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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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  • 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 the ratio of terephthaloyl chloride in the reaction process; this method divides the polymerization reaction into two stages, the first stage is the intermittent precondensation stage, because it is an intermittent polymerization, it will be inevitable Batch difference is generated, and the prepolymer formed has a higher apparent viscosity, which affects the precise metering and mixing of the second-stage continuous polymerization; the twin-shaft kneader reactor used in this method has no self-cleaning function, and the produced Accumulation will affect the continuous polymerization reaction in the second stage

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

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preparation example Construction

[0031] A preparation method for continuously preparing poly(p-phenylene terephthalamide) polymer, comprising the following steps:

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

[0033] (2) co-solvent-solvent and p-phenylenediamine and terephthaloyl chloride are continuously added to the mixer simultaneously, and flow into No. 1 twin-screw reactor after mixing; described p-phenylenediamine and terephthaloyl dichloride Acid chloride, its molar ratio is 1:1~1.01;

[0034] (3) The material flows into the mixing tank after being reacted in the No. 1 twin-screw reactor;

[0035] (4) oligomers and additives in the mixing tank are uniformly pumped into the No. 2 tw...

Embodiment 1

[0039] 7998.41kgN-methylpyrrolidone (NMP) solvent was added to 10m 3 In the dissolution kettle, after the solvent was heated up to 70°C, 695.51kg of anhydrous calcium chloride (CaCl 2 ) powder, stirred and dissolved for 4 hours, discharged into 30m 3 in a mixing tank. CaCl 2 -NMP solvent at 1086.74kg / h, p-phenylenediamine (PPD) powder at 56.74kg / h, and terephthaloyl chloride (TPC) melt at 106.52kg / h are continuously added to the mixer for mixing, and the inflow diameter is 125mm , The No. 1 twin-screw reactor with an aspect ratio of 7.2, a rotational speed of 200rpm, and a jacket temperature of 0°C, reacted in the reactor for 10s and then flowed into the mixing tank to form oligomers. The flow rate of oligomers was 1250kg / h Pump into the No. 2 twin-screw reactor with a diameter of 125mm, an aspect ratio of 7.2, a rotating speed of 200rpm, and a jacket temperature of 0°C. After reacting in the reactor for 10s, the inflow diameter is 400mm, and the aspect ratio is 10. No. 3 ...

Embodiment 2

[0041] 7998.41kgN-methylpyrrolidone (NMP) solvent was added to 10m 3 In the dissolution kettle, after the solvent was heated up to 70°C, 695.51kg of anhydrous calcium chloride (CaCl 2 ) powder, stirred and dissolved for 4 hours, discharged into 30m 3 in a mixing tank. CaCl 2 -NMP solvent at 1086.74kg / h, p-phenylenediamine (PPD) powder at 56.74kg / h, and terephthaloyl chloride (TPC) melt at 106.52kg / h are continuously added to the mixer for mixing, and the inflow diameter is 125mm The No. 1 twin-screw reactor with an aspect ratio of 7.2, a rotational speed of 200rpm, and a jacket temperature of 0°C, reacted in the reactor for 10s and then flowed into the mixing tank to form oligomers. The oligomers were flown at 1250kg / h, Liquid ammonia is simultaneously and continuously pumped at 16.05kg / h into the No. 2 twin-screw reactor with a diameter of 125mm, an aspect ratio of 7.2, a rotational speed of 200rpm, and a jacket temperature of 0°C. No. 3 twin-screw reactor with a diameter...

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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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