CN101723374A - Chlorosilane vapourizing mixed process and device - Google Patents

Chlorosilane vapourizing mixed process and device Download PDF

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Publication number
CN101723374A
CN101723374A CN200910310611A CN200910310611A CN101723374A CN 101723374 A CN101723374 A CN 101723374A CN 200910310611 A CN200910310611 A CN 200910310611A CN 200910310611 A CN200910310611 A CN 200910310611A CN 101723374 A CN101723374 A CN 101723374A
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CN
China
Prior art keywords
chlorosilane
hydrogen
vapourizing
interchanger
transfer lime
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
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CN200910310611A
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Chinese (zh)
Inventor
唐前正
张新
赵新征
卢涛
彭卡
李品贤
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LESHAN LEDIAN TIANWEI SILICAS CO Ltd
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LESHAN LEDIAN TIANWEI SILICAS CO Ltd
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Priority to CN200910310611A priority Critical patent/CN101723374A/en
Publication of CN101723374A publication Critical patent/CN101723374A/en
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Abstract

The invention discloses a chlorosilane vapourizing mixed process and a chlorosilane vapourizing mixed device which can improve the proportional control accuracy of hydrogen and chlorosilane in a chlorosilane vapourizing process. The chlorosilane vapourizing mixed device comprises a heat exchanger; a chlorosilane delivery pipe and a hydrogen delivery pipe are communicated with the tube pass/shell pass of the heat exchanger; the chlorosilane delivery pipe and the hydrogen delivery pipe are provided with a flow meter and a flow regulating valve respectively; and accordingly, the tube pass/shell pass of the heat exchanger is communicated with a heat supply system. The position in the heat exchanger corresponding to a joint of the chlorosilane delivery pipe and the heat exchanger is provided with a shunt which keeps a gap with the joint. The chlorosilane vapourizing mixed process comprises the following steps: metering the hydrogen and the chlorosilane respectively, and performing mixed vaporization in the heat exchanger to realize the complete vaporization of the gas mixture of the hydrogen and the chlorosilane and the proportional accuracy control of the hydrogen and the chlorosilane. The mixed process contributes to avoiding the waste of raw materials, improving and stabilizing the quality of polysilicon products, and realizing automation control.

Description

Chlorosilane vapourizing mixed process and device
Technical field
The present invention relates to chlorosilane and hydrogen hybrid technique and the device used in a kind of production of polysilicon.
Background technology
In production of polysilicon, the basic raw material of producing polysilicon is the chlorosilane and the hydrogen of rectification and purification, and chlorosilane and hydrogen need will be by a certain percentage the chlorosilane of gas phase to be mixed with hydrogen before entering reduction furnace, and this process is called chlorosilane vapourizing.
In traditional production of polysilicon technology, chlorosilane vapourizing carries out in bubbler and separator, its mixing process is: the chlorosilane that has certain liquid level in bubbler, in bubbler, feed hydrogen, make hydrogen carry out bubbling and vaporization mixing to chlorosilane, by separator the liquid chlorosilane in the gas is separated, and then send in the reduction furnace by the gas phase mixture that outlet conduit will be vaporized and mix.In the process of chlorosilane vapourizing, temperature by the chlorosilane of control in the bubbler and the pressure in the bubbler are controlled the ratio of hydrogen and chlorosilane in the gas phase mixture, control the inlet amount of reduction furnace by the flow of controlling gas phase mixture.
There is following shortcoming in this traditional vapourizing unit:
1, there is very mistake in the ratio control of hydrogen and chlorosilane, and the big back of error has a significant impact the quality of production of polysilicon;
2, in bubbler, chlorosilane is carried out the shortcoming that bubbling exists chlorosilane not vaporize fully by hydrogen;
3, the flow measurement to gas phase mixture is inaccurate, and flow is on the low side will to reduce the speed of growth of polycrystalline silicon rod, and flow is higher then to waste raw material.
Interchanger such as shell and tube evaporator are widely used in chemical industry, and wherein shell and tube heat exchanger often is provided with splitter in order to reach the purpose of uniform heat exchange in end socket, make each root tubulation that enters of the homogeneous media that enters tube side, with shell side medium heat-shift.
Summary of the invention
In order to overcome the big deficiency of ratio control error of hydrogen and chlorosilane in the existing chlorosilane vapourizing device, technical problem to be solved by this invention provides a kind of chlorosilane vapourizing mixed process and device that can improve hydrogen and chlorosilane ratio control precision in the chlorosilane vapourizing process.
The technical solution adopted for the present invention to solve the technical problems is: the chlorosilane vapourizing mixing device, comprise interchanger, chlorosilane transfer lime, hydrogen delivery tube are communicated with the tube side/shell side of this interchanger, all respectively be provided with under meter and flow control valve on chlorosilane transfer lime, the hydrogen delivery tube, correspondingly, the shell side/tube side of this interchanger is communicated with heat supply system.
Be provided with the splitter that has kept the gap with described Link Port corresponding to chlorosilane transfer lime and interchanger Link Port position in the described interchanger.
Described interchanger is a shell and tube evaporator, and chlorosilane transfer lime, hydrogen delivery tube are communicated with the tube side of this interchanger.
Described heat supply system is the steam cycle supply system.
Described interchanger is provided with the relief valve connection that is communicated with chlorosilane transfer lime, hydrogen delivery tube.
Described under meter adopts mass flowmeter.
The valve opening of described flow control valve is controlled by under meter.
The under meter interlock control that is provided with under meter that is provided with on the described chlorosilane transfer lime and the hydrogen delivery tube.
Chlorosilane vapourizing mixed process, the proportioning of regulating chlorosilane and hydrogen is earlier carried out the vaporization of the two again and is mixed.
The invention has the beneficial effects as follows: gasiform hydrogen and liquid chlorosilane can be controlled its flow by under meter and variable valve very easily, so be easy to control the ratio of hydrogen and chlorosilane, finished metering and formed proportioning before advancing vaporizer, the proportioning of this moment is very accurate, and operator are easy to operate; Utilize the interchanger heating that chlorosilane and hydrogen mixed gas can be vaporized fully, can bring up to comparatively high temps entering the stokehold, help the growth of polysilicon, avoid causing measuring inaccurate possibility because of in fact chlorosilane and hydrogen mixed gas in the incomplete vaporization exist two kinds of components, the material quantity that enters reduction furnace can accurately be controlled, avoid wastage of material, and helped realizing automatization control.
Description of drawings
Fig. 1 is the synoptic diagram of apparatus of the present invention.
Be labeled as 1-first Link Port, 2-second Link Port among the figure, the 3-mixed gas outlet, 4-relief valve connection, 5-splitter, the import of 6-steam cycle supply system, the outlet of 7-steam cycle supply system, 8-interchanger, 9-under meter, the 10-flow control valve, 11-chlorosilane transfer lime, 12-hydrogen delivery tube, 13-flow-control module.
Embodiment
The present invention is further described below in conjunction with drawings and Examples.
As shown in Figure 1, chlorosilane vapourizing mixing device of the present invention, comprise interchanger 8, chlorosilane transfer lime 11, hydrogen delivery tube 12 are communicated with the tube side/shell side of this interchanger 8, all respectively be provided with under meter 9 and flow control valve 10 on chlorosilane transfer lime 11, the hydrogen delivery tube 12, correspondingly, the shell side/tube side of this interchanger 8 is communicated with heat supply system.Chlorosilane transfer lime 11, hydrogen delivery tube 12 are communicated with the tube side/shell side of this interchanger 8, that is: or chlorosilane transfer lime 11, hydrogen delivery tube 12 is communicated with the tube side of this interchanger 8 simultaneously, heat supply system is communicated with the shell side of this interchanger 8 at this moment; Chlorosilane transfer lime 11, hydrogen delivery tube 12 are communicated with the shell side of this interchanger 8 simultaneously, and this moment, heat supply system was communicated with the tube side of this interchanger 8.
In this device, all respectively be provided with under meter 9 and flow control valve 10 on chlorosilane transfer lime 11, the hydrogen delivery tube 12, can realize vaporizing and mix preceding metering respectively, to realize that proportioning is regulated accurately; Chlorosilane transfer lime 11, hydrogen delivery tube 12 are communicated with the tube side/shell side of interchanger 8, enter interchanger 8 after, chlorosilane and hydrogen have realized that vaporization mixes.The present invention is by measuring mixing vaporization in interchanger 8 more earlier respectively with chlorosilane and hydrogen, realized the vaporization fully of chlorosilane and hydrogen mixed gas and the accurate control of chlorosilane and hydrogen ratio are helped avoiding wastage of material and raising and stable polysilicon product quality.
For thorough mixing chlorosilane and hydrogen, preferably in described interchanger 8, be provided with the splitter 5 that has kept the gap with described Link Port corresponding to chlorosilane transfer lime and interchanger Link Port 1 position, make rapidly vaporization and mix of liquid chlorosilane with hydrogen.
Consider that chlorosilane, hydrogen comparatively clean, less scaling, and consider to save cost, preferred described interchanger 8 is a shell and tube evaporator, chlorosilane transfer lime 11, hydrogen delivery tube 12 are communicated with the tube side of this interchanger.
Consider that the temperature requirement to chlorosilane and hydrogen mixed gas is not high in the whole technology, described heat supply system is preferably the steam cycle supply system, to save cost.
Consider security needs, for preventing superpressure, described interchanger 8 is provided with the relief valve connection 4 that is communicated with chlorosilane transfer lime 11, hydrogen delivery tube 12.
For understanding the material quantity that enters the vaporization mixing device intuitively, described under meter 9 should adopt mass flowmeter.
For ease of realizing control automatically and conveniently carry out the technology adjustment that the valve opening of described flow control valve 10 is by under meter 9 controls.For example, the valve opening of flow control valve 10 makes the gas that enters interchanger 8 can become the fixed proportioning by the demonstration Numerical Control of mass flowmeter 9.This proportioning generally adopts a mole proportioning.
Carry out the technology adjustment for further facilitating, the under meter 9 interlock controls that are provided with under meter 9 that is provided with on the described chlorosilane transfer lime 11 and the hydrogen delivery tube 12.Promptly the under meter 9 that is provided with on the under meter 9 that is provided with on the chlorosilane transfer lime 11 and the hydrogen delivery tube 12 is carried out ratio control, after utilizing Controlling System that the under meter 9 on transfer lime is wherein adjusted, under meter 9 on another transfer lime can be adjusted according to the proportioning ratio of predetermined chlorosilane and hydrogen in the flow-control module 13 immediately automatically, thereby reduce manually to adjust respectively the regulating error of two under meters 9, and synchronism is better, control more accurate, in addition, when process reform, can directly revise the proportioning ratio of flow-control module 13 interior predetermined chlorosilanes and hydrogen, realize proportioning adjustment chlorosilane and hydrogen.Flow-control module 13 can adopt existing automatic control technology realizations such as PLC controller.
As shown in Figure 1, chlorosilane vapourizing mixed process of the present invention, regulate the proportioning of chlorosilane and hydrogen earlier, carrying out the vaporization of the two again mixes, the proportioning of regulating chlorosilane and hydrogen is to realize by adjusting in the chlorosilane vapourizing mixing device of the present invention flow control valve 10 on chlorosilane transfer lime 11, the hydrogen delivery tube 12, and the vaporization of chlorosilane and hydrogen mixes and is to carry out in the interchanger 8 of chlorosilane vapourizing mixing device of the present invention.
As for the proportioning value of chlorosilane and hydrogen, be that those skilled in the art can select and determine according to reaction conditions.
Embodiment:
Utilize shell and tube evaporator to implement the present invention as interchanger of the present invention.
As shown in Figure 1, enter respectively in the interchanger 8 again after before entering interchanger 8, chlorosilane and hydrogen being regulated metering by flow control valve 10 and under meter 9 in the proportioning ratio of determining in the flow-control module 13 in transfer lime separately and mix, chlorosilane enters in the interchanger 8 by splitter 5 reflections by Link Port 1 and is filled in the upper cover of interchanger 8, hydrogen enters in the interchanger 8 by Link Port 2 and mixes with chlorosilane, the mixture of hydrogen and chlorosilane enters tube side, vaporized fully from the steam of steam cycle supply system import 6, gas mixture after the vaporization enters reduction furnace by mixed gas outlet 3, also be provided with a relief valve connection 4 in the upper cover side, and the installation safety valve, security incident takes place with superpressure preventing.

Claims (9)

1. chlorosilane vapourizing mixing device, comprise interchanger (8), it is characterized in that: chlorosilane transfer lime (11), hydrogen delivery tube (12) are communicated with the tube side/shell side of this interchanger (8) by first Link Port (1) and second Link Port (2) respectively, all respectively be provided with under meter (9) and flow control valve (10) on chlorosilane transfer lime (11), the hydrogen delivery tube (12), correspondingly, the shell side/tube side of this interchanger (8) is communicated with heat supply system.
2. chlorosilane vapourizing mixing device as claimed in claim 1 is characterized in that: be provided with the splitter (5) that has kept the gap with described Link Port corresponding to chlorosilane transfer lime and interchanger Link Port (1) position in the described interchanger (8).
3. chlorosilane vapourizing mixing device as claimed in claim 1 or 2 is characterized in that: described interchanger (8) is a shell and tube evaporator, and chlorosilane transfer lime (11), hydrogen delivery tube (12) are communicated with the tube side of this interchanger.
4. chlorosilane vapourizing mixing device as claimed in claim 1 or 2 is characterized in that: described heat supply system is the steam cycle supply system.
5. chlorosilane vapourizing mixing device as claimed in claim 1 or 2 is characterized in that: described interchanger (8) is provided with the relief valve connection (4) that is communicated with chlorosilane transfer lime (11), hydrogen delivery tube (12).
6. chlorosilane vapourizing mixing device as claimed in claim 1 or 2 is characterized in that: described under meter (9) adopts mass flowmeter.
7. chlorosilane vapourizing mixing device as claimed in claim 1 or 2 is characterized in that: the valve opening of described flow control valve (10) is controlled by under meter (9).
8. chlorosilane vapourizing mixing device as claimed in claim 7 is characterized in that: described chlorosilane transfer lime (11) is gone up the under meter (9) that is provided with and is gone up the under meter (9) of setting by flow-control module (13) interlock control with hydrogen delivery tube (12).
9. chlorosilane vapourizing mixed process is characterized in that: regulate the proportioning of chlorosilane and hydrogen earlier, carry out the vaporization of the two again and mix.
CN200910310611A 2009-11-30 2009-11-30 Chlorosilane vapourizing mixed process and device Pending CN101723374A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN200910310611A CN101723374A (en) 2009-11-30 2009-11-30 Chlorosilane vapourizing mixed process and device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN200910310611A CN101723374A (en) 2009-11-30 2009-11-30 Chlorosilane vapourizing mixed process and device

Publications (1)

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CN101723374A true CN101723374A (en) 2010-06-09

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285656A (en) * 2011-06-15 2011-12-21 四川新光硅业科技有限责任公司 Trichlorosilane vaporization device
CN102502647A (en) * 2011-10-31 2012-06-20 内蒙古盾安光伏科技有限公司 Polycrystalline silicon reduction system and feeding mode of reducing gas raw materials thereof
CN103950933A (en) * 2014-03-31 2014-07-30 中国恩菲工程技术有限公司 Polysilicon preparation method

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102285656A (en) * 2011-06-15 2011-12-21 四川新光硅业科技有限责任公司 Trichlorosilane vaporization device
CN102502647A (en) * 2011-10-31 2012-06-20 内蒙古盾安光伏科技有限公司 Polycrystalline silicon reduction system and feeding mode of reducing gas raw materials thereof
CN102502647B (en) * 2011-10-31 2013-11-06 内蒙古盾安光伏科技有限公司 Polycrystalline silicon reduction system and feeding mode of reducing gas raw materials thereof
CN103950933A (en) * 2014-03-31 2014-07-30 中国恩菲工程技术有限公司 Polysilicon preparation method
CN103950933B (en) * 2014-03-31 2016-08-17 中国恩菲工程技术有限公司 The method preparing polysilicon

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Application publication date: 20100609