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Preparation of polyisophthaloyl m-phenylene diamide spinning solution by using semi-continuous twin screw extruder

A technology of polym-phenylene isophthalamide spinning and isophthaloyl chloride, which is applied in the direction of spinning solution preparation, single-component polyamide artificial filament, etc., and can solve the problem that equimolar ratio is difficult to grasp, reaction Heat is not easy to remove, filtration is difficult, etc., to avoid the effect of molecular weight inhomogeneity

Inactive Publication Date: 2006-07-19
DONGHUA UNIV +1
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Problems solved by technology

Although this method can produce a spinning solution with low salt content, it will be difficult to filter when the molecular weight of the polymer is high
[0011] Moreover, solution polymerization basically adopts a discontinuous method, the heat of reaction is not easy to remove, and local overheating can easily lead to differences in molecular weight.
The continuous polymerization method disclosed in U.S. Patent No. 3287324 adopts the one-time feeding method of acid chloride, which has the disadvantage that the equimolar ratio is difficult to grasp

Method used

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  • Preparation of polyisophthaloyl m-phenylene diamide spinning solution by using semi-continuous twin screw extruder
  • Preparation of polyisophthaloyl m-phenylene diamide spinning solution by using semi-continuous twin screw extruder

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Embodiment 1

[0031] Dissolve one part of refined MPD in 8.7 parts of freshly distilled dry DMAC, add 1.7 parts of 60 °C refined IPC at -10 °C for prepolymerization to form a prepolymer containing hydrogen chloride, keep the temperature below 0 °C , After reacting for 20 minutes, add 0.27 parts of dry liquid ammonia under stirring at 0°C and keep it for 20 minutes to precipitate most of the hydrogen chloride, then press filter to remove the ammonium chloride crystals generated by the reaction, and keep the filtration temperature not exceeding 10°C . The filtrate and the remaining 0.177 parts of IPC enter a twin-screw extruder with a diameter of 25 mm, an aspect ratio of 1:40, and a rotational speed of 200 rpm, and the IPC is added in a molten state. Control the temperature of the twin-screw reactor below 50°C, extrude a colorless and transparent polymer for about 12 minutes, and then carry out the second neutralization, Ca(OH) 2 The amount is 0.084 parts. Finally, a polymer containing 19....

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Abstract

The semi-continuous twin screw preparation method of polyisophthaloyl m-phenylene diamide spinning solution uses twin screw extruder as main reactor and adopts the isophthaloyl dichloride double-charged and dried liquid ammonia as preveutralizing agent. The application of twin-screw extruder is favorable for system radiation problem, and prevents non-uniformity of polymer molecular weight distribution, and also id favorable for partially removing small molecular by-product in the polymerization system-hydrogen chloride gas. The length-to-diameter ratio of the twin-screw extruder is greater than 1:30. Said preparation method includes prepolymerization, preneutralization, filtration, polymerization and neutralization.

Description

technical field [0001] The invention relates to a semi-continuous twin-screw preparation of polym-phenylene isophthalamide spinning solution, more precisely, the preparation of poly-m-phenylene isophthalamide with a twin-screw extruder as the main reactor Amine spinning solution method. Background technique [0002] Polym-phenylene isophthalamide has excellent heat resistance and flame resistance, as well as excellent high-temperature electrical insulation properties, and is used to prepare fire-resistant and flame-resistant materials and high-use temperature insulating materials, such as fibers and paper. [0003] The existing method for preparing polym-phenylene isophthalamide is usually: [0004] 1) Interface polymerization [0005] m-Phenylenediamine and isophthaloyl chloride are reacted in a poor solvent of polym-phenylene isophthalamide, such as tetrahydrofuran, and then mixed with an aqueous solution containing an acid absorbent at a high speed, and the poly The po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01D1/02D01F6/60
Inventor 陈蕾扈益民刘兆峰朱富文胡祖明潘婉莲
Owner DONGHUA UNIV
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