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Method for preparing ethyl glycolate

A technology of glycolic acid ester and glyoxal, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problems of high raw material cost and easy polymerization of glycolic acid, and achieve stable product quality and reduce Raw material cost and effect of yield improvement

Active Publication Date: 2010-06-16
SHANGHAI SHISI CHEM PROD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a kind of preparation method of glycolic acid ester, to overcome the disadvantages of high raw material cost and easy polymerization of glycolic acid in the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Activation of the catalyst:

[0020] Add 1600g of 5wt% NH to the reactor with stirring and thermometer 4 NO 3 Solution, 200g of ZSM-5 molecular sieves (respectively marked as CatI, CatII, CatIII) with a silicon-aluminum ratio of 20, 30, and 35 were heated to reflux with stirring and maintained for 24 hours, cooled to room temperature, filtered, and the solid product obtained was obtained at 120 It was dried at ℃ for 5 hours, then placed in a resistance furnace, and activated at 350±5℃ for 2 hours to obtain 195 g of activated catalyst, which was cooled to room temperature for use.

[0021] (2) preparation of n-butyl glycolate:

[0022] In the pressure reactor with heating, stirring, thermometer, add 100g (0.71mol) 40wt% glyoxal aqueous solution respectively, the CatI activation catalyst that 5g step 1 obtains, 150g (2.11mol) n-butanol, heat while stirring Raise the temperature to 160±5°C, maintain the reaction for 0.5 hours, filter the reaction solution, remove th...

Embodiment 2

[0024] (1) Activation of catalyst: with embodiment 1.

[0025] (2) preparation of isooctyl glycolate:

[0026] In the pressure reactor with heating, stirring, thermometer, add 500g (3.55mol) 40wt% glyoxal respectively, 1600g (12.31mol) isooctyl alcohol, the CatII activation catalyst that 30g embodiment 1 obtains, heat while stirring Raise the temperature to 160±5°C, maintain the reaction for 0.5 hours, filter the reaction solution, remove the catalyst (recovery and reuse), and distill the filtrate under reduced pressure under the condition of 46mmHg, collect the 178-182°C fraction to obtain a colorless isooctyl glycolate liquid 520.57 g. The yield is 78%, the purity is 98%, the boiling point is 291-295°C, and the conversion rate of glyoxal is 100% as detected by HPLC.

Embodiment 3

[0028] (1) Activation of catalyst: with embodiment 1.

[0029] (2) preparation of benzyl glycolate:

[0030] In the pressure reactor with heating, stirring, thermometer, add 300g (2.07mol) 40wt% glyoxal respectively, 850g (7.86mol) benzyl alcohol, the CatIII activated catalyst that 10g embodiment 1 obtains, heat while stirring Raise the temperature to 160±5°C, maintain the reaction for 0.5 hours, filter the reaction liquid, remove the catalyst (recovery and reuse), and distill the filtrate under reduced pressure under the condition of 46mmHg, collect the fraction at 173-177°C, and obtain 254.86g of colorless benzyl glycolate liquid . The yield is 76%, the purity is 98%, the boiling point is 286-290° C. under the pressure of 14 mmHg, and the conversion rate of glyoxal is 100% as detected by HPLC.

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Abstract

The invention discloses a method for preparing ethyl glycolate. The method comprises the following steps of: refluxing HZSM-5 molecular sieves serving as a raw material in solution of NH4NO3, placing solid phase materials obtained by filtering in an electric resistance furnace for activation to obtain an activating catalyst; performing esterification reaction of aqueous solution of glyoxal serving as a raw material and a C4 to C8 unit alcohol in the presence of the activating catalyst in an atmosphere of nitrogen gas; and collecting a target product of ethyl glycolate from the reaction products. For the obtained ethyl glycolate, the yield is over 75 percent and the purity is over 98 percent. Compared with the prior art, the method uses the glyoxal to replace the glycolic acid as the raw material, thereby greatly lowering material cost, eliminating the self polymerization reaction which is difficultly avoided in the process of the glycolic acid and improving the yield of the target products; and the products obtained by the method is stable in quality, and the method is suitable for industrialized production.

Description

technical field [0001] The invention relates to a method for preparing glycolate, in particular to a method for preparing glycolate by using glyoxal as a starting material. Background technique [0002] Glycolic acid ester is an important class of chemical raw materials. It contains two functional groups, hydroxyl and ester, and can undergo various reactions. It has important applications in chemical synthesis and has a wide range of uses. Among them: n-butyl glycolate is a high boiling point solvent, which has good solubility in printing ink, dispersing binder and cleaning components, etc. It is widely used in paints, coatings and cosmetics, and can also be used as a synthetic anticancer drug Intermediate of isoharringtonine. Isooctyl glycolate is non-toxic, non-corrosive, harmless to the human body, does not pollute the environment, has strong cohesive force, no mildew, and no insects. It can be used as an emulsifier, thickener, stabilizer, sizing agent, and film-forming ...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/08
Inventor 宋振黄莹刘慧青吴晓旭
Owner SHANGHAI SHISI CHEM PROD
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