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Method for continuously preparing highly-pure poly(m-phenylene isophthalamide) resin solution

A technology of poly-m-phenylene isophthalamide and isophthaloyl chloride is applied in the industrialized continuous preparation of high-purity poly-m-phenylene isophthalamide resin solution and the field of polymer material production, and can solve the problem of high price, high cost and high cost. Corrosion, large engineering investment, etc.

Active Publication Date: 2016-10-26
SHANGHAI HUIBO NEW MATERIAL SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can meet the mixing requirements of different stages of polymerization and solve the heat dissipation problem. The polym-phenylene isophthalamide resin prepared by the continuous production method has a narrow molecular weight distribution, a stable inherent viscosity, and a viscosity of 2.0dl / More than g, it can meet the continuous and stable spinning requirements of polym-phenylene isophthalamide fiber; because the HCl produced in the reaction process is severely corrosive to commonly used stainless steel (such as 304, 316 and other stainless steels), and the prepared polym-phenylene isophthalamide The ash content of m-phenylenediamine phthalamide resin will increase. In order to reduce the corrosion of the equipment and improve the purity of the final resin product, it is better to use Hastelloy or titanium alloy to make the twin-screw polymerization reactor. The twin-screw polymerization reactor itself is processed High difficulty, complex structure, and high production costs lead to very expensive twin-screw polymerization reactors made of Hastelloy or titanium alloys and large engineering investment

Method used

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  • Method for continuously preparing highly-pure poly(m-phenylene isophthalamide) resin solution
  • Method for continuously preparing highly-pure poly(m-phenylene isophthalamide) resin solution
  • Method for continuously preparing highly-pure poly(m-phenylene isophthalamide) resin solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The production equipment used in this embodiment is as figure 2 As shown, the structural features of the device are as follows.

[0026] The device includes solvent metering delivery system, m-phenylenediamine metering delivery system, isophthaloyl chloride metering delivery system, twin-screw mixer 13, polymerization reactor 15 and resin solution storage tank 18, etc.; solvent metering delivery system includes solvent storage Tank 1, solvent delivery pump 3 and solvent mass flowmeter 5; m-phenylenediamine metering delivery system includes m-phenylenediamine storage tank 2, m-phenylenediamine delivery pump 4 and m-phenylenediamine mass flowmeter 6; The formyl chloride metering delivery system includes an isophthaloyl chloride storage tank 9, an isophthaloyl chloride delivery pump 10 and an isophthaloyl chloride mass flowmeter 11; their connection relationship is: the output port of the solvent storage tank 1 and the solvent delivery The input port of the pump 3 is con...

Embodiment 2

[0030] This embodiment adopts the same implementation device as that of Embodiment 1, but the process parameters are different.

[0031]The solid m-phenylenediamine (MPD) raw material is heated and melted at a temperature of 75°C into a fluid liquid molten state, and placed in the m-phenylenediamine storage tank 2 for standby; the solid isophthaloyl dichloride (IPC) raw material is in Heating and melting at a temperature of 55°C into a liquid molten state with fluidity, and placing it in the isophthaloyl chloride storage tank 9 for standby; the N,N-dimethylacetamide (DMAc) solvent in the solvent storage tank 1 is passed through the solvent After delivery pump 3 and solvent mass flow meter 5 are metered, enter from an input port 7 farthest away from output port 14 on the twin-screw mixer 13 at a flow rate of 330.12 mass parts per hour; m-phenylenediamine in the m-phenylenediamine storage tank 2 After the melt of diamine (MPD) is measured by the m-phenylenediamine delivery pump ...

Embodiment 3

[0034] This embodiment adopts the same implementation device as that of Embodiment 1, but the process parameters are different.

[0035] The solid m-phenylenediamine (MPD) raw material is heated and melted at 70°C into a fluid liquid molten state, and placed in the m-phenylenediamine storage tank 2 for standby; the solid isophthaloyl dichloride (IPC) raw material is in Heating and melting at a temperature of 50°C into a liquid molten state with fluidity, and placing it in the isophthaloyl chloride storage tank 9 for standby; the N,N-dimethylacetamide (DMAc) solvent in the solvent storage tank 1 is passed through the solvent After delivery pump 3 and solvent mass flowmeter 5 are metered, enter from an input port 7 farthest from output port 14 on the twin-screw mixer 13 at a flow rate of 390.01 parts by mass per hour; m-phenylenediamine in the m-phenylenediamine storage tank 2 After the melt of diamine (MPD) is measured by the m-phenylenediamine delivery pump 4 and the m-phenyle...

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Abstract

The invention relates to a method for continuously preparing a highly-pure poly(m-phenylene isophthalamide) resin solution. The method comprises the following steps: respectively metering and conveying a polar solvent, m-phenylenediamine and m-phthaloyl chloride, allowing above materials to enter a double screw mixer, mixing the materials, carrying out a preliminary reaction to generate oligomer, allowing the oligomer to enter a polymerization reactor from the bottom end, continuously carrying out the reaction for a period of time, and allowing the formed poly(m-phenylene isophthalamide) resin solution to flow out from the upper lateral part of the polymerization reactor. The method can reduce at least one double screw reactor needed in the prior art, reduces the device investment cost, and realizes continuous preparation of the poly(m-phenylene isophthalamide) resin solution with uniform viscosity and high purity.

Description

technical field [0001] The invention belongs to the field of polymer materials and relates to a production method of polymer materials. Specifically, it relates to a method suitable for industrial continuous preparation of high-purity polym-phenylene isophthalamide resin solution. Background technique [0002] Poly-m-phenylene isophthalamide is also called meta-aramid fiber or aramid fiber 1313. Meta-aramid fiber is one of the fastest-growing varieties of high-performance fibers today. It is a high-tech fiber with excellent comprehensive properties. It is widely used in protective clothing, honeycomb structure materials, electrical insulating paper and high-temperature filter materials, and is an important basic material in the fields of aerospace, electronics, communications, environmental protection, petrochemicals, marine development and special clothing. [0003] High-quality (uniform viscosity, high purity) polym-phenylene isophthalamide resin is an important prerequis...

Claims

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Application Information

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IPC IPC(8): C08G69/32
CPCC08G69/32
Inventor 刘岳新罗丹龚勇明罗建业胡艳君
Owner SHANGHAI HUIBO NEW MATERIAL SCI & TECH
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