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Method for synthesizing tributyl phosphate by sodium formate acid-binding method

A technology of tributyl phosphate and sodium formate, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Problems such as high alcohol consumption

Inactive Publication Date: 2011-03-30
JIANGXI SCI & TECH NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In industry, butanol and phosphorus oxychloride direct esterification method is generally used to synthesize tributyl phosphate. Since hydrogen chloride will be generated during the reaction process, in order to inhibit the further reaction of hydrogen chloride with butanol and phosphoric acid ester to generate chlorobutane, it is usually necessary to control Very low reaction temperature and high vacuum degree, and the consequence of high vacuum degree is to cause a large amount of volatilization of butanol, so that the unit consumption of butanol remains high, and the yield of tributyl phosphate is generally lower than 80%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Add 115.6g (1.7mol) of sodium formate and 115.0g (1.55mol) of butanol to a 500mL four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser and a dropping funnel, stir to dissolve them, and keep warm in an ice-water bath to 10 ℃, dropwise add 76.5g (0.5mol) phosphorus oxychloride from the dropping funnel, control the feeding rate to keep the temperature stable at about 10℃, after the dropwise addition, continue to insulate and stir for 20 minutes. Then it was changed into a distillation device, and first atmospheric distillation was carried out, and the fraction at about 101°C was collected as formic acid; then decompressed to -0.98Mpa (gauge pressure), and the fraction at about 170°C was collected as tributyl phosphate, and 125.0g was obtained. The yield was 94.0%, and the gas chromatography purity was 97.1%.

Embodiment 2

[0014] By the method of embodiment 1, the charging capacity of sodium formate is 105.4g (1.55mol), other steps are unchanged, obtains tributyl phosphate 122.8g, yield 92.3%, gas chromatography purity is 97.9%.

Embodiment 3

[0016] By the method of embodiment 1, the charging amount of butanol is 118.6g (1.6mol), other steps are unchanged, obtains tributyl phosphate 124.1g, yield 93.3%, gas chromatography purity is 98.2%.

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PUM

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Abstract

The invention discloses a method for synthesizing tributyl phosphate by a sodium formate aid-binding method. The method comprises the following steps of: dissolving sodium formate into butanol; adding phosphorus oxychloride dropwise into the solution at the temperature of between 5 and 15 DEG C, and then preserving the heat and reacting with stirring for 15 to 30 minutes; and then performing distillation: performing atmospheric distillation, collecting fraction at the temperature of between 100 and 105 DEG C to obtain formic acid, and then reducing pressure to -0.96 to -0.98Mpa, and collecting the fraction at the temperature of between 160 and 180 DEG C to obtain the tributyl phosphate. In the method for synthesizing the tributyl phosphate by the sodium formate acid-binding method, the sodium formate is weak acid strong alkali salt and has a certain alkaline and is reacted with hydrogen chloride to form sodium chloride and the formic acid, and the formic acid subjected to separation can be reacted with sodium hydroxide to form the sodium formate for cycling; and compared with the conventional method, the method has the advantages that vacuumization is not needed, the using amount of the butanol is close to a theoretical amount, the yield of the tributyl phosphate is high (the yield is over 92.0 percent), and the like.

Description

technical field [0001] The invention relates to a method for synthesizing tributyl phosphate by sodium formate acid-binding method. technical background [0002] Tributyl phosphate can be used as extractant for rare metals, solvent, plasticizer for chlorinated rubber and polyvinyl chloride, and industrial defoamer. It is an important chemical product. In industry, butanol and phosphorus oxychloride direct esterification method is generally used to synthesize tributyl phosphate. Since hydrogen chloride will be generated during the reaction process, in order to inhibit the further reaction of hydrogen chloride with butanol and phosphoric acid ester to generate chlorobutane, it is usually necessary to control Very low reaction temperature and high vacuum degree, and the consequence of high vacuum degree is to cause a large amount of volatilization of butanol, so that the unit consumption of butanol remains high, and the yield of tributyl phosphate is generally lower than 80% ....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11
Inventor 王晓季
Owner JIANGXI SCI & TECH NORMAL UNIV
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