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Preparation method of esterification reaction catalyst

The technology of esterification reaction and catalyst is applied in the field of preparation of esterification reaction catalyst, which can solve the problems of inability to participate in the esterification reaction of higher fatty acids, low catalyst activity, environmental pollution, etc., and achieves rich medium and large pore structure and high catalytic efficiency. , the effect of high acid content

Inactive Publication Date: 2017-04-26
HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology can overcome the disadvantages of the prior art that the esterification reaction catalyst pollutes the environment, is high in cost, has low catalyst activity, and cannot participate in the esterification reaction of higher fatty acids.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 415 g catalyst filter residue in the solution, add 18 g ZSM-5 type molecular sieve, 6.5 g A type molecular sieve under stirring state, add 39 ml of 6% phosphoric acid after stirring evenly, the pH value of the system is 3.3, reacts 60 at 40 ℃ min; lower the temperature of the reaction system to room temperature, add 12 ml of sodium silicate solution with a concentration of 50 g / L under stirring, adjust the pH of the system to 9.7, stir evenly to make a slurry, and spray-dry to form microspheres ; 100 g of microspheres were immersed in 300 ml of 5 wt% sulfuric acid solution for 12 h, and then dried at 120 °C; the dried material was calcined at 750 °C for 1 h to prepare catalyst A. The specific surface area of ​​the catalyst is 289.5 m 2 / g.

Embodiment 2

[0024] Add 155 g of catalyst filter residue into the solution, add 38.3 g of X-type molecular sieves and 117 ml of water under stirring, add 63 ml of 4% phosphoric acid after stirring evenly, the pH value of the system is 2.7, and react at 60 °C for 30 min; The temperature of the system was lowered to room temperature, and the pH value of the system was adjusted to 10.4 by adding a potassium silicate solution with a concentration of 100 g / L and 15 ml under stirring, and stirred evenly to make a slurry, which was formed into microspheres by spray drying; 70 g of microspheres Immerse in 140 ml, 7 wt% sulfuric acid solution, impregnate for 10 h, and then dry at 120 °C; roast the dried material at 650 °C for 4 h to prepare catalyst B. The specific surface of the catalyst is 231.2 m 2 / g.

Embodiment 3

[0026] Add 200 g of catalyst filter residue into the solution, add 3 g of Y-type molecular sieves under stirring, add 74 ml of 2% phosphoric acid after stirring, the pH value of the system is 2.6, react at 40 °C for 40 min; reduce the temperature of the reaction system to At room temperature, 11 ml of ammonium silicate solution with a concentration of 150 g / L was added under stirring to adjust the pH value of the system to 11.0, and stirred evenly to make a slurry, which was formed into microspheres by spray drying; 100 g of microspheres were immersed in 190 ml, 9 wt% sulfuric acid solution, impregnated for 5 h, and then dried at 120 °C; the dried material was calcined at 690 °C for 3 h to obtain catalyst C. The specific surface of the catalyst is 324.8m 2 / g.

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Abstract

The invention relates to a preparation method of an esterification reaction catalyst. The preparation method is characterized by including the steps: 1) adding catalyst filter residues in a container, adding molecular sieves and water under the stirring state, adding phosphoric acid solution after mixture is uniformly stirred, controlling a pH (potential of hydrogen) value of a system to be larger than or equal to 2.5, and reacting for 30-60min at the temperature ranging from 40 DEG C to 60 DEG C; 2) reducing the temperature of the reaction system of step 1) to indoor temperature, adding additive under the stirring state, controlling the pH value of the system to be 9.0-11.0, uniformly stirring to prepare slurry, atomizing, and drying to prepare atomizing microspheres; 3) soaking the atomizing microspheres in sulfuric acid solution, drying, and roasting to obtain the esterification catalyst. The preparation method of the catalyst is simple, low in cost and high in esterification rate, and the catalyst is easily separated, can be repeatedly used and has high popularization and application values.

Description

technical field [0001] The invention relates to a preparation method of an esterification reaction catalyst, which uses molecular sieves and catalyst filter residues as main raw materials to prepare the catalyst through molding, impregnating and roasting methods. The invention belongs to the technical field of catalyst preparation. Background technique [0002] Esterification is an important part of chemical production, an important way to synthesize raw materials and intermediates, and the main source of many daily and production supplies. In traditional esterification reactions, liquid acids are generally used as catalysts. Liquid acid catalysts are easy to cause problems such as equipment corrosion, many side reactions, complicated product separation, and a large amount of industrial wastewater, so they are gradually replaced by environmentally friendly solid acid catalysts. [0003] Chinese patent CN 102068972 A discloses a method for preparing a solid esterification c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/80B01J29/08B01J29/60B01J29/85C07C67/08C07C69/14
CPCC07C67/08B01J29/005B01J29/08B01J29/60B01J29/80B01J29/40B01J29/0308B01J29/7003B01J29/85B01J2229/18B01J2229/20B01J2229/40B01J35/615C07C69/14
Inventor 郑淑琴何理均唐课文任劭张建策彭祥唐铭俊潘登李洁
Owner HUNAN INSTITUTE OF SCIENCE AND TECHNOLOGY
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