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Preparation method of organic bismuth subgallate

A technology of organic acids and organic acid salts, which is applied in the field of fine chemical additives, can solve the problems of long production cycle, long production cycle, and high production cost, and achieve the effects of mild reaction conditions, high utilization of bismuth sources, and short production cycle

Inactive Publication Date: 2015-12-30
KITO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, because the price of bismuth is much higher than that of lead, mercury, tin, etc., and the synthesis process requirements of organic bismuth are high, and the yield is low, further causing the price of organic bismuth to be higher than that of catalysts such as lead, mercury, and tin. much higher price
[0003] The preparation method of bismuth organic acid in the prior art has the following defects: the synthesis process is relatively complicated, the synthesis conditions are relatively high, the production cost is high, and the product yield is low.
The method of preparing bismuth organic acid by using metal bismuth as bismuth source: first mix carboxylic acid or carboxylic acid anhydride with metal bismuth powder and hydrazine hydrate, heat to above 80°C, strictly control the temperature, and at the same time introduce air by bubbling method Oxidation reaction takes more than ten hours. This method has complex production process, difficult control of synthesis conditions, long production cycle, unsatisfactory product yield, and is not suitable for mass production.
The method of preparing bismuth organic acid by using bismuth oxide as a bismuth source: mainly using organic acid and bismuth oxide to react under high temperature for a long time to prepare bismuth organic acid. This method consumes a lot of energy, has a long production cycle and high production cost , the product color is darker, which is not conducive to the long-term development of the enterprise
The method for preparing bismuth organic acid using bismuth hydroxide as a bismuth source: directly using organic acid to react with bismuth hydroxide, this method has a low utilization rate of bismuth hydroxide, and has very strict requirements on the particle size of bismuth hydroxide, which is not suitable mass production

Method used

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Experimental program
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preparation example Construction

[0023] The preparation method of the bismuth organic acid of the present application comprises the steps of:

[0024] 1) Prepare organic acid salts from organic acids;

[0025] 2) mixing and stirring the prepared organic salt with bismuth nitrate pentahydrate and a cosolvent, blowing nitrogen gas, and heating to the reaction temperature for reaction;

[0026] 3) adding an organic solvent to extract the organic phase;

[0027] 4) Rinse with flushing water, filter, and distill to obtain bismuth organic acid.

[0028] In the method for preparing bismuth organic acid according to the present application, preferably, the organic acid is selected from one of isooctanoic acid, neodecanoic acid, naphthenic acid, lauric acid, stearic acid, and lauryl hydroxystearic acid. one or more; the co-solvent is selected from one or more of acetic acid, lactic acid, acetic anhydride, hydrochloric acid, nitric acid, sulfuric acid.

[0029] According to the preparation method of the bismuth orga...

Embodiment 1

[0036] Dissolve 24g of sodium hydroxide in 50g of water, then add 105g of neodecanoic acid to the reaction, then add 55g of bismuth nitrate pentahydrate and 27.5g of cosolvent acetic acid to it, stir evenly, ventilate nitrogen and heat up to 85°C, heat preservation reaction 5h, lower the temperature appropriately, add toluene, stand to separate layers, extract the organic phase, then wash the organic phase with water, filter it after washing, and then distill toluene and water under reduced pressure to finally obtain a relatively high viscosity distillate Yellow transparent liquid.

experiment example 2

[0038] Dissolve 24g of sodium hydroxide in 50g of water, then add 105g of neodecanoic acid to the reaction, then add 40g of bismuth nitrate pentahydrate and 20g of cosolvent acetic acid, stir evenly, ventilate nitrogen and heat up to 85°C, and keep the temperature for 5h , lower the temperature appropriately, add toluene, stand to separate layers, extract the organic phase, then wash the organic phase with water, filter it after washing, and then distill toluene and water under reduced pressure to finally obtain a higher viscosity light yellow Transparent liquid.

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PUM

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Abstract

The invention relates to a preparation method of organic bismuth subgallate. The preparation method comprises the following steps of preparing organic acid into organic acid salts; mixing and stirring the prepared organic acid salts with bismuth nitrate pentahydrate and a cosolvent; introducing nitrogen, and heating to a reaction temperature for reacting; adding an organic solvent, and extracting an organic phase; using washing water to wash, filtering and distilling to obtain the organic bismuth subgallate. According to the preparation method of the organic bismuth subgallate, disclosed by the invention, the organic solvent is added to purify and extract a product; washing to remove various water-soluble substances in the product; filtering to remove insoluble substances in the product; finally, performing reduced pressure distillation to remove the organic solvent and water in the product to finally obtain the bismuth subgallate with shallow color and better stability. The preparation method has the advantages of mild reaction conditions, low production cost, short production period, and high utilization rate of a bismuth source, and is suitable for large-batch production.

Description

technical field [0001] The invention belongs to the field of fine chemical additives, and relates to the preparation of organic bismuth catalysts, in particular to the preparation of organic acid bismuth catalysts. Background technique [0002] As a catalyst, bismuth organic acid is widely used as an accelerator for resin synthesis and a drier for paint. Due to its strong catalytic properties, environmental protection and non-toxicity, it is the best choice to replace toxic catalysts such as lead, mercury, and tin. However, because the price of bismuth is much higher than that of lead, mercury, tin, etc., and the synthesis process requirements of organic bismuth are high, and the yield is low, further causing the price of organic bismuth to be higher than that of catalysts such as lead, mercury, and tin. The price is much higher. [0003] The preparation method of bismuth organic acid in the prior art has the following defects: the synthesis process is relatively complicate...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/128C07C51/42
CPCC07C51/412C07C51/42C07C53/128
Inventor 王文蔡育涛陈能昌
Owner KITO CHEM CO LTD