Method for preparing strong acid type ion exchange fibers by sulfonating PP-ST-DVB fibers

A technology of PP-ST-DVB and ion exchange fibers, which is applied in the field of green environmental protection to improve the preparation of PP-ST-DVB-based strong acid ion exchange fibers, and can solve the problems of cumbersome, large amount of waste acid treatment, acid gradient leaching, etc.

Active Publication Date: 2015-08-26
河南省科学院同位素研究所有限责任公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problems in the prior art that a large amount of waste acid is produced during the sulfonation of concentrated sulfuric acid to prepare strong-acid ion exchange fibers, and the post-reaction treatment is cumbersome, and acid gradient leaching is required. The present invention proposes sulfonation of PP-ST-DVB fibers to prepare strong-acid type The process equipment improvement method of ion exchange fiber, in this method, the sulfonation reaction adopts step-by-step heating, the sulfonation liquid can be reused, and no waste acid is discharged; after the reaction is completed, the dichloroethane on the surface of the fiber can be directly removed by vacuum distillation Obtain strong acid ion exchange fibers without acid gradient washing

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1: the sulfonation process step of this example comprises:

[0021] (1) Get 1 kilogram of PP-ST-DVB fibers with a grafting rate of 180%, and use 10L 1,2-dichloroethane to swell in a reactor for 10 hours;

[0022] (2) After the PP-ST-DVB fiber is swollen, take it out and put it into the reaction kettle, and prepare 30L dichloroethane dilution solution of chlorosulfonic acid in the storage tank, which contains 0.8L chlorosulfonic acid, and use a chemical pump to sulfonate The liquid flows in slowly from the liquid storage tank through the bottom of the reactor. After the addition is completed, the chemical pump is turned on to make the reaction liquid spray out from the bottom of the reactor through the pipeline from the top of the reactor similar to the shower nozzle; the water bath circulation heating device is turned on to make the reaction The temperature in the kettle rises, and at the same time, the disc with holes is lowered to fully contact the sulfonat...

Embodiment 2

[0025] Embodiment 2: the sulfonation process step of this example comprises:

[0026] (1) Get 1 kilogram of PP-ST-DVB fibers with a graft rate of 150%, and use 15L of 1,2-ethylene dichloride to swell for 10 hours;

[0027] (2) After the PP-ST-DVB fiber is swollen, take it out and put it into the reaction kettle, and prepare 45L dichloroethane dilution solution of chlorosulfonic acid in the storage tank. The chlorosulfonic acid contains 0.6L, and the sulfonated The liquid flows in slowly from the liquid storage tank through the bottom of the reactor. After the addition is completed, the chemical pump is turned on to make the reaction liquid spray out from the bottom of the reactor through the pipeline from the top of the reactor similar to the shower nozzle; the water bath circulation heating device is turned on to make the reaction The temperature in the kettle rises, and at the same time, the disc with holes is lowered to fully contact the sulfonated liquid and the fiber; the...

Embodiment 3

[0030] Embodiment 3: the sulfonation process step of this example comprises:

[0031](1) Get 20 kilograms of PP-ST-DVB fibers with a graft rate of 120%, and use 20 L of 1,2-dichloroethane to swell for 10 hours; (2) Take out the PP-ST-DVB fibers after swelling and put them into the reaction In the kettle, prepare 30L of dichloroethane dilution of chlorosulfonic acid in the liquid storage tank, wherein chlorosulfonic acid contains 0.4L, use a chemical pump to slowly flow the sulfonated solution from the storage tank through the bottom of the reaction kettle, add After the completion, turn on the chemical pump to make the reaction liquid spray evenly from the bottom of the reaction kettle through the pipeline from the top of the reaction kettle similar to the shower nozzle; turn on the water bath circulation heating device to increase the temperature in the reaction kettle, and at the same time lower the hole disc to make the sulfur The chemical solution and the fiber are in full...

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Abstract

The invention discloses a method for preparing strong acid type ion exchange fibers by sulfonating PP-ST-DVB fibers. The method comprises the following steps: swelling the PP-ST-DVB fibers by using a swelling agent for 6-12 hours; then adding a sulfonating solution into the bottom of a reaction kettle and gradually heating to finish a sulfonating reaction; after the sulfonating reaction is finished, recycling the sulfonating solution into a solution storage tank; then, removing the swelling agent attached on the surfaces of the fibers by reduced pressure distillation; collecting and refluxing the volatile swelling agent into the solution storage tank; and after reduced pressure and distillation, obtaining PP-ST-DVB-based strong acid type ion exchange fibers and subpackaging for storage so as to avoid acid gradient washing. A certain amount of a dilution solution of chlorosulfonic acid is supplemented in the sulfonating solution and the sulfonating solution can be circularly utilized, so that the PP-ST-DVB fibers are continually sulfonated to prepare the strong acid type ion exchange fibers. The sulfonating method has the advantages that the preparation process is simple, the cost is obviously reduced, the acid solution gradient solution is not needed, no waste solutions are discharged, the sulfonating solution can be circularly utilized and the like.

Description

technical field [0001] The invention belongs to the technical field of ion exchange material preparation, and relates to an improvement method of process equipment for preparing strong-acid ion-exchange fibers by sulfonation of PP-ST-DVB fibers, which is a green and environmentally friendly improved PP-ST-DVB-based strong-acid ion-exchange fibers method of preparation. Background technique [0002] Ion-exchange fiber is a fibrous ion-exchange material. Due to its advantages of fast adsorption, high degree of purification, small water resistance, and convenient regeneration, it has broad applications in environmental protection, resource recovery, medicine, chemical industry, and metallurgy. Therefore, it has received more and more attention. [0003] At present, the methods for preparing strong acid ion exchange fibers reported in the literature include polymer chemical conversion method, polymer grafting monomer method, melt spinning method, etc., while using concentrated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/256B01J39/18D06M101/20B01J39/17
Inventor 张本尚陈海军赵惠东李坤豪王允张宏娜李召朋全彦君赵梅红丁光伟周从章
Owner 河南省科学院同位素研究所有限责任公司
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