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Method for phase transfer catalyzing synthesizing of 2-ethyl caproic acid stannous

A technology of phase transfer catalysis and stannous acid, applied in organic chemistry, carboxylate preparation, etc., can solve the problems of high reaction temperature, poor catalytic activity, high production cost, etc., achieve low reaction temperature, avoid oxidation and polymerization, and reduce viscosity small effect

Inactive Publication Date: 2015-07-08
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 certain problems: high reaction temperature (140-160°C), resulting in poor catalytic activity of the product and high production cost

Method used

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  • Method for phase transfer catalyzing synthesizing of 2-ethyl caproic acid stannous
  • Method for phase transfer catalyzing synthesizing of 2-ethyl caproic acid stannous

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The method for the synthesis of 2-ethylhexanoic acid stannous by phase transfer catalysis comprises the following steps:

[0018] (1) Add 192.5g of 2-ethylhexanoic acid, 89.7g of powdered stannous oxide, and 0.85g of 18-crown-6 into a 500mL flask equipped with a heating device, a stirring device, a condenser and a negative pressure port;

[0019] (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 45°C, start vacuuming, and the vacuum degree is less than 1013Pa. Increase the condensed water to continue to distill, continue to heat until the temperature reaches 85°C, control the temperature, maintain the temperature at 85±5°C, stop heating when there is no water drop in the condenser and the powdered stannous oxide in the flask completely disappears. , Obtain 270.2g pale yellow stannous 2-ethyl hexanoate.

[0020] The used 2-ethylhexanoic acid, stannous oxide, and 18-crow...

Embodiment 2

[0025] The method for the synthesis of 2-ethylhexanoic acid stannous by phase transfer catalysis comprises the following steps:

[0026] (1) Add 192.5g of 2-ethylhexanoic acid, 89.7g of powdered stannous oxide, and 0.85g of 18-crown-6 into a 500mL flask equipped with a heating device, a stirring device, a condenser and a negative pressure port;

[0027] (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 45°C, start vacuuming, and the vacuum degree is less than 1013Pa. Increase the condensed water to continue to distill, continue to heat until the temperature reaches 85°C, control the temperature, maintain the temperature at 85±5°C, stop heating when there is no water drop in the condenser and the powdered stannous oxide in the flask completely disappears. , Obtain 270g pale yellow stannous 2-ethyl hexanoate.

[0028] The used 2-ethylhexanoic acid, stannous oxide, and 18-crown-...

Embodiment 3

[0030] The method for the synthesis of 2-ethylhexanoic acid stannous by phase transfer catalysis comprises the following steps:

[0031] (1) Add 192.5g of 2-ethylhexanoic acid, 89.7g of powdered stannous oxide, and 0.35g of 18-crown-6 into a 500mL flask equipped with a heating device, a stirring device, a condenser and a negative pressure port;

[0032] (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 40°C, start vacuuming, and the vacuum degree is less than 1013Pa. Increase the condensed water to continue to distill, continue to heat until the temperature reaches 95°C, control the temperature, maintain the temperature at 90±5°C, stop heating when there is no water drop in the condenser and the powdered stannous oxide in the flask completely disappears. , Obtain 269g pale yellow stannous 2-ethyl hexanoate.

[0033] The used 2-ethylhexanoic acid, stannous oxide, and 18-crown-...

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Abstract

The invention discloses a method phase transfer catalyzing synthesizing of 2-ethyl caproic acid stannous, and belongs to the filed of organic synthesis. The method comprises the steps as follows: (1) adding 2-ethyl caproic acid, powdered stannous oxide and crown ether to a reactor with a condenser; (2) agitating and heating: heating the raw materials in the reactor in step (1) to reach 40 to 50 DEG C, starting to pump the vacuum, and distilling condensate water drop from the condenser, and continuously heating to reach 80 to 100 DEG C, and then controlling the temperature to at the temperature fluctuated not greater than 5 DEG C; stopping heating when no water strop is distilled from the condenser and the powdered stannous oxide in the reactor is completely removed, so as to obtain the 2-ethyl caproic acid stannous. According to the method disclosed by the invention, the 2-ethyl caproic acid and the powdered stannous oxide are reacted to obtain stannous octoate under the catalyzing of the crown ether; the reaction is carried out at low temperature; and the generation of wastewater can be avoided.

Description

technical field [0001] The invention relates to a method for synthesizing stannous 2-ethylhexanoate by phase transfer catalysis, belonging to the field of organic synthesis. Background technique [0002] Stannous 2-ethylhexanoate, also known as stannous octoate, is a light yellow transparent liquid or a yellow-brown paste, insoluble in water, soluble in petroleum ether, polyols, etc.; it is a basic catalyst for the production of polyurethane foam , Catalyst for room temperature curing silicone rubber, polyurethane rubber, and polyurethane coatings. It mainly promotes the reaction between isocyanate groups and active hydrogen such as hydroxyl groups and amine groups. The chemical properties are extremely unstable and easily oxidized. At present, stannous octoate is prepared by the saponification-metathesis method, and the problem with this method is that waste water is generated. [0003] Another production method of stannous octoate is: direct reaction with isooctanoic acid...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/128C07C51/41
Inventor 刘永军赵海争
Owner 沧州威达化工股份有限公司