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Method for preparing neopentylene glycol

A technology of neopentyl glycol and hydroxypivalaldehyde, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the problems of polluting the environment, high catalyst prices, rising production costs, etc. big effect

Inactive Publication Date: 2010-06-16
SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Wherein U.S. Patent 4250337 proposes the copper chromite catalyst method with barium as promoter, but at this moment, the service temperature of catalyst is as high as 170~200 ℃, and HPA is easy to decompose under such high temperature, so its NPG yield only has 87% %; Propose to use the mixture of copper oxide complexed copper chromate as catalyzer in the U.S. Patent 4855515, make cocatalyst with magnesium oxide, at this moment chromium content is higher in the catalyzer, service temperature is also on the high side (150~220 ℃), NPG yield If the rate is less than 90%, it is difficult to dispose the catalyst after it is discarded, and there is a possibility of polluting the environment; in European patent 343475, it is proposed to use platinum, ruthenium and tungsten as the catalyst, the reaction temperature is 80 ° C, and the mixture of water and alcohol is used as the solvent. The catalyst price of this system is high , leading to an increase in production costs

Method used

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  • Method for preparing neopentylene glycol
  • Method for preparing neopentylene glycol
  • Method for preparing neopentylene glycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020]Prepare 500ml of 2mol / L mixed solution of copper nitrate, zinc nitrate and aluminum nitrate, gradually add alkaline precipitant such as dilute ammonia solution 200ml at 60°C, and keep stirring the system to make the active components precipitate uniformly, filter the precipitate, Washing, drying at 100°C, tablet molding, and calcination at 400°C to obtain the Cu-Zn-Al catalyst precursor. Reduction conditions: In hydrogen atmosphere, rise from room temperature to 120°C at 1°C / min, stay for 2 hours, then rise to 140°C at 0.5°C / min, stay for 2 hours, then rise to 180°C at 0.5°C / min, Stay for 4 hours, lower the temperature, hydrogen pressure 0.3MPa; hydrogen flow rate 50ml / min. The reaction conditions and results of the Cu-Zn-Al catalyst are shown in Table 1, and the solvent used in the reaction is ethanol.

[0021] Table 1 Reaction performance of Cu-Zn-Al catalyst

[0022]

Embodiment 2

[0024] Prepare 500ml of 2mol / L mixed solution of copper nitrate, chromium nitrate and aluminum nitrate, gradually add alkaline precipitant such as dilute ammonia solution 200ml at 60°C, and keep stirring the system to make the active components evenly precipitate, filter the precipitate, Washing, drying at 100°C, adding 5% methyl cellulose to extrusion molding, and calcination at 400°C to obtain the Cu-Cr-Al catalyst precursor. Reduction conditions: Under hydrogen atmosphere, rise from room temperature to 120°C at 1°C / min, stay for 2 hours, then rise to 140°C at 0.5°C / min, stay for 2 hours, then rise to 200°C at 0.5°C / min, Stay for 4 hours, lower the temperature, hydrogen pressure 0.3MPa; hydrogen flow rate 50ml / min. The reaction conditions and results of the Cu-Cr-Al catalyst are shown in Table 2, and the solvent used in the reaction is methanol.

[0025] Table 2 Reaction performance of Cu-Cr-Al catalyst

[0026]

Embodiment 3

[0028] Prepare 100ml of 2mol / L copper nitrate and chromium nitrate mixed solution, gradually add 30g of formed γ-alumina carrier at 70°C, so that the active components are evenly loaded on γ-alumina, and place the mixed system at 80°C Stir and heat in a water bath to volatilize the solvent, dry at 100°C, and bake at 400°C to obtain the CuCr / alumina catalyst precursor. Reduction conditions: Under hydrogen atmosphere, rise from room temperature to 120°C at 1°C / min, stay for 2 hours, then rise to 140°C at 0.5°C / min, stay for 2 hours, then rise to 240°C at 0.5°C / min, Stay for 4 hours, lower the temperature, hydrogen pressure 0.3MPa; hydrogen flow rate 50ml / min. The reaction conditions and results of the CuCr / alumina catalyst are shown in Table 3, and the solvent used in the reaction is butanol.

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Abstract

The invention provides a method for preparing neopentylene glycol. In the method, in the presence of an organic solvent, hydroxyl pivalaldehyde(HPA) serving as a starting raw material undergoes a hydrogenation reaction in the presence of a copper-based catalyst to form the neopentylene glycol(NPG), wherein the reaction pressure is 1 to 5MPa, the reaction temperature is between 100 and 140 DEG C, a molar ratio of the hydrogen gas to the hydroxyl pivalaldehyde is 1-20:1, and the used organic solvent is saturated fatty alcohol or a mixture thereof. The conversion rate of the HPA in the raw material is over 99.5 percent, the selectivity of the generated NPG is over 97 percent, and the catalyst lifetime is over 2,000 hours.

Description

technical field [0001] The invention relates to the specialty of organic synthesis in the field of chemical industry, in particular to a method for preparing neopentyl glycol and a catalyst related to the method. Background technique [0002] Neopentyl glycol (NPG for short) is a typical neopentyl structural diol. The structure has two reactive primary alcohol hydroxyl groups at symmetrical positions in the molecule, which endows the molecule with good chemical reactivity and is easy to quickly participate in various chemical reactions such as esterification, condensation and oxidation. In addition, there is no specific neopentyl structure of α-hydrogen atom on the central carbon atom of NPG, which makes its downstream products have excellent hydrolysis resistance, thermal stability and light resistance. These excellent properties make NPG widely used: it can mainly produce polyester resin, polyurethane, powder coating and synthetic lubricating oil, etc. NPG derivatives ar...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/141
Inventor 王剑宁春利罗鸽施凯敏马建学褚小东邵敬铭
Owner SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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