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Production method of high-quality PPTA (poly(p-phenylene terephthalamide)) resin and PPD (p-phenylenediamine) stirring vessel

A technology of poly-p-phenylene terephthalamide and terephthaloyl chloride, which is applied in the direction of dissolution, dissolution, chemical instruments and methods, and can solve the problems of difficult control of molar ratio, temperature control of polymerization reaction, and quality of composite solvents. Fluctuation and other problems, to avoid repeated transfer, reduce corrosion, and easy to control the total molar ratio

Active Publication Date: 2019-06-21
HENAN SHENMA NYLON CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to provide a production method of high-quality poly-p-phenylene terephthalamide resin and a PPD dissolving kettle, which can effectively solve the fluctuations in the quality of the composite solvent, the molar ratio is difficult to control, the PPD is difficult to dissolve, and the polymerization temperature Control and other issues to achieve industrialized stable production

Method used

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  • Production method of high-quality PPTA (poly(p-phenylene terephthalamide)) resin and PPD (p-phenylenediamine) stirring vessel
  • Production method of high-quality PPTA (poly(p-phenylene terephthalamide)) resin and PPD (p-phenylenediamine) stirring vessel
  • Production method of high-quality PPTA (poly(p-phenylene terephthalamide)) resin and PPD (p-phenylenediamine) stirring vessel

Examples

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Effect test

Embodiment 1

[0038] A kind of production method of high-quality polyparaphenylene terephthalamide resin (PPTA), comprises the following steps:

[0039] (1) Mixed batch of NMP / CaCl2 composite solvent: first mix CaCl 2 Make it into an aqueous solution, then mix it with the solvent NMP, and remove the water after refining to obtain NMP / CaCl 2 Composite solvent (for the specific preparation process, please refer to patent 200810049483.9), under the condition of nitrogen blanketing, NMP / calcium chloride composite solvent, in the mixed batch tank at 95±5℃ for 3 days, relying on agitator and tank bottom pump Stir continuously and circulate, after batch mixing, the calcium chloride content is 8.0wt%, moisture 100PPm.

[0040] In order to prevent the moisture in the nitrogen from causing the moisture in the reaction system to exceed the standard and affect the reaction, the nitrogen index and dosage should be strictly controlled. The nitrogen dew point temperature must be lower than -70°C. Sligh...

Embodiment 2

[0048] A kind of production method of high-quality polyparaphenylene terephthalamide resin (PPTA), comprises the following steps:

[0049] (1) NMP / CaCl 2 Composite solvent mixed batch: NMP / calcium chloride composite solvent is not mixed batch, storage temperature is 95±5℃, calcium chloride content and moisture both fluctuate, calcium chloride content is 7.0-8.5%, moisture 100PPm; Nitrogen protection prevents the compound solvent from deteriorating;

[0050] (2) Preparation of p-phenylenediamine (PPD) solution: under the condition of nitrogen blanketing, add 1920kg of the composite solvent into the PPD dissolution kettle, make the stirring shaft 15 stir at a speed of 50 rpm, and pour into the PPD dissolution kettle through the feeding funnel 8 Add 100kg of PPD inside, feed circulating water from the water inlet 22 to make the dissolution temperature in the kettle 60°C, and get the PPD solution after fully dissolving for 1 hour, open the discharge valve on the discharge port 21...

Embodiment 3

[0056] A kind of production method of high-quality polyparaphenylene terephthalamide resin (PPTA), comprises the following steps:

[0057] (1) NMP / CaCl 2 Composite solvent mixed batch: under the condition of nitrogen blanketing, the NMP / calcium chloride composite solvent is mixed in the mixed batch tank at 95±5°C for 3 days, and it is stirred by the agitator and the tank bottom pump. , the calcium chloride content is 8.0%, the water content is 100PPm, and nitrogen is added in the tank to protect it from deterioration of the compound solvent;

[0058](2) Preparation of p-phenylenediamine (PPD) solution: under the condition of nitrogen blanketing, add 1920 kg of the composite solvent into the PPD dissolution kettle, stir the stirring shaft 15 at a speed of 40 rpm, and dissolve into the PPD through the feeding funnel 8 Add 100kg PPD into the kettle, dissolve at a temperature of 30°C, and obtain a PPD solution after fully dissolving for 1 hour. Open the discharge valve on the dis...

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Abstract

The invention provides a production method of high-quality PPTA (poly(p-phenylene terephthalamide)) resin and a PPD (p-phenylenediamine) stirring vessel, and belongs to the technical field of polymermaterials. The method for obtaining the high-quality PPTA resin comprises the following steps: blending of an NMP / CaCl2 complex solvent; preparation of a PPD solution; measuring of TPC (terephthaloylchloride); condensation polymerization; blank treatment. The PPD stirring vessel is also provided, PPD dissolution parameters such as temperature, stirring speed, dissolution time and the like are optimized, and all PPD can be dissolved and participate in the condensation polymerization. Pre-polymerization and the condensation polymerization are carried out in the same reactor, the technological process is short, the total molar ratio is easy to control, repeated transfer of materials is avoided, and influence of residues in the system on the molar ratio and influence of deterioration of deposited materials at dead corners of a conveying system on the reaction are avoided.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a production method of high-quality poly-p-phenylene terephthalamide resin and a PPD dissolving kettle. Background technique [0002] Polyparaphenylene terephthalamide resin (PPTA) is the raw material for preparing aramid 1414 fiber and pulp. Because of their high strength, high modulus, high temperature resistance, flame retardant and other excellent comprehensive properties, they have been widely used in military, aerospace, sports, communication, chemical, automotive and other fields. In 1972, Dupont Company carried out industrial production of PPTA type high-strength aramid fiber. The domestic development of high-strength aramid fibers began in the 1980s, but due to various internal and external factors, it was not until recent years that domestic industrial production has made great progress, and many special documents and patent reports have also been...

Claims

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Application Information

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IPC IPC(8): C08G69/32C08G69/28B01F1/00B01F7/16B01F15/02B01F15/06
Inventor 史红军赵铎张文广潘强郑淑昀王冬冬李晓峰陈聚良陈桂昌欧玲魏建毅赵辉孙浩杰董菲菲梁海军罗亚利晋卫国袁中良冯立伟尹胜利郑应山米朝圣陈聪段文蕊
Owner HENAN SHENMA NYLON CHEM
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