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Production method of high-yield transbutylene-2-acid

A high-yield, butene-based technology, applied in chemical instruments and methods, chemical recovery, carboxylate preparation, etc., can solve the problems of unrelated product cis-trans ratio, low yield of butene-2-acid, etc., to achieve Good fluidity, high catalytic activity and selectivity, good wear resistance

Active Publication Date: 2022-04-12
北京弗莱明科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The yields of butene-2-acid in the above-mentioned patents are all low, and none of the above-mentioned patents involves the cis-trans ratio of the product

Method used

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preparation example Construction

[0032] In the present invention, the preparation method of the supported silver catalyst preferably comprises the following steps:

[0033] impregnating the carrier in a soluble silver salt solution after first roasting to obtain an impregnated product;

[0034] The obtained impregnated product is sequentially dried and secondly calcined to obtain a supported silver catalyst.

[0035] In the present invention, the temperature of the first calcination is preferably 400-900°C, more preferably 500-800°C, and the time of the first calcination is preferably 1-6 h, more preferably 2-5 h; The invention pre-treats the carrier through the first calcination to decompose it into oxides to form the desired structure, and remove the moisture in the carrier, which is conducive to making the active components more uniformly attached to the surface of the carrier. The catalyst is easy to Lost with the solution; after the first roasting is completed, the present invention preferably cools the...

Embodiment 1

[0045] The catalyst used is Ag / TiO 2 Catalyst, the preparation method is co-precipitation method, the specific steps are as follows: 200 gTiO 2 (Anatase type, the specific surface area is about 80 m 2 / g) was roasted at 700 °C for 5 h, after cooling, mixed with 95.7 mL of silver nitrate solution with a concentration of 0.11 g / L, impregnated for 2 h, dried in an oven at 115 °C for 2 h, and then roasted at 450 °C for 4 h , to prepare Ag / TiO with a silver loading of 5% 2 Supported silver catalyst, the particle size is about 150 μm.

[0046] 70 g butene-2-aldehyde, 140 g ethyl acetate, 1.726 g Ag / TiO 2 The catalyst was added into the autoclave, and reacted with oxygen at room temperature (25 °C), the reaction pressure was 1 MPa, and after 7.8 hours of reaction, the conversion rate of butene-2-aldehyde was 95.73%, and the selectivity of butene-2-acid was 89.09%, the yield was 85.28%, the ratio of trans-butene-2-acid and cis-butene-2-acid in the product was 97:3, and the particl...

Embodiment 2

[0048] The catalyst that present embodiment adopts is Ag / TiO 2 Catalyst, the preparation method is the co-precipitation method, the specific steps are as follows: 200 g TiO 2 (Anatase type, the specific surface area is about 80 m 2 / g) was roasted at 700 °C for 5 h, after cooling, mixed with 95.7 mL of silver nitrate solution with a concentration of 0.11 g / L, impregnated for 2 h, dried in an oven at 115 °C for 2 h, and then roasted at 450 °C for 4 h , to prepare Ag / TiO with a loading of 5% 2 supported silver catalyst.

[0049] 70 g butene-2-aldehyde, 140 g ethyl acetate, 1.726 g Ag / TiO 2 The catalyst was added into the autoclave and reacted with oxygen at 40 °C. The reaction pressure was 1 MPa. After 7 h, the conversion rate of butene-2-aldehyde was 96.53%, the selectivity of butene-2-acid was 92.21%, and the yield is 89.01%, and the ratio of trans-butene-2-acid and cis-butene-2-acid in the product is 97:3.

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Abstract

The invention relates to the technical field of butenoic acid preparation, and provides a production method of high-yield transbutylene-2-acid. The method comprises the following steps: mixing butene-2-aldehyde, a solvent and a silver-loaded catalyst under an oxygen condition, and carrying out a catalytic oxidation reaction to obtain transbutene-2-acid; the solvent is an acetate solvent, and the carrier of the supported silver catalyst is ZrO2 and / or TiO2. The silver-loaded catalyst adopted by the invention has relatively high catalytic activity and selectivity, can be used for efficiently and continuously preparing the transbutene-2-acid, and is high in product yield, high in proportion of the transbutene-2-acid in the product, stable in activity and long in service life; the solvent adopted by the invention is low in toxicity and meets the green chemical requirements. Results of the embodiment show that when the transbutene-2-acid is prepared by adopting the method disclosed by the invention, the conversion rate of the butene-2-aldehyde is more than 95%, the selectivity of the butene-2-acid is more than 89%, and the proportion of the transbutene-2-acid in the product is more than 96%.

Description

technical field [0001] The invention relates to the technical field of crotonic acid preparation, in particular to a production method of high-yield trans-butene-2-acid. Background technique [0002] Butene-2-acid (structural formula is as follows) is an unsaturated fatty acid with cis and trans isomers. The molecule contains double bonds and carboxyl groups. It has strong reactivity and is widely used in industry. Uses: Mainly used to prepare various resins, fungicides, surface coatings, plasticizers, and also an important pharmaceutical intermediate and pesticide intermediate. [0003] [0004] At present, butene-2-acid is usually obtained by oxidation of butene-2-aldehyde, the basic principle is as follows: [0005] [0006] Since butene-2-aldehyde contains unsaturated double bonds, it is necessary to select catalysts and oxidation process conditions that can oxidize aldehyde groups without destroying double bonds. In existing reports, the oxidation of butene-2-al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/235C07C57/03B01J23/50
CPCY02P20/584
Inventor 刘伟王素素马龙龙高乐杜松松黄龙王海星陈建华崔长建和壮壮
Owner 北京弗莱明科技有限公司
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