A kind of technique of catalytically synthesizing tert-butyl acrylate

A technology of tert-butyl acrylate and acrylic acid, which is applied in the field of catalytic synthesis of tert-butyl acrylate, can solve the problems of catalyst performance decline, increase the cost of tert-butyl acrylate preparation, poor catalyst reuse, etc., and achieve high raw material utilization and excellent quality Low-temperature reactivity, selectivity, and excellent reusability

CN104844455BInactive Publication Date: 2016-06-22徐德良 +1
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2016-06-22
Estimated Expiration
Not applicable · inactive patent

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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.
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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 ...

Examples

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 the condition of 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 graduall...

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...