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Preparation method of supported solid acid catalyst for synthetizing fatty acid methyl esters

A solid acid catalyst, a technology of fatty acid methyl ester, which is applied in the directions of fatty acid esterification, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of high catalyst preparation cost, small catalyst specific surface, and many post-treatment processes. , to achieve the effect of good catalyst activity, reduced preparation cost, and reduced process steps

Inactive Publication Date: 2014-05-28
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to provide a supported solid acid catalyst for the heterogeneous catalyzed esterification reaction of fatty acid and methanol, and the synthesis of fatty acid methyl ester by the heterogeneous catalyzed transesterification reaction of fatty acid ester and methanol, so as to solve the problem of reaction temperature in the prior art High, the active species of the solid acid catalyst is easy to dissolve and detach during the reaction, the stability is poor, the specific surface of the catalyst is small, the mechanical strength is low, the catalyst preparation cost is high, the post-treatment process is many, and the production cost is high.

Method used

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  • Preparation method of supported solid acid catalyst for synthetizing fatty acid methyl esters
  • Preparation method of supported solid acid catalyst for synthetizing fatty acid methyl esters
  • Preparation method of supported solid acid catalyst for synthetizing fatty acid methyl esters

Examples

Experimental program
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Effect test

Embodiment 1

[0017] 7.70g Zr(NO 3 ) 4 ·5H 2 O was dissolved in 10mL distilled water, and 0.10g Nd(NO 3 ) 3 ·6H 2 O was dissolved in 2mL of distilled water, and then the above two solutions were prepared into a mixed solution, and 10g of 20-40 mesh SiO was added under stirring conditions. 2 Carrier, after ultrasonic degassing for 5 minutes, soaked in a water bath at 30°C for 24h, dried at 80°C, and then calcined at 600°C for 4h to obtain ZrO 2 -Nd 2 o 3 / SiO 2 carrier. Dissolve 0.31g (NH 4 ) 6 MoO 24 4H 2 O, the roasted ZrO 2 -Nd 2 o 3 / SiO 2 The carrier was impregnated in the sulfuric acid solution of ammonium molybdate for 2 hours, dried at 110°C, and calcined at 600°C for 2 hours to obtain solid acid 1# catalyst SO 4 2- -M o o 3 -ZrO 2 -Nd 2 o 3 / SiO 2 -2h, SO in its components 4 2- ,M o o 3 ,Nd 2 o 3 ,, ZrO2 , SiO 2 The mass ratio of MoO is 7.35%: 2.00%: 0.32%: 17.70%: 1, MoO 3 , ZrO 2 ,Nd 2 o 3 The total loading of the three components was 20%.

[00...

Embodiment 2

[0020] The step that prepares catalyst by embodiment 1 makes 2# solid acid catalyst SO 4 2- -MoO 3 -ZrO 2 -Nd 2 o 3 / SiO 2 -4h, the difference is: the calcination time of the catalyst is 4h, and the SO 4 2- ,M o o 3 ,Nd 2 o 3 ,, ZrO 2 , SiO 2 The mass ratio is 6.02%: 2.00%: 0.32%: 17.70%: 1. The activity test reaction and analysis conditions were the same as in Example 1, and the yield of methyl laurate was analyzed to be 98.4%.

Embodiment 3

[0022] The step that prepares catalyst by embodiment 1 makes 3# solid acid catalyst SO 4 2- -MoO 3 -ZrO 2 -Nd 2 o 3 / SiO 2 -6h, the difference is: the calcination time of the catalyst is 6h, and the SO in its components 4 2- , MoO 3 ,Nd 2 o 3 ,, ZrO 2 , SiO 2 The mass ratio is 3.86%: 2.00%: 0.32%: 17.70%: 1. The reaction and analysis conditions of the activity test were the same as in Example 1, except that the stirring and reflux time was 3 hours. The yield of methyl laurate was analyzed to be 94.0%.

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Abstract

A preparation method of a supported solid acid catalyst for synthetizing fatty acid methyl esters comprises the following steps: using SO4<2->, M0O3, ZrO2 and Nd2O3 as active components, using porous and high specific surface SiO2 of 20-40 mesh as a carrier, preparing the solid acid catalyst SO4<2->-M0O3-ZrO2-Nd2O3 / SiO2 according to an immersion method. The catalyst is used for synthetizing fatty acid methyl esters through the esterification reaction between fatty acid and methanol and the transesterification between the ester of fatty acid and methanol, and under the conditions of the normal pressure reaction, the reaction temperature of 55-65 DEG C and the reaction time of 2-8 h, the yield of the fatty acid methyl esters is high; the catalyst uses SiO2 as the carrier, so that the catalyst is more in ducts, larger in specific surface, and stronger in mechanical property, the use amount of the active components is reduced, and the preparation cost of the catalyst is reduced remarkably; the catalyst is easier to be separated from the product, the post-processing method is simpler, the process steps are reduced, and the production cost can be reduced remarkably.

Description

technical field [0001] The invention relates to a preparation method of a supported solid acid catalyst for synthesizing fatty acid methyl ester. Background technique [0002] Sulfuric acid, which is cheap, readily available and highly catalytically active, is widely used in industry to synthesize fatty acid methyl esters. However, there are disadvantages such as serious corrosion of equipment, large discharge of three wastes, complicated post-treatment, many by-products, and easy carbonization of organic matter at high temperature. Solid acid catalysts have attracted much attention because of their environmental friendliness and easy separation from products, and they have shown good catalytic activity in organic synthesis reactions such as esterification and transesterification. Sulfuric acid modified ZrO 2 Base solid acid is a commonly used solid acid catalyst. K.Suwannakarn et al reported the prepared ZrO in Journal of Catalysis255(2008) 279–286 2 SO 4 2- -ZrO 2 It...

Claims

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Application Information

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IPC IPC(8): B01J27/053C11C3/10
Inventor 童冬梅李秀琴李会娟胡常伟
Owner SICHUAN UNIV