Method for synthesizing methyl acrylate by means of filling catalysts in sections

A methyl acrylate and catalyst technology, applied in chemical instruments and methods, preparation of organic compounds, catalyst activation/preparation, etc., can solve problems such as low reaction conversion rate, and achieve the effects of improving conversion rate, improving reaction, and improving efficiency

Inactive Publication Date: 2009-11-11
HARBIN INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some people have also carried out related research on the aldol condensation synthesis of methyl acrylate for these two catalysts, but the problem of low conversion rate is common.

Method used

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  • Method for synthesizing methyl acrylate by means of filling catalysts in sections

Examples

Experimental program
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Effect test

Embodiment 1

[0024] In this example, 0.5g of lactic acid was dissolved in 5ml of hot water, and 0.5g of NH 4 VO 3 Add it into the lactic acid solution to make a vanadyl lactate solution, add 1.3g of phosphoric acid to make an impregnation solution, and then dissolve the chromatographic silica gel in 20ml of water. The two suspensions were stirred for 2 h to mix well. Evaporate the impregnating solution to dryness in a water bath, and dry it at 100°C until it becomes powdery. Then place it in a muffle furnace and burn at 200°C for 2 hours, at 300°C for 1 hour, and at 450°C for 3 hours to prepare the phosphorus vanadium catalyst. Under normal pressure, using the prepared catalyst with a V / P ratio of 1:2.5, the molar ratio of methyl acetate / formal is 1.6:1, and the feed space velocity is 3h -1 Methyl acrylate was reacted under certain conditions, the conversion rate of methylal was 15%, the selectivity of methyl acrylate was 72%, and the yield of methyl acrylate was 10.8%.

Embodiment 2

[0026] In this example, 35 ml of tetraethyl orthosilicate and 20 ml of absolute ethanol were stirred and heated to 60° C., and nitric acid was added dropwise to adjust the pH value to 3-4 to obtain a silica sol. 2g of Sb 2 o 3 Dissolve in 30ml of water, stir and add 5ml of triethanolamine as a stabilizer, then add 5ml of H 2 o 2 Produced Sb 2 o 5 Sol. Mix the silica sol and antimony gel and stir vigorously for 1 hour, adjust the pH value to 10 to prepare a mixed gel, add ammonium nitrate to dissolve the sol, raise the temperature to reflux, and react for 6 hours. Take out and dry in an oven at 80°C. Then put it in a muffle furnace to program the temperature to burn to obtain a white mixed gel, grind the mixed gel into 20-40 mesh, and impregnate 0.2g of CsNO 3 , and fired at 550°C for 3 hours to obtain Cs-Sb 2 o 5 / SiO 2 . Under the action of this catalyst, the methyl acetate / formaldehyde / molar ratio is 3:1, and the feed space velocity is 3h -1 Methyl acrylate was r...

Embodiment 3

[0028] The basic steps of this example are the same as those in Example 1, except that the two catalysts are loaded from top to bottom, and the phosphorus and vanadium are loaded in the third section, and the Cs-Sb 2 o 5 / SiO 2 The catalyst is loaded in the seventh section, the furnace temperature is set at 380°C, the molar ratio of methyl acetate / methylal is 1.6:1, and the feed space velocity is 3h -1 Methyl acrylate was reacted under the above conditions, the conversion rate of methylal at this time was 49.85%, the selectivity of methyl acrylate was 47.33%, and the yield of methyl acrylate was 23.59%.

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Abstract

The invention provides a method for synthesizing methyl acrylate by means of filling catalysts in sections; the method comprises the steps: methyl acetate and methylal are taken as raw materials for synthesizing methyl acrylate; the mole ratio of the methyl acetate to the methylal is 1:1 to 3:1; charging space velocity is 1 to 5h; the furnace temperature is fixed to be 350 DEG C to 420 DEG C; a reaction tube is divided into 9 sections; when two catalysts, i.e. phosphovanadate and Cs-Sb2O5 / SiO2, are filled in different sections from top to bottom, the phosphovanadate can be filled in the second section to the sixth section and the cesium or alkali metal catalyst can be filled in the second section to the ninth section; the conversion per pass of methylal is 30 percent to 50 percent; the selectivity of the methyl acrylate is 60 percent to 91 percent; and the yield per pass of the methyl acrylate is 40 percent to 50 percent. With the method for synthesizing the methyl acrylate by means of filling catalysts in sections, the reaction between the methyl acetate and the methylal can be further improved, the conversion rate of the methylal can be raised, and the yield of the target product, namely, the methyl acrylate, can be increased.

Description

(1) Technical field [0001] The invention relates to a chemical catalytic process, in particular to a method for synthesizing methyl acrylate. (2) Background technology [0002] Methyl acrylate is an important intermediate in organic synthesis and a monomer for synthesizing polymers. It is widely used in industries such as coatings, medicine, leather, papermaking, and adhesives. The main production methods of acrylic acid (ester): acrylonitrile hydrolysis method, propylene oxidation method, ketene method, among which propylene oxidation method accounts for a large proportion of the total production capacity of methyl acrylate. In addition, DuPont and Elf Ato jointly developed a new process for the production of acrylic acid using a moving bed reactor system. [0003] In the study, the synthesis of methyl acrylate with methyl acetate as raw material can usually be divided into two schemes, one is to use phosphorus vanadium catalyst to catalyze the reaction of methyl acetate a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/24B01J27/198B01J23/18B01J37/02G01N30/02G01N30/66
Inventor 荆涛孙德智田景芝邓启刚曹锐
Owner HARBIN INST OF TECH
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