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Preparation method of 2-tert-butylaminoethyl methacrylate

A technology of tert-butylaminoethyl methacrylate and methyl methacrylate is applied in the field of preparation of tert-butylaminoethyl methacrylate, and can solve the problems of high energy consumption, complicated azeotrope treatment process, and product and Catalyst loss and other problems, to achieve the effect of simple operation, saving resources and less equipment

Inactive Publication Date: 2018-09-25
李守莉
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction solution containing the catalyst is rectified, and the catalyst will remain in the heavy component at the bottom of the tower. The heavy component is usually processed by incineration, which causes the loss of products and catalysts. The azeotrope treatment process is complicated and energy-consuming

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The invention provides a technical scheme: a preparation method of tert-butylaminoethyl methacrylate, comprising the following steps:

[0020] S1: Transesterification, add methyl methacrylate, tert-butylethanolamine, polymerization inhibitor and solid base catalyst into the ten cubic reaction kettle, turn on the stirring device and heating device, and after 30 minutes of total reflux, control the temperature at the top of the tower to stabilize at 50 ℃, the azeotrope of methyl methacrylate and methanol is extracted from part of the reflux liquid until the transesterification reaction is completed, and the TBAEMA mixed solution containing solid alkali catalyst is extracted at the bottom of the tower;

[0021] S2: Centrifugal sedimentation, transfer the TBAEMA mixed solution in step 1 to a tubular high-speed centrifuge for centrifugal sedimentation, control the speed of the centrifuge to 12000r / min, after continuous centrifugation for 10min, collect the solid phase at the ...

Embodiment 2

[0026] The invention provides a technical scheme: a preparation method of tert-butylaminoethyl methacrylate, comprising the following steps:

[0027] S1: Transesterification, add methyl methacrylate, tert-butylethanolamine, polymerization inhibitor and solid base catalyst into the ten cubic reaction kettle, turn on the stirring device and heating device, and after 40 minutes of total reflux, control the temperature at the top of the tower to stabilize at 55 ℃, the azeotrope of methyl methacrylate and methanol is extracted from part of the reflux liquid until the transesterification reaction is completed, and the TBAEMA mixed solution containing solid alkali catalyst is extracted at the bottom of the tower;

[0028] S2: Centrifugal sedimentation, transfer the TBAEMA mixed solution in step 1 to a tubular high-speed centrifuge for centrifugal sedimentation, control the speed of the centrifuge to 15000r / min, continue centrifuging for 20min, collect the solid phase at the bottom and...

Embodiment 3

[0033] The invention provides a technical scheme: a preparation method of tert-butylaminoethyl methacrylate, comprising the following steps:

[0034] S1: Transesterification, add methyl methacrylate, tert-butylethanolamine, polymerization inhibitor and solid base catalyst into the ten cubic reaction kettle, turn on the stirring device and heating device, and after 50 minutes of total reflux, control the temperature at the top of the tower to stabilize at 60 ℃, the azeotrope of methyl methacrylate and methanol is extracted from part of the reflux liquid until the transesterification reaction is completed, and the TBAEMA mixed solution containing solid alkali catalyst is extracted at the bottom of the tower;

[0035] S2: Centrifugal sedimentation, transfer the TBAEMA mixed solution in step 1 to a tubular high-speed centrifuge for centrifugal sedimentation, control the speed of the centrifuge to 15000r / min, after continuous centrifugation for 30min, collect the solid phase at the ...

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PUM

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Abstract

The invention discloses a preparation method of 2-tert-butylaminoethyl methacrylate (TBAEMA). The preparation method comprises the following steps: S1, carrying out ester exchange; S2, centrifuging and depositing; S3, rectifying TBAEMA; S4, recycling methanol. According to the preparation method disclosed by the invention, a solid alkali catalyst is adopted; after reaction is finished, the catalyst is separated by adopting a centrifuging and depositing method and is repeatedly utilized; the yield of a product is improved and the dosage of the catalyst is reduced; the economic benefits are improved, resources are saved and emission is reduced.

Description

technical field [0001] The invention relates to the technical field of chemical production, in particular to a preparation method of tert-butylaminoethyl methacrylate. Background technique [0002] Tert-butylaminoethyl methacrylate (TBAEMA), also known as 2-tert-butylaminoethyl methacrylate, is used as a modifier for polymer materials. It is prepared by the transesterification reaction of cresol methacrylate and tert-butylaminoethanol, and can also be obtained by the direct esterification reaction of methacrylic acid and tert-butylaminoethanol. Lubricating oil additives and pigment colorants, etc. [0003] The preparation of tert-butylaminoethyl methacrylate by the transesterification reaction of methyl methacrylate and tert-butylethanolamine (R-OH) usually uses liquid catalysts such as organotin and titanate, and is gradually extracted from the top of the tower during the reaction process. The azeotrope of methanol and methyl methacrylate, after the reaction is completed,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/06C07C213/10C07C219/08
CPCC07C213/06C07C213/10C07C219/08
Inventor 李守莉
Owner 李守莉