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Production method for glycolic acid ester

A glycolic acid ester and production method technology, applied in the direction of carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve the problem of low selectivity of glycolic acid ester, achieve less side reactions, lower temperature, lower The effect of loss rate

Active Publication Date: 2012-08-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the low problem of glycolate ester selectivity that exists in the prior art

Method used

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  • Production method for glycolic acid ester
  • Production method for glycolic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Prepare the catalyst according to the content of 20 parts of Cu, 5 parts of Ag and 2 parts of Fe and the silicon oxide of the remainder, and its steps are as follows: (a) configure the mixed nitrate solution and sodium carbonate solution of copper, silver and iron of required concentration; (b) Co-precipitate the above solution at 70°C, stir continuously during the precipitation process, and pH=6 when the precipitation terminates; (c) Repeatedly wash the above precipitation slurry with deionized water until there is no Na + After adding silicon oxide carrier (specific surface area 150 square meters / gram) and concentration are 10% silica sol binding agent beating; Spherical shape; (e) Dry at 120°C for 6 hours and bake at 450°C for 4 hours. That is, the fluidized bed catalyst A was prepared.

[0022] The test is attached figure 1 The fluidized bed reactor device shown, using dimethyl oxalate as raw material, the reaction temperature is 200 ° C, the weight space velocity...

Embodiment 2

[0024] According to the various steps and conditions of [Example 1], the average diameter of the catalyst particles is 150 microns when the catalyst is molded, the particles are spherical, and the average specific surface area of ​​the carrier is 280 square meters per gram. The catalyst B thus obtained is 30 parts of Cu, 10 parts of Ag, 1 part of Fe and the rest of silicon oxide. The test is attached figure 1 The fluidized bed reactor device shown, using dimethyl oxalate as raw material, the reaction temperature is 170 ° C, the weight space velocity is 0.5 hours -1 , the hydrogen / ester molar ratio is 80:1, and the reaction pressure is under the condition of 2.8MPa, the raw material is contacted with the catalyst, and the reaction generates the effluent containing methyl glycolate, and the reaction result is: the transformation rate of dimethyl oxalate is 82 %, the selectivity of glycolate was 83%.

Embodiment 3

[0026] Prepare the catalyst according to the content of 40 parts of Cu, 3 parts of Ag and 15 parts of Fe and the silicon oxide and aluminum oxide of the balance, and its steps are as follows: (a) prepare the mixed nitrate solution and carbonic acid of copper, silver and iron of required concentration Sodium solution; (b) the above solution is co-precipitated at 65°C, stirring continuously during the precipitation process, and the pH=7 when the precipitation terminates; (c) repeatedly washing the above precipitation slurry with deionized water until there is no Na+ After adding alumina carrier (specific surface area 300 square meters / gram) and concentration are 15% silica sol binding agent beating; Spherical shape; (e) Dry at 120°C for 6 hours and bake at 450°C for 4 hours. That is, a fluidized bed catalyst C is obtained.

[0027] The test is attached figure 1 The fluidized bed reactor device shown, using dimethyl oxalate as raw material, the reaction temperature is 150°C, and...

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Abstract

The invention relates to a production method for glycolic acid ester, which mainly solves the technical problem in the prior art that the selectivity of the glycolic acid ester is low in the reaction process of preparing the glycolic acid ester through adding hydrogen in oxalic ester. According to the invention, the oxalic ester serves as raw materials, and at least one of water and C2-C5 alcohols is selected to serve as a terminating agent. The method comprises the following steps: (a), the raw materials enter from the bottom of a fluidized bed reactor to be in contact reaction with catalysts in a transition region and a dense-phase region of the fluidized bed reactor, so as to form an effluence I containing the glycolic acid ester and the catalysts; (b), the effluence I generated at the step (a) is in contact with the terminating agent at the bottom of a gas-solid quick separation region so as to form an effluence II which enters the gas-solid quick separation region at the upper part of the fluidized bed reactor and is subjected to gas-solid separation, and the sold catalyst enters a regenerator for regeneration; and (c), the catalyst from the regenerator returns the bottom of the fluidized bed reactor to continuously react. Due to the adoption of the technical scheme, the problem is better solved, and the method is suitable for industrial production of the glycolic acid ester.

Description

technical field [0001] The invention relates to a production method of glycolic acid ester, in particular to a method for generating glycolic acid ester through fluidized bed catalytic reaction catalyzed by dimethyl oxalate or diethyl oxalate. Background technique [0002] With its unique molecular structure: it has a-H, hydroxyl and ester functional groups at the same time, which makes it have the chemical properties of alcohol and ester, and can undergo carbonylation reaction, hydrolysis reaction, oxidation reaction, etc., and has become an important chemical raw material . Glycolate is an excellent solvent for many celluloses, resins, and rubbers. Its downstream products such as glycolic acid, glycine, dimethyl malonate and glyoxylic acid also have extensive application value. [0003] At present, there is no mature production process of environmentally friendly glycolic acid ester in China. It is still produced by the chloroacetic acid method, and the process is to mi...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/31
CPCY02P20/584
Inventor 刘俊涛王万民刘国强
Owner CHINA PETROLEUM & CHEM CORP
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