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Refining method for recovery of solvent and unpolymerized monomers in the production process of wet compound rubber

A production process and wet mixing technology, which is applied in the field of refining solvents and unpolymerized monomers in the wet mixing rubber production process, and can solve the problem of large loss of solvent monomers, large consumption of washing water, and failure to achieve polymerization Level requirements and other issues, to achieve the effect of low cost and simple operation

Active Publication Date: 2020-02-21
FUSHUN YIKESI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

If the above-mentioned existing refining and purification technology is adopted, ethanol is difficult to remove due to the good solubility of ethanol in the recovered mixture and the formation of an azeotrope with the solvent or monomer, so that the recovered solvent and unpolymerized monomer after refining are either Does not meet the requirements of polymerization grade (ethanol content is less than 0.0001wt%), or the consumption of washing water is large or the loss of solvent monomer is large, which makes it economically uneconomical

Method used

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  • Refining method for recovery of solvent and unpolymerized monomers in the production process of wet compound rubber
  • Refining method for recovery of solvent and unpolymerized monomers in the production process of wet compound rubber
  • Refining method for recovery of solvent and unpolymerized monomers in the production process of wet compound rubber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) the mixture (the water that contains 0.02wt% of water, the ethanol of 0.05wt% and other impurity with the solvent normal hexane that reclaims in the solution polymerization styrene-butadiene glue wet mixing process and unpolymerized monomer, the unpolymerized monomer Content is 0wt%) enters from the middle part of the rectifying tower that the number of theoretical plate is 20, wherein, mixture flow rate is 50000kg / h, rectifying tower operating pressure 0.1MPaG, reflux ratio 1, tower top temperature 65 ℃, tower bottom temperature 90 ℃; the mixture 1 of solvent and unpolymerized monomer is extracted at the bottom of the tower (the content of water and ethanol is all less than 0.0001wt%), and the azeotropic mixture 2 of solvent, unpolymerized monomer, ethanol and water is extracted at the top of the tower;

[0040] (2) Wash the azeotropic mixture 2 of the solvent, unpolymerized monomer, ethanol and water extracted from the top of the tower in step (1) with water (three...

Embodiment 2

[0053] (1) the solvent hexane that reclaims in the rare earth isoprene rubber glue wet mixing process and the mixture of unpolymerized monomer (containing the water of 0.02wt%, the ethanol of 0.05wt%, the isoprene of 1wt% and Other impurities) enter from the middle of a rectification tower with a theoretical plate number of 20, wherein the flow rate of the mixture is 50000kg / h, the operating pressure of the rectification tower is 0.2MPaG, the reflux ratio is 5, the temperature at the top of the tower is 68°C, and the temperature at the bottom of the tower is 100°C; A mixture 1 of solvent and unpolymerized monomer is taken out at the bottom of the tower (the content of water and ethanol is all less than 0.0001wt%), and an azeotropic mixture 2 of solvent, unpolymerized monomer, ethanol and water is taken out at the top of the tower;

[0054] (2) Wash the azeotropic mixture 2 of the solvent, unpolymerized monomer, ethanol and water extracted from the top of the tower in step (1) w...

Embodiment 3

[0067] (1) The mixture of solvent hexane and unpolymerized monomers recovered in the rare earth isoprene rubber glue wet mixing process (containing 0.02wt% of water, 0.2wt% of ethanol, 5wt% of isoprene and other Impurities) with a flow rate of 50000kg / h, first wash with an aqueous sodium hydroxide solution with a flow rate of 5000kg / h, a concentration of 0.2mol / L, and a temperature of 40°C, and then enter from the middle of a rectification tower with a theoretical plate number of 20. Rectification column operating pressure 0.2MPaG, reflux ratio 5, tower top temperature 68 ℃, tower bottom temperature 100 ℃; The mixture 1 of extraction solvent and unpolymerized monomer (the content of water and ethanol all is less than 0.0005wt%) at the bottom of the tower, The azeotropic mixture 2 of solvent, unpolymerized monomer, ethanol and water is withdrawn from the tower top;

[0068] (2) Wash the azeotropic mixture 2 of the solvent, unpolymerized monomer, ethanol and water extracted from...

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Abstract

The invention belongs to the technical field of novel rubber material production and particularly relates to a method for refining solvents and unpolymerized monomers recovered in a wet rubber compound production process. The method comprises the steps as follows: a mixture of the solvents and the unpolymerized monomers recovered in the wet rubber compound production process is added to a rectifying tower for rectification, a mixture 1 of the solvents and the unpolymerized monomers is extracted from the tower bottom, and an azeotropic mixture 2 of the solvents, the unpolymerized monomers, ethanol and water is extracted from the tower top; the mixture extracted from the tower top is washed so that the ethanol content is reduced to 0.0005wt% or below; the mixture extracted from the tower bottom is further subjected to separation or adsorption refining, and polymer-grade solvents and unpolymerized monomers are obtained; the washed mixture extracted from the tower top is mixed with a material entering the rectifying tower. The recycling rate of the solvents and the unpolymerized monomers is high, the loss rate of the recovered solvents and unpolymerized monomers is low, water consumption in the washing process is greatly reduced, and the recovered products including the solvents and the unpolymerized monomers have low ethanol content, meet the polymer-grade requirement and can be recycled.

Description

technical field [0001] The invention belongs to the technical field of production of new rubber materials, and in particular relates to a refining method for recovering solvents and unpolymerized monomers in the production process of wet mixing rubber. Background technique [0002] In 1991, the French Michelin company applied for the iconic "green tire" patent EP0501227A1. This patent uses highly dispersed silica as a tread rubber filler, and uses a specific process to blend silica and styrene-butadiene. The tires have achieved low rolling resistance, high wet skid resistance, high wear resistance and low noise at the same time, creating a precedent for "green tires". However, the traditional mixing process uses large mixing equipment, including internal mixers, kneaders, and open mills, to mix powdered fillers and additives into solid rubber. This kind of dry process has long mixing time, high energy consumption, more dust and poor dispersion, thus limiting the further imp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08J11/02C08L9/06C08L9/00
CPCC08J11/02C08J2309/00C08J2309/06
Inventor 李云涛
Owner FUSHUN YIKESI NEW MATERIAL