CN105084369B - A kind of recycling and processing device of chlorine-containing silane waste gas - Google Patents
A kind of recycling and processing device of chlorine-containing silane waste gas Download PDFInfo
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- CN105084369B CN105084369B CN201410166914.5A CN201410166914A CN105084369B CN 105084369 B CN105084369 B CN 105084369B CN 201410166914 A CN201410166914 A CN 201410166914A CN 105084369 B CN105084369 B CN 105084369B
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Abstract
The present invention provides a kind of recycling and processing device of chlorine-containing silane waste gas, including：Chlorosilane recovery unit, chlorosilane washing unit and tail gas emptying unit, the chlorosilane recovery unit are connected with chlorosilane washing unit, for the part chlorosilane gas in chlorine-containing silane waste gas to be reclaimed, and remainder of exhaust gas are delivered into chlorosilane washing unit；The chlorosilane washing unit is also connected with tail gas emptying unit, for the remaining chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas to be eluted, to remove the chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas, and the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas is delivered to tail gas emptying unit；The tail gas emptying unit is used to the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas being vented.Recycling and processing device of the present invention can fully reclaim the chlorosilane resource in waste gas, and and can carries out pollution-free processing to irretrievable chlorosilane in waste gas.
Description
Technical field
The present invention relates to Waste Disposal Technology field, and in particular to a kind of recycling and processing device of chlorine-containing silane waste gas.
Background technology
In polysilicon production process, because production needs, each process unit (such as purifying plant, reduction tail gas dry process
Retracting device, cold hydrogenation apparatus, reduction apparatus, tank field etc.) all inevitably to discharge a certain amount of tail gas (also referred to as useless
Gas).Constantly expanded with the production scale of polysilicon, tail gas (main component is nitrogen, hydrogen chloride, chlorosilane and hydrogen) discharge
Amount is also increased sharply therewith, on the one hand can largely waste the chlorosilane resource in tail gas；On the other hand because chlorosilane has contaminative,
Such as leak to cause seriously to pollute to environment, therefore, it is necessary to carries out respective handling to the tail gas formed in polysilicon production process
Normal discharge again afterwards.
At present, the exhaust gas processing device of domestic production of polysilicon producer generally comprises eluting column, spray pump and waste liquid pool, will
After tail gas collects and is sent into tail gas eluting column, the leacheate sprayed through spray pump is by hydrogen chloride soluble in water in tail gas, chlorine silicon
The elution such as alkane are got off, and not soluble in water and free of contamination hydrogen and nitrogen are directly vented after elution through exhaust port, elution
The waste liquid formed afterwards is directly transported to waste liquid pool.But the waste liquid moisture content that is formed after elution is high and has corrosivity so that
Transportation facility is easily corroded damage, and the waste residue in waste liquid is also easy to block transport pipeline, and waste liquid transport and manually drags for slag mistake
Pollution of the journey to surrounding environment is more serious.In addition, the leacheate (such as pure water or alkali lye) used in lessivation can not circulate
Utilize, cause leacheate dosage huge, so as to add the yield of waste liquid and processing cost.
The content of the invention
The technical problems to be solved by the invention are to be directed to the drawbacks described above in the presence of prior art, there is provided a kind of chloride
The recycling and processing device of silicone hydride waste gas, it can fully reclaim the chlorosilane resource in waste gas, and and can in waste gas to that can not reclaim
Chlorosilane carry out pollution-free processing.
Technical scheme used by solution present invention problem：
The recycling and processing device of the chlorine-containing silane waste gas includes：Chlorosilane recovery unit, chlorosilane washing unit and tail
Gas is vented unit,
The chlorosilane recovery unit is connected with chlorosilane washing unit, for by the part chlorine silicon in chlorine-containing silane waste gas
Alkane gas is reclaimed, and remainder of exhaust gas is delivered into chlorosilane washing unit；
The chlorosilane washing unit is also connected with tail gas emptying unit, for by the remaining chlorine silicon in the remainder of exhaust gas
Alkane gas and hydrogen chloride gas elute, to remove the chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas, and will
The remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas is delivered to tail gas emptying unit；
The tail gas emptying unit is used to the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas being vented.
Alternatively, the chlorosilane recovery unit includes the first recovery subelement, and its input receives the chlorine-containing silane
Waste gas, its output end are connected with recovery system and chlorosilane washing unit respectively, for making the portion in the chlorine-containing silane waste gas
Divide chlorosilane gas to form condensate liquid, and the condensate liquid is delivered to recovery system, and will not form the chloride of condensate liquid
Silicone hydride waste gas is delivered to chlorosilane washing unit as the remainder of exhaust gas.
Alternatively, the first recovery subelement uses forecooler, for the chlorine-containing silane waste gas to be cooled into -10 DEG C
~0 DEG C.
Alternatively, the chlorosilane recovery unit also includes the second recovery subelement, and its input receives the first recovery
The chlorine-containing silane waste gas for not forming condensate liquid of unit output, its output end is respectively through chlorosilane purification procedures and recovery system phase
Even, and it is connected with chlorosilane washing unit, for by the trichlorosilane in the chlorine-containing silane waste gas for not forming condensate liquid
Gas and dichlorosilane gas handle through chlorosilane purification procedures after absorbing and are delivered to recovery system again, and will not absorbed
And the chlorine-containing silane waste gas for not forming condensate liquid is delivered to chlorosilane washing unit as the remainder of exhaust gas.
Alternatively, the second recovery subelement includes absorption tower, the chlorine-containing silane waste gas for not forming condensate liquid from
The bottom inflow end on absorption tower enters, and silicon tetrachloride material enters from the top on absorption tower, and the silicon tetrachloride material is as suction
Liquid is received, for absorbing trichlorosilane gas and dichlorosilane gas in the chlorine-containing silane waste gas for not forming condensate liquid,
The absorbing liquid for having absorbed trichlorosilane gas and dichlorosilane gas purifies work after the discharge of the bottom on absorption tower through chlorosilane
Sequence processing is transported to recovery system again, is not absorbed by liquid absorption and does not form the chlorine-containing silane waste gas of condensate liquid as described surplus
Remaining waste gas is transported to chlorosilane washing unit after the discharge of the top outlet side on absorption tower.
Alternatively, the second recovery subelement also includes supercharger, and its input receives the first recovery subelement output
The chlorine-containing silane waste gas for not forming condensate liquid, its output end is connected with the bottom inflow end on absorption tower, for by the first recovery
The chlorine-containing silane exhaust gas for not forming condensate liquid of subelement output is to being delivered to absorption after 0.05MPaG~0.2MPaG
Tower.
Alternatively, the second recovery subelement also includes circulating pump, and its input has received absorb the bottom of the tower discharge
The absorbing liquid of trichlorosilane gas and dichlorosilane gas is absorbed, its output end at the top of absorption tower respectively with being connected, Yi Jijing
Chlorosilane purification procedures are connected with recovery system, for the trichlorosilane of the absorption gas and dichloro two for discharging absorb the bottom of the tower
The absorbing liquid of hydrogen silicon gas is pressurized to 0.3MPaG~1.0MPaG, and make in the absorbing liquid after supercharging mostly as circulation fluid
Absorption tower is back at the top of from absorption tower, and the fraction in the absorbing liquid after supercharging is purified as recovered liquid through chlorosilane
Recovery system is delivered to after process processing.
Alternatively, the second recovery subelement also includes deep freezer, and its input receives the circulation fluid of circulating pump output,
Its output end is returned at the top of absorption tower again with being connected at the top of absorption tower for the circulation fluid to be cooled to after -45 DEG C~-20 DEG C
It is back to absorption tower.
Alternatively, the chlorosilane washing unit includes eluting column, and the top in the eluting column is provided with spray head, uses
In making initial leacheate uniformly spray downwards, the remainder of exhaust gas of chlorosilane recovery unit output is from positioned at the lower section of spray head
Eluting column inlet end enter eluting column, the initial leacheate is by the remaining chlorosilane gas in the remainder of exhaust gas and chlorination
Hydrogen elutes and forms hydrolyzate, described to remove the chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas
Hydrolyzate is back to the spray head of eluting column as circulation fluid from the discharge of elution tower bottom and after the processing of sewage disposal process
In, the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas is transported to tail after the discharge of the top outlet side of eluting column
Gas is vented unit；Wherein, the spray volume of the initial leacheate need to meet from the described surplus of chlorosilane recovery unit output
Remaining waste gas enters the ejection time untill eluting column inlet end starts into the spray head that circulation fluid is back to eluting column first.
Alternatively, the spray head is additionally operable to make supplement leacheate uniformly spray downwards.
Alternatively, the chlorosilane washing unit also includes the stirring subelement positioned at elution tower bottom, for uniformly stirring
Mix the hydrolyzate.
Alternatively, the chlorosilane washing unit also includes force (forcing) pump, and its input receives the water of elution tower bottom discharge
Liquid is solved, its output end is connected through sewage disposal process with the spray head of eluting column, for will elute the hydrolyzate of tower bottom discharge
0.4MPaG~1.0MPaG is pressurized to, and the hydrolyzate after supercharging is back to the spray of eluting column after the processing of sewage disposal process
Drench in head.
Alternatively, the chlorosilane washing unit also includes mixing subelement, and its input receives chlorosilane recovery unit
The remainder of exhaust gas and part circulation fluid of output, its output end are connected with eluting column inlet end, for returning the chlorosilane
Receive the remainder of exhaust gas and part circulation fluid uniformly after mixing, then through eluting column inlet end enter eluting column of unit output.
Alternatively, the tail gas emptying unit uses water sealed tank, the top outlet side of eluting column and the inlet end of water sealed tank
It is connected, the output end of the force (forcing) pump is also connected with water seal upper end, most of through existing in the hydrolyzate after supercharging for making
It is back to after some conventional sewage treatment process processing in the spray head of eluting column, and makes the small portion in the hydrolyzate after supercharging
Divide and enter water sealed tank, and eluting column is back to after the discharge of the bottom of water sealed tank.
Beneficial effect：
Recycling and processing device of the present invention can will be exhausted in the chlorine-containing silane waste gas formed in polysilicon production process
Most of chlorosilane gas recovery, and a small amount of chlorosilane gas and hydrogen chloride gas that will be unable to fully reclaim are eluted by washing
Get off, and leacheate can recycle, so as to remove nearly all chlorosilane gas and the chlorination in chlorine-containing silane waste gas
Hydrogen, remaining free of contamination hydrogen and nitrogen can be directly vented, and meet the normal table operation of production of polysilicon.It can be seen that
Recycling and processing device of the present invention can improve the recovery utilization rate of the discarded object formed in polysilicon production process, and can be
On the premise of ensureing chlorosilane recovery quality, the chlorosilane gas in waste gas are reclaimed to the full extent；Prior art can also be overcome
The technical deficiency in processing procedure is eluted, realizes recycling for leacheate, thus reduces the dosage of leacheate, is reduced useless
The yield and processing cost of liquid (i.e. hydrolyzate)；It is additionally, since the waste liquid formed in lessivation and is passing through existing routine
Be back in the spray head of eluting column and recycle again as circulation fluid after the processing of sewage disposal process, thus the waste liquid of formation without
It need to transport, existing pollution problem and transportation facility is also just not present and is easily corroded damage, the waste residue in waste liquid easily blocks
The problems such as transport pipeline.
Brief description of the drawings
Fig. 1 is the structured flowchart of the recycling and processing device of chlorine-containing silane waste gas described in the embodiment of the present invention 1；
Fig. 2 is the operation principle schematic diagram of the recycling and processing device of chlorine-containing silane waste gas described in the embodiment of the present invention 2.
In figure：1- chlorine-containing silane waste gas；2- chilled brine forecoolers；3- chlorosilane condensate liquid；4- recovery systems；
The remaining chlorine-containing silane waste gas of 5-；6- superchargers；7- high pressure exhaust gas；8- absorption towers；9- silicon tetrachloride materials；10- is mixed
Close liquid；11- circulating pumps；12- deep freezers；13rd, 30,31- circulation fluids；14- recovered liquids；15- resin absorbing columns；16- chlorine
Silane purification procedures；The unrecovered gas of 17-；18- mixing subelements；19- eluting columns；20- stirs subelement；21- is sprayed
Head；22- supplements leacheate；23- hydrolyzates；24- force (forcing) pumps；25- the first highly pressured hydrolysis liquid；The highly pressured hydrolysis of 26- second
Liquid；27- unreacting gas；28- water sealed tanks；29- tail gas；32- sewage disposal processes.
Embodiment
To make those skilled in the art more fully understand technical scheme, with reference to the accompanying drawings and examples to this
Invention is described in further detail.
Embodiment 1：
As shown in figure 1, the present embodiment provides a kind of recycling and processing device of chlorine-containing silane waste gas, including：Chlorosilane reclaims
Unit, chlorosilane washing unit and tail gas emptying unit.
Wherein, the chlorine-containing silane waste gas includes the impurity such as nitrogen, hydrogen, hydrogen chloride gas, chlorosilane gas and B, P,
The impurity such as described B, P include：PCl3(phosphorus trichloride), PCl5(phosphorus pentachloride), BCl5(phosphoric boron) and PH3(hydrogen phosphide), with
And B (boron), P (phosphorus) chloride；Chlorosilane (chlorosilane) is silane (SiH4) in hydrogen atom be substituted by a chlorine atom both
Product afterwards, it is gas when chlorinty is low, is liquid when chlorinty is higher, formula SiHnCl4-n, n=0,1,2,3.
The chlorosilane recovery unit is connected with chlorosilane washing unit, for by the part chlorine silicon in chlorine-containing silane waste gas
Alkane gas is reclaimed, and remainder of exhaust gas is delivered into chlorosilane washing unit.
Specifically, the chlorosilane recovery unit includes the first recovery subelement, and its input receives the chlorine-containing silane
Waste gas, its output end are connected with recovery system (i.e. existing conventional chlorosilane recovery system) and chlorosilane washing unit respectively,
Recovery system is delivered to for making the part chlorosilane gas in the chlorine-containing silane waste gas form condensate liquid, and by the condensate liquid
System, recycled for recovery system, and the chlorine-containing silane waste gas for not forming condensate liquid is delivered to as the remainder of exhaust gas
Chlorosilane washing unit.
Preferably, the first recovery subelement uses forecooler, for the chlorine-containing silane waste gas to be cooled into -10 DEG C
~0 DEG C, so that the part chlorosilane gas in the chlorine-containing silane waste gas form condensate liquid.It is tests prove that described chloride
After the cooling of silicone hydride waste gas pre-cooled device, forming the chlorosilane gas of condensate liquid, to account for chlorosilane gas in the chlorine-containing silane waste gas total
More than the 20% of amount.(can reach more than 85% after the second recovery subelement) at normal atmospheric pressure, nitrogen is at -195.8 DEG C
Left and right is converted into liquid by gaseous state, and hydrogen is converted into liquid at -252.87 DEG C or so by gaseous state, hydrogen chloride -85 DEG C or so by
Gaseous state is converted into liquid, and chlorosilane is converted into liquid in the range of -10 DEG C~0 DEG C by gaseous state, therefore, using forecooler by institute
When stating chlorine-containing silane waste gas and being cooled to -10 DEG C~0 DEG C, part chlorosilane gas form condensate liquid, and nitrogen, hydrogen and hydrogen chloride
Gas also keeps gaseous state because temperature is not low enough, so as to by way of condensation by part chlorosilane gas from the chlorine-containing silane
Peeled away in waste gas, and be delivered to recovery system.Alternatively, the forecooler is air precooler, water precooler or vacuum
Forecooler.Because the freezing point of salt solution is lower than water, the chlorine-containing silane waste gas can be cooled to subzero, good refrigeration effect rapidly
And cost is low, therefore the forecooler is preferably chilled brine forecooler.
In order to further reclaim chlorosilane gas in the chlorine-containing silane waste gas for not forming condensate liquid, it is preferable that described
Chlorosilane recovery unit also includes the second recovery subelement, and its input is connected with the output end of the first recovery subelement, to connect
The chlorine-containing silane waste gas for not forming condensate liquid of the first recovery subelement output is received, its output end is respectively through existing conventional chlorine silicon
Alkane purification procedures (being realized using rectifying column etc., for removing the impurity such as B, P) are connected with recovery system, and are eluted with chlorosilane
Unit is connected, for by the trichlorosilane gas and dichlorosilane gas in the chlorine-containing silane waste gas for not forming condensate liquid
Recovery system is delivered to again through existing conventional chlorosilane purification procedures processing after absorption, and will not be absorbed and not formed cold
The chlorine-containing silane waste gas of lime set is delivered to chlorosilane washing unit as the remainder of exhaust gas.Wherein, it is delivered to recovery system
Dichlorosilane can react with silicon tetrachloride in counter be disproportionated in process in downstream and generate trichlorosilane, and trichlorosilane is purified
Available for producing polysilicon.Trichlorosilane gas and dichloro two in the chlorine-containing silane waste gas of condensate liquid are not being formed described in absorption
While hydrogen silicon gas, the impurity such as B, P can be also absorbed, therefore need to be through existing conventional chlorosilane purification procedures by impurity such as B, P
Remove, and in order to strengthen the removal effect of the impurity such as B, P, the second recovery subelement preferably includes resin absorbing column, is mingled with
The trichlorosilane gas and dichlorosilane gas for having the impurity such as B, P first adsorb through resin absorbing column, then through existing conventional chlorine
Recovery system is transported to after the processing of silane purification procedures.
Preferably, the second recovery subelement includes absorption tower, the chlorine-containing silane waste gas for not forming condensate liquid from
The bottom inflow end on absorption tower enters, and silicon tetrachloride material enters from the top on absorption tower, and the silicon tetrachloride material is as suction
Liquid (because the chlorinty of silicon tetrachloride is higher, therefore being in a liquid state) is received, is given up for absorbing the chlorine-containing silane for not forming condensate liquid
Trichlorosilane gas and dichlorosilane gas in gas, have absorbed the absorbing liquid of trichlorosilane gas and dichlorosilane gas
Handled after the discharge of the bottom on absorption tower through chlorosilane purification procedures and be transported to recovery system again, be not absorbed by liquid absorption and not
The chlorine-containing silane waste gas for forming condensate liquid is transported to chlorine as the remainder of exhaust gas after the discharge of the top outlet side on absorption tower
Silane washing unit.It is highly preferred that the operating pressure on the absorption tower is 0.05MPaG~0.2MPaG, absorbing liquid in absorption tower
Temperature be less than 25 DEG C, flow 30m3/ h~80m3/h。
Because high pressure is advantageous to absorption of the absorption tower to trichlorosilane gas and dichlorosilane gas, it is preferable that described
Second recovery subelement also includes supercharger, and its input is connected with the output end of the first recovery subelement, to receive first time
The chlorine-containing silane waste gas for not forming condensate liquid of subelement output is received, its output end is connected with the bottom inflow end on absorption tower, uses
In will not form the chlorine-containing silane exhaust gas of condensate liquid to 0.05MPaG~0.2MPaG described in the first recovery subelement output
After be delivered to absorption tower.
In order to ensure that absorption tower forced circulation absorbs, it is preferable that the second recovery subelement also includes circulating pump, and its is defeated
Enter end with absorb the bottom of the tower to be connected, to receive the trichlorosilane of the absorption gas and dichlorosilane gas of absorb the bottom of the tower discharge
Absorbing liquid, its output end respectively with absorption tower at the top of be connected, and through existing conventional chlorosilane purification procedures with recovery system
System is connected, and the absorbing liquid for having absorbed trichlorosilane gas and dichlorosilane gas for absorb the bottom of the tower to be discharged is pressurized to
0.3MPaG~1.0MPaG, and make major part (absorbing liquid 90%~99% accounted for after supercharging) conduct in the absorbing liquid after supercharging
Circulation fluid is back to absorption tower at the top of absorption tower, and makes the fraction (absorption accounted for after supercharging in the absorbing liquid after supercharging
Liquid 1%~10%) it is used as recovered liquid to be delivered to recovery system after existing conventional chlorosilane purification procedures processing, so circulation
Back and forth.Wherein, the specific ratio for the absorbing liquid that circulation fluid and recovered liquid account for after supercharging respectively need to be according in the absorbing liquid after supercharging
The content of silicon tetrachloride determines, specifically, need to ensure that the content of silicon tetrachloride in the absorbing liquid after supercharging is not less than 90%, enter
And ensure absorption tower to trichlorosilane gas and the assimilation effect of dichlorosilane gas.
Due to being back to absorption tower at the top of absorption tower mostly as circulation fluid in the absorbing liquid after supercharging, therefore inhale
Receiving the absorbing liquid in tower not only includes silicon tetrachloride material, in addition to circulation fluid, and the absorption trichlorine of absorb the bottom of the tower discharge
Trichlorosilane gas, dichlorosilane gas, silicon tetrachloride are contained in the absorbing liquid of hydrogen silicon gas and dichlorosilane gas
Material and circulation fluid, therefore also referred to as mixed liquor.
Because favors low temperature is in absorption of the absorption tower to trichlorosilane gas and dichlorosilane gas, it is preferable that described
Second recovery subelement also includes deep freezer, and its input is connected with the output end of circulating pump, to receive following for circulating pump output
Ring liquid, its output end at the top of absorption tower with being connected, for the circulation fluid to be cooled to after -45 DEG C~-20 DEG C again from absorption tower
Top is back to absorption tower.
It can be seen that the first recovery subelement through chlorosilane recovery unit and the second recovery are sub successively for the chlorine-containing silane waste gas
After unit, most of chlorosilane gas therein are recovered, only remaining nitrogen, hydrogen, hydrogen chloride gas and what is be not recovered lack
Amount chlorosilane gas (i.e. described remainder of exhaust gas) are discharged from the top outlet side on absorption tower and are transported to chlorosilane washing unit.
Wherein, absorption tower may absorb partial oxidation hydrogen, then unabsorbed hydrogen chloride gas will be from the top on absorption tower
Discharge and be transported to chlorosilane washing unit in outlet side.
It should be noted that the chlorosilane recovery unit can only include the first recovery subelement, second can be also only included
Subelement (its input directly receives the chlorine-containing silane waste gas) is reclaimed, can also include the first recovery subelement and second simultaneously
Reclaim subelement.
The chlorosilane washing unit is also connected with tail gas emptying unit, for the absorption tower of chlorosilane recovery unit to be arranged
Remaining chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas gone out elute, to remove in the remainder of exhaust gas
Chlorosilane gas and hydrogen chloride gas, and the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas is delivered to tail gas and put
Dummy cell.
Preferably, the chlorosilane washing unit includes eluting column, and the top in the eluting column is provided with spray head, uses
In making initial leacheate uniformly spray downwards, the remainder of exhaust gas of chlorosilane recovery unit output is from positioned at the lower section of spray head
Eluting column inlet end enter eluting column, the initial leacheate is by the remaining chlorosilane gas in the remainder of exhaust gas and chlorination
Hydrogen elute and formed hydrolyzate (hydrolyzate is the hydrolysate of chlorosilane, hydrogen chloride, main component be silicate,
The aqueous solution of silica and sodium chloride), to remove the chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas, the water
Liquid is solved from the discharge of elution tower bottom and processing (is realized) using filter press, filter etc. through existing conventional sewage treatment process
Afterwards, it is back in the spray head of eluting column as circulation fluid, so moves in circles, removes chlorosilane gas and hydrogen chloride gas
Remainder of exhaust gas tail gas emptying unit is transported to after the discharge of the top outlet side of eluting column；Wherein, the initial leacheate
Spray volume need to meet since the remainder of exhaust gas of chlorosilane recovery unit output enters eluting column inlet end to following
Ring liquid be back to first in the spray head of eluting column untill the ejection time because spray volume=ejection flow of initial leacheate
× time is sprayed, in the case where ejection flow is certain, spray volume is just determined by spraying the time, and spray volume meets above-mentioned ejection
During time conditions, the remainder of exhaust gas that can not only ensure from chlorosilane recovery unit output is opened into eluting column inlet end
Have what is uniformly sprayed downwards in time untill beginning into the spray head that circulation fluid is back to eluting column first, in eluting column always
Leacheate, it is also ensured that also have the leacheate uniformly sprayed downwards always in the cyclic process of circulation fluid, in eluting column.It is more excellent
Selection of land, the operating pressure of the eluting column are 0.01MPaG~0.05MPaG, and the temperature of leacheate is 25 DEG C~60 in eluting column
DEG C, flow 50m3/ h~150m3/h。
It is another on the one hand in order to maintain the water balance of circulation fluid because circulation fluid has water loss in its cyclic process
Aspect is in order to reduce the salinity of leacheate in eluting column, it is preferable that the spray head is additionally operable to make supplement leacheate equal downwards
Even ejection, and the amount of the supplement leacheate need to be according to the salinity of leacheate in the water balance degree and eluting column of circulation fluid
It is determined that.The initial leacheate and supplement leacheate can use pure water or alkali lye.
Certainly, the spray head can use multigroup, and every group may include multiple spray heads, and the plurality of spray head can form square
Battle array, such as circle matrix or square matrix, a portion spray head are used for initial leacheate and supplement the injection of leacheate, another portion
Shower nozzle is divided to be used for the injection of circulation fluid.
In order that the hydrolysis of the remaining chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas is more abundant, it is excellent
Selection of land, the chlorosilane washing unit also include the stirring subelement positioned at elution tower bottom, for hydrolysis described in uniform stirring
Liquid.
Meanwhile in order to ensure that circulation fluid can circulate well, it is preferable that the chlorosilane washing unit also includes pressurization
Pump, its input are connected with elution tower bottom, and to receive the hydrolyzate of elution tower bottom discharge, its output end is through existing routine
Sewage disposal process is connected with the spray head of eluting column, for by elute tower bottom discharge hydrolyzate be pressurized to 0.4MPaG~
1.0MPaG, and the hydrolyzate after supercharging is back to the spray head of eluting column after the processing of existing conventional sewage treatment process
In.Moreover, carrying out pressurized treatments to hydrolyzate by force (forcing) pump, hydrolyzate is also helped through existing conventional sewage treatment process
It is back to after processing in the spray head of eluting column, internal circulating load is larger.In addition, force (forcing) pump can also receive the warp of elution tower bottom discharge
The hydrolyzate after subelement is sufficiently stirred is stirred, is arranged such, when the amount of the remainder of exhaust gas of chlorosilane recovery unit output
When larger, remaining chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas can also hydrolyzed abundant, prevent the water to be formed
Substantial amounts of gas (remaining chlorosilane gas and hydrogen chloride gas in i.e. described remainder of exhaust gas) is carried secretly in solution liquid, and then prevents from adding
Press pump produces cavitation erosion.
In order to prevent the steam in eluting column from falling to go here and there to the pipe between eluting column inlet end and the top outlet side on absorption tower
In road, avoid steam that hydrolysis occurs with a small amount of chlorosilane gas in the remainder of exhaust gas of absorption tower discharge, and produce
Hydrolysate and block the pipeline, it is preferable that the chlorosilane washing unit also include mixing subelement, its input receive chlorine
The remainder of exhaust gas and part circulation fluid of silane recovery unit output, its output end is connected with eluting column inlet end, for making
The remainder of exhaust gas and part circulation fluid of chlorosilane recovery unit output enter uniformly after mixing, then through eluting column inlet end
Enter eluting column.That is, the part in circulation fluid is back in the spray head of eluting column, the blended subelement of another part
After uniformly being mixed with the remainder of exhaust gas of chlorosilane recovery unit output, enter eluting column from eluting column inlet end, wherein, warp
The circulation fluid that mixing subelement enters eluting column accounts for the remainder of exhaust gas that the ratio of circulation fluid total amount can discharge according to absorption tower
The amounts of middle chlorosilane gas determines, generally, the amount that blended subelement enters the circulation fluid of eluting column will be far fewer than straight
Connect the amount of the circulation fluid in the spray head for being back to eluting column.
It can be seen that chlorosilane recovery unit output the remainder of exhaust gas after chlorosilane washing unit, remaining chlorine therein
Silane gas and hydrogen chloride gas are leached, so as to remove the chlorosilane gas and hydrogen chloride gas in remainder of exhaust gas,
Only remaining nitrogen and hydrogen.
Tail gas emptying unit be used for by chlorosilane washing unit export described in remove chlorosilane gas and chlorination
The remainder of exhaust gas emptying of hydrogen.
Preferably, the tail gas emptying unit uses water sealed tank, the top outlet side of eluting column and the inlet end of water sealed tank
It is connected, the output end of the force (forcing) pump is also connected with water seal upper end, for making the major part in the hydrolyzate after supercharging (account for increasing
Hydrolyzate 90%~98% after pressure, the first highly pressured hydrolysis liquid can be called) after the processing of existing conventional sewage treatment process
Be back in the spray head of eluting column, and make in the hydrolyzate after supercharging fraction (account for supercharging after hydrolyzate 2%~
10%, the second highly pressured hydrolysis liquid can be called, the flow that need to ensure the second highly pressured hydrolysis liquid is 1m3/ h~5m3/ h) enter water seal
Tank, and eluting column is back to after the discharge of the bottom of water sealed tank, such as may return in the spray head of eluting column, also it may return to
Tower bottom is eluted, and then participates in circulation.Moreover, force (forcing) pump not only contribute to the first highly pressured hydrolysis liquid through existing conventional sewage at
It is back to after the processing of science and engineering sequence in the spray head of eluting column, also helps the second highly pressured hydrolysis liquid into tail gas emptying unit, and
Internal circulating load is larger.
The effect for setting water sealed tank is isolation air, avoids air from entering eluting column.Specifically, air is avoided from water sealed tank
Inlet end to the pipeline between eluting column outlet side enters in eluting column, and causes the oxygen in the hydrogen and air in eluting column
Mixing reaches explosion limit and explosion accident occurs.Moreover, the waste gas of eluting column discharge passes through (mainly comprising nitrogen and hydrogen)
It is vented again after water sealed tank, on the one hand, the moisture that can increase in emptying end gas (contains without moisture in the waste gas of water sealed tank
Measure relatively low), the hidden danger such as quick-fried is dodged so as to reduce, can also increase the humidity at water sealed tank outlet side, so as to prevent the hair of tempering phenomenon
It is raw；On the other hand, if also including micro chlorosilane gas in the waste gas of eluting column discharge, also can after water sealed tank is washed
The micro chlorosilane gas are thoroughly removed, so as to ensure only to be steamed in the tail gas of water sealed tank emptying comprising nitrogen, hydrogen and water
Gas.
Embodiment 2：
As shown in Fig. 2 the present embodiment provides a kind of recycling and processing device of chlorine-containing silane waste gas, including：Chilled brine is pre-
Cooler 2, supercharger 6, absorption tower 8, circulating pump 11, deep freezer 12, resin absorbing column 15, mixing subelement 18, eluting column 19, stir
Mix subelement 20, spray head 21, force (forcing) pump 24, water sealed tank 28.
The operation principle of the recycling and processing device is：
After chlorine-containing silane waste gas 1 enters chilled brine forecooler 2, which part chlorosilane gas form chlorosilane condensate liquid
3, and recovery system 4 is transported to, and remaining chlorine-containing silane waste gas 5 (does not form the chloride silicon of condensate liquid described in embodiment 1
Alkane waste gas) enter supercharger 6, turn into high pressure exhaust gas 7, high pressure exhaust gas 7 after supercharger 6 is pressurized to 0.05MPaG~0.2MPaG
Into after absorption tower 8, mixed with the silicon tetrachloride material 9 entered from the top of absorption tower 8 so that the trichlorine hydrogen in high pressure exhaust gas 7
The impurity such as silicon gas, dichlorosilane gas and B, P is absorbed by silicon tetrachloride material 9 and forms mixed liquor 10 and from absorption tower 8
Bottom discharge, and do not absorbed by absorption tower 8 unrecovered gas 17 (remainder of exhaust gas i.e. described in embodiment 1, including nitrogen, hydrogen,
Hydrogen chloride gas and a small amount of chlorosilane gas) discharged from the top outlet side on absorption tower 8, after mixed liquor 10 enters circulating pump 11
0.3MPaG~1.0MPaG is pressurized to, the mixed liquor 10 after wherein most supercharging enters deep freezer 12 as circulation fluid 13,
It is back to absorption tower 8, the mixing after fraction supercharging at the top of absorption tower again after deep freezer 12 is cooled to -45 DEG C~-20 DEG C
Liquid 10 is transported to recovery system after resin absorbing column 15 and chlorosilane purification procedures 16 carry out B, P removal of impurities successively
4, so move in circles；
The blended subelement 18 of unrecovered gas 17 of the top outlet side discharge on absorption tower 8 enters eluting column 19, initial leaching
Washing lotion and supplement leacheate (being referred to as leacheate 22) successively uniformly spray downwards from spray head 21, and in unrecovered gas 17
Hydrogen chloride gas and a small amount of chlorosilane gas occur hydrolysis and form hydrolyzate 23, and the agitated subelement 20 of hydrolyzate 23 is equal
Discharged after even stirring from the bottom of eluting column 19, and enter force (forcing) pump 24, force (forcing) pump 24 by hydrolyzate 23 be pressurized to 0.4MPaG~
1.0MPaG, and be pressurized after hydrolyzate in mostly as the first highly pressured hydrolysis liquid 25 through sewage disposal process 32 processing after
It is back to as the part of circulation fluid 31 in the spray head 21 of eluting column 19, the blended subelement 18 in part and unrecovered gas 17 are uniform
Eluting column 19 is entered back into after mixing, the fraction in hydrolyzate after supercharging is as the second highly pressured hydrolysis liquid 26 from water seal upper end
Into water sealed tank 28, and elution tower bottom is back to as circulation fluid 30 after the discharge of water seal pot bottom, so moved in circles, and
The unreacting gas 27 for having neither part nor lot in hydrolysis (remove chlorosilane gas and the residue of hydrogen chloride gas are given up described in embodiment 1
Gas, including nitrogen and hydrogen) discharged from the top outlet side of eluting column 19；
Eluting column 19 top outlet side discharge unreacting gas 27 through water sealed tank 28 washing after, formed tail gas 29 (including
Nitrogen, hydrogen and vapor), and discharged by the top outlet side of water sealed tank 28.
Other structures and effect in the present embodiment are all same as Example 1, repeat no more here.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses
Mode, but the invention is not limited in this.For those skilled in the art, the essence of the present invention is not being departed from
In the case of refreshing and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (12)
- A kind of 1. recycling and processing device of chlorine-containing silane waste gas, it is characterised in that including：Chlorosilane recovery unit, chlorosilane leaching Unit and tail gas emptying unit are washed,The chlorosilane recovery unit is connected with chlorosilane washing unit, for by the part chlorosilane gas in chlorine-containing silane waste gas Body is reclaimed, and remainder of exhaust gas is delivered into chlorosilane washing unit；The chlorosilane washing unit is also connected with tail gas emptying unit, for by the remaining chlorosilane gas in the remainder of exhaust gas Body and hydrogen chloride gas elute, and to remove the chlorosilane gas and hydrogen chloride gas in the remainder of exhaust gas, and will remove The remainder of exhaust gas of chlorosilane gas and hydrogen chloride gas is delivered to tail gas emptying unit；The tail gas emptying unit is used to the remainder of exhaust gas for removing chlorosilane gas and hydrogen chloride gas being vented；The chlorosilane washing unit includes eluting column, and the top in the eluting column is provided with spray head, for making initially to drench Washing lotion is uniformly sprayed downwards, and the initial leacheate uses pure water or alkali lye, and the residue of chlorosilane recovery unit output is given up Gas enters eluting column from the eluting column inlet end positioned at the lower section of spray head, and the initial leacheate is by the remainder of exhaust gas Remaining chlorosilane gas and hydrogen chloride gas elute and form hydrolyzate, to remove the chlorosilane gas in the remainder of exhaust gas Body and hydrogen chloride gas, the hydrolyzate are the hydrolysates of chlorosilane and hydrogen chloride, and main component is silicate, silica With the aqueous solution of sodium chloride, the hydrolyzate is from the discharge of elution tower bottom and after the processing of sewage disposal process, as circulation fluid Be back in the spray head of eluting column, so move in circles, remove the remainder of exhaust gas of chlorosilane gas and hydrogen chloride gas from Tail gas emptying unit is transported to after the top outlet side discharge of eluting column；Wherein, the spray volume of the initial leacheate need to expire Foot returns first since the remainder of exhaust gas of chlorosilane recovery unit output enters eluting column inlet end to circulation fluid Ejection time untill into the spray head of eluting column, the sewage disposal process are realized using filter press and filter；The chlorosilane washing unit also includes mixing subelement, and its input receives the described surplus of chlorosilane recovery unit output Remaining waste gas and part circulation fluid, its output end are connected with eluting column inlet end, for making the chlorosilane recovery unit output The remainder of exhaust gas and part circulation fluid enter eluting column uniformly after mixing, then through eluting column inlet end, to cause in circulation fluid A part be back in the spray head of eluting column, the blended subelement of another part exports described with chlorosilane recovery unit Enter eluting column from eluting column inlet end after the uniform mixing of remainder of exhaust gas.
- 2. recycling and processing device according to claim 1, it is characterised in that the chlorosilane recovery unit includes first time Receive subelement, its input receives the chlorine-containing silane waste gas, its output end respectively with recovery system and chlorosilane washing unit It is connected, for making the part chlorosilane gas in the chlorine-containing silane waste gas form condensate liquid, and the condensate liquid is delivered to Recovery system, and it is delivered to chlorosilane elution list using the chlorine-containing silane waste gas for not forming condensate liquid as the remainder of exhaust gas Member.
- 3. recycling and processing device according to claim 2, it is characterised in that the first recovery subelement uses precooling Device, for the chlorine-containing silane waste gas to be cooled into -10 DEG C~0 DEG C.
- 4. recycling and processing device according to claim 2, it is characterised in that the chlorosilane recovery unit also includes second Subelement is reclaimed, its input receives the chlorine-containing silane waste gas for not forming condensate liquid of the first recovery subelement output, and it is exported End is connected through chlorosilane purification procedures with recovery system respectively, and is connected with chlorosilane washing unit, for the non-shape by described in Through chlorosilane purification procedures after being absorbed into the trichlorosilane gas in the chlorine-containing silane waste gas of condensate liquid and dichlorosilane gas Processing is delivered to recovery system again, and will not be absorbed and do not form the chlorine-containing silane waste gas of condensate liquid as described remaining useless Gas is delivered to chlorosilane washing unit.
- 5. recycling and processing device according to claim 4, it is characterised in that the second recovery subelement includes absorbing Tower, the chlorine-containing silane waste gas for not forming condensate liquid enter from the bottom inflow end on absorption tower, and silicon tetrachloride material is from absorption The top of tower enters, and the silicon tetrachloride material gives up as absorbing liquid for absorbing the chlorine-containing silane for not forming condensate liquid Trichlorosilane gas and dichlorosilane gas in gas, have absorbed the absorbing liquid of trichlorosilane gas and dichlorosilane gas Handled after the discharge of the bottom on absorption tower through chlorosilane purification procedures and be transported to recovery system again, be not absorbed by liquid absorption and not The chlorine-containing silane waste gas for forming condensate liquid is transported to chlorine as the remainder of exhaust gas after the discharge of the top outlet side on absorption tower Silane washing unit.
- 6. recycling and processing device according to claim 5, it is characterised in that the second recovery subelement also includes supercharging Machine, its input receive the chlorine-containing silane waste gas for not forming condensate liquid of the first recovery subelement output, and its output end is with absorbing The bottom inflow end of tower is connected, for the chlorine-containing silane waste gas for not forming condensate liquid described in the first recovery subelement output to be increased Absorption tower is delivered to after being depressed into 0.05MPaG~0.2MPaG.
- 7. recycling and processing device according to claim 5, it is characterised in that the second recovery subelement also includes circulation Pump, its input receive the absorbing liquid for having absorbed trichlorosilane gas and dichlorosilane gas of absorb the bottom of the tower discharge, its Output end with being connected at the top of absorption tower, and is connected, for by absorption tower bottom through chlorosilane purification procedures with recovery system respectively Portion's discharge absorbed trichlorosilane gas and the absorbing liquid of dichlorosilane gas is pressurized to 0.3MPaG~1.0MPaG, and make Absorption tower is back at the top of absorption tower mostly as circulation fluid in absorbing liquid after supercharging, and makes the absorption after supercharging Fraction in liquid is delivered to recovery system as recovered liquid after the processing of chlorosilane purification procedures.
- 8. recycling and processing device according to claim 7, it is characterised in that the second recovery subelement also includes deep cooling Device, its input receive the circulation fluid of circulating pump output, and its output end at the top of absorption tower with being connected, for the circulation fluid is cold But to being back to absorption tower at the top of absorption tower again after -45 DEG C~-20 DEG C.
- 9. recycling and processing device according to claim 1, it is characterised in that the spray head is additionally operable to make supplement leacheate Uniformly spray downwards.
- 10. recycling and processing device according to claim 1, it is characterised in that the chlorosilane washing unit also includes position In the stirring subelement of elution tower bottom, for hydrolyzate described in uniform stirring.
- 11. recycling and processing device according to claim 1, it is characterised in that the chlorosilane washing unit also includes adding Press pump, its input receive the hydrolyzate of elution tower bottom discharge, spray of its output end through sewage disposal process and eluting column Head is connected, and for the hydrolyzate for eluting tower bottom discharge to be pressurized into 0.4MPaG~1.0MPaG, and makes the hydrolyzate after supercharging It is back to after the processing of sewage disposal process in the spray head of eluting column.
- 12. recycling and processing device according to claim 11, it is characterised in that the tail gas emptying unit uses water seal Tank, the top outlet side of eluting column are connected with the inlet end of water sealed tank, the output end of the force (forcing) pump also with water seal upper end phase Even, most of it is back to eluting column after the processing of existing conventional sewage treatment process for make in the hydrolyzate after supercharging In spray head, and the fraction in the hydrolyzate after supercharging is entered water sealed tank, and returned after the discharge of the bottom of water sealed tank To eluting column.
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| CN107441913A (en) * | 2016-05-30 | 2017-12-08 | 新特能源股份有限公司 | The exhaust treatment system and processing method of polysilicon production process |
| CN107648979A (en) * | 2016-07-26 | 2018-02-02 | 新特能源股份有限公司 | The method and system of tail gas in a kind of processing production of polysilicon |
| CN106276924B (en) * | 2016-08-22 | 2018-08-10 | 昆明理工大学 | Method that is a kind of while handling chlorosilane raffinate and exhaust gas |
| CN106731611A (en) * | 2017-01-10 | 2017-05-31 | 乐山职业技术学院 | A kind of polysilicon exhaust-gas treatment and residual heat using device and technique |
| CN106621757B (en) * | 2017-02-21 | 2022-09-16 | 德山化工（浙江）有限公司 | Chlorosilane analysis waste gas recovery treatment device and treatment method |
| CN107970756A (en) * | 2017-11-28 | 2018-05-01 | 南京德邦金属装备工程股份有限公司 | A kind of chlorosilane waste gas processing method |
| CN110143595A (en) * | 2019-06-04 | 2019-08-20 | 新疆大全新能源股份有限公司 | The recovery process of tail gas is restored in a kind of production of polysilicon |
| CN115414771A (en) * | 2022-08-11 | 2022-12-02 | 中国恩菲工程技术有限公司 | Tail gas treatment system and method for silicon-based electronic product production process |
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Application publication date: 20151125 Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2023990000586 Denomination of invention: A recovery and treatment device for waste gas containing chlorosilane Granted publication date: 20180209 License type: Common License Record date: 20230605 |