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Acrylic acid ester synthesis method

A synthetic method and acrylate technology, which is applied in the field of acrylate synthesis and can solve the problem of low selectivity of acrylate

Active Publication Date: 2017-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the problem of low selectivity of acrylate in the reaction of preparing acrylate by dehydration of existing 3-hydroxypropionate, and a new synthetic method of acrylate is provided, which has the advantages of high selectivity of acrylate advantage

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 1. Acquisition of catalyst

[0023] Silicon source (weight concentration is 40% silica sol), aluminum source (sodium metaaluminate), TBABr (tetrabutylammonium bromide) and water are mixed to obtain a mixture, and in molar ratio, SiO 2 :Al 2 o 3 :TBABr:H 2 O is 1.000:0.013:0.100:50.825; adjust the pH value to 12 with NaOH, stir for 20 minutes, put it into a reaction kettle, crystallize at 170°C for 3 days, quench, filter, wash with water until the pH value is 8, and Dry at 120°C for 12 hours to obtain the original ZSM-5 powder, then release the template at 600°C and exchange hydrogen to obtain HZSM-5. Join Al 2 o 3 , Tianqing powder, 0.3N nitric acid (HZSM-5 / Al 2 o 3 / Tian Qing powder = 1:1:0.1) extruded into rods, dried at 80°C for 5 hours, calcined at 500°C for 5 hours, and the product with 25-35 meshes was sieved as the H-ZSM-5 catalyst.

[0024] The molecular sieve silicon-aluminum atom molar ratio in the catalyst is 30.

[0025] 2. Synthesis of acrylate

...

Embodiment 2

[0029] 1. Acquisition of catalyst

[0030] Silicon source (weight concentration is 40% silica sol), aluminum source (sodium metaaluminate), TBABr (tetrabutylammonium bromide) and water are mixed to obtain a mixture, and in molar ratio, SiO 2 :Al 2 o 3 :TBABr:H 2 O is 1.000:0.013:0.100:50.825; adjust the pH value to 12 with NaOH, stir for 20 minutes, put it into a reaction kettle, crystallize at 170°C for 3 days, quench, filter, wash with water until the pH value is 8, and Dry at 120°C for 12 hours to obtain the original ZSM-5 powder, then release the template at 600°C and exchange hydrogen to obtain HZSM-5. Join Al 2 o 3 , Tianqing powder, 0.3N nitric acid (HZSM-5 / Al 2 o 3 / Tian Qing powder = 1:1:0.1) extruded into rods, dried at 80°C for 5 hours, calcined at 500°C for 5 hours, and the product with 25-35 meshes was sieved as the H-ZSM-5 catalyst.

[0031] The molecular sieve silicon-aluminum atom molar ratio in the catalyst is 30.

[0032] Mix the above shaped molecu...

Embodiment 3

[0039] 1. Acquisition of catalyst

[0040] Silicon source (weight concentration is 40% silica sol), aluminum source (sodium metaaluminate), TBABr (tetrabutylammonium bromide) and water are mixed to obtain a mixture, and in molar ratio, SiO 2 :Al 2 o 3 :TBABr:H 2 O is 1.000:0.013:0.100:50.825; adjust the pH value to 12 with NaOH, stir for 20 minutes, put it into a reaction kettle, crystallize at 170°C for 3 days, quench, filter, wash with water until the pH value is 8, and Dry at 120°C for 12 hours to obtain the original ZSM-5 powder, then release the template at 600°C and exchange hydrogen to obtain HZSM-5. Join Al 2 o 3 , Tianqing powder, 0.3N nitric acid (HZSM-5 / Al 2 o 3 / Tian Qing powder = 1:1:0.1) extruded into rods, dried at 80°C for 5 hours, calcined at 500°C for 5 hours, and the product with 25-35 meshes was sieved as the H-ZSM-5 catalyst.

[0041] The molecular sieve silicon-aluminum atom molar ratio in the catalyst is 30.

[0042] The above-mentioned shaped ...

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PUM

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Abstract

The present invention relates to an acrylic acid ester synthesis method. A purpose of the present invention is mainly to solve the problem of low selectivity of acrylic acid ester in the prior art. According to the present invention, by using the acrylic acid ester synthesis method, in the presence of a molecular sieve catalyst, 3-hydroxypropionate is subjected to dehydrating to obtain the acrylic acid ester; and with the technical scheme, the problem in the prior art is well solved, and the method can be used in the industrial production of the acrylic acid ester.

Description

technical field [0001] The present invention relates to the synthetic method of acrylate. Background technique [0002] Acrylate is an important organic chemical raw material. At present, the main synthesis method is to obtain acrylate through oxidation and esterification of propylene. With the technological progress in the field of biochemical industry and hydromethylation reaction, the source of 3-hydroxypropionate is increasingly Abundant, dehydration of 3-hydroxypropionate to prepare acrylate has become a new viable option. [0003] WO2013017904A1 (Improved Process of Dehydration Reactions) discloses a method for producing acrylic acid and methacrylic acid by catalytic dehydration of hydroxycarboxylic acid. The catalyst used is to load the active component of composite oxide containing W on a porous carrier, and the carrier is selected from TiO 2 , SiO 2 、Al 2 o 3 , ZrO 2 and Nb 2 o 5 at least one of the As one of the preferred embodiments, the catalyst active c...

Claims

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Application Information

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IPC IPC(8): C07C67/327C07C69/54B01J29/40B01J29/46B01J29/48
CPCB01J29/40B01J29/405B01J29/46B01J29/48B01J2229/18C07C67/327C07C69/54
Inventor 李晓明李云龙刘波吕建刚金照生周海春
Owner CHINA PETROLEUM & CHEM CORP
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