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Method for synthesizing hydroxyacetate through reactive rectification catalyzed by solid acid

A technology of glycolic acid ester and glycolic acid, which is applied in the field of synthesizing glycolic acid ester by reactive distillation catalyzed by solid acid, can solve the problems of long process flow, complicated purification process and equipment of synthetic raw material gas, limited application and development, etc.

Inactive Publication Date: 2016-08-10
EAST CHINA UNIV OF SCI & TECH
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  • Claims
  • Application Information

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Problems solved by technology

The raw material or product glycolic acid ester in method ④ and method ⑤ is essentially the intermediate product of synthesis gas to prepare ethylene glycol. The purification process and equipment of synthesis raw gas are complex and the process flow is long, which limits the application of this method to a certain extent And development
The defect of method ② is that there are few sources of pure glycolic acid, and the conversion rate of the single-pass esterification reaction is not very high

Method used

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  • Method for synthesizing hydroxyacetate through reactive rectification catalyzed by solid acid
  • Method for synthesizing hydroxyacetate through reactive rectification catalyzed by solid acid
  • Method for synthesizing hydroxyacetate through reactive rectification catalyzed by solid acid

Examples

Experimental program
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Effect test

Embodiment 1

[0023]Add 500mL of pure methanol solution into a 1000mL tower kettle (four-necked flask 1), and add 100mL glycolic acid methanol ethanol eluate into five 150mL jacketed reactors (8, 9, 10, 11, 12), respectively, where The molar ratio of methanol / glycolic acid is 5:1, and then 50g of treated and dried 732-type cation exchange resin (for the treatment method, please refer to the common conventional acid-base treatment method for ion exchange resins) is added to the five reactors as a solid acid catalyst. Open the condensed water valve of the tower top condenser 18, and feed cooling water; turn on the heating power supply of the tower kettle electric heating jacket 2, and carry out the temperature rise of the tower kettle 1 feed liquid; turn on the super water bath constant temperature tank 7 power supply for heating, adjust the temperature of the water bath and keep it constant at Around 80°C. In the experiment, the entire reactive distillation column can be allowed to react in...

Embodiment 2

[0031] The experimental raw materials and experimental conditions were the same as in Example 1, and the catalyst was changed to D001 type cation exchange resin. After the reaction, the total amount of feed liquid was 600 mL, which contained 175.8 g of glycolic acid. The total output of the tower kettle is 514.5g (volume 490mL), which contains 0.3677mol / L of glycolic acid and 4.227mol / L of methyl glycolate. Based on this calculation, the conversion rate of glycolic acid is 92.21%. The yield is 89.56%.

Embodiment 3

[0033] The catalyst used was 732 type cation exchange resin, and the experimental raw material was ethanol alcohol eluting liquid. Other experimental conditions were similar to those in Example 1. After the reaction, the total amount of feed liquid was 600mL, which contained 163.2g of glycolic acid. The total output of the tower kettle is 520.8g (volume 496mL), which contains 0.2913mol / L of glycolic acid and 4.032mol / L of ethyl glycolate. Based on this calculation, the conversion rate of glycolic acid is 93.27%. The yield is 93.15%.

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Abstract

A synthetic method for producing hydroxyacetate comprises: taking glycolic acid and alkanol as raw materials, taking 732-type and D001-type cation exchange resins as a solid acid catalyst, and using a reactive rectification column consisting of a rectification section, a stripping section, and a middle multi-kettle gas-liquid phase in sequence for continuous preparation of hydroxyacetate. The conversion rate and yield in an esterification process of hydroxyacetate is improved through controlling technical operation conditions, such as the mass ratio of glycolic acid to alkanol, the reaction temperature, and the consumption of the catalyst, in feeding. In a reactive rectification device, the operation conditions are that the mass ratio of alkanol to glycolic acid is 5:1, and each reactor has the reaction temperature being 70-80 DEG C, the column temperature being 90-110 DEG C, and the column top reflux ration being 0.3-0.5. The esterification conversion rate (based on hydroxyacetate) can reach more than 91%, and the yield of hydroxyacetate can normally reach more than 90%. Compared with a batch tank stirring esterification device in the prior art, the device in the method has large processing capacity and operational convenience, and is suitable for massive industrial production.

Description

technical field [0001] The present invention relates to a synthetic method of glycolic acid ester. Using alkanol and glycolic acid as raw materials, under the catalysis of cation exchange resins such as 732 type and D001 type, in the plate (or packing) tower section and multi-canister gas The invention relates to a method for synthesizing glycolate by continuous reactive distillation in reactive distillation equipment composed of liquid phase series reactors, which belongs to the field of reactive distillation separation and technology. Background technique [0002] Glycolic acid esters, including methyl glycolate, ethyl glycolate, (iso)propyl glycolate, butyl glycolate, etc., have important applications in the field of fine synthesis. For example, methyl glycolate, also known as methyl glycolate, methyl glycolate, etc., has low corrosion, low volatility, non-flammable, odorless, low toxicity, strong biodegradability, good metal chelation, The advantages of high water solub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/675B01J31/08
CPCY02P20/10
Inventor 施云海周忠雄梁善艾臻
Owner EAST CHINA UNIV OF SCI & TECH
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