Method for recycling dihydrate hexamethylene-1,6-sodium dithiosulfate from waste fluid by coupling crystallization

A technology of disodium dithiosulfate and hexamethylene dihydrate is applied in the field of recovering hexamethylene dihydrate-1 in waste liquid, and achieves the effects of easy operation and simple process

Active Publication Date: 2013-08-28
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention is to solve the existing method of preparing dihydrate hexamethylene-1,6-dithiosulfuric acid disodium salt after the reaction is completed and separated, the waste liquid still contains the active ingredient dihydrate hexamethylene-1,6 -The problem of dithiosulfuric acid disodium salt, and provide a kind of coupling crystallization to reclaim the method of dihydrate hexamethylene-1,6-dithiosulfuric acid disodium salt in the waste liquid

Method used

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  • Method for recycling dihydrate hexamethylene-1,6-sodium dithiosulfate from waste fluid by coupling crystallization
  • Method for recycling dihydrate hexamethylene-1,6-sodium dithiosulfate from waste fluid by coupling crystallization
  • Method for recycling dihydrate hexamethylene-1,6-sodium dithiosulfate from waste fluid by coupling crystallization

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specific Embodiment approach 1

[0025] Specific embodiment 1: In this embodiment, a method for coupling crystallization to reclaim dihydrate hexamethylene-1,6-dithiosulfate disodium salt in waste liquid is carried out according to the following steps:

[0026] 1. Preparation of solid residue: Concentrate the waste liquid under reduced pressure at a temperature of 30°C to 50°C and a vacuum of -0.09MPa to -0.15MPa until there is no distillate, and then at a temperature of 35°C to 45°C Drying for 2h to 3h under high temperature to obtain a solid residue;

[0027] 2. Dissolution and crystallization: put the solid residue obtained in step 1 in the crystallizer, then add water to the crystallizer, and raise the temperature to 73°C to 78°C at a stirring speed of 20rpm to 30rpm until the solid residue is completely dissolved. And at this temperature, add a dissolving agent preheated to 50°C to 60°C for elution and crystallization. After adding the eluent, continue to stir at a constant temperature for 1h to 2h to ob...

specific Embodiment approach 2

[0031] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the mass ratio of solid residue and water obtained in Step 1 described in Step 2 is 1:2.5. Others are the same as in the first embodiment.

specific Embodiment approach 3

[0032]Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the mass ratio of water to eluting agent described in step 2 is 1:20. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a method for recycling dihydrate hexamethylene-1, 6-sodium dithiosulfate from waste fluid by coupling crystallization, and relates to a method for recycling dihydrate hexamethylene-1,6-sodium dithiosulfate from waste fluid. The method is used for solving the problem that, in the existing preparation method of dihydrate hexamethylene-1,6-sodium dithiosulfate, after reaction and separation, the waste liquid still contains the effective constituent dihydrate hexamethylene-1,6-sodium dithiosulfate. A first method comprises the following steps of: 1, preparing solid residue; 2, performing dilution crystallization to get the dihydrate hexamethylene-1,6-sodium dithiosulfate. A second method comprises the following steps of: reducing pressure to concentrate the waste liquid, then, gradually adding preheated alcohol, maintaining system back flow, performing dilution crystallization, performing cooling crystallization on the crystallization mother liquor, after performing crystallization, filtering and drying to get the dihydrate hexamethylene-1,6-sodium dithiosulfate. A third method comprises the following steps of: 1, preparing solid residue; 2, preparing crystallization mother liquor; 3, performing dilution crystallization to get the dihydrate hexamethylene-1,6-sodium dithiosulfate. The method provided by the invention can be used for recycling the dihydrate hexamethylene-1,6-sodium dithiosulfate in the waste liquid.

Description

technical field [0001] The invention relates to a method for recovering dihydrated hexamethylene-1,6-dithiosulfuric acid disodium salt in waste liquid. Background technique [0002] Post-vulcanizing agent dihydrate hexamethylene-1,6-dithiosulfate disodium salt (Duralink HTS, Hexamethylene-1,6-bisthiosulfate Sodium dihydrate), chemical formula C 6 h 12 Na 2 o 6 S 4 2H 2 O, the molar mass is 390.43g / mol, and its structural formula is as follows: [0003] [0004] Widely used in the field of rubber, it can greatly improve the thermal stability of rubber and provide the actual performance of rubber. At present, in industry, the synthesis of this substance mainly takes the following route: [0005] [0006] After the preparation reaction is completed and separated, the waste liquid still contains a certain amount of active ingredient dihydrate hexamethylene-1,6-dithiosulfate disodium salt, and the coexisting substances include the remaining reaction product sodium th...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): C07C381/02C08L21/00C08K5/41
Inventor宋梁成杨春晖张晓磊
OwnerHARBIN INST OF TECH