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Method for preparing nonane diacid catalyzed by solid acid

A technology of solid acid catalysis and solid acid catalyst, which is applied in the preparation of carboxylate, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of expensive, difficult to recycle and reuse, and achieve an environmentally friendly effect.

Inactive Publication Date: 2007-11-28
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalyst 12-tungstophosphoric acid used in this method is a water-soluble acid, which exists in the water phase after the reaction, is difficult to recycle and reuse, and is expensive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Weigh a certain amount of ZrOCl with a molar ratio of 1:2 2 .8H 2 O and anhydrous AlCl 3 , dissolve with distilled water to make a mixed solution, add 28% ammonia water in the solution to adjust the pH to 10.0~11.0 to obtain a hydroxide precipitate, the precipitate is repeatedly washed and suction filtered after aging (stand overnight), until there is no chloride ion in the filtrate ( with AgNO 3 solution test). The resulting precipitate was dried at 110°C, ground, sieved with 100 mesh, and 0.5mol / LH 2 SO 4 Dipping for 12 hours. Filter, dry the filter cake at 110°C for 24 hours, and then burn at 500°C for 4 hours to obtain SO 4 2- ZrO 2 -Al 2 o 3 solid acid catalyst.

[0018] Add 100 grams of oleic acid, 10 grams of SO 4 2- / ZrO 2 -Al 2 o 3 Solid acid catalyst, 3 grams of cetyltrimethylammonium chloride. Stir and heat to 60°C, and pass air with an ozone concentration of 4g / L at a flow rate of 500ml / min. Add 200ml of 30% hydrogen peroxide ...

Embodiment 2

[0019] Embodiment two: a certain amount of TiCl 4 Dissolve in cyclohexane to make a 20% (W / V) solution. Under stirring, slowly add 28% ammonia solution dropwise to adjust the pH to 8-10 to obtain amorphous Ti(OH) 4 precipitation. The precipitate was statically aged for 24 hours, filtered, and washed repeatedly with ethanol and deionized water until there was no chloride ion (using AgNO 3 solution test). Dry at 110°C, grind, and sieve through 100 meshes, and use 0.5mol / LH 2 SO 4 Dipping for 12 hours. Filter, dry the filter cake at 110°C for 24 hours, and then burn at 500°C for 4 hours to obtain SO 4 2- / TiO 2 solid acid catalyst.

[0020] Add 100 grams of oleic acid, 10 grams of SO 4 2- / TiO 2 Solid acid catalyst, 3 grams of cetyltrimethylammonium chloride. Stir and heat to 60°C, inject ozone with a concentration of 10g / L at a flow rate of 500ml / min. Add 200ml of 10% hydrogen peroxide in batches, and control the temperature not to exceed 70°C. React at 65°C to 70...

Embodiment 3

[0021] Example 3: Grinding the 5A type macroporous molecular sieve into fine particles and sieving through a 60-mesh sieve to obtain fine gray powder. Dissolve the phosphotungstic acid solid equivalent to 1 / 5 of the mass of the 5A macroporous molecular sieve with distilled water equivalent to 1.5 times the volume of the 5A macroporous molecular sieve, and mix the above-mentioned 5A macroporous molecular sieve with the above-mentioned phosphotungsten at room temperature Mix the acid solution well and soak for 6 hours, dry at 110°C for 2 hours, and burn at 500°C for 3 hours to prepare the phosphotungstic acid-supported catalyst.

[0022] Add 100 grams of oleic acid, 8 grams of phosphotungstic acid supported catalyst, and 3 grams of cetyltrimethylammonium chloride into a 1000ml four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser. Stir and heat to 60°C, inject ozone with a concentration of 4g / L at a flow rate of 500ml / min. Add 200ml of 30% hyd...

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Abstract

The solid acid catalyzed process of preparing azelaic aid includes the following steps: mixing unsaturated fatty acid or mixed fatty acid produced through hydrolyzing animal and vegetable oil, solid acid catalyst and ammonium hexadecyl trimethyl chloride; stirring, heating to 50-70 deg.c, introducing gas mixture containing 2-10 wt% ozone in the flow rate of 500 ml / min, stepped adding 20-40 wt% concentration hydrogen peroxide solution at temperature controlled below 70 deg.c; heating to 95-110 deg.c for reaction for 5-12 hr; and separating the resultant liquid mixture and purifying to obtain pure azelaic aid. The used solid acid catalyst may be separated from other materials for reuse, and the process has facile materials and environment friendship, and is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing azelaic acid by using solid acid catalysis. Background technique [0002] Azelaic acid is a drug for the prevention and treatment of skin diseases, mainly used in the treatment of acne, chloasma and skin melanin deposition. It is also an important organic synthesis intermediate. It is also used in the synthesis of plasticizers in plastics and rubber industries, in the synthesis of low-temperature and high-speed lubricants in aviation fuels, and in the manufacture of electrolytic capacitors. [0003] The preparation of azelaic acid by using unsaturated fatty acids such as oleic acid and corresponding triglycerides such as castor oil and cottonseed oil is the main production method at present. [0004] In the method described in US5,336,793 by N.vaxnon S, etc., tungstic acid is used as a catalyst to oxidize oleic acid with 60% hydrogen peroxide to obtain a yield of 86% of azelaic acid. [0005] Montediso ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/13C07C51/285B01J27/053B01J29/78B01J21/04B01J21/06
Inventor 陈烨璞史春薇陈欣
Owner SHANGHAI UNIV
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