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A kind of preparation method of isoprene

A technology for isoprene and isobutylene, which is applied in the field of Pr-doped ceria catalyzing the reaction of isobutylene and formaldehyde solution to prepare isoprene, can solve the problems that need to be further improved, and achieves controllable reaction process, easy operation and reaction. The effect of simple process and simple separation process

Active Publication Date: 2021-09-21
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Recently, Nb 2 o 5 -P 2 o 5 (Appl Catal A: Gen 2012,441–442,21), heteropolyacid catalysts (Catal Sci Technol 2016,6,6354 and Reaction Kinetics, Mechanisms and Catalysis 2016,117,761) are used in the reaction of isobutene and formaldehyde to synthesize isobutene Medium, but the conversion rate and the selectivity of the target product need to be further improved

Method used

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  • A kind of preparation method of isoprene
  • A kind of preparation method of isoprene
  • A kind of preparation method of isoprene

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Embodiment 1

[0046] Example 1 Cerium nitrate and praseodymium nitrate are dissolved in water at a molar ratio of 99:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The concentration of the two metal ions in the aqueous solution sums to 1mol / L, and then under stirring conditions, at 25 At ℃, 38wt% ammonia water was added dropwise thereto, and the molar ratio of ammonia water to the sum of the moles of the two metal ions was 10:1, then stood, separated, washed with water and ethanol, dried, and then calcined at 300 °C for 2 hours, Available Pr-doped ceria catalyst (Pr doping amount 0.8wt%) is recorded as Pr-CeO 2 -99.

[0047] Fill 2g of 40-60 mesh Pr-doped ceria prepared above into a fixed-bed reactor, gasify isobutylene and formaldehyde aqueous solution and mix with N 2 Mixed, passed into a fixed bed as a reaction gas, wherein the volume fraction of isobutene and formaldehyde were 5% and 5% respectively; the mass space velocity of the catalyst was 0.3h -1 . T...

Embodiment 2

[0049] Dissolve cerium nitrate and praseodymium nitrate in water at a molar ratio of 49:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The sum of the concentrations of the two metal ions in the aqueous solution is 0.1mol / L. Add sodium hydroxide to it, the molar ratio of sodium hydroxide to the sum of the moles of the two metal ions is 5:1, then let it stand, separate, wash with water and ethanol, dry, and then roast at 500 °C for 4h, Available Pr-doped ceria catalyst (Pr doping amount 1.6wt%), denoted as Pr-CeO 2 -49.

[0050] Fill 40-60 mesh 2g of the above-mentioned Pr-doped ceria into a fixed-bed reactor, gasify isobutene and formaldehyde aqueous solution and mix with Ar, and pass it into the fixed bed as reaction gas, wherein the volume of isobutene and formaldehyde The fractions are 5% and 5% respectively; the mass space velocity of the catalyst is 0.3h -1 . The reaction was continuously fed at 200°C under a pressure of 0.5 atm. After the ...

Embodiment 3

[0052] Dissolve cerium nitrate and praseodymium nitrate in water at a molar ratio of 19:1 to obtain an aqueous solution of cerium nitrate and praseodymium nitrate. The concentration of the two metal ions in the aqueous solution is 0.05mol / L. Then, under stirring conditions, at 85°C, Add potassium hydroxide dropwise to it, the molar ratio of potassium hydroxide to metal ions is 3:1, then let stand, separate, wash with water and ethanol, dry, and then roast at 800°C for 8h to obtain Pr-doped dioxide The cerium catalyst (the doping amount of Pr is 4wt%) is denoted as Pr-CeO 2 -19.

[0053] 40-60 mesh 2g of the Pr-doped ceria prepared above is packed into a fixed-bed reactor, isobutene and trioxane methanol solution are gasified and mixed with He, and passed into the fixed bed as a reaction gas, wherein isobutene, The volume fraction of formaldehyde is 25% and 5% respectively; the mass space velocity of the catalyst is 1h -1 . The reaction was continuously fed at 250°C under a ...

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Abstract

The invention relates to a method for preparing isoprene. The method adopts isobutene and formaldehyde solution as reaction substrates, and under the action of a Pr-doped ceria catalyst, isoprene is prepared through Prins condensation-hydrolysis-dehydration process. The specific reaction process is as follows: a certain amount of isobutylene and a certain amount of formaldehyde solution are introduced into a certain amount of formed praseodymium-doped ceria catalyst through a fixed bed device, and react at a temperature not lower than 200 ° C to obtain isobutene pentadiene. The method can obtain isoprene from isobutene and formaldehyde solution in one step, and the catalyst has good stability. Wherein the yield of isoprene can reach up to 85%.

Description

technical field [0001] The invention relates to a method for preparing isoprene, in particular to preparing isoprene by catalyzing the reaction of isobutylene and formaldehyde solution with Pr-doped ceria. Background technique [0002] Isoprene, also known as 2-methyl-1,3-butadiene, is an irreplaceable and important monomer for synthetic natural rubber. A colorless liquid with a special odor, which is of great significance for the synthesis of regular polyisoprene. At present, in the industry, about 95% of isoprene is mainly obtained from C5 by-products in the process of petroleum steam cracking to ethylene through fractional extraction. The yield of this method is limited by the yield of petroleum-based ethylene. However, in the long run, with the development of more efficient ethylene production technologies, such as the development and utilization of shale gas, coal-to-olefins MTO, MTP technology, biomass-to-olefins technology, etc., will directly lead to the reduction ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C11/18C07C1/207B01J23/10
CPCB01J23/10C07C1/2072C07C11/18Y02P20/584
Inventor 王峰张志鑫王业红李书双张健
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI