CN102815710A - Solid raw material continuous feeding method of silicon tetrachloride hydrogenation reaction - Google Patents
Solid raw material continuous feeding method of silicon tetrachloride hydrogenation reaction Download PDFInfo
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- CN102815710A CN102815710A CN2012102854572A CN201210285457A CN102815710A CN 102815710 A CN102815710 A CN 102815710A CN 2012102854572 A CN2012102854572 A CN 2012102854572A CN 201210285457 A CN201210285457 A CN 201210285457A CN 102815710 A CN102815710 A CN 102815710A
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Abstract
The invention discloses a solid raw material continuous feeding method of a silicon tetrachloride hydrogenation reaction. The solid raw materials comprise silicon powder and a catalyst. The method comprises the steps that: (a) the silicon powder and the catalyst are mixed, such that a normal-pressure mixed material is obtained; (b) the normal-pressure mixed material is supplied into a metering tank, such that the normal-pressure mixed material with a predetermined amount is metered; with an atmospheric pressure regulating device, the normal-pressure mixed material in the metering tank is pressurized, such that the pressure is no less than the pressure in a silicon tetrachloride hydrogenation reactor, and a pressurized mixed material is obtained; (c) the pressurized mixed material is added into the silicon tetrachloride hydrogenation reactor, and is subjected to a reaction; and (d) with the atmospheric pressure regulating device, the atmospheric pressure in the metering tank is regulated such that the atmospheric pressure in the metering tank is no higher than the normal pressure, and the normal-pressure mixed material is received under normal pressure. Therefore, continuous feeding is realized. With the method provided by the invention, the solid raw materials are pressurized, and is delivered from a storage tank with a relatively low atmospheric pressure to the silicon tetrachloride hydrogenation reactor with a relatively high atmospheric pressure, such that continuous feeding is realized.
Description
Technical field
The present invention relates to the polysilicon preparing technical field, more specifically, the present invention relates to a kind of continuous feeding method of solid material of hydrogenation of silicon tetrachloride reaction.
Background technology
The a large amount of silicon tetrachloride as by-product that produces in the polysilicon production process, directly discharging can serious environment pollution.How the safe handling silicon tetrachloride has become " bottleneck " that restricts the polysilicon industry development.At present, the cold hydrogenation technology of silicon tetrachloride has solved the problem of polysilicon by product.
The cold hydrogenation technology of silicon tetrachloride is under certain temperature, pressure, and silicon tetrachloride, hydrogen and silica flour and Powdered catalyst add in the reactor drum, and silicon tetrachloride is converted into the raw material trichlorosilane of production of polysilicon, has realized the recycle of material.Because cold hydrogenation technology operating pressure is higher; Generally operation under 2.0-3.5MPa; And solid materials silica flour and catalyst need join in the reactor drum of high-voltage operation from low-voltage device; Pressure reduction is bigger, and under HTHP, inflammable and explosive operating mode, makes this solid materials add very difficulty of reactor drum.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or provides a kind of useful commerce to select at least.
For this reason, one object of the present invention is to propose a kind of continuous feeding method of implementing the solid material of the hydrogenation of silicon tetrachloride reaction simple, that feed is convenient, safe.
According to the continuous feeding method of the solid material of the hydrogenation of silicon tetrachloride of embodiment of the invention reaction, said solid material comprises silica flour and catalyzer, may further comprise the steps: a) said silica flour is mixed with said catalyzer, obtain the normal pressure mixture; B) with said normal pressure mixture the normal pressure mixture with metering predeterminable quantity is provided to the test tank; And the normal pressure mixture in the said test tank is pressurizeed through barometric control unit; Make its pressure more than or equal to the pressure in the hydrogenation of silicon tetrachloride reactor drum, the mixture that obtains pressurizeing; C) react in the mixture adding hydrogenation of silicon tetrachloride reactor drum with said pressurization; D) through said barometric control unit regulate in the said test tank air pressure so that the air pressure in the said test tank smaller or equal to normal pressure receiving said normal pressure mixture, thereby realize continuous feeding.
Continuous feeding method according to the solid material of the hydrogenation of silicon tetrachloride of embodiment of the invention reaction; Through solid material is pressurizeed, solid material is delivered to the higher hydrogenation of silicon tetrachloride reactor drum of air pressure from the lower storage tank of air pressure, realize continuous feeding; Thereby realize the continous-stable operation of hydrogenation; This method is simple to operate, and feed is effective, and safe.
In addition, the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, in said test tank, feed high pressure gas to increase the air pressure in the said test tank through said barometric control unit.
According to one embodiment of present invention, said high pressure gas are high pressure hydrogen.
According to one embodiment of present invention, discharge gas in the said test tank to reduce the air pressure in the said test tank through said air regulating device.
According to one embodiment of present invention, said normal pressure mixture offers said test tank through action of gravity.
According to one embodiment of present invention, said test tank is positioned at the top of said hydrogenation of silicon tetrachloride reactor drum.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, wherein:
Fig. 1 is the continuous feeding method flow synoptic diagram according to the solid material of the hydrogenation of silicon tetrachloride reaction of the embodiment of the invention;
Fig. 2 is according to used hydrogenation of silicon tetrachloride conversion unit structural representation in the continuous feeding method of the solid material of the hydrogenation of silicon tetrachloride reaction of the embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of said embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Be exemplary through the embodiment that is described with reference to the drawings below, be intended to be used to explain the present invention, and can not be interpreted as limitation of the present invention.
In description of the invention; It will be appreciated that; The orientation of indications such as term " " center ", " vertically ", " laterally ", " length ", " width ", " thickness ", " on ", D score, " preceding ", " back ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", " counterclockwise " or position relation are for based on orientation shown in the drawings or position relation; only be to describe with simplifying for the ease of describing the present invention; rather than the device or the element of indication or hint indication must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.
In addition, term " first ", " second " only are used to describe purpose, and can not be interpreted as indication or hint relative importance or the implicit quantity that indicates indicated technical characterictic.Thus, one or more a plurality of these characteristics can be shown or impliedly comprised to the characteristic that is limited with " first ", " second " clearly.In description of the invention, the implication of " a plurality of " is two or more, only if clear and definite concrete qualification is arranged in addition.
In the present invention, only if clear and definite regulation and qualification are arranged in addition, broad understanding should be done in terms such as term " installation ", " linking to each other ", " connection ", " fixing ", for example, can be to be fixedly connected, and also can be to removably connect, or connect integratedly; Can be mechanical connection, also can be to be electrically connected; Can be directly to link to each other, also can link to each other indirectly through intermediary, can be the connection of two element internals.For those of ordinary skill in the art, can understand above-mentioned term concrete implication in the present invention as the case may be.
In the present invention; Only if clear and definite regulation and qualification are arranged in addition; First characteristic second characteristic it " on " or D score can comprise that first and second characteristics directly contact, can comprise that also first and second characteristics are not directly contacts but through the contact of the additional features between them.And, first characteristic second characteristic " on ", " top " and " above " comprise first characteristic directly over second characteristic and oblique upper, or only represent that the first characteristic level height is higher than second characteristic.First characteristic second characteristic " under ", " below " and " below " comprise first characteristic directly over second characteristic and oblique upper, or only represent that the first characteristic level height is less than second characteristic.
At first combine Fig. 1 to describe continuous feeding method below according to the solid material of the hydrogenation of silicon tetrachloride of embodiment of the invention reaction.
Particularly, the continuous feeding method according to the solid material of the hydrogenation of silicon tetrachloride of embodiment of the invention reaction may further comprise the steps:
A) silica flour is mixed with catalyzer, obtain the normal pressure mixture;
B) with said normal pressure mixture the normal pressure mixture with metering predeterminable quantity is provided to the test tank; And the normal pressure mixture in the said test tank is pressurizeed through barometric control unit; Make its pressure more than or equal to the pressure in the hydrogenation of silicon tetrachloride reactor drum, the mixture that obtains pressurizeing;
C) react in the mixture adding hydrogenation of silicon tetrachloride reactor drum with said pressurization;
D) through said barometric control unit regulate in the said test tank air pressure so that the air pressure in the said test tank smaller or equal to normal pressure receiving said normal pressure mixture, thereby realize continuous feeding.
Continuous feeding method according to the solid material of the hydrogenation of silicon tetrachloride of embodiment of the invention reaction; Through solid material is pressurizeed, solid material is delivered to the higher hydrogenation of silicon tetrachloride reactor drum of air pressure from the lower storage tank of air pressure, realize continuous feeding; Thereby realize the continous-stable operation of hydrogenation; This method is simple to operate, and feed is effective, and safe.
According to one embodiment of present invention, in test tank, feed high pressure gas to increase the air pressure in the test tank through said barometric control unit.Advantageously, in one example, said high pressure gas are high pressure hydrogen, and said high pressure hydrogen passes through the pressurized with hydrogen pipe-line transportation to test tank.
According to one embodiment of present invention, discharge gas in the said test tank to reduce the air pressure in the said test tank through said barometric control unit.Preferably, but can link to each other with the tail gas source so that reduce the air pressure in the test tank on closed ground through the relief pipeline connected sum through the gas in said tail gas source discharge test tank.
About said normal pressure mixture being provided the method to the test tank do not have particular restriction, preferably, can the normal pressure mixture be placed the test tank top, offer test tank through action of gravity.Thus, can reduce the pressure requirement in the test tank, only need make that pressure can provide the normal pressure mixture to test tank smaller or equal to the pressure that the normal pressure mixture holds equipment in the test tank.
According to one embodiment of present invention, said test tank is positioned at the top of said hydrogenation of silicon tetrachloride reactor drum.Thus, also can the mixture in the test tank be joined in the hydrogenation of silicon tetrachloride reactor drum, reduce pressure requirement in the test tank through action of gravity.
Describe according to used hydrogenation of silicon tetrachloride conversion unit and solid material continuous feeding apparatus structure synoptic diagram thereof in the continuous feeding method of the solid material of the hydrogenation of silicon tetrachloride reaction of the embodiment of the invention below in conjunction with Fig. 2.
As shown in Figure 2, the solid material continuous feeding device of said hydrogenation of silicon tetrachloride reaction comprises the storage tank 10 and test tank 20 that is connected.
10 contain the solid material that hydrogenation of silicon tetrachloride reacts in the storage tank, and test tank 20 has the material outlet that said solid material is provided to the hydrogenation of silicon tetrachloride reactor drum, and test tank 20 is provided with barometric control unit with the air pressure in the accommodometer measuring tank 20.
Thus; Solid material continuous feeding device according to hydrogenation of silicon tetrachloride reaction of the present invention; Through on test tank 20, barometric control unit being set; Efficiently solve from the problem of the lower storage tank 10 feeding difficulty to the higher hydrogenation of silicon tetrachloride reactor drum of air pressure of air pressure, this feed device is simple in structure, and is easy to use and safe.
In one example, barometric control unit comprises: capstan 21 and relief pipeline 22.
But capstan 21 connected sums can link to each other with source of the gas so that increase the air pressure in the test tank 20 through in test tank 20, feeding high pressure gas on closed ground, but relief pipeline 22 connected sums can link to each other with the tail gas source so that reduce the air pressure in the test tank 20 through the gas of discharging in the test tank 20 to said tail gas source on closed ground.Advantageously; In one example, capstan 21 can be through the air pressure in the barometric control unit accommodometer measuring tank 20, when capstan 21 is communicated with source of the gas; Source of the gas feeds high pressure gas in test tank 20; Increase the air pressure in the test tank 20, when air pressure in the test tank 20 more than or equal to the hydrogenation of silicon tetrachloride reactor drum in during pressure, just can the solid material in the test tank 20 be delivered in the silicon tetrachloride reactor drum; When relief pipeline 22 is communicated with the tail gas source; Test tank 20 is discharged gas to the tail gas source; Reduce the air pressure in the test tank 20, when air pressure in the test tank 20 during smaller or equal to the air pressure in the storage tank 10, it is subsequent use the solid material in the storage tank 10 to be delivered to test tank 20.
In one example, also be provided with nitrogen pipeline 23 on the test tank 20.Thus, at storage tank 10 whens filling with substance, nitrogen pipeline 23 can break off storage tank 10 and reactor drum 30, and nitrogen plays protection gas.When storage tank 10 loading and unloading solid materialss; Its pressure is normal pressure, and the bottom reactor drum still is in step of reaction, and reactor pressure is higher; In order to prevent that gas is played a reversed role to storage tank 10 in the reactor drum; Test tank 20 pressure releases this moment are left nitrogen simultaneously to lower pressure, reactor drum is revealed the gas of coming take out of to relief pipeline 22.Nitrogen pipeline also can use in system's start-stop car displacement and accident, to play the pressure release effect.
In one example, storage tank 10 links to each other with test tank 20 through first connecting pipe 11, and first connecting pipe 11 is provided with first valve 111 to control the switching of first connecting pipe 11.Further; According to one embodiment of present invention; The material outlet of test tank 20 is connected with second connecting pipe, 23, the second connecting pipes 23 and is connected with said hydrogenation of silicon tetrachloride reactor drum, and second connecting pipe 23 is provided with second valve 231 to control the switching of second connecting pipe 23.Thus, through first valve 111 and second valve 231 can simple and effective control storage tank 10 and test tank 20, test tank 20 and hydrogenation of silicon tetrachloride reactor drum between the connected sum of connecting pipe closed, thereby the transmission of control material.
In one example, first valve 111 and second valve 231 are pneumatic moushroom valve, and further, according to one embodiment of present invention, the pneumatic moushroom valve on said first connecting pipe 11 and second connecting pipe 23 includes two.Thus, can control the connected sum closure of connecting pipe between storage tank 10 and test tank 20, test tank 20 and the hydrogenation of silicon tetrachloride reactor drum automatically through pressure difference through pneumatic moushroom valve.
In one example, storage tank 10 is positioned at test tank 20 tops.Thus, the solid material in the storage tank 10 can get into test tank 20 through gravity and pressure difference effect, has reduced air pressure requirement in the test tank 20.
Advantageously, in one example, test tank 20 is provided with WT-MSR to measure material content in the said test tank 20.Thus, can rationally control the amount of material transmission between storage tank 10 and test tank 20 and test tank 20 and the hydrogenation of silicon tetrachloride reactor drum.
In one example, said hydrogenation of silicon tetrachloride conversion unit comprises: hydrogenation of silicon tetrachloride reactor drum 30 (as shown in Figure 2) and solid material continuous feeding device.Hydrogenation of silicon tetrachloride reactor drum 30 has solid material import and products export; Said solid material continuous feeding device is the solid material continuous feeding device according to the described hydrogenation of silicon tetrachloride reactor drum of the foregoing description; Wherein, the material outlet of test tank 20 links to each other with the solid material import of hydrogenation of silicon tetrachloride reactor drum 30.Because the solid material continuous feeding device according to the hydrogenation of silicon tetrachloride reactor drum of the embodiment of the invention has above-mentioned technique effect, therefore, also has the corresponding techniques effect according to the hydrogenation of silicon tetrachloride reactor drum of the embodiment of the invention.
Below in conjunction with the continuous feeding flow process of specific embodiment description according to the solid material of the hydrogenation of silicon tetrachloride reaction of the embodiment of the invention.
At first, silica flour is mixed in storage tank 10 with catalyzer, obtain the normal pressure mixture.
Open first valve 111 on first connecting pipe 11, storage tank 10 is communicated with test tank 20,, the normal pressure mixture is delivered in the test tank 20 through the effect of gravity differential pressure.
Regulating barometric control unit makes capstan 21 be communicated with source of the gas; Source of the gas feeds high pressure gas in test tank 20; Increase the air pressure in the test tank 20, when air pressure in the test tank 20 more than or equal to hydrogenation of silicon tetrachloride reactor drum 30 in during pressure, open second valve 231 on second connecting pipe 23; Test tank 20 is communicated with silicon tetrachloride reactor drum 30, the mixture of pressurization in the test tank 20 is delivered in the silicon tetrachloride reactor drum 30 reacts.
Regulating barometric control unit makes relief pipeline 22 be communicated with the tail gas source; Test tank 20 is discharged gas to the tail gas source, reduces the air pressure in the test tank 20, when air pressure in the test tank 20 during smaller or equal to the air pressure in the storage tank 10; Open first valve 111 on first connecting pipe 11; Storage tank 10 is communicated with test tank 20, and it is subsequent use that the normal pressure mixture in the storage tank 10 is delivered to test tank 20, realizes continuous feeding.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete characteristic, structure, material or the characteristics of description can combine with suitable manner in any one or more embodiment or example.
Although illustrated and described embodiments of the invention; Those having ordinary skill in the art will appreciate that: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (6)
1. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction, said solid material comprises silica flour and catalyzer, it is characterized in that, may further comprise the steps:
A) said silica flour is mixed with said catalyzer, obtain the normal pressure mixture;
B) with said normal pressure mixture the normal pressure mixture with metering predeterminable quantity is provided to the test tank; And the normal pressure mixture in the said test tank is pressurizeed through barometric control unit; Make its pressure more than or equal to the pressure in the hydrogenation of silicon tetrachloride reactor drum, the mixture that obtains pressurizeing;
C) react in the mixture adding hydrogenation of silicon tetrachloride reactor drum with said pressurization;
D) through said barometric control unit regulate in the said test tank air pressure so that the air pressure in the said test tank smaller or equal to normal pressure receiving said normal pressure mixture, thereby realize continuous feeding.
2. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction according to claim 1 is characterized in that, in said test tank, feeds high pressure gas to increase the air pressure in the said test tank through said barometric control unit.
3. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction according to claim 2 is characterized in that said high pressure gas are high pressure hydrogen.
4. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride according to claim 1 reaction is characterized in that, discharges gas in the said test tank to reduce the air pressure in the said test tank through said air regulating device.
5. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction according to claim 1 is characterized in that said normal pressure mixture offers said test tank through action of gravity.
6. the continuous feeding method of the solid material of hydrogenation of silicon tetrachloride reaction according to claim 1 is characterized in that said test tank is positioned at the top of said hydrogenation of silicon tetrachloride reactor drum.
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| CN2012102854572A CN102815710A (en) | 2012-08-10 | 2012-08-10 | Solid raw material continuous feeding method of silicon tetrachloride hydrogenation reaction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112717835A (en) * | 2020-12-16 | 2021-04-30 | 亚洲硅业(青海)股份有限公司 | Hydrogenation reaction system and method for improving conversion rate of hydrogenation reaction |
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| CN2643991Y (en) * | 2003-07-09 | 2004-09-29 | 陈忠丽 | Adding apparatus of catalyzer |
| CN201372206Y (en) * | 2009-02-27 | 2009-12-30 | 比亚迪股份有限公司 | Facility for preparing trichlorosilane by silicon tetrachloride |
| CN201427041Y (en) * | 2009-07-01 | 2010-03-24 | 禹城绿健生物技术有限公司 | High pressure charging non-return hydrogenator |
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2012
- 2012-08-10 CN CN2012102854572A patent/CN102815710A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2643991Y (en) * | 2003-07-09 | 2004-09-29 | 陈忠丽 | Adding apparatus of catalyzer |
| CN201372206Y (en) * | 2009-02-27 | 2009-12-30 | 比亚迪股份有限公司 | Facility for preparing trichlorosilane by silicon tetrachloride |
| CN201427041Y (en) * | 2009-07-01 | 2010-03-24 | 禹城绿健生物技术有限公司 | High pressure charging non-return hydrogenator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112717835A (en) * | 2020-12-16 | 2021-04-30 | 亚洲硅业(青海)股份有限公司 | Hydrogenation reaction system and method for improving conversion rate of hydrogenation reaction |
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Application publication date: 20121212 |