CN101757831B - Trichlorosilane tail gas variable-pressure adsorption equipment and process thereof - Google Patents
Trichlorosilane tail gas variable-pressure adsorption equipment and process thereof Download PDFInfo
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- CN101757831B CN101757831B CN2010101126757A CN201010112675A CN101757831B CN 101757831 B CN101757831 B CN 101757831B CN 2010101126757 A CN2010101126757 A CN 2010101126757A CN 201010112675 A CN201010112675 A CN 201010112675A CN 101757831 B CN101757831 B CN 101757831B
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Abstract
The invention discloses trichlorosilane tail gas variable-pressure adsorption equipment, and a process thereof. The adsorption equipment comprises a resolution gas heat exchanger, wherein the resolution gas heat exchanger is provided with a raw material gas inlet pipe and a gas outlet pipe; and the gas outlet pipe is connected with an adsorption device. The adsorption process comprises the steps that: the raw material tail gas first enters the resolution gas heat exchanger to exchange heat, then enters a heater to be heated up to a temperature of 70+/-2 DEG C and finally enters the adsorption equipment to be absorbed; and after the adsorption, the purified hydrogen gas flows out of a purifying gas tube and is delivered to an HCL synthetic system to take part in HCL synthesis, and the resolution gas enters the resolution gas exchanger from a resolution gas tube to exchange heat and then enters a resolution gas buffer tank and is delivered to a trichlorosilane synthetic system to be recycled.
Description
Technical field
The present invention relates to a kind of trichlorosilane tail gas treatment facility and treatment process thereof, relate to a kind of trichlorosilane tail gas variable-pressure adsorption equipment and technology thereof specifically, belong to chemical technology field.
Background technology
In trichlorosilane technology, vent gas treatment is the difficult problem of puzzlement trichlorosilane industry, and the volume fraction of each main component of technique of trichlorosilane synthetic tail gas is respectively, and HCl 10%; H
285%; SIHCl
32%; SICl
42%; Other are 1% years old.Though the boiling point of trichlorosilane is 31.8 ℃, very easy being condensed, but its volume fraction in tail gas only is 5.4%, according to the Dao Er law of partial pressure, the stagnation pressure of admixture of gas equals the dividing potential drop sum of every kind of gas in the mist, as calculated, when tail gas pressure was 0.11-0.12MPa, its dividing potential drop only was 0.00594-0.00648MPa, so low branch is pressed under normal temperature or the not too low temperature, is difficult to be condensed.Its corresponding temperature is-28～-30 ℃.As seen,, very low temperature will be arranged, so just must consume a large amount of energy, and the retracting device volume be also bigger if want most of trichlorosilane condensation in the tail gas is got off.The direct emptying of these tail gas meeting serious environment pollution can bring very big potential safety hazard simultaneously in addition.At present trichlorosilane producer is to handling that tail gas is taked:
The one, comprehensive recovering process: uncooled hydrogen chloride, hydrogen return the hydrogen chloride synthesis system, and hydrogen mixes by a certain percentage with chlorine, and burning generates hydrogen chloride, recycles.Adopt this method to make the technological process of synthesis procedure open circuit become closed cycle, improve utilization rate of raw materials, removed the raw material unit consumption low, realized that no waste gas discharges, thoroughly solved problem of environmental pollution.But, the micro-chlorosilane that contains in the tail gas easily with hydrogen chloride in the water reaction generate the solid silica blocking pipe, trichlorosilane enters the yield reduction that synthetic furnace can cause trichlorosilane in addition.
The 2nd, drip washing neutralisation treatment method: hydrogen chloride, hydrogen and a spot of uncooled chlorosilane send the tail gas eluting column, spray absorption with big water gaging, hydrogen chloride is dissolved in the water, chlorosilane hydrolysis such as trichlorosilane generate silica and water-soluble hydrogen chloride, hydrochloride aqueous solution discharging in NaOH and after up to standard.This method technology is simple, technology maturation, and small investment, the input amount of the NaOH by the control water yield of spray system and neutralization pond also can realize qualified discharging well.Shortcoming is hydrogen chloride and hydrogen not to be carried out the secondary utilization, makes to consume to increase.The reaction of chlorosilane in the tail gas and water generates water-fast silica and hydrochloric acid in addition, the water-soluble hydrochloric acid that also forms of while hydrogen chloride, and three wastes treating capacity is big.
The 3rd, tail gas adsorption treatment method: utilize of the suction-operated of adsorbents such as active carbon to chlorosilane.Behind the chlorosilane process active carbon of hydrogen chloride in tail gas, hydrogen and a small amount of not liquefaction, chlorosilane wherein is just by charcoal absorption, after charcoal absorption is saturated, by Steam Heating, deviate from the chlorosilane of absorption, together send piece-rate system to separate with sintetics.The hydrogen chloride that is not adsorbed becomes byproduct hydrochloric acid and sells outward after water absorbs.Remaining hydrogen send the hydrogen chloride synthesis system to generate hydrogen chloride with the chlorine burning by a certain percentage and recycles.On the basis of reclaiming a spot of chlorosilane, the hydrogen chloride in the tail gas becomes hydrochloric acid after being absorbed by water, has not only solved the problem of acid water discharging, has increased byproduct hydrochloric acid simultaneously, has increased economic benefit.This method is had relatively high expectations to active carbon, and steam consumption is bigger, and economy is relatively poor.
Summary of the invention
The problem to be solved in the present invention provides a kind of zero-emission that can realize tail gas, reduces the trichlorosilane tail gas variable-pressure adsorption equipment of environmental pollution, and it is recycling that the accessory substance hydrogen of trichlorosilane reaction is obtained, and saves cost, increases economic efficiency.
For addressing the above problem, the present invention institute by the following technical solutions:
A kind of trichlorosilane tail gas variable-pressure adsorption equipment comprises and separates the gassing heat exchanger that the described gassing heat exchanger of separating is provided with unstripped gas air inlet pipe and escape pipe, is connected with adsorbent equipment on escape pipe.
Below be the invention further improvement of these options:
Described adsorbent equipment comprises four absorbers that are installed in parallel, and described absorber is provided with the purified gas pipeline and conciliates the gassing pipeline, described parsing feed channel with separate the gassing heat exchanger and be communicated with.
Further improve:
Be provided with heater in the position of resolving between gas heat exchanger and the absorber on the described escape pipe.
Further improve:
Described purified gas pipeline is provided with equalizer tank.
Further improve:
Described parsing feed channel is provided with vavuum pump.
Further improve:
The described gassing heat exchanger of separating is provided with and separates gassing and go out pipe, goes out to be equipped with on the pipe and separates the gassing surge tank separating gassing, separates the gassing surge tank and is provided with and separates the gassing efferent duct.
Further improve:
Be provided with cooler and compressor on the gassing efferent duct separating, compressor is arranged on cooler and separates between the gassing surge tank.
The present invention also provides a kind of trichlorosilane tail gas pressure swing adsorption technique, and this technology may further comprise the steps:
A raw material tail gas at first enters separates the gassing heat exchanger, enters the heater temperature after heating after the heat exchange and is controlled at 70 ℃ ± 2 ℃:
B and then enter four absorbers and adsorb;
Purified hydrogen after the C absorption is come out by the purified gas pipeline, and delivering to the HCL synthesis system by pipeline, to participate in HCL again synthetic;
Stripping gas after the D absorption enters by the parsing feed channel and separates the gassing heat exchanger, after the heat exchange, enters and separates the gassing surge tank, is delivered in the trichlorosilane synthesis system by compressor, recycles again.
Below be the further improvement of the present invention to above-mentioned technology:
Among the step C: the purified hydrogen after the absorption is come out by the purified gas pipeline, be introduced into equalizer tank and all press, and then delivering to the HCL synthesis system by pipeline, to participate in HCL again synthetic.
The present invention adopts such scheme, has following advantage:
1, separates the gassing heat exchanger because the stripping gas after the absorption enters by the parsing feed channel, after the heat exchange, enter and separate the gassing surge tank, deliver to participation absorption again in the system by compressor, realize the zero-emission of tail gas, made whole production technology reach sealing and circulating, significantly reduced environmental pollution.
2, because the purified hydrogen after the absorption is come out by the purified gas pipeline, delivering to the HCL synthesis system by pipeline, to participate in HCL again synthetic; The accessory substance hydrogen of trichlorosilane reaction has been obtained recycling, provided cost savings, improved economic benefit.
3, the tail gas component that absorbs is unreacted small amount of H CL, the trichlorosilane and the silicon tetrachloride that get off of total condensation not completely, the gas that these absorb, again participate in reaction by the HCL surge tank that compressor is delivered in the trichlorosilane system, utilize the HCL that reclaims to participate in reaction, can reduce production costs; And silicon tetrachloride adds the conversion ratio that can improve the main reaction trichlorosilane in the reaction system to, suppresses the generation of side reaction silicon tetrachloride, has improved product yield, has reduced environmental pollution.
The invention will be further described below in conjunction with drawings and Examples:
Description of drawings
Accompanying drawing 1 is the process chart of the embodiment of the invention;
Accompanying drawing 2 is an I place enlarged drawing in the accompanying drawing 1;
Accompanying drawing 3 is an II place enlarged drawing in the accompanying drawing 1.
Among the figure: 1-separates the gassing heat exchanger; The 2-heater; 3,31,32,33-absorber; The 4-equalizer tank; The 5-vavuum pump; 6-resolver surge tank; The 7-compressor; The 8-cooler; 11-unstripped gas air inlet pipe; The 12-escape pipe; 34-purified gas pipeline; 35-resolves feed channel; 36-separates gassing and goes out pipe; 61-separates the gassing efferent duct; 18,1A, 2A, 3A, 4A, 5A, 6A, 7A, 1B, 2B, 3B, 4B, 5B, 6B, 7B, 1C, 2C, 3C, 4C, 5C, 6C, 7C, 1D, 2D, 3D, 4D, 5D, 6D, 7D, 101,102-valve.
The specific embodiment
Embodiment, as shown in Figure 1, a kind of trichlorosilane tail gas variable-pressure adsorption equipment, comprise and separate gassing heat exchanger 1, the described gassing heat exchanger 1 of separating is provided with unstripped gas air inlet pipe 11 and escape pipe 12, on escape pipe 12, be connected with adsorbent equipment, described adsorbent equipment comprises four absorbers that are installed in parallel 3, absorber 31, absorber 32 and absorber 33, described absorber 3, absorber 31, absorber 32 and absorber 33 are provided with shared purified gas pipeline 34 and conciliate gassing pipeline 35, on the connecting pipe between described purified gas pipeline 34 and the absorber 3 valve 2A is installed, on the connecting pipe between purified gas pipeline 34 and the absorber 31 valve 2B is installed, on the connecting pipe between purified gas pipeline 34 and the absorber 32 valve 2C is installed, on the connecting pipe between purified gas pipeline 34 and the absorber 33 valve 2D is installed, resolve on the connecting pipe between feed channel 35 and the absorber 3 valve 7A is installed, resolve on the connecting pipe between feed channel 35 and the absorber 31 valve 7B is installed, resolve on the connecting pipe between feed channel 35 and the absorber 32 valve 7C is installed, resolve on the connecting pipe between feed channel 35 and the absorber 33 valve 7D is installed.
Described parsing feed channel 35 with separate gassing heat exchanger 1 and be communicated with, described escape pipe 12 is provided with heater 2, described purified gas pipeline 34 is provided with equalizer tank 4, described parsing feed channel 35 is provided with two vavuum pumps 5, the described gassing heat exchanger 1 of separating is provided with and separates gassing and go out pipe 36, go out to be equipped with on the pipe 36 and separate gassing surge tank 6 separating gassing, separating gassing surge tank 6 is provided with and separates gassing efferent duct 61, be provided with cooler 8 and two compressors 7 on the gassing efferent duct 61 separating, compressor 7 is arranged on cooler 8 and separates between the gassing surge tank 6.
A kind of trichlorosilane tail gas pressure swing adsorption technique, this technology may further comprise the steps:
Raw material tail gas enters under 0.35MPa ,-10 ℃ of conditions and separates gassing heat exchanger 1, enters heater 2 temperature after heating after the heat exchange and is controlled at 70 ℃ ± 2 ℃; Raw material tail gas and then enter in the absorber 3.
As Fig. 2, shown in Figure 3, each course of work is as follows in the cycle period of absorber 3:
1, absorption:
Open valve 1A and valve 2A, unstripped gas enters absorber 3 by valve 1A, and by absorber 3, impurity composition is adsorbed unstripped gas in the process from bottom to top under operating pressure, and the hydrogen that is not adsorbed flows out by valve 2A.When the absorption forward position that is adsorbed impurity moved to the certain position of absorber 3, valve-off 1A and valve 2A stopped unstripped gas and enter with product and export.Adsorb forward position to the port of export between also leave the one section adsorbent that not by impurity taken in the absorber 3 this moment.
Step time of implementation :≤180s, pressure process: 0.4MPa.
2, first order isostasy is fallen:
After absorber 3 stops adsorption step, Open valve 5A and valve 18, make absorber 3 and resolver surge tank 6 carry out isostasy, the absorption forward position of absorber 3 advances to port of export direction in the pressure equalizing, but still its port of export of no show, when pressure equated substantially, step all falls in valve-off 5A and valve 18, to be finished.
Step time of implementation :≤45s, pressure process: drop to 0.3MPa by 0.4MPa.
3, second level isostasy is fallen:
Absorber 3 one all falls after step finishes, Open valve 4A and valve 4C, absorber 3 ports of export are linked to each other with the port of export of absorber 32, carry out isostasy, further reclaim dead space gas in the absorber 3, when this step finished, the pressure of absorber 3 and absorber 32 reached balance basically, the impurity absorption forward positions no show port of export still in this moment absorber 3.
Step time of implementation :≤45s, pressure process: drop to 0.18MPa by 0.34MPa.
4, forward put pressure:
After absorber 3 two equal steps finish, continue Open valve 4A, while Open valve 6D, residual gas still washes absorber 33 by valve 4A along Way out in the absorber 3, when absorber 3 pressure drop to 0.08MPa, valve-off 4A, valve 101 and valve 6D, this moment, absorber 3 interior impurity absorption forward positions just arrived the port of export.
Step time of implementation :≤45s, pressure process: drop to 0.08MPa by 0.18MPa.
5, the reverse pressure of putting:
Step time of implementation :≤40s, pressure process: drop to 0.02MPa by 0.08MPa.
6, find time:
7, second level isostasy liter:
After evacuation step finishes, valve-off 6A, valve 7A, valve 102 immediately, Open valve 4A, valve 4C make absorber 3 ports of export link to each other with absorber 32 simultaneously, carry out the isostasy liter, when these two absorber pressure equate substantially, valve-off 4A.
Step time of implementation :≤45s, pressure process: rise to 0.18MPa by 0.02MPa.
8, first order isostasy liter:
Two all rise step and finish after, Open valve 5A and valve 18, valve 5A links to each other with resolver surge tank 6 ports of export, carries out the isostasy liter, absorber 3 pressure further raise.When absorber 3 equates substantially with resolver surge tank 6 pressure, valve-off 5D and valve 18.
Step time of implementation :≤45s, pressure process: 0.18MPa is to 0.34MPa.
9, finally boost:
Finally boosting of absorber 3 is to use product gas, and product gas enters absorber 3 through valve 102 and valve 5A by the port of export, finally makes absorber 3 pressure reach or reach adsorptive pressure substantially, valve-off 5A.After this step, regenerative process is all over, and and then just circulates next time.
Step time of implementation :≤45s, pressure process rises to 0.5MPa by 0.34MPa.
So far, absorption, the regenerative process of absorber 3 are all over, and and then just circulate next time.
After absorber 3 was finished, absorber 31, absorber 32, absorber 33 repeated the adsorption process of absorber 3 successively, after the absorption of four absorbers once more from absorber 3, the repetitive cycling adsorption process.
Stripping gas after the absorption enters by parsing feed channel 35 and separates gassing heat exchanger 1, after the heat exchange, enters and separates gassing surge tank 6, deliver to participation absorption again in the system by compressor 7, realize the zero-emission of tail gas, made whole production technology reach sealing and circulating, significantly reduced environmental pollution.
Claims (3)
1. a trichlorosilane tail gas variable-pressure adsorption equipment comprises and separates gassing heat exchanger (1), and the described gassing heat exchanger (1) of separating is communicated with unstripped gas air inlet pipe (11) and escape pipe (12), it is characterized in that: be communicated with adsorbent equipment on escape pipe (12);
Described adsorbent equipment comprises four absorbers that are installed in parallel, and described absorber is provided with purified gas pipeline (34) and conciliates gassing pipeline (35), described parsing feed channel (35) with separate gassing heat exchanger (1) and be communicated with;
Described escape pipe (12) is provided with heater (2); Described purified gas pipeline (34) is communicated with equalizer tank (4); Described parsing feed channel (35) is provided with vavuum pump (5);
The described gassing heat exchanger (1) of separating is provided with and separates gassing and go out pipe (36), separates gassing and goes out pipe (36) and be communicated with and separate gassing surge tank (6), separates gassing surge tank (6) and is communicated with and separates gassing efferent duct (61);
Be provided with cooler (8) and compressor (7) on the gassing efferent duct (61) separating, compressor (7) is arranged on cooler (8) and separates between the gassing surge tank (6).
2. trichlorosilane tail gas pressure swing adsorption technique, it is characterized in that: this technology may further comprise the steps:
A, raw material tail gas at first enter separates gassing heat exchanger (1), enters heater (2) temperature after heating after the heat exchange and is controlled at 70 ℃ ± 2 ℃;
B and then enter four absorbers and adsorb successively;
Purified gas after C, the absorption is come out by purified gas pipeline (34), and delivering to the HCL synthesis system, to participate in HCL again synthetic;
Stripping gas after D, the absorption enters by parsing feed channel (35) and separates gassing heat exchanger (1), after the heat exchange, enters and separates gassing surge tank (6), is delivered in the trichlorosilane synthesis system by compressor (7).
3. a kind of trichlorosilane tail gas pressure swing adsorption technique according to claim 2, it is characterized in that: among the step C: the purified gas after the absorption is come out by purified gas pipeline (34), be introduced into equalizer tank (4) and all press, and then delivering to the HCL synthesis system by pipeline, to participate in HCL again synthetic.
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| CN2010101126757A CN101757831B (en) | 2010-02-10 | 2010-02-10 | Trichlorosilane tail gas variable-pressure adsorption equipment and process thereof |
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| CN2010101126757A CN101757831B (en) | 2010-02-10 | 2010-02-10 | Trichlorosilane tail gas variable-pressure adsorption equipment and process thereof |
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| CN108926960A (en) * | 2018-08-31 | 2018-12-04 | 四川永祥新能源有限公司 | A kind of processing method of cold hydrogenated tail gas |
| CN109529534B (en) * | 2018-12-27 | 2021-05-04 | 西南化工研究设计院有限公司 | Method and device for purifying organic silicon fractionation tail gas and recycling organic silicon monomers |
| CN109573950A (en) * | 2019-01-31 | 2019-04-05 | 内蒙古通威高纯晶硅有限公司 | A kind of Analytic Tower hydrogen chloride recovery system and technique |
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| CN101357292B (en) * | 2007-07-31 | 2012-07-04 | 中国恩菲工程技术有限公司 | Method for recovering tail-gas generated during producing polycrystalline silicon using silicon tetrachloride |
| CN101254387A (en) * | 2007-12-04 | 2008-09-03 | 魏玺群 | Voltage transformation adsorption method for separating mixture gas containing hydrogen and chloro-silicane and/or hydrogenchloride mixture gas |
| US20090166173A1 (en) * | 2007-12-31 | 2009-07-02 | Sarang Gadre | Effluent gas recovery process for silicon production |
| CN101279178B (en) * | 2008-01-04 | 2010-11-24 | 广州吉必盛科技实业有限公司 | Method and device for recovering H2 in tail gas produced during trichlorosilane production |
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Owner name: SHANDONG XINLONG TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: SHANDONG XINLONG SILICAS INDUSTRY SCIENCE AND TECHNOLOGY CO., LTD. Effective date: 20140212 |
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