Preparation method of methacrylate products

A technology of methyl methacrylate and methacrylic acid, applied in the field of preparation of methacrylate products, can solve the problems of high power consumption, no mention of the recovery of azeotrope methyl methacrylate, etc. Investment, easy automation control, high product quality effect

Active Publication Date: 2013-01-02
苏州和创化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The above-mentioned foreign patents that adopt the transesterification process all adopt the batch reaction rectification process, focusing on the research of catalyst and polymerization inhibitor. In the patent, there is no mention of the recovery of methyl methacrylate in the azeotrope, and the

Method used

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  • Preparation method of methacrylate products
  • Preparation method of methacrylate products
  • Preparation method of methacrylate products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] The reactor is two tank reactors in series, each volume is 5 liters, and the rectification tower is Φ50×2.5 and the height is 800mm. Light removal tower Φ50×2.5, height 1000mm. Weight-removing tower Φ50×2.5, height 800mm.

[0039] The raw materials are methyl methacrylate and allyl alcohol.

[0040] The catalyst is dibutyltin dilaurate.

[0041] The polymerization inhibitor is 2,2,6,6-tetramethyl-4-hydroxypiperidine-1-oxynitride free radical.

[0042] The entrainer is n-pentane.

[0043] Methyl methacrylate, allyl alcohol and the reused polymerization inhibitor and catalyst are mixed continuously with a metering pump and enter reactor A, wherein the flow of methyl methacrylate is 600g / h, and the flow of allyl alcohol is 260g / h , Catalyst and polymerization inhibitor flow rate 90g / h (catalyst concentration is 50%, polymerization inhibitor concentration 2%). Reactor A is heated up, and the azeotrope of methyl methacrylate and methanol generated enters the azeotropic ...

Embodiment 2

[0047] The reactor is two tank reactors in series, each volume is 5 liters, and the rectification tower is Φ50×2.5 and the height is 800mm. Light removal tower Φ50×2.5, height 1000mm. Weight-removing tower Φ50×2.5, height 800mm.

[0048] The raw materials are methyl methacrylate and allyl alcohol.

[0049] The catalyst is dibutyl tin dilaurate and allyl titanate, and the ratio of the two is 4:1.

[0050] The polymerization inhibitor is tetramethylpiperidine nitroxide free radical phosphite triester and hydroquinone, and the ratio of the two is 2:1.

[0051] The entrainer is n-hexane.

[0052] Methyl methacrylate, allyl alcohol and the reused polymerization inhibitor and catalyst are mixed continuously with a metering pump and enter reactor A, wherein the flow of methyl methacrylate is 600g / h, and the flow of allyl alcohol is 260g / h , Catalyst and polymerization inhibitor flow rate 90g / h (catalyst concentration is 50%, polymerization inhibitor concentration 2%). Reactor A ...

Embodiment 3

[0056] The reactor is two tank reactors connected in series, each volume is 6000 liters, and the rectification tower is Φ500×5 and the height is 8000mm. Light removal tower Φ500×5mm, height 10000mm. Weight-removing tower Φ500×5mm, height 8000mm.

[0057] The raw materials are methyl methacrylate and allyl alcohol.

[0058] The ratio of the catalyst dibutyltin oxide to allyl titanate is 4:1.

[0059] The polymerization inhibitor is copper dibutyldithiocarbamate and hydroquinone, and the ratio of the two is 2:1.

[0060] The entrainer is cyclohexane.

[0061] Use a metering pump to continuously mix methyl methacrylate, allyl alcohol and recycled inhibitors and catalysts into reactor A, wherein the flow of methyl methacrylate is 700kg / h, and the flow of allyl alcohol is 320kg / h , Catalyst and polymerization inhibitor flow rate 90g / h (catalyst concentration is 50%, polymerization inhibitor concentration 2%). The material in reactor A is heated up, and the generated azeotrope ...

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Abstract

The invention discloses a preparation method of methacrylate products, which comprises the following steps: adopting a reaction device comprising at least two reaction kettles connected in series, taking methyl methacrylate and alcohol as raw materials, using a catalyst and a polymerization inhibitor for assistance, placing the methyl methacrylate, the alcohol, the catalyst and the polymerization inhibitor into the reaction kettles, heating and reacting to generate the methacrylate products and methanol; then separating and purifying to obtain the products. The preparation method provided by the invention adopts a coupling process of reactive rectification and azeotropic rectification to couple the reactive rectification of the methyl methacrylate and the alcohol with the azeotropic rectification of the methyl methacrylate in an azeotrope formed in recycling of the methyl methacrylate and the alcohol so as to reduce the device investment, decrease the energy consumption and increase the yield rate. By adopting the technology provided by the invention, the proportion of the materials is decreased, the efficiency of the reactor is improved, the technological process is simplified, the reaction condition is mild, the operation is simple, the conversion rate is high, and the product quality is high and stable.

Description

technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of methacrylate products. Background technique [0002] Methacrylates are widely used in coating resins, ink resins, adhesives, PMMA sheets, oil additives, paper, leather, water treatment and textile finishing agents and other industries. [0003] Introduced the preparation technology of methacrylic acid ester in the U.S. Patent 5072027, this patent adopts methyl methacrylate and alcohol to carry out transesterification reaction under the effect of catalyst and polymerization inhibitor, and catalyzer needs to be filtered, and filtration time can be controlled by the catalyzer The water content is shortened, and the catalyst of the transesterification reaction is lithium hydroxide after heating and drying. [0004] US Patent No. 5183930 introduces a catalyst for the transesterification process. The catalyst is a transition metal element, and the ca...

Claims

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Application Information

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IPC IPC(8): C07B41/12C07C67/03C07C67/54C07C69/54C07C213/06C07C219/08
CPCY02P20/10
Inventor 安丰发李虹
Owner 苏州和创化学有限公司
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