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Catalyst for preparing p-tertbutyl benzaldehyde and preparation method

A p-tert-butyl catalyst technology, applied in the field of selective oxidation of p-tert-butyl toluene to synthesize p-tert-butyl benzaldehyde as a catalyst and its preparation, can solve the problems of limited application, many reaction steps, equipment corrosion, etc., and achieve high Selectivity and activity, improved catalytic activity, less corrosive effect on equipment

Active Publication Date: 2014-12-31
SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The traditional stoichiometric oxidation method is in MnO 2 , concentrated H 2 SO 4 Directly oxidize p-tert-butyltoluene to synthesize p-tert-butylbenzaldehyde under the influence of the action. This process has disadvantages such as equipment corrosion and serious pollution, high production cost, and difficult separation of products.
Although the process of benzyl chloride hydrolysis is mature, there are many reaction steps and the yield is low, and the product contains a small amount of organic chlorine that is not easy to remove, which is carcinogenic, and a large amount of sodium chloride or calcium chloride will be produced in the subsequent processing section waste water, so it causes serious pollution to the environment; in addition, because the products produced by this process contain chlorine, it also limits its application in fields such as spices and medicine
[0004] In the Chinese patent documents whose announcement numbers were CN1944368A and CN101058071A, there was a report on the synthesis of p-tert-butylbenzaldehyde by hydrogenation of methyl p-tert-butylbenzoate. , synthesis of aromatic aldehydes after hydrogenation, but the process is relatively complicated and the yield is low
However, the method for preparing p-tert-butylbenzaldehyde by the catalytic oxidation of a single active component catalyst that has been used in the field at present also has the problem that the conversion rate of the reactant and the selectivity of the product are low in the reaction process

Method used

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  • Catalyst for preparing p-tertbutyl benzaldehyde and preparation method

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Experimental program
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Effect test

Embodiment 1

[0026] 1. Titanium dichloride (Cp2TiCl 2 ) as the titanium source, accurately weigh 1.5g of titanocene dichloride and dissolve it in 50g of chloroform (CHCl 3 ), stir well until it completely dissolves into a red transparent solution to obtain solution A; weigh 6g of MCM-41 and add it to 100g of chloroform, then drop 1.5g of triethylamine into it and stir for 8min to obtain a suspension Solution B: add solution A dropwise to suspension B, and after fully stirring, filter with a vacuum filter bottle, dry the filtered solid in the air for 6 hours, and then roast it in the air at 550°C for 3 hours to obtain 4%Ti-MCM-41 catalyst;

[0027] 2. Accurately weigh 0.85g of cobalt acetate [Co(OOCCH 3 ) 2 4H 2 0], dissolved in 40 milliliters of ethylene glycol solution, then weighed 5g of 4%Ti-MCM-41 obtained in the above preparation steps and added to Co(OOCCH 3 ) 2 4H 2 0 ethylene glycol solution, stir evenly to make it fully wet, let it stand for 24 hours, vacuumize at 200°C for...

Embodiment 2

[0029] 1. Accurately weigh 2.0g titanocene dichloride and dissolve it in 70g chloroform, stir well until it completely dissolves into a red transparent solution to obtain solution A; weigh 5.7g MCM-41 and add it to 160g chloroform, Then 1.4g of triethylamine was dropped into it and stirred for 5min to obtain suspension B. Add solution A dropwise to suspension B, stir well until the suspension turns yellow; filter and dry in the air, and then roast in air at 500°C for 4 hours to obtain 5% Ti grafted MCM-41 catalyst;

[0030] 2. Accurately weigh 1.17g of cobalt acetate, dissolve it in 30ml of ethylene glycol solution, then weigh 4g of 4%Ti-MCM-41 obtained in the above preparation steps and add it to the ethylene glycol solution of cobalt acetate, and stir evenly , make it fully wet, let stand for 30 hours, vacuumize at 200°C for 4h, and roast the dry solid at 550°C for 4h to prepare 4%Ti-5%Co-MCM-41 catalyst.

Embodiment 3

[0032] 1. Accurately weigh 2.0g of titanocene dichloride and dissolve it in 100g of chloroform, stir well until it completely dissolves into a red transparent solution to obtain solution A; weigh 8.0g of HMS and add it to 180g of chloroform, then Add 2.0 g of triethylamine dropwise, and stir for 10 minutes to obtain suspension B; add solution A to suspension B dropwise, and stir well. After suction filtration, it was dried in the air, and then calcined at 550°C for 3 hours in the air to obtain the 4% Ti grafted HMS catalyst.

[0033] 2. Accurately weigh 1.33g of cobalt acetate, dissolve it in 45ml of ethylene glycol solution, then weigh 6g of the 4% Ti grafted HMS catalyst obtained in the above preparation steps and add it to the ethylene glycol solution of cobalt acetate, and stir evenly , make it fully wet, let it stand for 24 hours, vacuumize at 230°C for 3h, and roast the dry solid at 600°C for 3h to prepare 4%Ti-4%Co-HMS catalyst.

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Abstract

The invention relates to a catalyst for preparing p-tertbutyl benzaldehyde and a preparation method, wherein the preparation raw materials comprise a titanium source, cobalt salt, a mesoporous molecular sieve, triethylamine, a solvent, an alcohol impregnant and the like. According to the invention, the catalyst containing two active constituents, namely, titanium and cobalt, is prepared by taking the mesoporous molecular sieve as a carrier, and loading the active constituents by combining a grafting method with an impregnation method; the catalyst is high in selectivity and activity; the conversion rate of the reactants in a reaction for preparing p-tertbutyl benzaldehyde via catalytic oxidation is up to more than 45%, and the selectivity of the product is up to more than 90%.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and relates to a catalyst for selectively oxidizing p-tert-butyltoluene to synthesize p-tert-butylbenzaldehyde under mild conditions and a preparation method thereof. Background technique [0002] 4-tert-Butylbenzaldehyde is an important intermediate in chemical synthesis, widely used in medicine, dyestuffs, fragrances, pesticides, printing and dyeing auxiliaries and other industries, and is in great demand in the synthesis of flavors and fragrances lyral . [0003] The traditional stoichiometric oxidation method is in MnO 2 , concentrated H 2 SO 4 Directly oxidize p-tert-butyltoluene under the action to synthesize p-tert-butylbenzaldehyde. This process has the disadvantages of equipment corrosion and serious pollution, high production cost, and difficult separation of products. Although the process of benzyl chloride hydrolysis is mature, there are many reaction...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/03B01J35/10C07C47/542C07C45/36
Inventor 张金峰张存社周魁沈寒晰蓝伟
Owner SHAANXI RES DESIGN INST OF PETROLEUM CHEM IND
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