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Method for preparing neopentyl glycol

A technology of neopentyl glycol and dimethyl, which is applied in the chemical industry and can solve the problems of long steps, low yield of neopentyl glycol, and low yield.

Inactive Publication Date: 2011-11-23
淄博新华-百利高制药有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN1301685A proposes a kind of method for preparing neopentyl glycol by ibuprofen production by-product 2,2-dimethyl-3-chloropropanol, with 2, the still of 2-dimethyl-3-chloropropanol The raffinate is used as a raw material, and the epoxidation reaction is carried out under strong alkali conditions to obtain 2,2-dimethyl-1,3-epoxypropane; 2,2-dimethyl-1,3-epoxypropane is Under hydrolysis to get neopentyl glycol, but the yield of neopentyl glycol is less than 70%
CN101407447A has described a kind of 3 that produces in naproxen production process, and 3-dimethyl propylene oxide adopts acid hydrolysis, alkali neutralization, adds entrainer rectification to remove water, and filtration desalination obtains neopentyl glycol, step long and low yield

Method used

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  • Method for preparing neopentyl glycol
  • Method for preparing neopentyl glycol
  • Method for preparing neopentyl glycol

Examples

Experimental program
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Effect test

Embodiment 1

[0022] In the epoxidation reactor, feed intake contains 2,2-dimethyl-3-chloropropanol residue 100g (wherein 2,2-dimethyl-3-chloropropanol content is 30g), first heated to 85°C ; According to 0.5% of 2,2-dimethyl-3-chloropropanol, add dodecyltrimethylammonium chloride 0.15g, 2,2-dimethyl-3-chloropropanol: sodium hydroxide Add 30.47g of 45% sodium hydroxide solution at a molar ratio of 1: 1.4, and distill the generated 2,2-dimethyl-1,3-epoxypropane while reacting and collect it in the reservoir. Raise the temperature to 110°C, while controlling the temperature at the top of the tower to not exceed 75°C, stop the reaction until no more distillate comes out, and the reaction time is 6 hours. Add 150g of distilled water and 1.5g of sulfuric acid into the low-pressure hydrolysis reactor, and heat up to 55°C. While the epoxidation reaction is taking place, the 2,2-dimethyl-1,3-epoxypropylene collected in the reservoir is Add slowly into the hydrolysis reactor for reaction, and then ...

Embodiment 2

[0024] In the epoxidation reactor, feed intake contains 2,2-dimethyl-3-chloropropanol residue 100g (wherein 2,2-dimethyl-3-chloropropanol content is 30g), first heated to 85°C ; According to 3% of 2,2-dimethyl-3-chloropropanol, add cetyltrimethylammonium chloride 0.90g, 2,2-dimethyl-3-chloropropanol: sodium hydroxide Add 26.12g of 45% sodium hydroxide solution at a molar ratio of 1: 1.2, and distill the generated 2,2-dimethyl-1,3-epoxypropane while reacting and collect it in the reservoir, gradually depending on the reaction rate. Raise the temperature to 108°C, while controlling the temperature at the top of the tower to not exceed 75°C, stop the reaction until no more distillates come out, and the reaction time is 5.5 hours. Add 150g of distilled water and 1.5g of sulfuric acid into the low-pressure hydrolysis reactor, raise the temperature to 40°C, and pressurize to 0.3MPa. The 2,2-dimethyl-1,3-propylene oxide collected in the reservoir was slowly added into the hydrolysis...

Embodiment 3

[0026] In the epoxidation reactor, feed intake contains 2,2-dimethyl-3-chloropropanol solution 100g (wherein 2,2-dimethyl-3-chloropropanol content is 30g), first heated to 85°C; 1% of 2,2-dimethyl-3-chloropropanol amount adds dodecyltriethylammonium chloride 0.30g, 2,2-dimethyl-3-chloropropanol: sodium hydroxide molar ratio Add 30.47g of 45% sodium hydroxide solution at 1:1.4, and distill the generated 2,2-dimethyl-1,3-epoxypropane while reacting and collect it in the storage tank, and gradually heat up to 106°C, while controlling the temperature at the top of the tower to not exceed 75°C, until no more distillate comes out to stop the reaction, and the reaction time is 6.0 hours. Add 100g of distilled water, 3.6g of sulfuric acid, and 1.80g of polyethylene glycol PEG2000 into a low-pressure hydrolysis reactor, raise the temperature to 60°C and pressurize to 0.4MPa, and collect the 2,2-bis Methyl-1,3-epoxypropane was slowly added into the hydrolysis reactor; after the additio...

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Abstract

The invention relates to a method for preparing neopentyl glycol. The byproduct 2,2-dimethyl-3-chloropropanol, which is generated in the process of producing ibuprofen and the like, is used as the raw material to prepare neopentyl glycol through epoxidation and hydrolysis under the action of a phase-transfer catalyst. The method comprises the following steps: adding a quaternary ammonium salt or polyethylene glycol phase-transfer catalyst to 2,2-dimethyl-3-chloropropanol under alkaline conditions to carry out epoxidation, thereby generating 2,2-dimethyl-1,3-epoxy propane; and adding the quaternary ammonium salt or polyethylene glycol phase-transfer catalyst under acidic conditions to prepare neopentyl glycol at high yield by atmospheric or pressurized hydrolysis.

Description

Technical field: [0001] The invention belongs to the field of chemical industry, and relates to a kind of waste liquid containing 2,2-dimethyl-3-chloropropanol shown in formula (I) produced in the production process of ibuprofen as raw material to prepare formula (III) ) The method of neopentyl glycol shown. Background technique: [0002] Neopentyl glycol is mainly used in the production of saturated polyester resins, and its derivatives are widely used in the fields of coatings, automobiles, textiles, pesticides, plastics and petroleum. Saturated polyester resin produced from neopentyl glycol, its unique neopentyl structure makes powder coatings and high-solid coatings prepared from it have excellent fluidity, flexibility, chemical stability, and weather resistance performance, chlorine resistance, thermal stability and resistance to ultraviolet radiation. With the strengthening of people's awareness of environmental protection, the rapid development of environmental prot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/10
CPCY02P20/52
Inventor 吕志果郭振美刘义勇
Owner 淄博新华-百利高制药有限责任公司