Preparation method for methoxyethyl methacrylate

A technology of methoxyethyl methacrylate and methyl methacrylate, which is applied in the field of preparation of methoxyethyl methacrylate, and can solve problems such as increased reaction by-products, impact on product quality, loss of polymerization inhibition, etc. , to achieve the effect of improving product quality and yield, not affecting product color, and reducing polymer content

Inactive Publication Date: 2012-02-15
里光
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when these inhibitors are specifically applied to the transesterification reaction of MMA and methoxyethanol to prepare methoxyethyl methacrylate, they have their own shortcomings.
Such as hydroquinone, the dosage is large, the cost is high, and the polymerization inhibition effect must be shown when there is oxygen dissolved in the monomer, and it will be entrained in the product during distillation, which will affect the quality of the product; hydroquinone monomethyl Ether has a good polymerization inhibition effect only on free radicals with strong electron donation, and will lose its polymerization inhibition effect under high temperature conditions; phenothiazine is easy to oxidize and change color, so it is easy to be oxidized during production, resulting in a change in product color ; Piperidinol nitroxide free radical or piperidinol nitroxide free radical phosphite, the polymerization inhibition effect is better, but the price is high, and sometimes used alone, the reaction by-products will increase; copper salt inhibitors are not easy to dissolve , easy to crystallize, often block the pipeline, and have a certain degree of corrosion to the equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Add 1184kg methyl methacrylate and 450kg methoxyethanol to the reactor, add 44kg catalyst (mixed by sodium cyanate and magnesium hydroxide at a weight ratio of 2:1), add 4.4kg Polymerizing agent (mixed from tetramethylpiperidine nitroxide free radical phosphite triester and hydroquinone in a weight ratio of 2:1).

[0025] Start stirring, heat up, and when the temperature in the reactor rises to 90-100°C, the top of the tower starts to discharge, full reflux, and when the temperature at the top of the tower is stable at 62-64°C, start the top reflux ratio system, and the reflux ratio is 6: 1-6:2. By adjusting the reflux ratio, the temperature at the top of the tower is stabilized at 63-70°C. When the temperature of the kettle rises to 115-125°C and the temperature at the top of the tower rises significantly, stop heating, cool down, and take samples for analysis.

[0026] The total product in the kettle is 1288kg, the composition (determined by gas chromatogra...

Embodiment 2

[0032]Example 2: Add 1316kg methyl methacrylate and 400kg methoxyethanol to the reactor, add 86kg catalyst (mixed by sodium cyanate and barium oxide at a weight ratio of 5:1), add 8.6kg polymerization inhibitor Agent (by dibutyl dithiocarbamate copper and hydroquinone mixed in a weight ratio of 2:1).

[0033] Start stirring, heat up, and when the temperature in the reactor rises to 90-100°C, the top of the tower starts to discharge, full reflux, and when the temperature at the top of the tower is stable at 62-64°C, start the top reflux ratio system, and the reflux ratio is 6: 1-6:2. By adjusting the reflux ratio, the temperature at the top of the tower is stabilized at 63-70°C. When the temperature of the kettle rises to 115-125°C and the temperature at the top of the tower rises significantly, stop heating, cool down, and take samples for analysis.

[0034] The total product in the kettle is 1348kg, the composition (determined by gas chromatography):

[0035] Methanol 0.10% ...

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PUM

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Abstract

The invention discloses a preparation method for methoxyethyl methacrylate. The method comprises the following steps of: reacting methyl methacrylate and methoxy ethanol serving as raw materials by using a reactive rectification transesterification process in the presence of a catalyst and a polymerization inhibitor; performing azeotropic distillation to timely remove methanol produced by reaction; distilling an obtained reaction product containing methoxyethyl methacrylate under a reduced pressure condition; and removing excessive methyl methacrylate and then removing the catalyst and the polymerization inhibitor to obtain a methoxyethyl methacrylate product, wherein the catalyst is a composite catalyst, and the polymerization inhibitor is a composite polymerization inhibitor. The preparation method has the advantages of good catalysis effect, short reaction time, high reaction efficiency, good polymerization inhibition effect, high reaction kettle efficiency, high product quality and yield and the like.

Description

1. Technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of methoxyethyl methacrylate. 2. Background technology [0002] Methoxyethyl methacrylate is an important two-component acrylate adhesive and thermosetting acrylic resin, as well as a solution-polymerized or suspension-polymerized monomer and comonomer. Mainly used in marine coatings, biomaterials and paper industry. The preparation methods of methoxyethyl methacrylate in the prior art mainly include esterification and transesterification. [0003] TQ225.241 introduces a method to prepare solid superacid SO by precipitation-impregnation method 4 2- / TiO 2 As a catalyst, a method for synthesizing methoxyethyl methacrylate. The method adopts an esterification process route, and the activity of the catalyst decreases significantly after being recycled twice. [0004] TQ433.436 introduces a method of synthesizing methoxyethyl acryl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/03
CPCY02P20/10
Inventor 里光
Owner 里光
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