Preparation of allyl methacrylate

A technology of allyl methacrylate and methyl methacrylate, applied in the field of preparation of allyl methacrylate, can solve the problem of unsatisfactory allyl methacrylate, high price of polymerization inhibitor, inability to recycle, etc. problems, to achieve the effect of shortening the reaction time, high activity and better use effect

Inactive Publication Date: 2009-07-22
上海和创化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Most of the above-mentioned foreign patents using the transesterification process are aimed at some methacrylate products. Due to the high activity of allyl methacrylate, most catalytic systems are not ideal for the synthesis of allyl methacrylate. Mo

Method used

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  • Preparation of allyl methacrylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Add 1380g methyl methacrylate and 348g allyl alcohol in the reaction kettle, add 50g dibutyltin oxide as a catalyst, add 5g tetramethylpiperidinyl nitroxide free radical phosphite triester as a polymerization inhibitor.

[0037] Start stirring, heat up, and when the temperature inside the reactor 1 rises to 92-95°C, the top of the first-stage rectification tower 2 starts to discharge and fully reflux, and when the temperature at the top of the tower is stable at 62-64°C, start the top reflux ratio system , the reflux ratio is 6:1~6:2, by adjusting the reflux ratio, the temperature at the top of the tower is controlled at 62~64°C. When the temperature of the reactor reaches 109~115°C, stop heating and cool down.

[0038] Move the reaction solution to the separation tank 4, and carry out vacuum distillation and separation through the secondary rectification tower 5, and remove excess methyl methacrylate under the condition of 10-15kPa, and then remove the excess methyl meth...

Embodiment 2

[0040] 1500g of methyl methacrylate and 580g of allyl alcohol were added into the reactor 1, 43g of dibutyl tin laurate was added as a catalyst, and 4g of tetramethylpiperidinyl nitroxide radical phosphite was added as a polymerization inhibitor.

[0041] Start stirring, heat up, and when the temperature in the reactor 1 rises to 92-95°C, the top of the first-stage rectification tower 2 starts to discharge and fully reflux. When the top of the tower is stable at 62-64°C, the top reflux ratio system is opened. The reflux ratio is 6:1~6:2. By adjusting the reflux ratio, the temperature at the top of the tower is controlled at 62~64°C. When the temperature of the reactor reaches 109~115°C, stop heating and cool down.

[0042] Move the reaction solution to the separation tank 4, and carry out vacuum distillation and separation through the secondary rectification tower 5, and remove excess methyl methacrylate under the condition of 10-15kPa, and then remove the excess methyl methacr...

Embodiment 3

[0044] Add 2500g methyl methacrylate and 580g allyl alcohol to reactor 1, add a mixture of 120g dibutyltin oxide and tetrabutyl titanate (the ratio of the two is 3:1) as a catalyst, add 12g dibutyltin oxide A mixture of copper dithiocarbamate and hydroquinone (the ratio of the two is 2:1) is used as a polymerization inhibitor.

[0045] Start stirring, heat up, and when the temperature inside the reactor 1 rises to 92-95°C, the top of the first-stage rectification tower 2 starts to discharge and fully reflux, and when the temperature at the top of the tower is stable at 62-64°C, start the top reflux ratio system , the reflux ratio is 6:1~6:2, by adjusting the reflux ratio, the temperature at the top of the tower is controlled at 62~64°C. When the temperature of the reactor reaches 109~115°C, stop heating and cool down.

[0046] Move the reaction solution to the separation tank 4, and carry out vacuum distillation and separation through the secondary rectification tower 5, and r...

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PUM

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Abstract

The invention relates to a preparation method of allyl methacrylate. Methyl methacrylate and allyl alcohol are taken as raw materials; in the presence of a catalyst and a polymerization inhibitor, the reactive distillation transesterification technology is adopted for reaction, thus obtaining a reaction product containing allyl methacrylate; the reaction product is distilled under the condition of pressure reduction; after extra methyl methacrylate is removed, the catalyst and the polymerization inhibitor are removed so as to obtain the allyl methacrylate. The preparation method adopts a novel recyclable catalytic system, thereby reducing the cost of the catalyst; the novel combined polymerization inhibitor is adopted, thereby lowering the cost of the polymerization inhibitor; and the reactive distillation technology is adopted and the produced methanol is removed in time, thereby quickening the reaction pace to produce the product and improving the efficiency of a reactor.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of allyl methacrylate. Background technique [0002] Allyl methacrylate is an important cross-linking agent that can provide effective bifunctional cross-linking in the second stage, polymers modified with allyl methacrylate have good chemical resistance, impact strength, Hardness and low shrinkage, widely used in dental materials, industrial paints, silicone intermediates, elastomers and some vinyl and acrylic polymer systems. [0003] The preparation methods of allyl methacrylate in the prior art mainly include esterification and transesterification. [0004] CN1410412 discloses a kind of synthetic method of allyl methacrylate, the method adopts the process route of esterification method, with methacrylic acid and allyl alcohol as raw materials, with p-toluenesulfonic acid as catalyst, in the polymerization inhibitor terephthalate Allyl methacr...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/03B01J31/12
CPCY02P20/10
Inventor 安丰发
Owner 上海和创化学股份有限公司
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