Bis-diol monoalkyl ether formaldehyde preparation method

A technology for diol monoalkyl ether and monoalkyl ether, which is applied in the field of preparing diglycol monoalkyl ether formal, can solve the problems such as difficulty in filtration and recovery of catalysts, reduce harm to human body, and improve product quality. Quality and effect of reducing waste water discharge

Active Publication Date: 2018-03-23
ANHUI XINYUAN CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

CN104974021A has reported the method for preparing di-lower alkoxymethane by sulfuric acid modification treatment nano-scale HZSM-5 catalyst, the catalyst has high activity, good selectivity and long service life, but it is more difficult to filter and recover the catalyst
However, the acetal exchange reaction under this condition must depend on the existence of the pyrrole ring. The same experiment was carried out with benzaldehyde ethylene glycol acetal, and it was found that the acetal exchange reaction cannot occur

Method used

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  • Bis-diol monoalkyl ether formaldehyde preparation method
  • Bis-diol monoalkyl ether formaldehyde preparation method
  • Bis-diol monoalkyl ether formaldehyde preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 156.4g of diethoxymethane, 81.2g of diethylene glycol butyl ether, and 0.8g of phosphotungstic acid into a 500mL four-neck flask equipped with a thermometer, a magnetic rotor, and a condenser tube, stir and heat up to 80°C, and the reaction time is 90min Reaction finishes, and reactant is layered, reclaims lower layer catalyst and recycles; Upper layer liquid removes excess diethoxymethane and ethanol through decompression distillation, obtains light yellow two diethylene glycol butyl ether formal crude product 103.5g, gas chromatography According to analysis, the content of diethylene glycol butyl ether formal is 68.9%, and the content of diethylene glycol butyl ether is 11.8%. The crude product can be refined to obtain bisdiethylene glycol butyl ether formal with a purity greater than 98%.

Embodiment 2

[0027] Add 156.1g of diethoxymethane, 81.4g of diethylene glycol butyl ether, and 0.8g of phosphotungstic acid into a 500mL four-neck flask equipped with a thermometer, a magnetic rotor, and a condenser tube, stir and heat up to 75°C, and the reaction time is 90min Reaction finishes, and reactant is layered, reclaims lower layer catalyst and recycles; Upper layer liquid removes excess diethoxymethane and ethanol through decompression distillation, obtains light yellow two diethylene glycol butyl ether formal crude product 102.4g, gas chromatography According to analysis, the content of diethylene glycol butyl ether formal is 66.4%, and the content of diethylene glycol butyl ether is 13.5%. The crude product can be refined to obtain bisdiethylene glycol butyl ether formal with a purity greater than 98%.

Embodiment 3

[0029] Add 156.5g of diethoxymethane, 81.3g of diethylene glycol butyl ether, and 0.8g of phosphotungstic acid into a 500mL four-neck flask equipped with a thermometer, a magnetic rotor, and a condenser tube, stir and heat up to 70°C, and the reaction time is 90min Reaction finishes, and reactant is layered, reclaims lower layer catalyst and recycles; Upper layer liquid removes excess diethoxymethane and ethanol through decompression distillation, obtains light yellow two diethylene glycol butyl ether formal crude product 101.8g, gas chromatography According to analysis, the content of diethylene glycol butyl ether formal is 65.9%, and the content of diethylene glycol butyl ether is 14.1%. The crude product can be refined to obtain bisdiethylene glycol butyl ether formal with a purity greater than 98%.

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Abstract

The invention discloses a bis-diol monoalkyl ether formaldehyde preparation method. The bis-diol monoalkyl ether formaldehyde can be prepared by the steps: utilizing methylene diethyl ether and diolmonoalkyl ether as raw materials and performing transacetalation under the catalysis of phosphotungstic acid. According to the preparation method disclosed by the invention, the bis-diol monoalkyl ether formal is synthesized from a phosphotungstic acid catalyst; the catalyst has the advantages of small use amount, high catalytic activity, small corrosion to equipment and easiness in being separated from products; recycling the catalyst is achieved; the preparation method is a high-efficiency, green and environment-friendly production method. The methylene diethyl ether is utilized to replace formaldehyde as the raw material, so that pollution of the formaldehyde to the environment and harm of the formaldehyde to the human body are greatly reduced; wastewater emission is reduced, product quality is improved, and a green chemistry idea is met.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and specifically relates to a method for preparing double glycol monoalkyl ether formal by using a phosphotungstic acid catalyst through an acetal exchange reaction. Background technique [0002] Acetal compounds play a very important role in daily production and life. Due to its unique glycol ether structure, double glycol monoalkyl ether formal has a wide range of uses in solvents, plasticizers, thinners, etc. . [0003] Take bis (diethylene glycol butyl ether) formal (BDEGBF) as an example. BDEGBF is a light yellow liquid with a relatively elegant taste. The CAS number is 143-29-3 and the molecular formula is C 17 h 36 o 6 , the relative molecular mass is 336.46, and the density is 0.968g / cm 3 , with a boiling point of 392.3°C and a structural formula as follows: [0004] [0005] BDEGBF is mainly used as diluent and non-reactive plasticizer (TP-90B) for coatings suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/48C07C43/30
CPCC07C41/48C07C43/30Y02P20/584
Inventor 朱新宝邵冲张小祥付博李俊胡明华魏民
Owner ANHUI XINYUAN CHEM
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