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Method for preparing tributyl borate by utilizing reactant n-butyl alcohol as water-carrying agent

A technology for tributyl borate and n-butanol, which is applied in the field of preparing tributyl borate by organic synthesis, can solve the problems of high operation risk, high toxicity of water-carrying agent, difficult recovery and processing, etc., and achieves improved conversion rate and low cost , the effect of easy operation

Inactive Publication Date: 2012-11-07
SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the synthesis of tributyl borate is mainly obtained by adding boric acid and n-butanol as raw materials to esterify the water-carrying agent. The disadvantages are that the water-carrying agent is highly toxic, the operation is dangerous, and the system is complex and difficult to recycle.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 250ml round bottom flask with a water separator, 21g of boric acid and 136.5g of n-butanol were added. The mixture was placed in an oil bath and heated to 110°C to start the reflux reaction until no more water came out. The reactant was fractionated under reduced pressure with a 25cm fractionating column to collect the product at 130°C-136°C / 8.113KPa, the content of tributyl borate was 99.15%, and the yield was 85.9%.

Embodiment 2

[0021] In a 1000ml round bottom flask with a water separator, add boric acid 84g and n-butanol 588g. The mixture was placed on a heating mantle and heated to 112 °C to start the reflux reaction until no more water came out. The reactant was fractionated under reduced pressure with a 25cm fractionating column to collect the product at 130°C-136°C / 8.113KPa, the content of tributyl borate was 99.05%, and the yield was 85.5%.

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Abstract

The invention provides a method for preparing tributyl borate by utilizing a reactant n-butyl alcohol as a water-carrying agent. The method comprises the following preparation processes of: a: adding boric acid and the n-butyl alcohol which are taken as raw materials into a reactor; b: adding the n-butyl alcohol taken as the water-carrying agent into the reactor to react; in a reaction process, discharging water generated in the reaction out by a water distributor in time to obtain a rough product of the tributyl borate; and c: utilizing a fractional column to carry out decompression fraction to separate the tributyl borate, and recycling the n-butyl alcohol. The n-butyl alcohol disclosed by using the method is used as the raw material of esterification reaction and is also used as the water-carrying agent; the reaction temperature is increased so as to be good for carrying out the esterification reaction and the conversion rate of the reaction is improved; the defects that the toxin is great and the operation danger is great when benzene, toluene or carbon tetrachloride is used as the water-carrying agent can be overcome; the recycled n-butyl alcohol can be circularly utilized; and the tributyl borate with the content of being more than 99.0% can be obtained by utilizing the fractional column to carry out the decompression fraction.

Description

technical field [0001] The invention relates to a method for preparing tributyl borate by organic synthesis, in particular to a method for preparing tributyl borate by using the reactant n-butanol as a water-carrying agent. Background technique [0002] Tributyl borate is an intermediate for the preparation of borohydride compounds, used in the synthesis of lubricating oil additives, fire retardants, adhesion promoters, rubber additives, semiconductor boron diffusers and desiccants for anhydrous systems, and can also be used as flame retardants, It is used in automobile brake fluid and special surfactant, and has a wide range of applications. At present, the synthesis of tributyl borate is mainly obtained by adding boric acid and n-butanol as raw materials and adding water-carrying agent to esterify. The disadvantages are that the water-carrying agent is highly toxic, the operation is dangerous, and the system is complex and difficult to recycle. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C07F5/04
Inventor 梁嘉鸣
Owner SHENYANG INSTITUTE OF CHEMICAL TECHNOLOGY
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