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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
  • Description
  • 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 the boron, phosphorus, vanadium, aluminum and potassium five-component catalyst is not effective for condensation The selectivity of isoprene in the reaction product is still very low, it is difficult to produce industrially

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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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preparation example Construction

[0038] The invention provides a kind of preparation method of solid acid catalyst, comprises the following steps:

[0039] a) mixing the raw material of the auxiliary agent and the carrier in the first solvent and carrying out the first loading, and then drying and first roasting to obtain the catalyst precursor;

[0040] b) performing a second load on the catalyst precursor and the metal compound obtained in step a) in a second solvent to obtain a catalyst intermediate;

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

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

Embodiment 1

[0096] 7.8g H 3 BO 3 , 8.5mL H 3 PO 4 and 130mL deionized water were placed in a 500mL round bottom flask, when H 3 BO 3 After completely dissolving, add 80g of silicon dioxide to it while stirring, then connect the round bottom flask to the mixing device, at 95°C, make B and P elements evenly mixed into the silicon dioxide, after loading for 0.5h, Raise the temperature to 120°C, evaporate the moisture in the carrier loaded with additives, place 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 on the carrier to obtain the catalyst precursor;

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

[0098] Raise the temperature to 125°C, evaporate the water to dryness, place the catalyst interme...

Embodiment 2

[0102] 7.8g H 3 BO 3 , 8.5mL H 3 PO 4 and 130mL deionized water were placed in a 500mL round bottom flask, when H 3 BO 3 After completely dissolving, pour 80g of silica while stirring, connect the round-bottomed flask to the mixing device, load it at a temperature of 20°C for 8 hours, raise the temperature to 120°C, and evaporate to dryness the moisture in the carrier loaded with additives , placing the dry carrier loaded with additives in a muffle furnace, and performing the first calcination at 350° C. for 0.5 h, so that B and P elements are fully reacted and fixed on the carrier to obtain a 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 2h to obtain a catalyst intermediate;

[0104] Raise the temperature to 125°C, evaporate the moisture in the catalyst intermediate, and then add 130mL of concentrated ammonia water with ...

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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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