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Method for synthesizing tributyl phosphate

A technology of tributyl phosphate and a synthesis method, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as increased burden, no promotion effect, etc., and achieves high yield Effect

Inactive Publication Date: 2011-05-04
洛阳市中达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method uses an excessive amount of butanol, which increases the burden on post-treatment; when sodium carbonate or sodium hydroxide is added to neutralize HCl, the esterification reaction has ended and does not promote the reaction.

Method used

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  • Method for synthesizing tributyl phosphate

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Experimental program
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Effect test

Embodiment 1

[0019] Add 280.0 g (3.4 mol) of sodium acetate and 230.0 g (3.1 mol) of butanol in sequence into a 1000 mL four-necked flask equipped with a mechanical stirrer, a thermometer, a condenser and a dropping funnel, stir to dissolve, and keep warm in an ice-water bath to 10 ℃, drop 153.0g (1mol) phosphorus oxychloride from the dropping funnel, control the feeding rate to keep the temperature stable at 10 ℃, finish adding within 15min, continue to insulate and stir for 60 minutes; remove the generated sodium chloride by filtration, Then atmospheric pressure distillation, collect the acetic acid cut of about 120 ℃; Reduce again to-0.98Mpa (gauge pressure), collect the cut of 170 ℃ to be tributyl phosphate, obtain 248.0g, yield is 93.2%, gas chromatography purity is 98.2%. The tributyl phosphate yield described in this patent all refers to the yield calculated with phosphorus oxychloride.

Embodiment 2

[0021] By the method for example 1, the charging capacity of sodium acetate is changed into 254g (3.1mol), and phosphorus oxychloride is added dropwise in 60min, then continues reaction 15min. Other methods remained unchanged, 241.1 g of the product was obtained, the yield was 90.6%, and the purity by gas chromatography was 98.3%.

Embodiment 3

[0023] By the method of example 1, the charging capacity of butanol is changed into 237.2g (3.2mol), and phosphorus oxychloride is added dropwise in 30min, then continues to react 45min, and other methods are unchanged, obtains product 248.5g, and yield is 93.4 %, the gas chromatography purity is 98.3%.

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Abstract

The invention discloses a method for synthesizing tributyl phosphate by carrying out direct esterification on butanol and phosphorus oxychloride. The method for synthesizing the tributyl phosphate is characterized by comprising the following steps: dissolving sodium acetate solution in the butanol to prepare solution; dropwise adding the phosphorus oxychloride to the solution for reaction at a temperature is 10-30 DEG C; continuously enabling the mixture to be subject to reaction for 15-60 minutes after finishing dropwise adding the phosphorus oxychloride; and distilling to obtain the target product of tributyl phosphate. Compared with the traditional method for synthesizing the tributyl phosphate, the method for synthesizing the tributyl phosphate provided by the invention has the advantages that vacuumization is omitted, other solvents are not used, the use amount of the butanol is close to the theoretical use amount, and the yield of the tributyl phosphate is high.

Description

technical field [0001] The invention relates to a phosphate synthesis technology, in particular to a synthesis method of tributyl phosphate. Background technique [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. [0003] In industry, tributyl phosphate is generally synthesized by direct esterification of butanol and phosphorus oxychloride. Since hydrogen chloride is generated during the reaction, in order to inhibit the further reaction of hydrogen chloride with butanol and phosphoric acid ester to form chlorobutane, it is usually necessary to control the reaction at a very low level. Temperature and higher vacuum, the consequence of high vacuum 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 张建国吕鸿雁
Owner 洛阳市中达化工有限公司
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