Preparation and purification of diborane

A technology of diborane and potassium borohydride, applied in the field of preparation and purification of diborane, can solve problems such as unfavorable lithium borohydride

Inactive Publication Date: 2001-08-22
HONEYWELL INTPROP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

From thermodynamic considerations, the reaction of lithium borohydride with boron trifluoride is more favorable than with sodiu

Method used

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  • Preparation and purification of diborane
  • Preparation and purification of diborane
  • Preparation and purification of diborane

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0026] Fifty grams of potassium borohydride was wrapped in a glove bag under helium and placed in a cylindrical stainless steel reactor R (volume 195 cc) with flanges at each end. The reactor is closed by fitting a flange with a closed valve. The reactor assembly is placed into a jacketed empty cylinder-like vessel. Purifier P is a stainless steel bubbler (volume 972cc) fitted with inclined tubes, with inlet and outlet valves with VCR components welded on top. The purifier is filled more than half full with potassium borohydride pellets through the fill port. Filling of the purifier is performed in a glove bag with helium flow. The fill port is closed with a 1 / 2" VCR cap. Figure 1 shows the reactor and purifier connections. All parts of the apparatus including the reactor and purifier are to be evacuated. To dry the potassium borohydride, heat the purify slightly while evacuating P. The jacketed vessel surrounding the reactor was filled with dry ice. The surrounding of the ...

example 2

[0028] The procedure of Example 1 was repeated except that the purifier P with potassium borohydride was kept at room temperature. Samples were collected through the purifier up to a pressure of 53 Torr for IR scanning. The spectrum shows only a small amount of diborane and no BF3. However, at a pressure of 14 Torr, a sample containing diborane and some boron trifluoride was collected through bypass line B and through purifier P; the spectrum of this sample was similar to Fig. 2b. These results indicate that the scrubber removes BF3 completely at room temperature, but diborane has some differences. Example 3

example 3

[0029] The procedure of Example 1 was repeated except that the clarifier was filled with soda lime (a mixture of sodium hydroxide, calcium oxide, and calcium hydroxide). Cool the reactor and purifier to dry ice temperature. Samples were collected up to a pressure of 51 Torr from the reactor and passed through the purifier, and samples were collected up to a pressure of 19 Torr bypassing the purifier. Comparing the IR scans of these samples revealed that the scrubber was able to remove boron trifluoride from the diborane / boron trifluoride mixture. However, an imbalance in the conversion of some diborane to noncondensable hydrogen with soda lime was observed. Comparative Example 4

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Abstract

BF3, CO2 or both are removed from a mixture containing these gases with B2H6 by contacting the mixture with an inorganic hydroxide such as LiOH. B2H6 is synthesized by contacting BF3 with KBH4.

Description

technical field [0001] The present invention relates to the preparation and purification of diborane. technical background [0002] Diborane (B 2 h 6 ) is a flammable gas used in semiconductors as a p-type dopant and is also used in the boro-phosphate-silicate glass forming process. Diborane forms a variety of complexes with Lewis bases, such as boron-tetrahydrofuran, dimethyl boron sulfide, and various amine boranes. These compounds are widely used as selective reducing agents in pharmaceutical synthesis, fine organic chemicals, and electroless metal plating baths. [0003] At room temperature, diborane slowly decomposes to diborane and its physical state changes from gas to solid, causing process variability and equipment failure. To reduce decomposition, diborane is sometimes delivered as an enveloped gas mixture, or at cryogenic temperatures such as dry ice. Another solution to the decomposition problem is to utilize the point-of-use production of diborane. However...

Claims

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Application Information

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IPC IPC(8): C01B6/10C01B6/34C01B9/08C01B33/04C01B35/02
CPCY02C10/08C01B9/08C01B6/10C01B35/02C01B6/34
Inventor D·S·拉约里尔
Owner HONEYWELL INTPROP
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