A kind of method that prepares 1,3-dibasic alcohol by prins condensation reaction

A condensation reaction and dihydric alcohol technology, which is applied in the field of preparing 1,3-dihydric alcohol, can solve the problems of complex catalyst preparation, easy deactivation of catalyst, low yield, etc., and achieves good catalytic conversion effect, high selectivity, Highly active effect

Active Publication Date: 2017-10-20
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are problems in the preparation route of 1,3-dihydric alcohol, such as long route, low yield, complex catalyst preparation and difficult separation, and easy deactivation of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] CeO obtained by co-precipitation method 2 -ZrO 2 The process is as follows: 17.4g of cerium nitrate hexahydrate and 2.31g of zirconium oxynitrate (the molar ratio of cerium and zirconium is 4:1) are dissolved in 100mL water respectively, the two solutions obtained are mixed, ammonia solution (the volume ratio of ammonia water to water is 1:1) adjust pH=11, stir at room temperature for 4 hours, filter and separate the resulting precipitate, wash with deionized water three times, dry the filter cake in an oven at 100°C overnight, and roast at 500°C for 4 hours to obtain the composite metal oxide CeO 2 -ZrO 2 . In a 250ml Teflon-lined reactor, add 60mmol38% formaldehyde solution, 3g catalyst and 10ml water respectively, pour 0.9MPa isobutylene into it, stir and react at 150°C for 2h, after the reaction, detect the product by chromatography, 3- The yield of methyl-1,3-butanediol is shown in Table 1.

Embodiment 2

[0021] CeO obtained by co-precipitation method 2 -ZrO 2 The process is as follows: 17.4g of cerium nitrate hexahydrate and 2.31g of zirconium oxynitrate (the molar ratio of cerium and zirconium is 4:1) are dissolved in 100mL water respectively, the two solutions obtained are mixed, ammonia solution (the volume ratio of ammonia water to water is 1:1) adjust pH=11, stir at room temperature for 4 hours, filter and separate the resulting precipitate, wash with deionized water three times, dry the filter cake in an oven at 100°C overnight, and roast at 500°C for 4 hours to obtain the composite metal oxide CeO 2 -ZrO 2 . In a 250ml Teflon-lined reactor, add 60mmol38% formaldehyde solution, 3g catalyst and 10ml water respectively, pour into 0.9Mpa propylene, stir and react at 180°C for 12h, after the reaction, chromatographically detect the product, 1, The yield of 3-butanediol is shown in Table 1.

Embodiment 3

[0023] CeO obtained by co-precipitation method 2 -ZrO 2 The process is as follows: 17.4g of cerium nitrate hexahydrate and 2.31g of zirconium oxynitrate (the molar ratio of cerium and zirconium is 4:1) are dissolved in 100mL water respectively, the two solutions obtained are mixed, ammonia solution (the volume ratio of ammonia water to water is 1:1) adjust pH=11, stir at room temperature for 4 hours, filter and separate the resulting precipitate, wash with deionized water three times, dry the filter cake in an oven at 100°C overnight, and roast at 500°C for 4 hours to obtain the composite metal oxide CeO 2 -ZrO 2 . In a 250ml Teflon-lined reaction kettle, add 60mmol38% formaldehyde solution, 3g catalyst and 10ml water respectively, pour into 0.9Mpa ethylene, stir and react at 200°C for 12h, after the reaction, chromatographically detect the product, 1, 3-Propanediol yield is shown in Table 1.

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PUM

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Abstract

The invention relates to a method for preparing 1,3-dihydric alcohols through Prins condensation reaction. The method adopts olefin and formaldehyde aqueous solution as reaction substrates, and directly prepares 1,3-diol under the catalysis of an acidic composite metal oxide. The reaction process is as follows: After mixing the formaldehyde aqueous solution with the catalyst, put it into a pressure vessel and seal it, pour in olefin gas, stir, the reaction temperature is higher than 80°C, and the reaction time is longer than 2h. After the reaction, the catalyst and the reaction system are easy to separate and can be reused. The yield of 1,3-diol can reach up to 90% in the second cycle.

Description

technical field [0001] The invention relates to a method for preparing 1,3-diol through Prins condensation reaction, in particular to the preparation of 1,3-diol through condensation and hydrolysis of formaldehyde and olefin. Background technique [0002] 1,3-diol has important uses in medicine, chemical industry, fuel, etc. It is mainly used as a monomer of polyester and polyurethane, as well as a solvent, antifreeze or protective agent, and is also an important pharmaceutical intermediate and organic synthesis intermediate. 1,3-propanediol can be used to synthesize paint, it can also synthesize 3-hydroxypropionic acid and malonic acid through air oxidation, and react with urea to synthesize cyclic carbonate. 1,3-Butanediol can be used as the raw material of polyester resin and alkyd resin, it can also be used for the synthesis of plasticizer, and it can also be used as wetting agent and softener. [0003] Methods for the preparation of 1,3-diols have been reported. CN87...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C29/38C07C31/20
CPCY02P20/582
Inventor 王峰王业红徐杰张健张晓辰
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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