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Preparation method of diborane

A technology of diborane and boron trichloride, applied in the field of preparation of diborane, can solve the problems of long process and high cost, and achieve the effects of cost saving, raw material cost saving and low price

Active Publication Date: 2021-04-13
SHANDONG GUOBANG PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The above methods all use sodium borohydride and boron trichloride or boron trifluoride to react in a solvent to prepare diborane. In actual commercial applications, sodium borohydride uses the Schlesinger method, that is, sodium hydride and trimethyl borate are heated at high temperature. After the reaction, it is hydrolyzed, extracted and concentrated with isopropylamine, and sodium borohydride is a high-value product. The above methods all have the problems of long process and high cost

Method used

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  • Preparation method of diborane

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Embodiment 1

[0032] A preparation method for diborane, specifically comprising the following steps:

[0033] (1) Condensation reaction: Add 40g of sodium hydride to a 1000mL four-necked flask, pass nitrogen gas, use nitrogen to replace the air in the flask for 2 to 3 times, add 60g of tetrahydrofuran, stir, let stand for 1h, use nitrogen to dissolve tetrahydrofuran Press out the flask and repeat once. Take 200g of tetrahydrofuran, put it into the flask, slowly heat up the oil bath to 68°C, slowly add 109.12g of trimethyl borate dropwise, the dropwise addition is completed in 1.5h, keep it under full reflux for 5h, the sodium hydride solution turns from silvery white to off-white, and 125.93g is obtained Sodium trimethoxyborohydride, the yield is 99.12% based on sodium hydride.

[0034] (2) Metathesis reaction: control the temperature of the mixed solution of sodium trimethoxyborohydride tetrahydrofuran to 70°C, slowly add 384.48 g of 20% boron trichloride tetrahydrofuran solution dropwise...

Embodiment 2

[0038] A preparation method for diborane, specifically comprising the following steps:

[0039] (1) Condensation reaction: Add 40g of sodium hydride into a 1000mL four-neck flask, replace with nitrogen for 2 to 3 times, then slowly raise the temperature to 68°C, slowly add 109.12g of trimethyl borate dropwise, complete the dropwise addition in 1.5h, and keep warm under full reflux After 5 hours, the sodium hydride solution changed from silvery white to off-white to obtain 121.40 g of sodium trimethoxyborohydride, with a yield of 95.55% based on sodium hydride.

[0040] (2) Metathesis reaction: control the temperature of the mixed solution of sodium trimethoxyborohydride tetrahydrofuran to 70°C, slowly add 335.93 g of 20% boron trichloride tetrahydrofuran solution dropwise, and complete the dropwise addition in 1.5 hours, and keep it under total reflux for 7 hours to obtain diborane Crude. Use a three-stage ultra-low temperature vent condenser to cool, and the cooling temperat...

Embodiment 3

[0044] A preparation method for diborane, specifically comprising the following steps:

[0045] (1) Condensation reaction: Add 40g of sodium hydride to a 1000mL four-neck flask, replace with nitrogen 2 to 3 times, add 120g of tetrahydrofuran, stir, let stand for 1h, use nitrogen to press tetrahydrofuran out of the flask, and repeat once. Take 200g of tetrahydrofuran, put it into the flask, slowly heat up the oil bath to 68°C, slowly add 109.12g of trimethyl borate dropwise, the dropwise addition is completed in 1.5h, keep it under full reflux for 5h, the sodium hydride solution turns from silvery white to off-white, and 123.68g is obtained Sodium trimethoxyborohydride, the yield is 97.35% based on sodium hydride.

[0046] (2) Metathesis reaction: Control the temperature of the mixed solution of sodium trimethoxyborohydride tetrahydrofuran to 70°C, slowly add 342.25 g of 20% boron trichloride tetrahydrofuran solution dropwise, and complete the dropwise addition in 1.5 hours, an...

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Abstract

The invention provides a preparation method of diborane, and solves the technical problems of unreasonable preparation method, high raw material price, complex product purification operation, high cost, low yield and unsuitability for industrial production. The preparation method of diborane takes sodium hydride, trimethyl borate and boron trichloride as initial raw materials, and tetrahydrofuran as a reaction solvent, and carries out condensation reaction and a double decomposition reaction to obtain the diborane. The method can be widely applied to the technical field of diborane preparation.

Description

technical field [0001] The invention relates to the technical field of diborane preparation, in particular to a preparation method of diborane. Background technique [0002] Diborane (B2H6) is used as a dopant for gaseous impurity sources, ion implantation and boron-doped oxidation diffusion in the electronics industry. It is mainly used as a dopant in the production of P-type semiconductor chips, so it is widely used in semiconductor integration. Circuits, liquid crystal displays, semiconductor light-emitting devices and solar cells and other industries; because of its high-value energy, it can also be used as a high-energy fuel for rockets and missiles; due to its electron-deficient characteristics, it can produce a variety of networks with Lewis base Compounds, such as boron-tetrahydrofuran and various amine boranes, are used to prepare selective reducing agents commonly used in organic synthesis, and have a wide range of applications in the fields of organic synthesis, m...

Claims

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Application Information

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IPC IPC(8): C01B6/10
CPCC01B6/10
Inventor 廖仕学康卫兵李芳陆华文段良鹏
Owner SHANDONG GUOBANG PHARMA
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