Preparation for p-benzoquionone dioxime

A technology of p-benzoquinone dioxime and p-benzoquinone, which is applied in oxime preparation, organic chemistry and other directions, can solve the problems of complicated steps, sewage discharge in the synthesis process, product purity limitation, etc., and achieves high reaction yield, high product purity, and waste. The effect of less liquid discharge

Inactive Publication Date: 2008-03-26
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method step is loaded down with trivial details, needs two sets of devices of cooling and heating, and productive rate is lower (about 60%), and product purity is subjected to the limitation (≤95%) of this synthetic method, contains more impurity, and owing to employing sodium nitrite, Environmentally unfriendly reagents such as sulfuric acid lead to serious pollution during the synthesis process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] In the first step, put 4.0g of p-benzoquinone, 5.4g of calcium carbonate, and 10.0g of hydroxylamine chloride into the reactor, add 80ml of ethanol and 20ml of water, and stir evenly. React at 70° C. for 3 h. After the reaction is complete, the product is evaporated in vacuo to remove the solvent.

[0013] In the second step, add 60ml of water and 11.3g of hydrochloric acid with a mass fraction of 36.5% into the container after removing the solvent, stir evenly for 5min, then filter the product with suction, wash with water, and dry to obtain 4.05g of the product. Through high-performance liquid chromatography analysis, compared with the standard sample, the product purity reaches more than 99%. The target product yield was 79.2%.

Embodiment 2

[0015] In the first step, put 4.0g of p-benzoquinone, 4.1g of calcium carbonate, and 10.0g of hydroxylamine chloride into the reactor, add 80ml of ethanol and 20ml of water, and stir evenly. React at 70° C. for 3 h. After the reaction is complete, the product is evaporated in vacuo to remove the solvent.

[0016] In the second step, add 60ml of water and 11.3g of hydrochloric acid with a mass fraction of 36.5% into the container after removing the solvent, stir evenly for 5min, then filter the product with suction, wash with water, and dry to obtain 4.49g of the product. Through high-performance liquid chromatography analysis, compared with the standard sample, the product purity reaches more than 99%. The target product yield was 87.9%.

Embodiment 3

[0018] In the first step, put 4.0g of p-benzoquinone, 3.4g of calcium carbonate, and 10.0g of hydroxylamine chloride into the reactor, add 80ml of ethanol and 20ml of water, and stir evenly. React at 70° C. for 3 h. After the reaction is complete, the product is evaporated in vacuo to remove the solvent.

[0019] In the second step, add 60ml of water and 11.3g of hydrochloric acid with a mass fraction of 36.5% into the container after removing the solvent, stir evenly for 5 minutes, then filter the product with suction, wash with water, and dry to obtain 4.77g of the product. Through high-performance liquid chromatography analysis, compared with the standard sample, the product purity reaches more than 99%. The target product yield was 93.3%.

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PUM

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Abstract

The present invention relates to catalytic synthesis process of p-benzoquinone dioxime, belongs to the field of organic synthesis technology, and is especially catalytic synthesis process of p-benzoquinone dioxime with p-benzoquinone and hydroxylamine chloride as material and calcium carbonate as catalyst and in certain temperature. P-benzoquinone dioxime, p-benzoquinone and hydroxylamine chloride are first reacted in alcohol inside a reactor; and through the subsequent vacuum evaporation to eliminate solvent, adding HCl and water through stirring and suction filtering, product is obtained. The process has high yield, high product purity, mild reaction condition, low energy consumption, environment friendship, and cheap and reuseable catalyst.

Description

technical field [0001] The present invention relates to a method for catalytically synthesizing p-benzoquinone dioxime. To be precise, it uses p-benzoquinone and hydroxylamine chloride as raw materials, and uses calcium carbonate as a catalyst to catalyze the synthesis of p-benzoquinone dioxime in the next step at a certain temperature. The method belongs to the technical field of organic synthesis. Background technique [0002] P-benzoquinone dioxime is a cross-linking agent, which has the characteristics of easy dispersion in the rubber compound, fast vulcanization speed, high tensile strength of the rubber compound, heat resistance, ozone resistance, and good electrical insulation. It can be used as a polymerization inhibitor for acrylic acid agent, metallic glass hot-melt adhesive, olefin copolymer crosslinking regulator, organic monomer stabilizer and self-vulcanizing adhesive. Oxidants (Pb 3 o 4 , PbO 2 ) has an activation effect and improves the thermal resistance...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/22C07C249/08
Inventor 单永奎贺峥侯亚伟孔爱国赵新华
Owner EAST CHINA NORMAL UNIV
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