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Production process of polyisophthaloyl metaphenylene diamine polymer

A polym-phenylene isophthalamide, production process technology, applied in the production process field of poly-m-phenylene isophthalamide polymer, can solve difficult to grasp and control, inaccurate control, increasing colloid Difficulty of filtering etc.

Inactive Publication Date: 2014-01-08
东莞市灿森新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the prior art, the preparation method of polym-phenylene isophthalamide polymer comprises a polymerization step, simultaneously generates by-product hydrogen chloride, neutralization step, neutralizes hydrogen chloride in the step polymerization step with an alkaline earth metal compound, The reaction produces alkaline earth metal chlorides that can be dissolved in the reaction system, and the neutralization reaction is carried out in a twin-screw extruder, such as the Chinese invention patent No. "200610118482.6", "Preparation of polym-phenylene isophthalamide spinning solution As shown in the Chinese invention patent of the "method", the neutralization step in the production process of polym-phenylene isophthalamide polymer is completed by one neutralization reaction step, and in the neutralization reaction process, the neutralization The reaction is difficult to grasp and control in the control of the neutralization end point of the polymer colloid
Because if the pH value of neutralization is very low, it will affect the stability of the polymer. If the pH value is required to be around 7, because the closer to the end point, the more moderate the reaction, it is easy to cause slight alkaline earth in the neutralized polymer. The excess of metal oxides or hydroxides exists. Since this excess is a powder suspension and insoluble in the polymer colloid, it will inevitably cause difficulties in the subsequent filtration of the polymer colloid.
Due to the inability to accurately control the neutralization end point of the polymer colloid, more impurities such as powdery suspended solids remain in the polymer, which increases the difficulty of colloid filtration, increases the complexity and processing difficulty of the subsequent process, and also reduces the quality of the obtained polymer. worse, so there is a need to improve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A kind of production technique of polym-phenylene isophthalamide polymer, comprises the following steps,

[0024] In the diamine dissolving step, m-phenylenediamine is added to a temperature of 20-60 degrees in an amide polar organic solvent, and m-phenylenediamine is dissolved in an amide polar organic solvent; in a preferred embodiment, m-phenylene The diamine is selected from polymer grade m-phenylenediamine, and the amide polar organic solvent is selected from dimethylacetamide solution, and the dimethylacetamide solution made from 6 to 8 parts of weight of dry dimethylacetamide is mixed with 1 Part weight of polymeric grade m-phenylenediamine is added to the dimethylacetamide solution, and the temperature of the solution is controlled at 20-30 degrees;

[0025] In the normal temperature polymerization step, the temperature of the solution obtained in the diamine dissolving step is controlled at 20-40 degrees, and isophthaloyl dichloride is added under the reaction ...

Embodiment 2

[0032] A kind of specific production technique of polym-phenylene isophthalamide polymer, comprises the following steps,

[0033] In the diamine dissolving step, m-phenylenediamine is selected from polymer grade m-phenylenediamine, amide polar organic solvent is selected from dimethylacetamide solution, and dimethylacetamide made from 7.8 parts by weight of dry dimethylacetamide Acetamide solution, 1 part by weight of polymeric grade m-phenylenediamine is added to the dimethylacetamide solution, and the temperature of the solution is controlled at 20-30 degrees;

[0034] In the normal temperature polymerization step, continuously and slowly the polymerization grade isophthaloyl dichloride of 1.88 parts by weight;

[0035]In the rough control neutralization reaction step, corresponding to 1 part by weight of m-phenylenediamine in the diamine dissolution step, 0.65 parts by weight of alkaline earth metal oxide or hydroxide is added, and in a preferred embodiment, corresponding t...

Embodiment 3

[0039] A kind of specific production technique of polym-phenylene isophthalamide polymer, comprises the following steps,

[0040] In a tank reactor with stirring and jacket, add 1 part by weight of polymer-grade m-phenylenediamine to 7.8 parts by weight of dry dimethylacetamide, control the temperature at 20-30 degrees, and continuously Slowly add 1.88 parts by weight of polymeric isophthaloyl chloride for polymerization, and the hydrogen chloride generated is continuously neutralized with 0.65 parts by weight of calcium hydroxide dimethylacetamide solution, wherein calcium hydroxide and dimethyl The weight ratio of acetamide is 1:2, the temperature is controlled below 70 degrees, and then 0.07 parts by weight of diethylamine-dimethylacetamide solution is used for continuous neutralization reaction. The weight ratio of diethylamine and dimethylacetamide The ratio is 1:2, and the resulting colloidal polymer of polyisophthaloyl dichloride m-phenylenediamine has a polymer concent...

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PUM

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Abstract

The invention discloses a production process of a polyisophthaloyl metaphenylene diamine polymer. The production process comprises a diamine dissolution step, a normal-temperature polymerization reaction step, a coarse control neutralization reaction step and a fine control neutralization reaction step. According to the production process, the neutralization reaction can be better controlled and especially the finishing of the neutralization reaction can be controlled in such a way that a polymer is neutralized by respectively adding different neutralizing agents in two steps, more than 80% of neutralization reaction is completed in the first coarse control neutralization reaction step and the rest of neutralization reaction is completed by using diethylamine, so that the polymer with excellent neutralization quality is obtained, and the subsequent filtering and processing difficulties of a colloid are reduced.

Description

technical field [0001] The invention relates to the technical field of production technology of polym-phenylene isophthalamide polymer, in particular to a production technology of poly m-phenylene isophthalamide polymer. Background technique [0002] In the prior art, the preparation method of polym-phenylene isophthalamide polymer comprises a polymerization step, simultaneously generates by-product hydrogen chloride, neutralization step, neutralizes hydrogen chloride in the step polymerization step with an alkaline earth metal compound, The reaction produces alkaline earth metal chlorides that can be dissolved in the reaction system, and the neutralization reaction is carried out in a twin-screw extruder, such as the Chinese invention patent No. "200610118482.6", "Preparation of polym-phenylene isophthalamide spinning solution As shown in the Chinese invention patent of the method ", the neutralization steps in the production process of polym-phenylene isophthalamide polyme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32C08G69/46
Inventor 钟彤
Owner 东莞市灿森新材料有限公司
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