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Solid superstrong acid catalyst of esterification of preparation thereof

A technology of solid superacid and esterification reaction, which is applied in the direction of physical/chemical process catalyst, carboxylate preparation, chemical instruments and methods, etc. It can solve the problems of large amount of esterification reaction catalyst, high cost, and harsh preparation conditions. Achieve the effects of easy control of preparation conditions, extended life, and convenient preparation conditions

Inactive Publication Date: 2005-10-12
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a catalyst that does not pollute the environment, is easy to prepare, has high catalytic activity, good selectivity, long life, and good product color, aiming at the shortcomings of the existing esterification reaction catalysts, such as large consumption, high cost, and harsh preparation conditions. Solid Superacid Catalyst System SO 4 2- / Ti-Al-M-O, M is a kind of rare earth element (Re, Tm, La), to replace this traditional catalyzer of sulfuric acid, another purpose of the present invention is to provide the preparation method of this catalyzer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Catalyst preparation

[0020] Stir and mix the two salt solutions with the atomic ratio of Ti and Al of 1:0.3 (the molar content of Al is 23%) at room temperature, and use NH 3 ·H 2 O to adjust the pH of the solution to 10, age for 8 hours, filter and wash with suction, dry at 383-413K for 15-24 hours, and grind to ≤200 mesh. Then use 0.1mol·L -1 Tm(NO 3 ) 3 Solution according to 15ml·g -1 The ratio of reflux state impregnated 2h, with 0.5mol L -1 H 2 SO 4 Solution according to 10ml·g -1 Immerse for 20min, dry at 393K for 3h, bake at 653K for 5h in an air atmosphere, and store in a desiccator.

[0021] Catalytic synthesis of TOPM

[0022] Weigh 0.1 g (accounting for 1.8% of the average anhydride weight) of the catalyst, weigh 5.5 g of pyromellitic anhydride, and weigh 27 ml of isooctyl alcohol into a three-necked flask. Insert a thermometer, a reflux condenser, and a water separator into the three-necked flask, start timing from the beginning of reflux, and the...

Embodiment 2

[0024] Catalyst preparation

[0025] Stir and mix the two salt solutions with the atomic ratio of Ti and Al of 1:0.7 (the molar content of Al is 41.2%) at room temperature, and use NH 3 ·H 2 O to adjust the pH of the solution to 6, age for 8 hours, filter and wash with suction, dry at 383-393K for 24 hours, grind to ≤200 mesh, and then use 0.2mol·L -1 Tm(NO 3 ) 3 Solution according to 15ml·g -1 After impregnating for 50min in the reflux state, use 0.5mol·L -1 H 2 SO 4 Solution according to 10ml·g -1 Immerse in the ratio of 20min, dry at 393K for 2h, grind to ≤200 mesh, bake at 773K for 5h in air atmosphere, and store in a desiccator.

[0026] Catalytic synthesis of TOPM

[0027] The esterification reaction was carried out according to the method of Example 1, the reaction temperature was 169-185° C., and the reaction yield was 99.3%.

Embodiment 3

[0029] At room temperature, stir and mix the two salt solutions with the atomic ratio of Ti and Al of 1:1 (the molar content of Al is 50%) and mix them evenly with NH 3 ·H 2 O to adjust the pH value of the solution to 8, age for 6 hours, filter and wash with suction, dry at 383K for 24 hours, grind to ≤200 mesh, and then use 0.2mol·L -1 La(NO 3 ) 3 Solution according to 15ml·g -1 After immersing in the reflux state for 20min, use 0.1mol·L H 2 SO 4 The solution was impregnated at a ratio of 10ml·g for 25min, dried at 393K for 1h, ground to ≤200 mesh, calcined at 873K for 5h in an air atmosphere, and then stored in a desiccator.

[0030] Catalytic synthesis of TOPM

[0031] Esterification is carried out according to the method of example 1, and reaction temperature is 165~189 ℃, and reaction yield is 98.0%

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Abstract

An ultra-strong solid acid catalyst used for esterifying reaction to synthesize tetraisooctyl sym-phenyltetraformate (TOPM) from sym-phenyl tetraformic dianhydride and isooctanol is prepared from titanium sulfate, aluminium nitrate, sulfuric acid and RE salt. Its formula is SO4 / Ti-Al-M-O, where M is chosen from Re, Tm and La. Its advantages are high activity and selectivity, long service life and low reaction temp.

Description

technical field [0001] The invention relates to a solid superacid catalyst for esterification reaction and a preparation method thereof, in particular to a solid superacid catalyst modified with rare earth for esterification reaction and a preparation method thereof. Background technique [0002] Carboxylate is an important organic compound. It can not only be used as a raw material for organic synthesis, but also an important fine chemical product. It is widely used in spices, daily chemicals, food, medicine, rubber, paint and other industries. With the rapid development of science and technology and the improvement of people's living standards, people's demand for it is also increasing. The traditional synthetic method of this product is to use corresponding carboxylic acid and alcohol as raw materials, and adopts concentrated sulfuric acid as catalyst to prepare. Although the use of concentrated sulfuric acid as catalyst has the advantages of low price and high activity, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053C07C67/00
Inventor 管国锋万辉谭强
Owner NANJING TECH UNIV
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