Continuous benzoxazine preparation device and method

A benzoxazine and microwave heating device technology, applied in the field of polymer chemistry, can solve the problems of limited production capacity, labor consumption, low production efficiency, etc., and achieves short reaction time, improved reaction speed, and improved productivity and production speed. Effect

Pending Publication Date: 2018-08-17
成都科宜高分子科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, benzoxazine is prepared by a batch method, which is characterized in that the raw materials required for the reaction are loaded into the reactor once, and then reacted in it, and after a certain period of time, the required reaction level is reached and then unloaded. All reaction materials, including mainly reaction products and a small amount of unconverted raw materials, belong to batch batch production method, which is complicated to operate, consumes a lot of labor, has low production efficiency and limited production capacity

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  • Continuous benzoxazine preparation device and method

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Effect test

Embodiment 1

[0034] like figure 1As shown, the device for the continuous preparation of benzoxazine of the present invention has a structural composition comprising: at least two material mixing tanks 1, a microwave heating device 2, a tubular reactor 3, a ceramic membrane separator 4, and an oil-water separator 5 , waste water tank 6, controller 7 and scraper type thin film evaporator 12. Wherein, the liquid level gauge 8 and the buzzer 9 are set on the material mixing tank 1, the controller 7 is connected with the liquid level gauge 8 and the buzzer 9 respectively, and the controller controls the buzzer based on the liquid level information detected by the liquid level gauge. buzzer on or off. Each material mixing tank is provided with an agitator 13 . Each material mixing tank is connected to the feed port of the tubular reactor, and an infusion pump 10 and a flow meter 11 are provided on the connecting pipeline between each material reaction tank and the tubular reactor. The tubular...

Embodiment 2

[0038] The method for preparing benzoxazine by adopting the above-mentioned device for continuously preparing benzoxazine comprises the following steps:

[0039] Step S1, preparation of raw materials: add toluene as a solvent to two material mixing tanks (material mixing tank A and material mixing tank B); then add phenol, formaldehyde and aniline in sequence; the amount of toluene in the material mixing tank accounts for The total mass of all reaction materials is 30%, the mass ratio of phenol, formaldehyde and aniline is 94:60:93, the stirring is started, the raw materials are fully mixed and dissolved in toluene solvent.

[0040] Step S2, turn on the microwave heating device, control the temperature in the heating chamber at 70°C, adjust the flow rate of the material mixing tank A obtained in step S1, and then continuously inject the mixed reaction liquid into the tubular reactor through the infusion pump A; because in this At high temperature, phenol, aldehyde, and amine w...

Embodiment 3

[0047] The method for preparing benzoxazine by means of a device for continuously preparing benzoxazine comprises the steps of:

[0048] Step S1, prepare raw materials: add toluene respectively in two material mixing tanks (material mixing tank A and material mixing tank B) as a solvent; then add bisphenol A, paraformaldehyde and aniline in sequence; the toluene in the material mixing tank The dosage accounts for 30% of the total mass of all reaction materials in the tank, the mass ratio of bisphenol A, paraformaldehyde, and aniline is 228:120:186, start stirring, fully mix the raw materials and dissolve them in toluene solvent.

[0049] Step S2, turn on the microwave heating device, control the temperature in the heating chamber at 75°C, adjust the flow rate of the material mixing tank A obtained in step S1, and then continuously inject the mixed reaction liquid into the tubular reactor through the infusion pump A; because in this At high temperature, phenol, aldehyde, and am...

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Abstract

The invention discloses a continuous benzoxazine preparation device and method. The device comprises at least two material mixing tanks, a microwave heating device, a tubular reactor, a ceramic membrane separator, an oil-water separator, a scraper film evaporator, a wastewater tank and a controller. Each material mixing tank is provided with a liquid level meter and a buzzer. The method includes:starting microwave heating, pumping mixed reaction liquid in one of the material mixing tank into the tubular reactor, stopping an infusion pump in operation when the liquid level in the tank reachesa lowest value and the corresponding buzzer alarms, and starting the other infusion pump to continue delivering the mixed reaction liquid into the tubular reactor to enable the reaction liquid to continuously enter the tubular reactor; pumping a material after reaction into the ceramic membrane separator, separating to obtain a primary benzoxazine product, pumping into the scraper film evaporator,and purifying to obtain benzoxazine. By continuous reaction, the method has advantages of short reaction time, high yield, high production speed, narrowness in benzoxazine molecular weight distribution and high purity.

Description

technical field [0001] The invention belongs to the field of polymer chemistry, and in particular relates to a device and method for continuously preparing benzoxazine. Background technique [0002] The benzo six-membered heterocyclic compound--benzoxazine monomer synthesized by Mannich reaction using phenolic compounds, primary amine compounds and aldehydes as raw materials, can undergo ring-opening polymerization under the action of heating and / or catalysts to form Spatial network structure. Benzoxazine does not release small molecules during molding and curing, and the product has low porosity and close to zero shrinkage. It has excellent high temperature resistance, and the glass transition temperature (Tg) is above 150°C; after benzoxazine ring-opening polymerization, it has good electrical insulation properties; benzoxazine can be solidified and formed under appropriate temperature conditions, and has Good mechanical properties. [0003] Benzoxazine is widely used i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D265/36C07D265/16
CPCC07D265/36C07D265/16
Inventor 张锋高英菊王翔宇
Owner 成都科宜高分子科技有限公司
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