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

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

CN102206339AActive 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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  • 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

Patent Timeline
05 Oct 2011
Publication
CN102206339A
IPC
D01F6/60; C08G69/32
Inventors
刘岳新; 周文奎