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Method for preparing stannous octoate by pressurizing

A technology of stannous octoate and isooctanoic acid, applied in the directions of carboxylate preparation, carboxylate preparation, chemical instruments and methods, etc., can solve the problems of difficult large-scale application, high production cost, high solution temperature, and achieve good product quality , The effect of reducing production cost and short process

Active Publication Date: 2019-10-15
云南锡业研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem that exists is that a small amount of spongy tin is precipitated at the cathode in the electrolysis process, which leads to a low direct yield of tin (about 89%), and the voltage of the electrolytic cell reaches more than 17V. high
This method is non-aqueous solution synthesis, and the product has high purity, but there are problems such as the regeneration of triethylamine and the recovery and utilization of methanol, and the preparation of anhydrous stannous chloride, etc., the cost is high, and it is difficult to apply on a large scale

Method used

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  • Method for preparing stannous octoate by pressurizing
  • Method for preparing stannous octoate by pressurizing
  • Method for preparing stannous octoate by pressurizing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The method for preparing stannous octoate under pressure, in a 3L autoclave, add 1.4L of water, then add 660g of liquid isooctanoic acid, start stirring and then add 500g of tin flower, the liquid-solid mass ratio is 4:1. Cover the autoclave, heat and control the reaction pressure to 1.0MPa (the reaction pressure is the pressure of water vapor pressure and the hydrogen generated by the reaction), the reaction temperature is 180±5°C, and the reaction time is 6 hours. After the reaction, three layers of substances appear , the lowermost layer is solid stannous octoate (intermediate product), the middle layer is water, and the uppermost layer is unreacted isooctanoic acid. The liquid and solid are separated, and the solution is settled again to release the intermediate stannous octoate in the lower layer. The aqueous solution used in the closed reaction is only the carrier, and the residual acid and the aqueous solution are added with isooctanoic acid and then returned to ...

Embodiment 2

[0027] Pressurize the method for preparing stannous octoate, in 3L autoclave, add 1.4L water, add 440g isooctanoic acid again, open and stir and add 300g tin flower again, liquid-solid mass ratio is 6:1, autoclave capping, heating and Control the reaction pressure to 1.2MPa, the reaction temperature is 155±5°C, and the reaction time is 5 hours. After the reaction, the liquid and solid are separated, and the solution is settled again. Then return to the autoclave and continue to pressurize to prepare stannous octoate.

[0028] Add water and wash the stannous octoate intermediate product, and the supernatant is taken away, and the stannous octoate after washing is added in the distillation still to remove moisture, obtains 640g stannous octoate product, and product reaches following product quality standard.

[0029]

Embodiment 3

[0031] The method for preparing stannous octoate under pressure, in a 3L autoclave, add 1.8L water, then add 220g isooctanoic acid, start stirring and then add 200g tin powder, the liquid-solid mass ratio is 10:1, the autoclave is covered, heated and Control the reaction pressure to 1.5MPa, the reaction temperature is 200±5°C, and the reaction time is 4 hours. After the reaction, the liquid and solid are separated, and the solution is settled again. The intermediate product of stannous octoate is released from the lower layer. Then return to the autoclave and continue to pressurize to prepare stannous octoate.

[0032] Add water and wash the stannous octoate intermediate product, and the supernatant is taken away, and the stannous octoate after washing is added in the distillation still to remove moisture, obtains the 300g stannous octoate product, and the product reaches the following product quality standards.

[0033]

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PUM

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Abstract

The invention discloses a method for preparing stannous octoate by pressurizing. The method comprises the following steps: feeding isocaprylic acid, purity tin and water into a closed container according to a proportion, wherein the liquid-solid mass ratio of a solution to the purity tin is (4 to 10) to 1, and the amount of the isocaprylic acid is 110 percent of the theoretical quantity; subsequently, heating, and carrying out closed reaction on the isocaprylic acid and the purity tin at the pressure of greater than or equal to 1.0 MPa and the reaction temperature of greater than or equal to 150 DEG C for greater than or equal to 4 hours to synthesize the stannous octoate at a step, wherein three layers of substances are produced after reaction, the lowermost layer is solid stannous octoate, the middle layer is water and the uppermost layer is unreacted isocaprylic acid; carrying out solid-liquid separation, and taking out the stannous octoate at the lowermost layer. The method disclosed by the invention has the advantages of short process flow, low production cost, energy conservation and environmental protection; in addition, a final product is ensured to have high purity and good product quality.

Description

technical field [0001] The invention relates to the technical fields of hydrometallurgy and chemical industry, in particular to a preparation method of stannous octoate. Background technique [0002] The chemical name of stannous octoate is stannous 2-ethylhexanoate, which is a chemical product of tin 。 Because stannous octoate is easily hydrolyzed in both acidic and alkaline aqueous solutions, the stable pH value range is small, and it is easily oxidized and decomposed by oxygen in the air and other oxidants, and its preparation is relatively difficult. There are two ways to achieve large-scale production: saponification synthesis and electrolysis. [0003] The saponification synthesis method is to firstly react isooctanoic acid with sodium hydroxide to obtain sodium octanoate, then add stannous chloride solution to react with sodium octanoate to obtain stannous octanoate, or mix isooctanoic acid with stannous chloride solution, and then add hydrogen Sodium oxide solution...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C53/126
CPCC07C51/418C07C51/412C07C53/126
Inventor 苏瑞春黄迎红张雄林杨习文
Owner 云南锡业研究院有限公司
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