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Method used for catalyzed synthesis of tert-butyl acrylate

A technology for tert-butyl acrylate and acrylic acid, which is applied in the field of catalytic synthesis of tert-butyl acrylate, can solve the problems of increasing the preparation cost of tert-butyl acrylate, decreasing the catalytic performance of the catalyst, poor reuse of the catalyst, etc., and achieves excellent low-temperature reaction activity and selection. The effect of high stability, high utilization rate of raw materials, and excellent reusability

Inactive Publication Date: 2015-08-19
徐德良 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But adopt this method to prepare tert-butyl acrylate, its catalyst reuse aspect performance is relatively poor, after 3 times of repeated use, the catalytic performance of its catalyst obviously descends, and esterification rate drops to about 90% from initial 98%, thereby improves The preparation cost of tert-butyl acrylate

Method used

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  • Method used for catalyzed synthesis of tert-butyl acrylate
  • Method used for catalyzed synthesis of tert-butyl acrylate
  • Method used for catalyzed synthesis of tert-butyl acrylate

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preparation example Construction

[0029] Following examples or comparative examples relate to nanometer solid superacid SO 4 2－ / SnO 2 The preparation method comprises the steps:

[0030] (1) Nano-SnO 2 Preparation: under vigorous stirring, 0.15mol / L of SnCl 4 The solution is added dropwise to 2.5% ammonia water containing a dispersant polyethylene glycol, and the pH of the solution is kept at about 9. After the dropwise addition, Sn(OH) was obtained 4 sol, aged in a water bath at 70°C for 10 h to obtain SnO 2 gel. Wash thoroughly with distilled water until Cl-free - , vacuum filtration. The resulting filter cake was replaced with n-butanol for moisture. Disperse the filter cake in 10 times of n-butanol, stir and mix it and carry out azeotropic distillation. When the temperature reaches the water-n-butanol azeotropic temperature of 92.4°C, the water molecules in the colloid will be removed in the form of azeotrope , as the distillation proceeds, the temperature of the system gradually increases until...

Embodiment 1

[0033] A kind of preparation technology that catalyzes the synthesis of tert-butyl acrylate with strong acidic cation exchange resin combination product as catalyst, carries out successively according to the following steps:

[0034] 1) acrylic acid, made of nano-solid superacid SO 4 2－ / SnO 2 , strong acidic cation exchange resin A, strong acidic cation exchange resin B and strong acidic cation exchange resin C catalyst composition, polymerization inhibitor A, polymerization inhibitor B are added in the airtight reaction kettle, and the isobutylene of liquefaction is added dropwise to carry out Esterification reaction;

[0035] 2) After the dropwise addition is completed, keep warm;

[0036] 3) After the heat preservation is completed, the closed reaction kettle is depressurized, filtered, and the liquid components are extracted into the rectification tower;

[0037] 4) sequentially separate by-product tert-butyl alcohol, diisobutylene and target product tert-butyl acryla...

Embodiment 2

[0044] A kind of preparation technology that catalyzes the synthesis of tert-butyl acrylate with strong acidic cation exchange resin combination product as catalyst, carries out successively according to the following steps:

[0045] 1) acrylic acid, made of nano-solid superacid SO 4 2－ / SnO 2 , strong acidic cation exchange resin A, strong acidic cation exchange resin B and strong acidic cation exchange resin C catalyst composition, polymerization inhibitor A, polymerization inhibitor B are added in the airtight reaction kettle, and the isobutylene of liquefaction is added dropwise to carry out Esterification reaction;

[0046] 2) After the dropwise addition is completed, keep warm;

[0047] 3) After the heat preservation is completed, the closed reaction kettle is depressurized, filtered, and the liquid components are extracted into the rectification tower;

[0048] 4) sequentially separate by-product tert-butyl alcohol, diisobutylene and target product tert-butyl acryla...

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Abstract

The invention relates to a method used for catalyzed synthesis of tert-butyl acrylate. The method comprises following steps successively:1) acrylic acid, a catalyst combination, a polymerization inhibitor A, and a polymerization inhibitor B are delivered into a sealed reaction kettle, and liquefied isobutylene is added dropwise for esterification, wherein the catalyst combination is composed of nanosolid superacid SO<4><2-> / SnO<2>, Amberlyst-15, D001 resin, and NKC-9 resin; 2) after adding, heat preservation is carried out; 3) after heat preservation, the sealed reaction kettle is subjected to pressure relief, an obtained mixture is subjected to filtration, and an obtain liquid ingredient is pumped into a rectifying tower; and 4) by-products tert-butyl alcohol, diisobutylene, and the target product tert-butyl acrylate are obtained via separation successively. Yield of tert-butyl acrylate is higher than 98%; reuse ratio of the catalyst is high; the method is simple; and no pollution is caused.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a process for catalytically synthesizing tert-butyl acrylate. Background technique [0002] Tert-butyl acrylate, its structural formula is Tert-butyl acrylate is an extremely important chemical basic raw material and intermediate. Because of its unique and highly active polar molecule, unsaturated double bond and carboxylate (-COOR) structure, it can be derived into many kinds It has a polymer formula with good performance, and can prepare plastic, cross-linked and other polymers through emulsion polymerization, solution polymerization, copolymerization and other processing methods. Its strong polymer cohesion, good transparency, and clear film formation make it have great potential in the modification of various chemicals. It is used in coatings, coatings, papermaking, non-woven fabrics, super absorbent materials, Detergents, synthetic fibers, synthetic ...

Claims

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Application Information

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IPC IPC(8): C07C69/54C07C67/04
CPCC07C67/04C07C69/54
Inventor 徐德良丁峰
Owner 徐德良
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