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Synthetic method of bismuth isocaprylate

A technology of bismuth isooctanoate and a synthesis method, which is applied in chemical instruments and methods, carboxylate preparation, carboxylate preparation, etc., can solve the problems of high reaction temperature, poor catalytic activity, high production cost, etc., and achieve the reduction of reaction temperature, Good catalytic activity, the effect of improving the reaction yield

Inactive Publication Date: 2016-11-16
沧州威达化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This route does not produce "three wastes", but there are also certain problems: the reaction temperature is as high as 160 ° C to 180 ° C, resulting in poor catalytic activity of the product and high production costs

Method used

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  • Synthetic method of bismuth isocaprylate
  • Synthetic method of bismuth isocaprylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A kind of synthetic method of bismuth isooctanoate, comprises the following steps:

[0025] (1) Add 185.8g of isooctanoic acid, 100g of powdered bismuth oxide, and 0.2g of catalyst into a 500ml flask equipped with heating device, stirring device, condenser and negative pressure port;

[0026] (2) Turn on the heating and stirring device, and the stirring speed is greater than 130rpm. When the raw material in the flask in step (1) is heated to 80°C, start vacuuming. Increase the condensed water to continue to distill, continue heating until the temperature reaches 115°C, maintain the temperature at 110°C~120°C, stop heating when there is no water droplet distilling out in the condenser and the powdered bismuth oxide in the flask completely disappears, the reaction is over, and 274g Pale yellow bismuth isooctanoate liquid.

[0027] The used isooctanoic acid, bismuth oxide and catalyst used in this embodiment are all industrial products with a purity greater than 99%.

[...

Embodiment 2

[0034] A kind of synthetic method of bismuth isooctanoate, comprises the following steps:

[0035] (1) Add 185.8g of isooctanoic acid, 100g of powdered bismuth oxide, and 0.2g of catalyst into a 500ml flask equipped with heating device, stirring device, condenser and negative pressure port;

[0036] (2) Turn on the heating and stirring device, and the stirring speed is greater than 130rpm. When the raw material in the flask in step (1) is heated to 80°C, start vacuuming. Continue to distill out condensed water as the temperature rises, continue heating until the temperature reaches 115°C, maintain the temperature at 110°C to 120°C, stop heating when no water droplet distills out in the condenser and the powdered bismuth oxide in the flask completely disappears, and the reaction ends to obtain 274.2 g Pale yellow bismuth isooctanoate liquid.

[0037] The used isooctanoic acid, bismuth oxide and catalyst used in this embodiment are all industrial products with a purity greater ...

Embodiment 3-9

[0039] The synthetic method of the bismuth isooctanoate of embodiment 3-9 is the same as embodiment 2, and the quality of the bismuth isooctanoate product of gained is as follows.

[0040] Table 2

[0041] Example

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Abstract

The invention relates to the technical field of organic synthesis, in particular to the technical field of synthesis of organic bismuth compounds, and particularly discloses a synthetic method of bismuth isocaprylate. The synthetic method is characterized in that the bismuth isocaprylate is generated by enabling an isocaprylic acid to react with powdery bismuth oxide under the action of a catalyst, and the catalyst is a composite solid superacid SO4<2-> / ZrO2-TiO2-Fe203, wherein a mass ratio of Fe, Ti and Zr is 2:3:1. According to the synthetic method disclosed by the invention, the synthesis reaction temperature is low, a reaction process is kept in negative pressure, a reaction product is condensed by water and is distilled out, economization and environment protection are realized, and the generated bismuth isocaprylate has good catalytic activity in polyurethane synthesis.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to the technical field of synthesis of organic bismuth compounds. Background technique [0002] Bismuth isooctanoate is a light yellow liquid, insoluble in water, soluble in petroleum ether, polyols, etc. It is an environmentally friendly polyurethane catalyst, used in the catalytic synthesis of polyurethane resins, adhesives, coatings, elastomers, etc., mainly for isocyanate groups The reaction with active hydrogen such as hydroxyl group and amine group has a strong promoting effect. At present, bismuth isooctanoate is prepared by the saponification-metathesis method, and the problem with this method is that waste water is produced. [0003] Another production method of bismuth isooctanoate is: use isooctanoic acid and bismuth oxide to react directly, and after evaporating a small amount of water, the finished product is obtained. This route does not produce "three wast...

Claims

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Application Information

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IPC IPC(8): C07C51/41C07C53/128B01J27/053
CPCB01J27/053C07C51/412C07C53/128
Inventor 王彤陈冬旭陈凌霞马力马越林马铁
Owner 沧州威达化工股份有限公司