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Synthetic method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol

A synthesis method and technology of cyclobutanediol, applied in two fields, can solve problems such as complicated process and many side reactions, and achieve the effect of simple reaction process, simple composition and easy preparation

Active Publication Date: 2016-07-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention proposes a kind of synthetic method of 2,2,4,4-tetramethyl-1,3-cyclobutanediol, to solve 2,2,4,4-tetramethyl-1,3 - Hydrogenation of cyclobutanedione needs to be dissolved in a solvent and fed together, resulting in complex process and many side reactions

Method used

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  • Synthetic method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol
  • Synthetic method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol
  • Synthetic method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol

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Embodiment 1

[0065] Put 212.5 grams of copper nitrate (Cu(NO 3 ) 2 ·3H 2 O), 36.5 grams of zinc nitrate (Zn(NO 3 ) 2 6H 2 O), 73.5 grams of aluminum nitrate (Al(NO 3 ) 3 9H 2 O) and 10 grams of chromic acid (CrO 3 ) was dissolved in 800 ml of distilled water. Under heating and stirring, use alkali solution (sodium hydroxide, sodium carbonate or ammonia water) to neutralize to PH = 7, and at the same time, precipitates are formed. After filtering and washing, dry at 120°C for 5 hours, bake at 400°C for 4 hours, and shape. Catalyst I was reduced in a hydrogen stream at 300°C for 4 hours before use.

Embodiment 2

[0067] Put 121.4 grams of copper chloride (CuCl 2 2H2O), 127.8 grams of zinc nitrate (Zn(NO 3 ) 2 6H 2 O), 147 grams of aluminum nitrate (Al(NO 3 ) 3 9H 2 O) and 5 grams of chromic acid (CrO 3 ) was dissolved in 800 ml of distilled water. Under heating and stirring, use alkali solution (sodium hydroxide, sodium carbonate or ammonia water) to neutralize to PH = 7, and at the same time, precipitates are formed. After filtering and washing, dry at 120°C for 5 hours, and bake at 400°C for 4 hours to shape. The catalyst code is DLW-66. Catalyst II was reduced in hydrogen flow at 300°C for 4 hours before use.

Embodiment 3

[0069] Put 151.8 grams of copper nitrate (Cu(NO 3 ) 2 ·3H 2 O), 109.5 grams of zinc nitrate (Zn(NO 3 ) 2 ·6H 2 O), 95.6 grams of aluminum nitrate (Al(NO 3 ) 3 9H 2 O) and 7 grams of chromic acid (CrO 3 ) was dissolved in 800 ml of distilled water, under heating and stirring, neutralized to PH=7 with alkaline solution (sodium hydroxide, sodium carbonate or ammonia water), and a precipitate was formed at the same time, after filtering and washing, it was dried at 120°C for 5 hours, Baking at 400°C for 4 hours to shape. Catalyst III was reduced at 300°C for 4 hours in a hydrogen stream before use.

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PUM

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Abstract

The invention provides a synthetic method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol. The synthetic method is a highly selective conversion method of 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanedione into 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol. The synthetic method comprises the following steps: using 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanedione as a reaction raw material; and carrying out hydrogenation reaction of the 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanedione so as to generate 2, 2, 4, 4-tetramethyl-1, 3-cyclobutanediol. Catalysts utilized in the reaction comprise copper, zinc, aluminum and chromium elements. Weighed by weights of oxides of the copper, zinc, aluminum and chromium elements, weight of the copper oxide accounts for 40-70 parts of the total weight of the catalysts; weight of the zinc oxide accounts for 10-35 parts of the total weight of the catalysts; weight of the aluminum oxide accounts for 10-20 parts of the total weight of the catalysts; and weight of the chromium oxide accounts for 5-10 parts of the total weight of the catalysts. The synthetic method disclosed by the invention is simple in processes and relatively fewer in side effects.

Description

technical field [0001] The invention relates to a synthesis method of 2,2,4,4-tetramethyl-1,3-cyclobutanediol. Specifically, 2,2,4,4-dimethyl-1,3-cyclobutanedione is used as raw material to obtain 2,2,4,4-dimethyl-1,3 -The method of cyclobutanediol, this process technique is simple, and conversion rate is high. Background technique [0002] 2,2,4,4-Tetramethyl-1,3-cyclobutanediol is an aliphatic diol mainly used in the synthesis of high-performance polyesters to replace polycarbonate; the glass transition of traditional polyesters The low temperature limits its application in medium and high temperature fields. The addition of CBDO can significantly improve the glass transition temperature of polyester, improve weather resistance and transparency. [0003] So far, the more typical and mature methods in the world for synthesizing 2,2,4,4-tetramethyl-1,3-cyclobutanediol are to split isobutyric anhydride or isobutyric acid into two Methyl ketene is collected and polymerized ...

Claims

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Application Information

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IPC IPC(8): C07C35/04C07C29/145B01J23/86
Inventor 史君程光剑娄阳李学张晓琳黄集钺王洪星李志宇曹微石鸣彦韩秋萍琼伟格赵晶
Owner PETROCHINA CO LTD
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