Method for preparing vinyl cyanide/methacrylic acid copolymer

A technology of methacrylic acid and acrylonitrile, applied in the field of preparation of acrylonitrile/methacrylic acid copolymer, can solve the problem of difficult to become high-performance foam plastic, high polymer foam plastic with poor mechanical properties and low chain link ratio, etc. problem, to achieve the effect of low water absorption, good stability and high heat resistance temperature

Inactive Publication Date: 2014-04-09
王少辉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since methacrylic acid is a hydrophilic monomer, the resulting high polymer and its foam plastics have poor mechanical properties and high water absorption.
As the polymerization proceeds, since more methacrylic acid enters the copolymer in the previous stage, less and less methacrylic acid enters the copolymer; more and more acrylonitrile enters the copolymer, and the acrylonitrile chain in the copolymer The segment ratio is relatively large, and there are many homopolymerized segments of acrylonitrile; at this time, the obtained material is brittle and difficult to process; in the whole polymer, the proportion of chain segments adjacent to the nitrile group and carboxyl group is small, and it is difficult to become a high-performance foam plastic

Method used

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  • Method for preparing vinyl cyanide/methacrylic acid copolymer
  • Method for preparing vinyl cyanide/methacrylic acid copolymer
  • Method for preparing vinyl cyanide/methacrylic acid copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] In a 5-liter reaction kettle equipped with a reflux condenser, temperature control equipment, and stirring equipment, vacuumize and inject nitrogen, and then vacuumize and inject nitrogen for three consecutive times; add 2.4 liters of acrylonitrile and 1.55 liters of methyl Acrylic acid, 3.6 grams of azobisisobutyronitrile.

[0035] Start stirring, the stirring speed is 30 rpm, the temperature of the reactor is raised to 50°C, and the polymerization reaction is started;

[0036] Half an hour after the polymerization reaction, centrifugal separation, continuous separation or intermittent separation, the separated liquid is refluxed into the reactor;

[0037] During the reaction, the mixture of methacrylic acid and initiator azobisisobutyronitrile, wherein the initiator azobisisobutyronitrile content is 0.9 grams per liter; slowly and continuously injected into the reactor by a metering pump, the injection speed is 1.5 milliliters / liter Minutes, keep the ratio of the two...

Embodiment 2

[0042]In a 5-liter reactor equipped with a reflux condenser, temperature control equipment, and stirring equipment, vacuumize, inject nitrogen, and then vacuumize, inject nitrogen; three times in a row. Add 3 liters of acrylonitrile, 0.97 liters of methacrylic acid, and 100 grams of azobisisobutyronitrile into the kettle. Start stirring at 30 rpm, and the reaction kettle is heated to 30 degrees Celsius.

[0043] Half an hour after the polymerization reaction, centrifugal separation, continuous separation or intermittent separation, the separated liquid is refluxed into the reactor;

[0044] During the reaction, 73.8 milliliters of acrylic acid, acrylonitrile and initiator azobisisobutyronitrile mixture were injected into the reactor every half hour; Content 25 g / L.

[0045] Its following operation steps are identical with embodiment one.

[0046] The solid obtained in the above steps is weighed to obtain 562 grams; during the reaction process, the following three samples ar...

Embodiment 3

[0048] In a 5-liter reactor equipped with a reflux condenser, temperature control equipment, and stirring equipment, vacuumize, inject nitrogen, and then vacuumize, inject nitrogen; three times in a row. Add 2.8 liters of acrylonitrile, 0.6 liters of methacrylic acid, and 1.42 grams of dibenzoyl peroxide into the kettle. Start stirring at 30 rpm, and the reaction kettle is heated to 60 degrees Celsius.

[0049] During the reaction process, at intervals of 30 minutes, use a horizontal scraper centrifugal separation device to separate the copolymer for 30 minutes; the separated liquid is returned to the reactor;

[0050] During the reaction, inject 30 milliliters of the mixture of methacrylic acid and initiator dibenzoyl peroxide into the reactor every 20 minutes; wherein the initiator dibenzoyl peroxide content is 0.6 g / liter; keep two single body proportions.

[0051] Its following operation steps are identical with embodiment one.

[0052] The solid obtained in the above s...

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Abstract

The invention relates to a method for preparing vinyl cyanide / methacrylic acid copolymer. The method comprises the following steps of: under inert gas protection, filling polymerized monomer vinyl cyanide and methacrylic acid into a reaction kettle; heating an initiator at the temperature of between 30 and 60 DEG C to start a polymerization reaction, wherein with the polymerization reaction, the proportion of the polymerized monomer in the polymerized mixture is changed; supplementing polymerized monomer methacrylic acid which is quickly consumed or a mixture of two polymerized monomers into the polymerized mixture, and keeping the proportion of the polymerized monomer in the polymerized mixture, wherein the supplementation speed is slower than or equal to the speed of the polymerization reaction; and filtering and distilling to obtain the vinyl cyanide / methacrylic acid copolymer. The method has the advantage that: the methacrylic acid monomer and vinyl cyanide polymerized monomer which are low in cost and relatively big in reactivity ratio difference are used for synthesizing the copolymer of which the ratio of nitrile group to carboxyl group is constant, the molar ratio is 1 to 1 approximately, and the neighboring chain proportion of the vinyl cyanide and the methacrylic acid is relatively high.

Description

technical field [0001] The invention relates to a preparation method of an acrylonitrile / methacrylic acid copolymer. Background technique [0002] The sandwich sandwich structure is a sandwich structure that uses resin-based composite materials as the skin and foam plastic or honeycomb as the core; this structure has the advantages of light weight, high specific stiffness and high specific strength; currently the sandwich structure is used in military and civilian applications. The products have been widely used, and the main application directions are: wind turbine blades, aircraft, helicopter wings, large ships, radome, etc. The high-performance structural foam plastics that can be used in the sandwich sandwich structure of composite materials include polyvinyl chloride, polyacrylonitrile / styrene, poly(meth)acrylimide (PMI), and the like. [0003] Polyimide (PI) is a super engineering plastic with excellent comprehensive properties (250 degrees high temperature can work f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/46C08F220/06C08F8/48
Inventor 王少辉
Owner 王少辉
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