Solid acid catalyst and preparation method thereof, and preparation method of diolefin compound

A solid acid catalyst and catalyst technology, applied in the direction of catalyst carrier, chemical instrument and method, physical/chemical process catalyst, etc., can solve the problems of difficult industrial production and low selectivity of isoprene, and achieve low toxicity and high yield Effects of selectivity and productivity improvement

Active Publication Date: 2014-04-16
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The research results show that the regeneration performance of the boron, phosphorus, vanadium, aluminum and potassium five-component catalyst is improved compared with the boron and phosphorus two-component catalyst, but t

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  • Solid acid catalyst and preparation method thereof, and preparation method of diolefin compound
  • Solid acid catalyst and preparation method thereof, and preparation method of diolefin compound
  • Solid acid catalyst and preparation method thereof, and preparation method of diolefin compound

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Example Embodiment

[0038] The present invention provides a method for preparing a solid acid catalyst, which includes the following steps:

[0039] a) After mixing the auxiliary raw material and the carrier in the first solvent, perform the first loading, and then perform drying and first calcination to obtain the catalyst precursor;

[0040] b) The catalyst precursor and the metal compound obtained in step a) are subjected to a second loading in a second solvent to obtain a catalyst intermediate;

[0041] c) subjecting the catalyst intermediate obtained in step b) to a second calcination to obtain a solid acid catalyst.

[0042] In the present invention, the auxiliary agent raw material and the carrier are mixed in the first solvent and then the first loading is carried out, followed by drying and the first calcination to obtain the catalyst precursor. In the present invention, there is no special restriction on the order of adding the auxiliary raw material and the carrier to the first solvent. Prefer...

Example Embodiment

[0095] Example 1

[0096] 7.8g H 3 BO 3 , 8.5mL H 3 PO 4 And 130mL deionized water in a 500mL round bottom flask, when H 3 BO 3 After dissolving completely, add 80g of silica while stirring, then connect the round-bottomed flask to the slurry mixing device, and mix the elements B and P into the silica at 95°C. After loading for 0.5h, Raise the temperature to 120°C, evaporate the water in the carrier loaded with additives, put the dried carrier loaded with additives in a muffle furnace, and perform the first calcination at 300°C for 8 hours to make B and P elements Fully react and fix to the carrier to obtain the catalyst precursor;

[0097] Add 130mL containing 2g Li to the catalyst precursor containing B and P elements 2 O deionized aqueous solution, continue to react in a slurry mixing device at 90°C for 2 hours to obtain a catalyst intermediate;

[0098] The temperature is increased to 125°C, the water is evaporated, the catalyst intermediate is placed in a muffle furnace, and th...

Example Embodiment

[0101] Example 2

[0102] 7.8g H 3 BO 3 , 8.5mL H 3 PO 4 And 130mL deionized water in a 500mL round bottom flask, when H 3 BO 3 After dissolving completely, pour 80g of silica while stirring, connect the round-bottomed flask to the slurry mixing device, load at a temperature of 20℃ for 8h, raise the temperature to 120℃, and evaporate the water in the carrier loaded with additives , Put the dry carrier with auxiliary agent in a muffle furnace, and perform the first calcination at 350°C for 0.5h to fully react the B and P elements and fix them on the carrier to obtain the catalyst precursor;

[0103] Add 130mL containing 2g Li to the catalyst precursor containing B and P elements 2 O deionized aqueous solution, continue to react in a slurry mixing device at 90°C for 2 hours to obtain a catalyst intermediate;

[0104] Raise the temperature to 125°C, evaporate the water in the catalyst intermediate, and then add 130mL of concentrated ammonia water with a mass concentration of 36% to a wa...

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Abstract

The invention provides a solid acid catalyst which comprises the following components: metallic oxide, auxiliaries and a carrier, wherein the auxiliaries comprise boric oxide and phosphorus oxide. The solid acid catalyst provided by the invention can catalyze the condensation reaction of a carbonyl compound with a structure shown in the formula (I) and a monoolefin compound with a structure shown in the formula (II), so as to prepare a diene compound. The solid acid catalyst provided by the invention has relatively high product selectivity, the side reaction during the condensation reaction is reduced and the productivity of the diene compound is improved; the solid acid catalyst provided by the invention has high catalytic activity and a relatively high conversion rate; moreover, the solid acid catalyst provided by the invention has low toxicity, and is long in service life and good in regenerability, thereby being applicable to industrial production.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a solid acid catalyst, a preparation method thereof and a preparation method of a diolefin compound. Background technique [0002] Diolefin compounds are unsaturated hydrocarbons containing two carbon-carbon double bonds. The main use of isoprene in diene compounds is to produce isoprene rubber, butyl rubber, pharmaceutical and pesticide intermediates, synthetic lubricating oil additives, rubber vulcanizing agents, etc. [0003] In the prior art, the preparation methods of isoprene mainly include dehydrogenation method, synthesis method and extraction method, wherein the synthesis method includes isobutylene-formaldehyde method, acetylene-acetone method and propylene dimerization method. According to the different reaction processes, the isobutylene and formaldehyde method can also be divided into two-step method and one-step method. Among them, the two-step method is...

Claims

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Application Information

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IPC IPC(8): B01J27/18B01J27/182B01J27/19B01J27/198B01J27/186B01J27/185B01J27/187B01J32/00C07C11/18C07C2/86
Inventor 张贺新张学全白晨曦张春雨张梦辉于琦周毕吉福代全权那丽华董博胡庆娟
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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