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Synthesis method of 1-benzylpyridinium-3-carboxylate

A technology of benzylnicotinic acid and a synthesis method is applied in the synthesis field of alkaline cyanide-free zincate galvanizing additives, can solve the problems of dark red color, poor water solubility of products, long reaction time and the like, and achieves short reaction time , good throwing and deep plating ability, low cost effect

Active Publication Date: 2015-01-14
湖北吉和昌化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] If simply synthesized according to the above process without adding other catalysts and buffers, the reaction time will be long, the color of the obtained product will be dark red or even black, and there will be a large amount of black viscous substance, the product will not be water soluble, and will have opalescence after dilution

Method used

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  • Synthesis method of 1-benzylpyridinium-3-carboxylate
  • Synthesis method of 1-benzylpyridinium-3-carboxylate
  • Synthesis method of 1-benzylpyridinium-3-carboxylate

Examples

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Embodiment 1

[0021] Add 2.2kg of deionized water to a 5L four-neck flask, add 0.4kg of sodium hydroxide to dissolve, then slowly add 1.23kg of nicotinic acid at 40°C, continue to stir and dissolve, and gradually add 5gK 2 CO 3 , 5g trioctylmethyl ammonium chloride, 10g boric acid, the solution is neutral, and the temperature is raised to 80°C, and 1.26kg of benzyl chloride is started to be added dropwise, at a temperature of 80-90°C. After 4 hours, the reaction was completed, and the benzyl nicotinic acid onium salt was obtained as a light yellow transparent liquid.

Embodiment 2

[0024] Add 480g of deionized water to a 1L four-neck flask, add 80g of sodium hydroxide to dissolve, then slowly add 240g of nicotinic acid at 50°C, continue to stir and dissolve, and gradually add 1g of NaOH 2 CO 3 , 0.5g tetrabutylammonium bromide, 5g sodium bicarbonate, the solution is weakly alkaline, heat up to 70°C, start to add 200g of benzyl chloride dropwise, the dropwise addition temperature is 70-80°C, after the dropwise addition is completed, keep the temperature at this temperature After 2 hours, the reaction was completed, and the benzyl nicotinic acid onium salt was obtained as a yellow transparent liquid. The concentration is 90.17%.

Embodiment 3

[0026] Add 520g of deionized water to a 1L four-neck flask, add 80g of sodium hydroxide to dissolve, then slowly add 246g of nicotinic acid at 60°C, continue to stir and dissolve, and gradually add 3g of K 2 CO 3 , 1g of bromogeramine, 6g of sodium acetate, the solution is weakly alkaline, the temperature is raised to 80°C, and 240g of benzyl chloride is started to be added dropwise at a temperature of 80-95°C. After the addition is completed, the temperature is kept at this temperature for 1 hour. Benzylnicotinium salt, the appearance is a yellow transparent liquid. The concentration is 91.26%.

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Abstract

The invention discloses a synthesis method of 1-benzylpyridinium-3-carboxylate. The 1-benzylpyridinium-3-carboxylate is obtained by performing a chemical reaction on benzyl chloride, nicotinic acid and sodium hydroxide serving as raw materials; fully dissolving the sodium hydroxide in water; adding the nicotinic acid; stirring to fully dissolve; adding a composite catalyst and a buffer; dropwise adding the benzyl chloride and continuously reacting for 1-2 hours after the dropwise adding is finished so as to obtain the 1-benzylpyridinium-3-carboxylate, wherein the composite catalyst is a mixture of K2CO3 or Na2CO3 and quaternary ammonium salt; the quaternary ammonium salt is one or more of tetrabutylammonium bromide, benzyltriethylammonium chloride, dodecyl trimethyl ammonium chloride, methyl trioctyl ammonium chloride, hexadecyl trimethyl ammonium bromide and bromogeramine; the buffer is one of sodium bicarbonate, sodium carbonate, sodium acetate and boric acid. The synthesis method has the advantages of high yield, short reaction time, low cost, high product purity, no environment pollution during production and environmental friendliness.

Description

technical field [0001] The invention relates to a synthesis method of an alkaline cyanide-free zincate zinc plating additive, in particular to a synthesis method of benzyl nicotinic acid onium salt. Background technique [0002] At present, the most commonly used galvanizing processes are cyanide galvanizing, acid cyanide-free galvanizing and alkaline cyanide-free galvanizing. In view of the toxicity of cyanide and the increasingly stringent environmental protection requirements, cyanide galvanizing has been gradually eliminated. [0003] The acid cyanide-free galvanizing and alkaline cyanide-free galvanizing have their own advantages and disadvantages. The advantages of acid cyanide-free galvanizing are: high galvanizing efficiency, high brightness, no irritating smell, and its process can also be used for cast iron and high carbon steel. At the same time, it also has the disadvantages of poor throwing and deep plating ability, difficult passivation of the coating, and hi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/80C07D213/803
Inventor 付远波陈彰评宋文超杨威周世骏李玉梁明瑞涛高成
Owner 湖北吉和昌化工科技有限公司
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