Device for continuous preparation of poly(p-phenylene terephthalamide) polymer and preparation method

A technology of poly-p-phenylene terephthalamide and polymers, which is applied in the field of polymer material manufacturing and industrial continuous preparation of poly-p-phenylene terephthalamide polymers. Continuous polymerization precision metering and mixing, reduced reactivity and other issues, to achieve the effect of continuous and stable spinning

Active Publication Date: 2011-10-05
上海舟汉纤维材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method overcomes the adverse effects of weather and operation on the water content of the polymerization solvent system, and realizes continuous, airtight, and clean production. However, in this method, the p-phenylenediamine powder is completely dissolved in a solvent containing a co-solvent first. After industrial production, Since p-phenylenediamine stays in the solvent containing co-solvent for a long time, the activation of co-solvent will make p-phenylenediamine darker and reduce its reactivity, thus affecting the poly-p-phenylenediamine terephthalamide polymer And the color of the fiber also affects

Method used

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  • Device for continuous preparation of poly(p-phenylene terephthalamide) polymer and preparation method
  • Device for continuous preparation of poly(p-phenylene terephthalamide) polymer and preparation method
  • Device for continuous preparation of poly(p-phenylene terephthalamide) polymer and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0031] A preparation method for continuous preparation of poly(p-phenylene terephthalamide) polymer comprises the following steps:

[0032] (1) A co-solvent with a concentration of 4-12% by mass percentage is dissolved in one or a mixture of N-methylpyrrolidone, dimethylacetamide, N-ethylpyrrolidone, and diethylacetamide In the solvent of, a co-solvent-solvent system is formed; the co-solvent is chloride, which is one of calcium chloride, magnesium chloride, and lithium chloride or a mixture thereof;

[0033] (2) The co-solvent-solvent, p-phenylenediamine and terephthaloyl chloride are continuously added to the mixer at the same time, and flowed into the first twin-screw reactor after mixing; said p-phenylenediamine and p-xylylenediamine The molar ratio of acid chloride is 1:1~1.01;

[0034] (3) After reacting in the No. 1 twin-screw reactor, the materials flow into the mixing tank;

[0035] (4) The oligomers and additives in the mixing tank are uniformly pumped into the second twin-...

Example Embodiment

[0038] Example 1:

[0039] 7998.41kg N-methylpyrrolidone (NMP) solvent is added to 10m 3 In the dissolving kettle, after the solvent is heated to 70℃, add 695.51kg of anhydrous calcium chloride (CaCl 2 ) Powder, stir to dissolve for 4 hours, discharge 30m 3 Mixing tank. CaCl 2 -NMP solvent at 1086.74 kg / h, p-phenylenediamine (PPD) powder at 56.74 kg / h, and terephthaloyl chloride (TPC) melt at 106.52 kg / h are continuously added to the mixer for mixing, and the inflow diameter is 125 mm , The first twin-screw reactor with a length-to-diameter ratio of 7.2, a rotation speed of 200 rpm, and a jacket temperature of 0°C. After reacting in this reactor for 10 seconds, it flows into the mixing tank to form oligomers. The flow rate of oligomers is 1250kg / h. Pump into the second twin-screw reactor with a diameter of 125mm, an aspect ratio of 7.2, a rotation speed of 200rpm, and a jacket temperature of 0°C. After reacting for 10 seconds in the reactor, the inflow diameter is 400mm and the a...

Example Embodiment

[0040] Example 2:

[0041] 7998.41kg N-methylpyrrolidone (NMP) solvent is added to 10m 3 In the dissolving kettle, after the solvent is heated to 70℃, add 695.51kg of anhydrous calcium chloride (CaCl 2 ) Powder, stir to dissolve for 4 hours, discharge 30m 3 Mixing tank. CaCl 2 -NMP solvent at 1086.74 kg / h, p-phenylenediamine (PPD) powder at 56.74 kg / h, and terephthaloyl chloride (TPC) melt at 106.52 kg / h are continuously added to the mixer for mixing, and the inflow diameter is 125 mm The first twin-screw reactor with a length-to-diameter ratio of 7.2, a rotation speed of 200 rpm, and a jacket temperature of 0°C, reacted in this reactor for 10 seconds and then flows into the mixing tank to form oligomers. The oligomers flow at 1250 kg / h. Liquid ammonia was continuously pumped into the second twin-screw reactor with a diameter of 125mm, a length-to-diameter ratio of 7.2, a rotation speed of 200 rpm, and a jacket temperature of 0°C at 16.05kg / h. The reactor was reacted for 10 secon...

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Abstract

A device for continuous preparation of poly(p-phenylene terephthalamide) polymer and a preparation method belong to the field of polymer materials, and relate to the polymer material manufacturing technology. The invention is characterized in that: the poly(p-phenylene terephthalamide) polymer is prepared by using the preparation device and through the following steps: preparing a cosolvent-solvent system; proportionally and simultaneously adding the cosolvent-solvent, p-phenylenediamine and terephthaloyl chloride into a No.1 mixer, mixing and allowing the mixture to flow into a twin screw reactor; successively allowing the mixture to flow into a subsequent mixer and a No.2 twin screw reactor till a light-yellow breadcrumb-like mixture is extruded from a No.3 twin screw reactor, pulverizing the mixture, washing by water, and drying to obtain the poly(p-phenylene terephthalamide) polymer. The method of the invention can solve the problems of deepened color and decreased reactivity of p-phenylenediamine caused by long-term storage in a cosolvent-containing solvent; the combination of a plurality of twin screw reactors meets the mixing requirements of the polycondensation reaction at different stages and provides a logarithmic viscosity of above 6.5 dl/g; the performance requirements for industrial continuous preparation are met.

Description

technical field [0001] The invention belongs to the field of polymer materials and relates to polymer material manufacturing technology. Specifically, it relates to a device suitable for industrial continuous preparation of poly(p-phenylene terephthalamide) polymers and its preparation method. Background technique [0002] Poly-paraphenylene terephthalamide fiber is also called para-aramid fiber. Para-aramid fiber is the most widely used and most demanded fiber among high-performance fibers in the world. The first choice for special protective materials, widely used in aerospace, aviation, military industry, electromechanical, construction, automobile, sporting goods and other fields. [0003] High-quality poly-p-phenylene terephthalamide polymer is an important prerequisite for preparing high-quality poly-p-phenylene terephthalamide fibers. The poly-p-phenylene terephthalamide polymer in the present invention The chemical structure of the body is as follows: [0004] ...

Claims

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Application Information

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IPC IPC(8): D01F6/60C08G69/32
Inventor 刘岳新周文奎金伟
Owner 上海舟汉纤维材料科技股份有限公司
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