CN102814095B - Processing method of tail gas of trichlorosilane synthesis - Google Patents
Processing method of tail gas of trichlorosilane synthesis Download PDFInfo
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Abstract
The invention discloses a processing method of tail gas of trichlorosilane synthesis. The method comprises the steps that: (a) the trichlorosilane synthesis tail gas is subjected to a sedimentation treatment; the trichlorosilane synthesis tail gas obtained after the sedimentation treatment is filtered by using a gas filtering device, such that solid impurities in the gas are removed, wherein a ceramic filtering core is provided in the gas filtering device; (b) the filtered trichlorosilane synthesis tail gas is condensed, such that liquid chlorosilane and a gas-phase mixture of hydrogen and hydrogen chloride are obtained; and (c) the mixture of hydrogen and hydrogen chloride is absorbed by using an absorbing agent, such that hydrogen chloride is absorbed, and high-purity hydrogen is obtained. According to the method provided by the invention, the gas filtering device with the ceramic filtering core is adopted. The filtering device has excellent properties of high-temperature resistance and corrosion resistance. The material of the filtering device is table, such that no influence is caused on polysilicon product quality.
Description
Technical field
The present invention relates to polysilicon production process technical field, more specifically, the present invention relates to a kind of processing method of technique of trichlorosilane synthetic tail gas.
Background technology
China's present stage polysilicon project technology more than 85% all belongs to Siemens process technology, in this technical process, has numerous system to need to carry out gas filtration.Specifically have: producing trichloro hydrosilicon by hydrogenation of silicon tetrachloride system, trichlorosilane synthesis system, reduction tail gas dry process recovery system etc.
The general filter adopted is cloth envelop collector at present, and in process of production, finds that cloth envelop collector exists following several shortcoming:
1, cloth envelop collector resistance to elevated temperatures is poor.Especially, in trichlorosilane synthesis system and producing trichloro hydrosilicon by hydrogenation of silicon tetrachloride system, find that cloth envelop collector is very easy to occur breakage, cause filter effect degradation, finally cause follow-up system to block;
2, cloth envelop collector is easily damaged, just causes the Dust Capacity in gas to roll up, finally causes product quality to occur declining to a great extent;
3, cloth envelop collector is expensive, and the filter material of current import is converted on finished product filter bag, and every cost per square meter reaches more than 1000 yuan;
4, the filter material poor corrosion resistance of cloth envelop collector, support member easily corrodes in maintenance process simultaneously, cause maintenance difficulty, and the cost of overhaul is high.
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 at least provides a kind of useful business to select.
For this reason, one object of the present invention is to propose the processing method that a kind of good filtration effect, cost are low, implement technique of trichlorosilane synthetic tail gas easily.
Processing method according to the technique of trichlorosilane synthetic tail gas of the embodiment of the present invention comprises the following steps: a) described technique of trichlorosilane synthetic tail gas is carried out settlement treatment, and utilize gas-filtering device to filter the technique of trichlorosilane synthetic tail gas after settlement treatment, with removing solid impurity wherein, wherein, ceramic element is provided with in described gas-filtering device; B) technique of trichlorosilane synthetic tail gas after filtration is carried out condensation, with the hydrogen of chlorosilane and gaseous state obtaining liquid and the mixture of hydrogen chloride; And c) mixture of hydrogen and hydrogen chloride is adsorbed by adsorbent, to adsorb hydrogen chloride wherein, obtain high-purity hydrogen.
According to the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the present invention, owing to adopting the gas-filtering device being provided with ceramic element, this filter has high temperature resistant, corrosion resistant good characteristic, and stable material quality, can not impact polysilicon product quality.
In addition, following additional technical characteristic can also be had according to the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the present invention:
According to one embodiment of present invention, in step a), the intake air temperature of described gas-filtering device is controlled in 250 ~ 300 DEG C.
According to one embodiment of present invention, the admission pressure of described gas-filtering device is 0.05 ~ 0.3MPa.
According to one embodiment of present invention, the charge flow rate of described gas-filtering device is 500 ~ 2000Nm
3/ h.
According to one embodiment of present invention, described gas-filtering device comprises the upper cover connected successively from top to bottom, vertical tube part and low head, wherein, the top of described filter is provided with gas outlet for discharging the gas after filtration and bottom is provided with slag-drip opening for discharging waste residue, the bottom of described vertical tube part is provided with the air inlet for importing gas to be filtered in described straight tube, and the top of described air inlet is provided with filter house, described filter house comprises the floral disc being provided with through hole and the ceramic element be located in described through hole, the described gas-filtering device for the treatment of technique of trichlorosilane synthetic tail gas also comprises: heat exchange jacket, described heat exchange jacket is located at the outside of described vertical tube part, the bottom of described heat exchange jacket is provided with heat transferring medium import and top is provided with heat transferring medium outlet.
According to one embodiment of present invention, described through hole is multiple, and described multiple through hole is uniformly distributed along the radial and axial of described floral disc, is equipped with described ceramic element in each described through hole.
According to one embodiment of present invention, the number of described through hole and described ceramic element is configured to the flow control of described gas at 0.01 ~ 0.2m/s.
According to one embodiment of present invention, described ceramic element is fixed on described floral disc by securing member, described securing member comprises retainer ring and gland, described retainer ring is welded on described floral disc and the endoporus of described retainer ring is corresponding with described through hole, and described gland snaps onto the top of described ceramic element and is connected to be fixed in described through hole by described ceramic element with described retainer ring.
According to one embodiment of present invention, described ceramic element is aluminium oxide filter core.
According to one embodiment of present invention, the filtering accuracy of described aluminium oxide filter core is 800 ~ 1500 orders.
According to one embodiment of present invention, be also provided with air inlet endless tube and deflection plate in described vertical tube part, described air inlet endless tube is connected with described air inlet, and described deflection plate is between described ceramic element and described air inlet endless tube.
According to one embodiment of present invention, described air inlet endless tube is interval with multiple outlet equably, and described deflection plate has multiple, described multiple deflection plate rises and being circumferentially uniformly distributed at described vertical tube part along the spiral inner wall of described vertical tube part.
According to one embodiment of present invention, described vertical tube part is provided with access hole, and described access hole is positioned at the top of described filter house.
According to one embodiment of present invention, described gas outlet is located at the top of described upper cover and described slag-drip opening is located at the bottom of described low head.
Additional aspect of the present invention and advantage will part provide in the following description, and part will become obvious from the following description, or be recognized by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage will become obvious and easy understand from accompanying drawing below combining to the description of embodiment, wherein:
Fig. 1 is the schematic flow sheet of the processing method of technique of trichlorosilane synthetic tail gas according to the embodiment of the present invention;
Fig. 2 is the gas-filtering device structural representation according to the embodiment of the present invention;
Fig. 3 is the gas-filtering device ceramic element distribution schematic diagram according to the embodiment of the present invention;
Fig. 4 is the gas-filtering device ceramic element securing member schematic diagram according to the embodiment of the present invention;
Fig. 5 is the trichlorosilane synthesis system schematic diagram according to the embodiment of the present invention;
Fig. 6 is the trichlorosilane synthesis system handling process schematic diagram according to the embodiment of the present invention.
Detailed description of the invention
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has element that is identical or similar functions from start to finish.Be exemplary below by the embodiment be described with reference to the drawings, be intended to for explaining the present invention, and can not limitation of the present invention be interpreted as.
In describing the invention, it will be appreciated that, term " " center ", " longitudinal direction ", " transverse direction ", " length ", " width ", " thickness ", " on ", D score, " front ", " afterwards ", " left side ", " right side ", " vertically ", " level ", " top ", " end " " interior ", " outward ", " clockwise ", orientation or the position relationship of the instruction such as " counterclockwise " are based on orientation shown in the drawings or position relationship, only the present invention for convenience of description and simplified characterization, instead of indicate or imply that the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore limitation of the present invention can not be interpreted as.
In addition, term " first ", " second " only for describing object, and can not be interpreted as instruction or hint relative importance or imply the quantity indicating indicated technical characteristic.Thus, be limited with " first ", the feature of " second " can express or impliedly comprise one or more these features.In describing the invention, the implication of " multiple " is two or more, unless otherwise expressly limited specifically.
In the present invention, unless otherwise clearly defined and limited, the term such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, above-mentioned term concrete meaning in the present invention can be understood as the case may be.
In the present invention, unless otherwise clearly defined and limited, fisrt feature second feature it " on " or D score can comprise the first and second features and directly contact, also can comprise the first and second features and not be directly contact but by the other characterisation contact between them.And, fisrt feature second feature " on ", " top " and " above " comprise fisrt feature directly over second feature and oblique upper, or only represent that fisrt feature level height is higher than second feature.Fisrt feature second feature " under ", " below " and " below " comprise fisrt feature directly over second feature and oblique upper, or only represent that fisrt feature level height is less than second feature.
First the flow process of the processing method according to technique of trichlorosilane synthetic tail gas of the present invention is described with reference to figure 1 below.
Particularly, comprise the following steps according to the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the present invention:
A) described technique of trichlorosilane synthetic tail gas is carried out settlement treatment, and utilize gas-filtering device to filter the technique of trichlorosilane synthetic tail gas after settlement treatment, to remove solid impurity wherein, wherein, in described gas-filtering device, be provided with ceramic element;
B) technique of trichlorosilane synthetic tail gas after filtration is carried out condensation, with the hydrogen of chlorosilane and gaseous state obtaining liquid and the mixture of hydrogen chloride; And
C) mixture of hydrogen and hydrogen chloride is adsorbed by adsorbent, to adsorb hydrogen chloride wherein, obtain high-purity hydrogen.
Thus, according to the processing method of the technique of trichlorosilane synthetic tail gas of the embodiment of the present invention, owing to adopting the gas-filtering device being provided with ceramic element, this filter has high temperature resistant, corrosion resistant good characteristic, and stable material quality, can not impact polysilicon product quality, thus can filter and obtain the higher hydrogen of purity.
In order to ensure the normal operation of filter, improve filter efficiency, preferably, the intake air temperature that can control gas-filtering device is 250 ~ 300 DEG C, and admission pressure is 0.05 ~ 0.3MPa, and charge flow rate is 500 ~ 2000Nm
3/ h.
The gas-filtering device in above-described embodiment is specifically described below in conjunction with accompanying drawing.
As shown in Figure 2, preferably, this gas-filtering device can comprise: the upper cover 10 connected successively from top to bottom, vertical tube part 20, low head 30 and heat exchange jacket 40.
Wherein, the top of described gas-filtering device is provided with gas outlet 11 for discharging the gas after filtration and bottom is provided with slag-drip opening 31 for discharging waste residue, the bottom of vertical tube part 20 is provided with the air inlet 21 for importing gas to be filtered in described straight tube, and the top of air inlet 21 is provided with filter house, filter house comprises the floral disc 22 that is provided with through hole and establishes ceramic element 23 in through-holes, heat exchange jacket 40 is located at the outside of vertical tube part 20, and the bottom of heat exchange jacket 40 is provided with heat transferring medium import 41 and top is provided with heat transferring medium outlet 42.
Thus, according to above-mentioned gas filter, owing to have employed ceramic element 23, gas-filtering device is had high temperature resistant, corrosion resistant good characteristic, and stable material quality, can not impact polysilicon product quality; Ceramic element 23 can, according to the requirement of filtering accuracy, produce the filter core of different accuracy, and ceramic element 23 be simply shaping, and large-scale production is easy, cheap; Gas-filtering device outside is provided with heat exchange jacket 40, can ensure filtration temperature, effectively prevents the condensation of gas, also can effectively prevent portion temperature too high, cause the damage of built-in securing member.
Further contemplate cost and mass production problem, in one example, preferably, ceramic element 23 is aluminium oxide filter core.Thus, the ceramic element 23 of this material both can meet high temperature resistant, corrosion resistant requirement, and easily large-scale production, can reduce production cost further.
In one example, as shown in Figure 3, through hole is multiple, and multiple through hole is uniformly distributed along the radial and axial of floral disc 22, is equipped with ceramic element 23 in each through hole.Thus, by arranging multiple through hole, can by filtration duct separately, the size according to heat exchange area and floral disc 22 arranges that ceramic element 23 reaches filter effect, avoids occurring filtering duct blocking and overall non-serviceable situation, improves the practicality of filter.
Consider the problem of gas volume and filter area, in one example, the number of through hole and ceramic element 23 is configured to the flow control of described gas at 0.01 ~ 0.2m/s.Thus, gas can be made under this flow velocity to be filtered more fully.
In one example, as shown in Figure 4, ceramic element 23 is fixed on floral disc 22 by securing member, described securing member comprises retainer ring 241 and gland 242, retainer ring 241 is welded on floral disc 22 and the endoporus of retainer ring 241 is corresponding with through hole, and gland 242 snaps onto the top of ceramic element 23 and is connected to be fixed in through hole by ceramic element 23 with retainer ring 241.Thus, ceramic element 23 can be fixed on floral disc 22, and fixed form is reasonable, conveniently carries out dismantling, installing, reduces maintenance difficulty.
In one example, the filtering accuracy of described aluminium oxide filter core is 800 ~ 1500 orders.Thus, the larger dust of order number can be filtered out as required.
In one example, be also provided with air inlet endless tube 25 and deflection plate 26 in vertical tube part 20, air inlet endless tube 25 is connected with air inlet 21, and deflection plate 26 is between ceramic element 26 and air inlet endless tube 25.Further, according to one embodiment of present invention, air inlet endless tube 25 is interval with equably multiple outlet 251, and deflection plate 26 has multiple, multiple deflection plate 26 rises and being circumferentially uniformly distributed at vertical tube part 20 along the spiral inner wall of vertical tube part 20.Thus, air inlet endless tube 25 and deflection plate 26 effectively can ensure air inlet uniformity, and reach and promote that filtration core filters uniform object, meanwhile, the dust in air-flow can act on lower part sedimentation at deflection plate 26, reaches the effect alleviating filtration core load.
Advantageously, in one example, vertical tube part 20 is provided with access hole 27, and access hole 27 is positioned at the top of described filter house.Thus, by arranging access hole 27, conveniently can carry out trouble hunting, not needing detaching equipment.
In one example, gas outlet 11 is located at the top of upper cover 10 and slag-drip opening 31 is located at the bottom of low head 30.Thus, so that the deslagging of filter, the process of detaching equipment can be eliminated.
The trichlorosilane synthesis system of the processing method adopting technique of trichlorosilane synthetic tail gas of the present invention is described below in conjunction with Fig. 5.
As shown in Figure 5, described trichlorosilane synthesis system comprises trichlorosilane synthesizer and tail gas treatment device, synthesis tail gas from described trichlorosilane synthesizer is carried out vent gas treatment by described tail gas treatment device, preferably, described tail gas treatment device can comprise the sedimentation device 50, gas-filtering device 60, condenser 70 and the adsorption tower 80 that connect successively
Wherein, gas-filtering device 60 is the gas-filtering device according to above-described embodiment, and gas-filtering device 60 flows to condenser 70 after being filtered by the synthesis tail gas from sedimentation device 50, condenser 70 is for being separated into the chlorosilane of liquid and the hydrogen of gaseous state and hydrogen chloride by the synthesis tail gas after filtering, adsorption tower 80 for adsorptive gaseous hydrogen chloride, to obtain hydrogen.
Because the gas-filtering device above-mentioned according to the present invention has above-mentioned technique effect, therefore, above-mentioned trichlorosilane synthesis system also has corresponding technique effect, and can be filtered by this system and obtain the higher hydrogen of purity.
The flow process of the processing method of technique of trichlorosilane synthetic tail gas in above-mentioned trichlorosilane synthesis system is specifically described below in conjunction with embodiment and accompanying drawing.
Embodiment 1
As shown in Figure 6, first silica flour and hydrogen chloride are passed into trichlorosilane synthesizer and carry out trichlorosilane synthesis, then synthesis tail gas is carried out sedimentation by sedimentation device 50 to gather dust to remove high chlorosilane wherein and solid impurity, synthesis tail gas component is chlorosilane, hydrogen and hydrogen chloride.
Gas after sedimentation being gathered dust passes into gas-filtering device 60 and filters, and the intake air temperature controlling gas-filtering device 60 is 250 ~ 300 DEG C, and admission pressure is 0.05 ~ 0.3MPa, and charge flow rate is 500 ~ 2000Nm
3/ h, filtering accuracy is 800 ~ 1500 orders.
Gas after filtration is passed into condenser 70 and carries out condensation, the synthesis tail gas after filtering being separated into the chlorosilane of liquid and the hydrogen of gaseous state and hydrogen chloride, being passed into the adsorptive gaseous hydrogen chloride of adsorption tower 80, obtaining high-purity hydrogen.High-purity hydrogen carries out synthesis and obtains hydrogen chloride, and hydrogen chloride can be used as raw material and silica flour carries out trichlorosilane synthesis.
In the description of this description, specific features, structure, material or feature that the description of reference term " embodiment ", " some embodiments ", " example ", " concrete example " or " some examples " etc. means to describe in conjunction with this embodiment or example are contained at least one embodiment of the present invention or example.In this manual, identical embodiment or example are not necessarily referred to the schematic representation of above-mentioned term.And the specific features of description, structure, material or feature can combine in an appropriate manner in any one or more embodiment or example.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (10)
1. a processing method for technique of trichlorosilane synthetic tail gas, is characterized in that, comprises the following steps:
A) described technique of trichlorosilane synthetic tail gas is carried out settlement treatment, and utilize gas-filtering device to filter the technique of trichlorosilane synthetic tail gas after settlement treatment, to remove solid impurity wherein, wherein, in described gas-filtering device, be provided with ceramic element;
B) technique of trichlorosilane synthetic tail gas after filtration is carried out condensation, with the hydrogen of chlorosilane and gaseous state obtaining liquid and the mixture of hydrogen chloride; And
C) mixture of hydrogen and hydrogen chloride is adsorbed by adsorbent, to adsorb hydrogen chloride wherein, obtains high-purity hydrogen,
Described gas-filtering device comprises the upper cover, vertical tube part and the low head that connect successively from top to bottom, wherein,
The top of described gas-filtering device is provided with gas outlet for discharging the gas after filtration and bottom is provided with slag-drip opening for discharging waste residue,
The bottom of described vertical tube part is provided with the air inlet for importing gas to be filtered in described straight tube, and the top of described air inlet is provided with filter house, and described filter house comprises the floral disc being provided with through hole and the ceramic element be located in described through hole,
The described gas-filtering device for the treatment of technique of trichlorosilane synthetic tail gas also comprises:
Heat exchange jacket, described heat exchange jacket is located at the outside of described vertical tube part, the bottom of described heat exchange jacket is provided with heat transferring medium import and top is provided with heat transferring medium outlet, step a) in, the intake air temperature of described gas-filtering device is controlled in 250 ~ 300 DEG C, the admission pressure of described gas-filtering device is 0.05 ~ 0.3MPa, and the charge flow rate of described gas-filtering device is 500 ~ 2000Nm
3/ h.
2. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, is characterized in that, described through hole is multiple, and described multiple through hole is uniformly distributed along the radial and axial of described floral disc, is equipped with described ceramic element in each described through hole.
3. the processing method of technique of trichlorosilane synthetic tail gas according to claim 2, is characterized in that, the number of described through hole and described ceramic element is configured to the flow control of described gas at 0.01 ~ 0.2m/s.
4. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, it is characterized in that, described ceramic element is fixed on described floral disc by securing member, described securing member comprises retainer ring and gland, described retainer ring is welded on described floral disc and the endoporus of described retainer ring is corresponding with described through hole, and described gland snaps onto the top of described ceramic element and is connected to be fixed in described through hole by described ceramic element with described retainer ring.
5. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, is characterized in that, described ceramic element is aluminium oxide filter core.
6. the processing method of technique of trichlorosilane synthetic tail gas according to claim 5, is characterized in that, the filtering accuracy of described aluminium oxide filter core is 800 ~ 1500 orders.
7. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, it is characterized in that, also be provided with air inlet endless tube and deflection plate in described vertical tube part, described air inlet endless tube is connected with described air inlet, and described deflection plate is between described ceramic element and described air inlet endless tube.
8. the processing method of technique of trichlorosilane synthetic tail gas according to claim 7, it is characterized in that, described air inlet endless tube is interval with multiple outlet equably, and described deflection plate has multiple, described multiple deflection plate rises and being circumferentially uniformly distributed at described vertical tube part along the spiral inner wall of described vertical tube part.
9. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, is characterized in that, described vertical tube part is provided with access hole, and described access hole is positioned at the top of described filter house.
10. the processing method of technique of trichlorosilane synthetic tail gas according to claim 1, is characterized in that, described gas outlet is located at the top of described upper cover and described slag-drip opening is located at the bottom of described low head.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106215575A (en) * | 2016-08-31 | 2016-12-14 | 芜湖恒耀汽车零部件有限公司 | Automobile tail gas filtering device ceramic membrane filter material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103449446B (en) * | 2013-08-23 | 2015-05-20 | 中国恩菲工程技术有限公司 | Method for preparing trichlorosilane |
| CN113117442B (en) * | 2020-01-10 | 2023-05-02 | 新疆新特晶体硅高科技有限公司 | Tail gas treatment method and system in polysilicon production |
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