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Preparation method of diethylaminoethyl methacrylate

A technology of diethylaminoethyl methacrylate and methyl methacrylate, which is applied in the field of preparation of diethylaminoethyl methacrylate, can solve problems such as polymerization, and reduce polymer content and production volume , the effect of reducing the dosage

Inactive Publication Date: 2012-03-21
里光
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the above-mentioned inhibitors are used, there are different degrees of polymerization phenomena.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Example 1: Add 923kg of methyl methacrylate and 600kg of diethylaminoethanol to reactor 1, add 22.8kg of lead tetroxide as a catalyst, and add 1.5kg of composite inhibitor (from tetramethylpiperidine nitrogen oxide Free radical phosphite triester and hydroquinone are mixed in a weight ratio of 2:1).

[0017] Turn on the stirring, heat up, and when the temperature in the reactor rises to 100-110°C, the top of the tower begins to discharge and reflux. When the temperature at the top of the tower stabilizes at 62-64°C, turn on the reflux system at the top of the tower, the reflux ratio is 6:1 -8:1, adjust the reflux ratio to stabilize the temperature at the top of the tower at 62-70°C. When the temperature of the kettle rises to between 120-140°C and the temperature at the top of the tower rises significantly, stop heating, cool down, and sample for analysis.

[0018] The product in the kettle obtained a total of 1287kg of diethylaminoethyl methacrylate:

[0019] Composition (de...

Embodiment 2

[0025] Example 2: Add 1128kg of methyl methacrylate and 600kg of diethylaminoethanol to the reactor 1, and add 12.1kg of catalyst (mixed with lead oxide and calcium titanate in a weight ratio of 3:1, add 1.7kg Compound polymerization inhibitor (made by mixing copper dibutyl dithiocarbamate and hydroquinone in a weight ratio of 2:1).

[0026] Turn on the stirring, heat up, and when the temperature in the reactor rises to 100-110°C, the top of the tower begins to discharge and reflux. When the temperature at the top of the tower stabilizes at 62-64°C, turn on the reflux system at the top of the tower, the reflux ratio is 6:1 -8:1, adjust the reflux ratio to stabilize the temperature at the top of the tower at 62-70°C. When the temperature of the kettle rises to between 120-140°C and the temperature at the top of the tower rises significantly, stop heating, cool down, and sample for analysis.

[0027] A total of 1468kg of diethylaminoethyl methacrylate was obtained from the product in...

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PUM

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Abstract

The invention discloses a preparation method of diethylaminoethyl methacrylate, which comprises the following steps that: methyl methacrylate and 2-ethyl aminoethanol are used as raw materials and are reacted in the presence of a catalyst and a polymerization inhibitor by adopting a reactive distillation ester exchange process, and methanol generated by the reaction is timely removed by azeotropic distillation; the obtained reaction product containing diethylaminoethyl methacrylate is distilled under reduced pressure conditions; after excess methyl methacrylate is removed, the catalyst and the polymerization inhibitor are removed to obtain a diethylaminoethyl methacrylate product; and the catalyst is one of lead oxides and / or one of metal titanates, and the polymerization inhibitor is a compound polymerization inhibitor. The preparation method has the advantages of good catalytic effect, short reaction time, high reaction efficiency, good polymerization inhibition, high efficiency of a reaction kettle, high product quality and yield and the like.

Description

1. Technical Field [0001] The invention belongs to the technical field of chemical synthesis, and specifically relates to a preparation method of diethylaminoethyl methacrylate. 2. Background technology [0002] Due to its reactive amino groups and polymerizable vinyl groups, diethylaminoethyl methacrylate can increase adhesion, thermosetting, crosslinking and coloring properties of dyes and pigments. It is widely used in the preparation of thermosetting coatings and antistatic agents. , Dyeing auxiliaries, lubricant additives, adhesives, leather processing agents, combustion aids, etc. [0003] At present, there are three main methods for preparing diethylaminoethanol methacrylate. One is acylation. He Lingzhi et al. introduced one in "Fine Chemical Intermediates" (2009, vol.39, No.6). Take methacrylic acid and oxalyl chloride as raw materials, first synthesize methacrylic acid chloride by oxalyl chloride method, then use diethylaminoethanol and methacrylic acid chloride as raw m...

Claims

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Application Information

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IPC IPC(8): C07C219/08C07C213/06
CPCY02P20/10
Inventor 里光
Owner 里光
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