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Method for synthesizing dipentaerythritol from mono-pentaerythritol

A technology for dipentaerythritol and monopentaerythritol, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of low synthesis yield of dipentaerythritol, expensive reaction raw materials, complicated reaction steps and the like, and achieves good industrial production. Prospects, high product quality, the effect of avoiding organic solvents

Inactive Publication Date: 2012-12-05
SHANGHAI BEIKAI IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0019] The technical problem to be solved in the present invention is to provide a synthesis method of dipentaerythritol, which solves the problems in the prior art that the reaction raw materials are expensive, the reaction steps are cumbersome, and the synthesis yield of dipentaerythritol is low

Method used

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  • Method for synthesizing dipentaerythritol from mono-pentaerythritol
  • Method for synthesizing dipentaerythritol from mono-pentaerythritol

Examples

Experimental program
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Embodiment 1

[0041] Add 136g of pentaerythritol, 155mL of 85wt% aqueous formic acid and 67.6g of polyphosphoric acid in a 500mL reaction flask with a water separation device, place at 120 o C oil bath, ventilation operation, under the protection of nitrogen, react for 8h, after the reaction, directly raise the temperature to 160o C, continue to separate a small amount of water, after reacting for 4 hours, cool down to 80 o C, add 180 mL of ethanol, change the water separation device to a reflux device, and reflux for 3 hours, a large amount of white insoluble matter is precipitated. After the reaction, filter and dry to obtain the crude product of dipentaerythritol. The reaction product was analyzed by high performance liquid phase, and the content of each substance was calculated based on pentaerythritol. The results are shown in Table 1.

Embodiment 2

[0043] Add 136g of pentaerythritol, 155mL of 85wt% aqueous formic acid and 34.4g of p-toluenesulfonic acid in a 500mL reaction flask with a water separator, place at 120 o C oil bath, ventilation operation, under the protection of nitrogen, react for 6h, after the reaction, directly raise the temperature to 160 o C, continue to separate a small amount of water, after reacting for 4 hours, then cool down to 80 o Add 180 mL of ethanol at C, change the water separation device to a reflux device, and reflux for 3 hours, a large amount of white insoluble matter precipitates out. After the reaction, the crude product of dipentaerythritol was obtained after filtration and drying. The reaction product was analyzed by high performance liquid phase, and the yield of each substance was calculated based on pentaerythritol. The results are shown in Table 1.

Embodiment 3

[0045] Add 136g of pentaerythritol, 155mL of 85wt% aqueous formic acid and 19.2g of methanesulfonic acid in a 500mL reaction flask with a water separator, place at 120 o C oil bath, ventilation operation, under the protection of nitrogen, react for 8h, after the reaction, directly raise the temperature to 170 o C, continue to separate a small amount of water, after reacting for 4 hours, then cool down to 80 o Add 180 mL of ethanol at C, change the water separation device to a reflux device, and reflux for 3 hours, a large amount of white insoluble matter precipitates out. After the reaction, the crude product of dipentaerythritol was obtained after filtration and drying. The reaction product was analyzed by high performance liquid phase, and the yield of each substance was calculated based on pentaerythritol. The results are shown in Table 1.

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Abstract

The invention discloses a method for synthesizing dipentaerythritol from mono-pentaerythritol. According to the method, pentaerythritol is used as a raw material and is subjected to a three-step continuous reaction of esterification, intermolecular condensation and interchange esterification to obtain a crude dipentaerythritol product. A synthetic process disclosed by the invention has the advantages that no special requirement on production equipment is set, reaction raw materials are low in price and easily obtained, the reaction process is simple, no separation of an intermediate is needed and the synthesis of the dipentaerythritol by the three-step continuous reaction is realized. The crude dipentaerythritol product synthesized by the method is subjected to high performance liquid chromatography, and the analysis result shows that the synthetic yield of the dipentaerythritol is as high as 40-50 percent and 10-30 percent of tripentearythritol as a byproduct is obtained; and the pentaerythritol obtained by a conventional separation method is higher in purity. The method disclosed by the invention has a favorable industrial production prospect.

Description

technical field [0001] The invention relates to a method for synthesizing dipentaerythritol from monopentaerythritol, in particular to a method for synthesizing dipentaerythritol through three-step continuous reactions of esterification reaction, intermolecular condensation reaction and transesterification reaction using pentaerythritol as a raw material. Background technique [0002] Dipentaerythritol is a solid polyol compound whose structural formula is as follows: [0003] [0004] Dipentaerythritol molecules contain multiple hydroxyl groups, which can undergo esterification, nitration, halogenation reactions, etc. to form functional compounds with unique application properties. They are widely used in the polymer industry, coating industry, printing and textile industry, aerospace industry, and can be used in production Fire and flame retardant materials, synthetic high-grade coatings and lubricating base oils, etc. [0005] Dipentaerythritol, as a raw material of e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/13C07C41/18
Inventor 秦威李俊秀
Owner SHANGHAI BEIKAI IND
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