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Synthesis method of tributyl borate

A technique for the synthesis of tributyl borate and its synthesis method, which is applied in the field of synthesis of tributyl borate, can solve the problems of long hours of operation for water removal and recovery of n-butanol, easy occurrence of mono-substitution and di-substitution products, and influence on product purity, etc. Achieve the effects of avoiding water generation and water removal problems, less components, and reducing operating time

Pending Publication Date: 2022-05-13
BEIJING GREENCHEM TECH
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  • Claims
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Problems solved by technology

[0005] However, the method for preparing tributyl borate with boric acid and n-butanol in the prior art also has some disadvantages: it needs to consume a large amount of butanol with water, resulting in long working hours and large energy consumption for subsequent n-butanol dehydration and recovery operations; Longer, generally takes 20 to 26 hours to complete a cycle; and water is generated during the reaction process, if the water is not removed in time or not completely, it will lead to incomplete reaction, prone to single substitution and secondary substitution products, affecting the product purity

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  • Synthesis method of tributyl borate
  • Synthesis method of tributyl borate
  • Synthesis method of tributyl borate

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preparation example Construction

[0026] The invention provides a synthetic method of tributyl borate, which is suitable for industrial production, comprising: under the condition of acid catalysis, trimethyl borate shown in formula (I) undergoes transesterification reaction with butanol to obtain formula (II ) shown tributyl borate. Reaction formula of the present invention is as follows:

[0027]

[0028] Reaction mechanism of the present invention is as follows:

[0029]

[0030] An oxygen atom on the trimethyl borate is combined with a hydrogen ion to form an oxonium ion, and then the butanol has a nucleophilic attack on the boron atom, and at the same time, a methanol molecule is lost, and the substitution reaction of the butoxy group to the methoxy group is completed. In the same way, the other two methoxyl groups are replaced by butoxyl groups accordingly, finally obtaining tributyl borate.

[0031] The system after the reaction in the present invention is simple, and the components are only tri...

Embodiment 1

[0043]Under the protection of nitrogen, 615 g of n-butanol and 10 g of p-toluenesulfonic acid were added to a 1 L four-necked flask, the temperature was raised to 65° C., and 200 g of trimethyl borate was slowly added. After the addition, keep warm at 65°C for 3.5 hours, take a sample and send the gas phase, the conversion of trimethyl borate to tributyl borate is complete, and the reaction is complete. 400.0 g of tributyl borate was obtained by rectification at a controlled temperature of 40-55°C and a pressure of -0.1--0.08 mpa, with a yield of 92.3% and a GC purity of 99.95%. And recover n-butanol through rectification, and the recovered n-butanol is directly applied to the next reaction. figure 1 It is the nuclear magnetic spectrum of the tributyl borate prepared by embodiment 1.

Embodiment 2

[0045] Under nitrogen protection, 738 g of n-butanol (partially recovered from Example 1) and 10 g of p-toluenesulfonic acid were added to a 1 L four-necked flask, and the temperature was raised to 70° C., and 200 g of trimethyl borate was slowly added. After the addition, keep warm at 70°C for 3.5 hours, take a sample and send the gas phase, the conversion of trimethyl borate to tributyl borate is complete, and the reaction is complete. Control the temperature at 40-55°C and pressure -0.1--0.08mpa to obtain 400.9g of tributyl borate through rectification, with a yield of 92.5% and a GC purity of 99.87%. And recover n-butanol through rectification, and the recovered n-butanol is directly applied to the next reaction.

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Abstract

The invention relates to a synthesis method of tributyl borate, which is prepared by carrying out transesterification on trimethyl borate serving as an initial raw material and butanol under the catalysis of acid. No water is generated in the reaction process, water removal is not needed, and the problems of long time consumption, high energy consumption and the like in subsequent butanol recovery and water removal in the prior art are solved. According to the method, only a slightly excessive amount of butanol is used, a large amount of butanol does not need to be consumed as a water-carrying agent, the recycled butanol can be directly used for the next reaction, water removal is not needed, the operation time is greatly shortened, and the energy consumption is reduced. After the reaction is completed, the system is simple, the components are few, a high-purity and high-yield product can be obtained through one-time continuous rectification by using simple rectification equipment, the process operation is simplified, the production period is greatly shortened, and the method is particularly suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to a synthesis method of tributyl borate, which belongs to the technical field of organic synthesis. Background technique [0002] Tributyl borate is a colorless and clear liquid, which can be used to prepare boron hydride intermediates, semiconductor boron diffusion sources, fire retardants, adhesives, and dehydration desiccants for anhydrous systems. [0003] The current production method of tributyl borate is usually using boric acid and n-butanol as starting raw materials. After the reaction is completed, the excess n-butanol is evaporated by carrying water through butanol, and finally the tributyl borate is obtained by distillation under reduced pressure. For example, the journal paper "Synthesis of Tributyl Borate" published in "Chemical Industry and Engineering" publicly reported that tributyl borate was synthesized by using n-butanol and boric acid as raw materials by microwave radiation, and investigated catalysts, water-...

Claims

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Application Information

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IPC IPC(8): C07F5/04
CPCC07F5/04
Inventor 宫宁瑞
Owner BEIJING GREENCHEM TECH
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