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CN-122010664-A - Preparation method of isobutylbenzene

CN122010664ACN 122010664 ACN122010664 ACN 122010664ACN-122010664-A

Abstract

The invention provides a preparation method of isobutylbenzene, which comprises the step of carrying out contact reaction on gaseous toluene, propylene and hydrogen in a microchannel reactor under the condition of gas-solid reaction and in the presence of a catalyst, wherein the active components of the catalyst comprise alkali metal and Cu. The method can react under the gas-solid contact reaction condition, so that the catalyst and the reaction product are not required to be separated, the reaction product is not required to be separated after the catalyst is deactivated by water or methanol (because the reaction speed of water or alcohol and alkali metal is high, a great amount of heat is released, the risk of fire is caused, the risk of the method is great), the method can react under the condition of lower pressure, and compared with the pressure (2-4 mpa) required by the traditional kettle type reaction, the pressure is greatly reduced.

Inventors

  • JIANG JIAN
  • MIAO CHANGXI
  • LU YUANJIAO
  • SUN QING
  • SONG LEI

Assignees

  • 中国石油化工股份有限公司
  • 中石化（上海）石油化工研究院有限公司

Dates

Publication Date
20260512
Application Date
20241111

Claims (10)

  1. 1. A preparation method of the isobutylbenzene is characterized by comprising the step of carrying out contact reaction on gaseous toluene, propylene and hydrogen in a microchannel reactor under the condition of gas-solid reaction in the presence of a catalyst, wherein the active components of the catalyst comprise alkali metal and Cu.
  2. 2. The preparation method according to claim 1, wherein, The inner diameter of the channel of the micro-channel reactor is 2-5 mm.
  3. 3. The process according to claim 1 or 2, wherein the catalyst is used in the preparation of the catalyst, The alkali metal content is 0.1-20wt%, preferably 14-18wt%, and/or The copper content is 0.1-15 wt%, preferably 0.5-10 wt%.
  4. 4. The process according to any one of claim 1 to 3, wherein, The alkali metal is selected from Na and/or K, preferably the alkali metal comprises K and Na; More preferably, the process is carried out, The weight ratio of sodium to potassium is (0.01-10): 1, preferably (0.1-5): 1, and/or Based on the total weight of the catalyst, the weight of sodium is 0.5-10wt% and the weight of potassium is 3-15wt%.
  5. 5. The production method according to any one of claims 1 to 4, wherein the catalyst is a supported catalyst comprising a carrier and the active component supported on the carrier.
  6. 6. The preparation method according to claim 5, wherein, The support is selected from one or more of alumina, silica, molecular sieves X and molecular sieves Y, preferably one or more of alumina, molecular sieves X, more preferably one or more of gamma-alumina, molecular sieves X, and/or The particle size of the carrier is 500-1000 μm.
  7. 7. The production method according to any one of claims 1 to 6, wherein the production method of the catalyst comprises: (1) The copper source is contacted with the carrier for impregnation, and the obtained solid is dried, roasted and reduced to obtain a catalyst precursor; (2) An alkali metal melt is mixed with the catalyst precursor under vacuum.
  8. 8. The process according to claim 7, wherein in the step (1), Drying at 100-150℃, and/or The roasting temperature is 450-650 ℃, and/or The reduction condition comprises reduction in a hydrogen atmosphere, wherein the reduction temperature is 150-300 ℃.
  9. 9. The production method according to any one of claims 1 to 8, wherein the conditions of the contact reaction include: the molar ratio of toluene to propylene is (0.05-2.5): 1, preferably (0.3-2.0): 1; The molar ratio of toluene to hydrogen is (10-3) 1; The contact is carried out under anhydrous and anaerobic conditions, and/or The weight space velocity of toluene is 0.1-3.5 h -1 , preferably 0.2-2.5 h -1 .
  10. 10. The production method according to any one of claims 1 to 9, wherein the conditions of the contact reaction include: A temperature of 150 to 300 ℃, preferably 170 to 250 ℃, and/or The pressure is 0.1 to 1.0MPa, preferably 0.2 to 0.8MPa.

Description

Preparation method of isobutylbenzene Technical Field The invention relates to a preparation method of isobutylbenzene. Background Ibuprofen (isobutylbezene, IBB for short) is a main intermediate for synthesizing ibuprofen (Profe or Brufen) which is an anti-inflammatory, antipyretic and analgesic medicine for human. Ibuprofen is used as an anti-inflammatory, antipyretic and analgesic drug for treating rheumatic arthritis, osteoarthritis, toothache, neuralgia and the like, has good curative effects on inflammation, fever and pain after gynaecological and obstetrical operations, and has small adverse reaction and can be taken for a long time. At present, other commonly used antipyretic analgesic drugs have many problems, such as unstable action of some domestic acetaminophen oral preparations, unsatisfactory high-fever effect and short antipyretic action time, and aspirin and compound preparations thereof have large side effects on digestive tracts and blood systems, and can cause the Reye's syndrome of children and the like, so the ibuprofen has very broad market application prospect. Among the numerous synthetic routes for the synthesis of ibuprofen, almost all routes require the use of the intermediate ibuprofen. The synthetic process route of the isobutylbenzene is dozens of routes up to now, but most of the synthetic process routes are laboratory preparation methods, and the raw materials are not easily available although the synthetic process can be industrialized. The existing synthesis process of the isobutylbenzene mainly comprises a side chain alkylation reaction process of toluene and propylene under the catalysis of alkali metal. In 1950, the scientists of Pines and the like firstly propose that alkyl aromatic hydrocarbon and micromolecular olefin are subjected to side chain alkylation reaction under the catalysis of strong alkali. The strong base catalyst is composed of alkali metal or alkali metal hydride and promoter. The promoter may be aromatic hydrocarbon, benzonitrile, pyridine or chloralkane, etc., and its main function is to induce alkali metal or its oxide to form metal organic compound to attack alkylbenzene. In the prior industry, toluene and propylene are mainly used for synthesizing the isobutylbenzene under the action of an alkali metal potassium-sodium catalyst. Because the method uses the metal potassium-sodium catalyst, water or alcohol is required to inactivate the catalyst in the synthesis process, and the safety risk is high. In addition, the industrial synthesis of the isobutylbenzene by batch kettle reaction is generally not realized in continuous production. Disclosure of Invention Aiming at the problems existing in the prior art, the invention provides a preparation method of the isobutylbenzene. The method can effectively reduce the safety risk, realize the continuous synthesis of the isobutylbenzene, and can obtain higher conversion rate and selectivity under the low pressure condition. In order to achieve the aim, the invention provides a preparation method of the isobutylbenzene, which comprises the step of carrying out contact reaction on gaseous toluene, propylene and hydrogen in a microchannel reactor under the condition of gas-solid reaction in the presence of a catalyst, wherein the active components of the catalyst comprise alkali metal and Cu. The method can react under the gas-solid contact reaction condition, so that the catalyst and the reaction product are not required to be separated, the reaction product is not required to be separated after the catalyst is deactivated by water or methanol (because the reaction speed of water or alcohol and alkali metal is high, a great amount of heat is released, the risk of fire is caused, the risk of the method is great), the method can react under the condition of lower pressure, and compared with the pressure (2-4 mpa) required by the traditional kettle type reaction, the pressure is greatly reduced. The method solves the defects that the isobutyl benzene in the prior art cannot be continuously produced and the safety risk in the prior art is high, and realizes continuous production and reduces the safety risk through a microchannel fixed bed reaction process. Detailed Description The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein. The following detailed description of embodiments of the invention is provided, but it should be noted that the scope of the invention is not limited by these embodiments, but is defined by the appended claims. All publications, patent applications, patents, and oth