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Process for hydrogenation of a silicon tetrahalide and silicon to trihalosilane

a technology of trihalosilane and hydrogenation process, which is applied in the direction of halogenated silanes, inorganic chemistry, chemistry apparatus and processes, etc., can solve the problems of increasing capital cost and operating cost, increasing capital cost, and increasing capital cost, so as to improve heat integration, increase reaction rate, and yield the effect of trihalosilan

Inactive Publication Date: 2012-07-05
LORD STEPHEN MICHAEL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0008]Systems incorporating the invention provide higher yield of the trihalosilane, lower fabrication cost lower cost of operation, high consumption of feed silicon flexible size distribution requirements for the feed metallurgical grade silicon and a flexible operation.
[0010]In accordance with a preferred embodiment of the invention, an apparatus for hydrogenation of a silicon tetrahalide and silicon to trihalosilane comprises: a vessel with no internal flow distribution, one or more gas entries, one or more solids entries, one or more solids drains, one or more gas / solids exits and fresh surface generation by jet grinding. Also further disclosed is a process for choosing a set of operating conditions to take full advantage of the apparatus and an example of improved heat integration. This apparatus has the advantages of higher reaction rates, higher yields of trihalosilane and lower capital and operating costs by better heat integration with the remainder of the process.

Problems solved by technology

Delaying the mixing to the mixing plenum increases the capital cost and operating cost because it makes heat recovery from the hot effluent gases more difficult and causes operational problems.
The silicon tetrahalide frequently contains significant traces of the trihalosilane and dihalosilane which can decompose to silicon inside the tetrahalide heaters causing plugging.
Using two separate preheaters increases the capital cost compared to a single train and makes it more difficult to recover heat from the exhaust gas which increases the use of utilities.
The provision of a distribution means increases capital cost.
The lower yield of commercial reactors can be attributed to the design of the distribution means and selection of typical fluidized bed operating conditions which cause bypassing of the silicon by large bubbles of reacting gas which means some of the reacting gas has a very short residence time.
The comminution increases reaction rate and yield but the Bade method of using a ball mill makes it difficult and expensive to implement at the high pressure, 500 psig, and high temperature, 500° C., needed for this reaction.

Method used

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  • Process for hydrogenation of a silicon tetrahalide and silicon to trihalosilane
  • Process for hydrogenation of a silicon tetrahalide and silicon to trihalosilane
  • Process for hydrogenation of a silicon tetrahalide and silicon to trihalosilane

Examples

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example 1

[0030]The gas inlet composition is as in Table 1

[0031]ε is the voidage at Umb=0.4

[0032]g is the acceleration of gravity=980 m / s2

[0033]Dp is the diameter of the particle=To be calculated

[0034]ρp is the particle density=2.33 g / cc

[0035]ρf is the fluid density.=0.0218 g / cc

[0036]μf is the viscosity of the fluid=0.00024 poise

[0037]U is the max. superficial velocity=0.11 m / sec=Umb

Therefore the desired minimum average particle size=444 microns. Since MGS is quite angular this particle size should be adjusted by dividing by the sphericity which is typically about 0.86. This gives the average particle size, 516 microns as measured by sieve analysis. Further standard population balance calculations can be made to allow for the shrinkage of the particle due to reaction and the decrease in size due to attrition to arrive at the required minimum average particle size for the feed to the reactor. Once a reasonable estimate has been obtained for the correct particle size for the feed, a test may ...

example 2

[0038]A reactor 10 meters long was charged with a 7 m high bed using MGS of a nominal 750 micron size. The reactor was run for 120 hours under the conditions of Table 1 and batches of metallurgical grade silicon were added once per hour to maintain level. At the end of the run a sample of the MGS in the bed was taken from the bed and analyzed and the results are shown below.

TABLE 2Weight % of Particles in a sieve size rangeSieve sizeParticleMicronsWt % 0-500.03% 50-1000.24%100-1500.61%150-2000.96%200-2500.94%250-3002.44%300-3505.16%350-4003.85%400-4505.49%450-5007.53%500-55010.02% 600-60013.01% 650-65014.88% 650-70016.52% 700-75015.24% 750-8003.08%

The average particle size was calculated at 538 microns

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Abstract

A process of hydrogenation of a silicon tetrahalide and silicon to a trihalosilane comprising: providing a vessel with at least one inlet and one outlet with a plurality of silicon particles located in a bed inside the vessel and feeding a mixture of gases consisting primarily of a silicon tetrahalide and hydrogen. A calculational procedure is provided where the flow rate of the gases and the incoming size of the silicon particulates are chosen so that at least 90% of the volume of the bed is free of bubbles after allowance for decrease in particle size due to the reaction and attrition resulting in a higher yield of the trihalosilane.

Description

[0001]This is a Divisional of application Ser. No 12 / 291,115, filed Nov. 05, 2008, now U.S. Pat. No. ______, issued ______, 2012.BACKGROUND OF THE INVENTION[0002]This invention relates generally to the field of high purity silicon production and more specifically to an apparatus and process for hydrogenation of a silicon tetrahalide and silicon to trihalosilane.[0003]Trihalosilanes such as SiHCl3 and SiHBr3 were first made by the reaction of silicon with the respective hydrogen halide, HCl or HBr, at a temperature of approximately 350° C. and at approximately atmospheric pressure. Yields from this reaction are typically very high, the literature showing yields in excess of 90%, with the remainder being silicon tetrahalide. The trihalosilane most commonly used is trichlorosilane which is purified and decomposed to form very pure silicon. This decomposition reaction also forms the silicon tetrahalide which thus builds up in the process. Various measure have been taken to minimize the ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C01B33/107
CPCB01J8/1827C01B33/10773C01B33/1071B01J8/24
Inventor LORD, STEPHEN MICHAEL
Owner LORD STEPHEN MICHAEL
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