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Process for preparing o-phenylphenol sodium salt

A kind of o-phenylphenol sodium and a preparation process technology, applied in the field of preparation of o-phenylphenol sodium salt, can solve the problems of high energy consumption for decompression dehydration, poor product appearance, unsuitable crystallization, etc., and achieve the effect of reducing energy consumption

Inactive Publication Date: 2011-05-18
淄博润博化工销售有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the conversion rate of the o-phenylphenol solution washed with sodium carbonate aqueous solution is relatively low, and the obtained product is in an aqueous solution, the energy consumption of dehydration under reduced pressure is relatively large, and it is not suitable for crystallization, and the obtained product has a poor appearance, generally Red or a little black, the yield is relatively low, and it is not easy to operate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 1000ml of petroleum ether and 50ml of isopropanol into a 2000ml four-necked reaction bottle, add 170g of o-phenylphenol (1mol) with a content of 99.6%, heat up and stir to fully dissolve it, cool down to room temperature, and slowly add refined hydrogen Sodium oxide solution (about 1.1mol), after the dropwise addition, stir slowly for 5-6 hours, squeeze and suction filter, rinse the reaction bottle with 200ml of petroleum ether and wash the filter cake, after the filter cake is centrifuged and vacuum-dried at 48°C The finished product is obtained, and the filtrate is reused. After the filtrate is used many times, crystals will be precipitated, which can be extracted with water and recycled at atmospheric pressure. The product is a white powder with a purity of 96%. mp: 57-58°C.

Embodiment 2

[0024] Put 900ml of toluene and 100ml of tetrahydrofuran into a 2000ml four-necked reaction flask, add 170g of o-phenylphenol (1mol) with a content of 99.6%, heat up and stir to fully dissolve it, cool down to room temperature, and slowly add the refined sodium hydroxide solution dropwise (about 1.1mol), after the dropwise addition, stir at a slow speed for 5-6 hours, squeeze and filter, rinse the reaction bottle with 200ml petroleum ether and wash the filter cake, after the filter cake is centrifuged and vacuum-dried at 48°C, the finished product is obtained , and the filtrate was reused. After the filtrate is used many times, crystals will be precipitated, which can be extracted with water and recycled at atmospheric pressure. The product is white powder with a purity of 95.6%. mp: 57-58°C.

Embodiment 3

[0026] Put 900ml of petroleum ether and 100ml of methyl isobutyl ketone into a 2000ml four-necked reaction flask, add 170g of o-phenylphenol (1mol) with a content of 99.6%, heat up and stir to fully dissolve it, cool to room temperature, and slowly dropwise add Refined sodium hydroxide solution (about 1.1mol), after the dropwise addition, stir slowly for 5-6 hours, squeeze and suction filter, rinse the reaction bottle with 200ml of petroleum ether and wash the filter cake, after the filter cake is centrifuged at 48°C The finished product is obtained after vacuum drying, and the filtrate is reused. After the filtrate is used many times, crystals will be precipitated, which can be extracted with water and recycled at atmospheric pressure. The product is white powder with a purity of 95.2%. mp: 56.5-58°C.

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Abstract

The invention relates to a method for preparing o-phenylphenol sodium salt. The method comprises the following steps of: dissolving o-phenylphenol in an organic solvent; directly dropwise adding sodium hydroxide solution; directly separating an obtained product out of an organic phase; and filtering and drying to obtain a product, wherein the organic solvent is a mixed solvent of a polar solvent and a non-polar solvent in a volume ratio of 1:0.03-1:0.3, preferably between 1 to 0.05 and 1 to 0.1; the non-polar solvent is an aromatic hydrocarbon solvent or an aliphatic hydrocarbon solvent; and the polar solvent is an ester solvent, a ketone solvent, an alcohol solvent or an ether solvent. By the method, the appearance of the o-phenylphenol sodium salt can be effectively improved and the content is more than or equal to 99 percent; and the method has the advantages of easily controlled reaction conditions, simple preparation process, energy conservation, emission reduction and the like.

Description

technical field [0001] The invention relates to the preparation of o-phenylphenol sodium salt, in particular to a preparation process of adding sodium hydroxide solution dropwise to an organic solution of o-phenylphenol sodium and directly filtering to obtain o-phenylphenol sodium. Background technique [0002] The use of o-phenylphenol sodium salt is mainly as antiseptic and fungicide, antifungal agent. Mainly used in citrus. my country stipulates that it can be used for citrus preservation, the maximum usage amount is 0.95g / kg, and the residual amount is not more than 12mg / kg. The method of use is different from that of OPP (07202). Mainly adopt immersion, spray or tank washing with 0.3% to 2% aqueous solution. It is also possible to add 0.68% to 2% to the wax and then spray it. [0003] Regarding the preparation of o-phenylphenol sodium salt, the traditional process is to extract o-phenylphenol from the residue of phenol production, and react in aqueous solution to ob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/235C07C37/66
Inventor 颜如和于兵甄美静于成
Owner 淄博润博化工销售有限公司