CN109081351A - A kind of processing system and method for the high-boiling components that cold hydrogenation system generates - Google Patents
A kind of processing system and method for the high-boiling components that cold hydrogenation system generates Download PDFInfo
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- CN109081351A CN109081351A CN201811012403.2A CN201811012403A CN109081351A CN 109081351 A CN109081351 A CN 109081351A CN 201811012403 A CN201811012403 A CN 201811012403A CN 109081351 A CN109081351 A CN 109081351A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
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Abstract
The invention discloses the processing systems and method of a kind of high-boiling components that cold hydrogenation system generates, the processing system includes sequentially connected polychlorostyrene silane weight-removing column, weight-removing column condenser, weight-removing column return tank, weight-removing column reflux pump, preheater, polychlorostyrene silane cracker and chlorosilane evaporator, polychlorostyrene silane weight-removing column material inlet connects high-boiling components input channel, and chlorosilane evaporator gas vent passes to knockout tower.It is equipped with catalyst alkalinity quaternary amine base macro porous crosslinking resin in polychlorostyrene silane cracker, is constantly passed through hydrogen chloride cracked gas in polychlorostyrene silane cracker, the high-boiling components in polychlorostyrene silane cracker react to obtain chlorosilane mixture with hydrogen chloride cracked gas.The method of the present invention process flow is simple, high-boiling components are realized from purification, cracking again to the step of separation, avoid prior art high-boiling components hydrolysis influence caused by environment, chlorosilane raw material needed for the chlorosilane that high-boiling components crack can be used as organosilicon production, reduces the production cost of polysilicon.
Description
Technical field
The present invention relates to a kind of processing systems of high-boiling components that cold hydrogenation system matched with polysilicon production process generates
And method, belong to polysilicon preparation technical field.
Background technique
Global production of polysilicon prevailing technology uses improved Siemens, and this method is with SiHCl3In high temperature H2In environment also
Original, which is deposited on silicon core, forms polysilicon, the tail gas H of reduction furnace discharge2、SiHCl3、SiCl4、SiH2Cl2With HCl by separating
Recycling afterwards.The cold hydrogenation process of mating improved Siemens is by SiCl4, Si powder and H2In 500 DEG C of temperature and 1.5MPa
Under pressure condition, SiHCl is converted by being catalyzed reaction3.In the crude product trichlorosilane that cold hydrogenation process obtains, containing a large amount of
Silicon tetrachloride and a small amount of high-boiling components, metal chloride, it is therefore desirable to separating-purifying be carried out to trichlorosilane, which generally exists
It is completed in rectifying column.
In the actual production process, the high-boiling components 99% isolated from tower bottom of rectifying tower are polychlorostyrene silane, are handled it
Usually pass through a large amount of STC (SiCl of concentration and recovery4) be hydrolyzed together with solid impurities such as metal chlorides afterwards, consumption chlorine member
Element is more.Hydrolysis neutralizes the calcium chloride generated and needs to be handled with concentration technology with high salt, and energy consumption is higher；Hydrolyze the salt generated
Acid needs to be neutralized with lye；Hydrolysis generates a large amount of silicon mud after neutralizing, and needs buried processing, not only can be to environment
It pollutes, meanwhile, it will also result in the waste of a large amount of chlorine and Si element, be unfavorable for the sustainable development of production of polysilicon.
Summary of the invention
In view of this, in view of the deficiencies of the prior art, the present invention provides a kind of place of high-boiling components that cold hydrogenation system generates
System and method are managed, the wasting of resources is reduced, reduce environmental pollution.
In order to solve the above technical problems, technical solution of the present invention provide firstly a kind of cold hydrogenation system generate it is high boiling
The processing system of object, it includes sequentially connected polychlorostyrene silane weight-removing column, weight-removing column condenser, weight-removing column return tank, weight-removing column
Reflux pump, preheater, polychlorostyrene silane cracker and chlorosilane evaporator, it is defeated that polychlorostyrene silane weight-removing column material inlet connects high-boiling components
Enter pipeline, chlorosilane evaporator gas vent passes to knockout tower.
Based on above system, the present invention also provides a kind of processing methods of high-boiling components that cold hydrogenation system generates, it is wrapped
Include following steps:
(1) high-boiling components of the rectifying column extraction in cold hydrogenation system rectification section enter polychlorostyrene silicon through high-boiling components input channel
Beavy metal impurity is got rid of in alkane weight-removing column enters back into polychlorostyrene silane cracker；
(2) catalyst alkalinity quaternary amine base macro porous crosslinking resin, polychlorostyrene silane cracker are equipped in polychlorostyrene silane cracker
Interior to be constantly passed through hydrogen chloride cracked gas, the high-boiling components in polychlorostyrene silane cracker react to obtain chlorine silicon with hydrogen chloride cracked gas
Alkane mixture；
(3) by the chlorosilane mixture that step (2) obtains be input in chlorosilane evaporator heating evaporation be after gas again
It is separated by knockout tower up to silicon tetrachloride and trichlorosilane.
Further, the high-boiling components that rectifying column produces in the step (1) should remove before entering polychlorostyrene silane weight-removing column
Metal chloride therein.Because of metal chloride, especially alchlor, it is during pipeline exports, due to temperature
It gradually decreases, alchlor can crystallize, and the alchlor of crystallization becomes larger while silicon powder being wrapped in inside crystal, gradually
Fouling and block pipeline, cause system shutdown, service conduits.
Preferably, the metal chloride in high-boiling components is removed using the method for cooling and stirring sedimentation separation.By cold
But it stirs, high-boiling components and metal chloride form suspension, and suspension can be by alchlor from high-boiling components through sedimentation separation
It separates, avoids alchlor and crystallize the case where the blocking pipeline that become larger.
Further, the general formula of step (2) the neutral and alkali quaternary amine base macro porous crosslinking resin is Ry-NHx, x=0~2, R
For Long carbon chain.The use granularity of the macro porous crosslinking resin is 0.5~0.9mm.Select alkaline quaternary amine base macro porous crosslinking resin conduct
Catalyst because itself has the amino of catalytic action, while being solid-state, can be in fixed bed arrangement in cracker, will not
It is come out with sewage discharge, the consequence of sewage treatment burden can not be handled or increase by avoiding sewage.
The common catalyst of polychlorostyrene silane cracking reaction is the n,N-Dimethylaniline of liquid in the prior art, it can be with
Sewage discharge, but sewage treatment can not handle the catalyst, lead to the pollution of environment.
Amino has the work of open catalytic activation to chemical bonds such as Si-Si, Si-Cl, Si-C of chlorosilane, polychlorostyrene silane
With, it is allowed to become the very high free group of activity, and these free groups can easily be combined into new molecule, this is also weak
Basic amine group resin can play the essential reason of anti-disproportionation.Therefore can just be used to be catalyzed polychlorostyrene silane using this characteristic
Si-Si bond open, single silicon chlorosilane is cracked into, below with catalyst R-NH2For illustratively reaction process of the invention
Principle:
Compared with prior art, it is miscellaneous to pass through the heavy metal that polychlorostyrene silane weight-removing column eliminates in high-boiling components first by the present invention
Matter, the specific functional groups for avoiding catalyst in beavy metal impurity and cracker generate apparent complexing colour developing phenomenon, cause to urge
The excessive consumption and poisoning of agent；By selecting suitable cracked gas and catalyst, catalyst emission is avoided to environment
Caused by pollute, while also ensuring that polychlorostyrene silane is cracked into the lysis efficiency of chlorosilane.The method of the present invention process flow is simple,
High-boiling components are realized from purification, cracking again to the step of separation, prior art high-boiling components is avoided and hydrolyzes the shadow caused by environment
It rings, chlorosilane raw material needed for the chlorosilane that high-boiling components crack can be used as organosilicon production reduces the production of polysilicon
Cost.
Detailed description of the invention
Fig. 1 is the flow diagram of the processing system for the high-boiling components that the cold hydrogenation system of the present invention generates.
Marginal data:
1- high-boiling components input channel；2- polychlorostyrene silane weight-removing column；3- weight-removing column condenser；4- weight-removing column return tank；5- is de-
Weight tower reflux pump；6- preheater；7- polychlorostyrene silane cracker；8- chlorosilane evaporator；9- knockout tower.
Specific embodiment
It is with reference to the accompanying drawing and specific real in order to make those skilled in the art more fully understand technical solution of the present invention
Applying mode, the present invention is described in further detail.
Referring to Fig. 1, the present invention provides a kind of processing systems of high-boiling components that cold hydrogenation system generates, it includes successively connecting
Polychlorostyrene silane weight-removing column 2, weight-removing column condenser 3, weight-removing column return tank 4, weight-removing column reflux pump 5, preheater 6, the polychlorostyrene silicon connect
Alkane cracker 7 and chlorosilane evaporator 8,2 material inlet of polychlorostyrene silane weight-removing column connect high-boiling components input channel 1, and chlorosilane steams
Hair 8 gas vent of tank passes to knockout tower 9.
The process flow of above-mentioned processing system are as follows: the high-boiling components of the rectifying column extraction in cold hydrogenation system rectification section are (excellent
High-boiling components after choosing removal metal chloride) enter in polychlorostyrene silane weight-removing column 2 through high-boiling components input channel 1, the weight of hardly possible volatilization
Metal impurities are retained in dropping liq, and high-boiling components are evaporated to gas phase, rise to weight-removing column tower top constantly to complete a huge sum of money
Belong to the separation of impurity, gas phase high-boiling components enter weight-removing column condenser 3 and are condensed into liquid, and condensate liquid enters in weight-removing column return tank 4
Storage, the effect through reflux pump 5, a part of condensate liquid return in weight-removing column 2, and the preheated device 6 of remainder condensate liquid is heated to
It is input to after reaction temperature and cracking reaction occurs under the effect of the catalyst with cracked gas in polychlorostyrene silane cracker 7 obtains chlorine
Silane mixture, chlorosilane mixture are input to heating evaporation in chlorosilane evaporator 8 and separate to pass through knockout tower 9 after gas again
Obtain silicon tetrachloride and trichlorosilane.
Based on above-mentioned processing system, a kind of processing method for the high-boiling components that cold hydrogenation system generates provided by the invention, it
The following steps are included:
(1) high-boiling components of the rectifying column extraction in cold hydrogenation system rectification section enter polychlorostyrene silicon through high-boiling components input channel
Beavy metal impurity is got rid of in alkane weight-removing column enters back into polychlorostyrene silane cracker；
(2) catalyst alkalinity quaternary amine base macro porous crosslinking resin, polychlorostyrene silane cracker are equipped in polychlorostyrene silane cracker
Interior to be constantly passed through hydrogen chloride cracked gas, the high-boiling components in polychlorostyrene silane cracker react to obtain chlorine silicon with hydrogen chloride cracked gas
Alkane mixture；
(3) by the chlorosilane mixture that step (2) obtains be input in chlorosilane evaporator heating evaporation be after gas again
It is separated by knockout tower up to silicon tetrachloride and trichlorosilane.
Illustrate the effect of the method for the present invention with specific embodiment below, high-boiling components used in following embodiments be Sichuan forever
The tower bottoms that rectification section 6# rectifying column produces in the auspicious cold hydrogenation system of new energy Co., Ltd is through 90~130 DEG C of step-up temperature
It is obtained after the most of silicon tetrachloride of concentration removal, again after cooling and stirring removal metal chloride, high-boiling components are poly- in tower bottoms
The content of chlorosilane is 14%, and the group after heating concentration is divided into 0.8% STC, 6.3% HCl, and remainder is polychlorostyrene silane.
Embodiment 1:
High-boiling components are heated to 90 DEG C through preheater after weight-removing column removes removing heavy-metal impurities and enter in polychlorostyrene silane cracker,
It is equipped with catalyst alkalinity quaternary amine base macro porous crosslinking resin (solid-state) in polychlorostyrene silane cracker, is passed through in polychlorostyrene silane cracker
Cracked gas (hydrogen chloride), polychlorostyrene silane cracker interior reaction temperature are 90 DEG C, pressure 0.2MPa, high-boiling components and cracking gas
Precursor reactant obtains chlorosilane mixture, and it is to lead to after gas again that chlorosilane mixture is input to heating evaporation in chlorosilane evaporator again
Knockout tower is crossed to separate up to silicon tetrachloride and trichlorosilane.The chlorosilane amount obtained with gas-chromatography test cracking reaction, specifically
It see the table below 1.
Embodiment 2:
High-boiling components are heated to 90 DEG C through preheater after weight-removing column removes removing heavy-metal impurities and enter in polychlorostyrene silane cracker,
Polychlorostyrene silane cracker is provided with catalyst benzonitrile (liquid), and cracking gas (hydrogen), polychlorostyrene are passed through in polychlorostyrene silane cracker
Silane cracker interior reaction temperature is 90 DEG C, and pressure 0.2MPa, high-boiling components react to obtain chlorosilane mixture with cracked gas,
It is to separate four chlorinations to obtain the final product by knockout tower again after gas that chlorosilane mixture is input in chlorosilane evaporator heating evaporation again
Silicon and trichlorosilane.The chlorosilane amount obtained with gas-chromatography test cracking reaction, is specifically shown in the following table 1.
Embodiment 3:
High-boiling components are heated to 90 DEG C through preheater after weight-removing column removes removing heavy-metal impurities and enter in polychlorostyrene silane cracker,
Polychlorostyrene silane cracker is provided with catalyst 1,6- hexamethylene diamine (liquid), is passed through cracking gas (chlorine) in polychlorostyrene silane cracker,
Polychlorostyrene silane cracker interior reaction temperature is 90 DEG C, pressure 0.2MPa, and high-boiling components, which react to obtain with cracked gas chlorosilane, to be mixed
Close object, it is to separate to obtain the final product four by knockout tower again after gas that chlorosilane mixture is input in chlorosilane evaporator heating evaporation again
Silicon chloride and trichlorosilane.The chlorosilane amount obtained with gas-chromatography test cracking reaction, is specifically shown in the following table 1.
Embodiment 4:
High-boiling components are heated to 90 DEG C through preheater after weight-removing column removes removing heavy-metal impurities and enter in polychlorostyrene silane cracker,
Polychlorostyrene silane cracker is provided with catalyst n, accelerine (liquid), is passed through cracking gas (chlorine in polychlorostyrene silane cracker
Change hydrogen), polychlorostyrene silane cracker interior reaction temperature is 90 DEG C, and pressure 0.2MPa, high-boiling components react to obtain chlorine with cracked gas
Silane mixture, it is after gas again by knockout tower separation that chlorosilane mixture is input in chlorosilane evaporator heating evaporation again
Up to silicon tetrachloride and trichlorosilane.The chlorosilane amount obtained with gas-chromatography test cracking reaction, is specifically shown in the following table 1.
The cracking of table 1 front and back high-boiling components and chlorosilane degree (%)
DCS: dichlorosilane, TCS: trichlorosilane, STC: silicon tetrachloride.
The main component general formula of concentration high-boiling components meets SinCl2N+2 (n > 1).
As can be seen from the above table, the yield of STC of the present invention is higher than embodiment 2 and 3, slightly below embodiment 4, but the present invention
Catalyst is granular solid, can be in fixed bed arrangement, will not be discharged with sewage, the catalyst of excess-three embodiment is liquid
State is discharged with sewage, increases sewage treatment burden.
To sum up, the method for the present invention process flow is simple, realizes high-boiling components from purification, cracking again to the step of separation, keeps away
Prior art high-boiling components hydrolysis influence caused by environment is exempted from, the chlorosilane that high-boiling components crack can be used as organosilicon production
Required chlorosilane raw material, reduces the production cost of polysilicon.
It should be pointed out that above-mentioned preferred embodiment is not construed as limitation of the present invention, protection scope of the present invention
It should be defined by the scope defined by the claims..For those skilled in the art, this hair is not being departed from
In bright spirit and scope, several improvements and modifications can also be made, these improvements and modifications also should be regarded as protection of the invention
Range.
Claims (6)
1. a kind of processing system for the high-boiling components that cold hydrogenation system generates, it is characterised in that: including sequentially connected polychlorostyrene silane
Weight-removing column, weight-removing column condenser, weight-removing column return tank, weight-removing column reflux pump, preheater, polychlorostyrene silane cracker and chlorosilane steam
Tank is sent out, polychlorostyrene silane weight-removing column material inlet connects high-boiling components input channel, and chlorosilane evaporator gas vent passes to knockout tower.
2. a kind of processing method for the high-boiling components that cold hydrogenation system generates, it is characterised in that: the following steps are included:
(1) high-boiling components of the rectifying column extraction in cold hydrogenation system rectification section enter polychlorostyrene silane through high-boiling components input channel and take off
Beavy metal impurity, which is got rid of, in weight tower enters back into polychlorostyrene silane cracker；
(2) it is equipped with catalyst alkalinity quaternary amine base macro porous crosslinking resin in polychlorostyrene silane cracker, in polychlorostyrene silane cracker not
It is open close enter hydrogen chloride cracked gas, the high-boiling components in polychlorostyrene silane cracker react to obtain chlorosilane with hydrogen chloride cracked gas mixed
Close object；
(3) chlorosilane mixture that step (2) obtains is input in chlorosilane evaporator heating evaporation is to pass through after gas again
Knockout tower separates up to silicon tetrachloride and trichlorosilane.
3. the processing method for the high-boiling components that a kind of cold hydrogenation system according to claim 2 generates, it is characterised in that: described
The high-boiling components that rectifying column produces in step (1) should remove metal chloride therein before entering polychlorostyrene silane weight-removing column.
4. the processing method for the high-boiling components that a kind of cold hydrogenation system according to claim 3 generates, it is characterised in that: use
The method of cooling and stirring sedimentation separation removes the metal chloride in high-boiling components.
5. the processing method for the high-boiling components that a kind of cold hydrogenation system according to claim 2 generates, it is characterised in that: described
The general formula of step (2) neutral and alkali quaternary amine base macro porous crosslinking resin is Ry-NHx, x=0~2, R are Long carbon chain.
6. the processing method for the high-boiling components that a kind of cold hydrogenation system according to claim 2 generates, it is characterised in that: described
The granularity of step (2) neutral and alkali quaternary amine base macro porous crosslinking resin is 0.5~0.9mm.
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Cited By (5)
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| CN109908621A (en) * | 2019-04-12 | 2019-06-21 | 四川永祥多晶硅有限公司 | Slurry separates preposition transportation system and method |
| CN110627069A (en) * | 2019-10-22 | 2019-12-31 | 中国恩菲工程技术有限公司 | System for handle chlorosilane raffinate |
| CN110627071A (en) * | 2019-11-12 | 2019-12-31 | 四川永祥新能源有限公司 | Polychlorosilane processing apparatus in polycrystalline silicon production |
| CN113149017A (en) * | 2021-04-15 | 2021-07-23 | 宁夏胜蓝化工环保科技有限公司 | Complexing agent for removing aluminum from polycrystalline silicon high-boiling residues and application method thereof |
| CN114147033A (en) * | 2020-09-05 | 2022-03-08 | 中国石油化工股份有限公司 | High-boiling-point substance continuous washing system and process |
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| CN113149017A (en) * | 2021-04-15 | 2021-07-23 | 宁夏胜蓝化工环保科技有限公司 | Complexing agent for removing aluminum from polycrystalline silicon high-boiling residues and application method thereof |
| CN113149017B (en) * | 2021-04-15 | 2022-06-17 | 宁夏胜蓝化工环保科技有限公司 | Complexing agent for removing aluminum from polycrystalline silicon high-boiling residues and application method thereof |
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Application publication date: 20181225 Assignee: Sichuan Yongxiang Energy Technology Co.,Ltd. Assignor: SICHUAN YONGXIANG NEW ENERGY Co.,Ltd. Contract record no.: X2023510000014 Denomination of invention: A treatment system and method for high boiling substances generated by a cold hydrogenation system Granted publication date: 20210511 License type: Common License Record date: 20230816 |