: 201110083107.3) embodiment 1-3 corresponding test condition and method described in No. 8 test, coordination polymerization prepares linear poly(styrene-ethylene) alternating copolymer, uses GPC Measured by the method (using polystyrene as the standard sample, mobile phase is 1,2-C 6 D. 4 Cl 2 , the temperature is 145°C): M n 42,000, molecular weight distribution coefficient (M w / M n ) is 2.07, use 1 HNMR method records (solvent is C 2 D. 2 Cl 4 , the temperature is 120°C, PS mol%=4A ar / (5A al +A ar ), where A ar Represents the number of protons in the benzene ring of the polystyrene component, A al Represents the number of protons in the aliphatic chain (including the ethylene of the polyethylene component and the polystyrene component): the content of the polystyrene component is 47mol% (mole percent), which is converted into a mass content of 76.7% (equal to 104.15 ×47 / (104.15...

Embodiment 2

[0022] Still adopt the linear poly(styrene-ethylene) alternating copolymer described in embodiment 1, the sulfonation step of alcohol-soluble cationic exchange resin is as follows: 1) 500g linear poly(styrene-ethylene) alternating copolymer ( Containing 383.5g of polystyrene components (3.68mol in total), put it into a 20L glass reactor, add 6.0L (about 7400g) of dichloroethane, heat to 50-55°C, stir for 50 minutes, and then completely dissolve into Clarified solution; 2) In a 10L three-neck flask (ice-water bath) with nitrogen protection and an outlet connected to a drying tube, add 2400mL (about 2970g) dichloroethane and 1650g acetic anhydride (content 99%, 16.0mol) in sequence , stirred for a while, then added dropwise 1110g concentrated sulfuric acid (content 98%, 11.0mol), and the control was completed dropwise in about 45 minutes; Stirring and reacting for about 120 minutes, naturally warming up to room temperature, obtained completely clear fresh reaction solution of ace...

Embodiment 3

[0025]First refer to the test conditions and methods described in the No. 9 test corresponding to the Chinese invention patent application (application number: 201110083107.3) embodiment 1-3, coordinate polymerization to prepare linear poly(styrene-ethylene) alternating copolymers, use GPC Measured by method: M n 35,000, molecular weight distribution coefficient (M w / M n ) is 2.16, use 1 According to the HNMR method, the content of the polystyrene component is 37 mol%, and the converted mass content is 68.6%.

[0026] The sulfonation steps of alcohol-soluble cation exchange resin are as follows: 1) 500g linear poly(styrene-ethylene) alternating copolymer (343g containing polystyrene component, 3.3mol in total) is put into a 20L glass reactor, Add 6.4L (about 7900g) of dichloroethane, heat to 45-50°C, stir for 80 minutes, and dissolve into a clear liquid; Add 1200mL (about 1480g) of dichloroethane and 852g of acetic anhydride (content 99%, 8.26mol) in sequence, stir for a ...

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Abstract

The invention discloses a manufacturing method of alcohol soluble sulfonic acid type cation exchange resin. Linear poly(styrene-ethylene) alternating copolymers are used as raw materials and are completely dissolved in dichloroethane; then, an acetylsulfuric acid solution generated by concentrated sulfuric acid and acetic anhydride is dropwise added; homogeneous sulfonation reaction is implemented; then, reaction products are extruded into water containing a dispersant and sodium hydroxide through a stainless steel high-pressure spray nozzle; the mixture is fast scattered into a suspension system by a stirring paddle with a cutting function; finally, reduced pressure distillation is performed to recover dichloroethane; suspended particles are drained, and are then washed by deionized waterfor many times; after the draining, forced air drying is performed; the alcohol soluble sulfonic acid type cation exchange resin product is obtained. The cation exchange resin product prepared by themethod has the advantages that the particle size and the inside sulfonic acid group distribution are uniform; the cation exchange resin product can be completely dissolved in low-toxicity organic alcohol; the manufacturing process is simple, compact and efficient; the cost is low; the large-scale industrial production can be easily realized.

Description

technical field [0001] The invention belongs to the field of functional polymer materials, in particular to a poly(styrene-ethylene) alternating copolymer, which can be completely dissolved in alcohol organic solvents, has a strong acidic sulfonic acid functional group, and can rapidly generate Functional resin material for cation exchange and its manufacturing method. Background technique [0002] Linear polymer materials containing sulfonated polystyrene components (also known as sulfonated polystyrene-based polymers), due to their ability to be highly swellable in aqueous solutions, moderately soluble in organic solvents, and strongly hydrophilic , fast cation exchange and other physical and chemical properties, it is widely used in various fields such as hydrophilic membrane preparation, water treatment, construction, environmental protection, energy, and medicine. For example, as the main material or auxiliary additive material of negatively charged membranes for hydro...

Claims

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Application Information

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IPC IPC(8): C08F8/36C08F212/08B01J39/20
CPCB01J39/20C08F8/36C08F212/08
Inventor 雷引林高章华陈飞李南文廖家友殷锦邓承毅
Owner 雷引林