CN109384233A - A method of for handling silicon polymer - Google Patents
A method of for handling silicon polymer Download PDFInfo
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- CN109384233A CN109384233A CN201811525561.8A CN201811525561A CN109384233A CN 109384233 A CN109384233 A CN 109384233A CN 201811525561 A CN201811525561 A CN 201811525561A CN 109384233 A CN109384233 A CN 109384233A
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- silicon
- silicon polymer
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- hydrogen chloride
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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
- C01B33/10742—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by hydrochlorination of silicon or of a silicon-containing material
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Abstract
The present invention relates to a kind of methods for handling silicon polymer, it includes using ionic liquid as catalyst, using silicon polymer and anhydrous hydrogen chloride as raw material, silicon polymer and anhydrous hydrogen chloride are reacted under conditions of 30-180 DEG C, 0.02-1.2MPa in the reactor, obtain the chlorosilane product containing 1 silicon atom.The present invention has can be the advantages of improving polysilicon and organosilicon by-product higher boiling polymer throughput simultaneously, reducing catalyst attrition, eliminate environmental pollution.
Description
Technical field
The present invention relates to polysilicon preparation and organosilicon preparation fields, and in particular in a kind of polysilicon and organosilicon production
The cleavage method of by-product silicon polymer.
Background technique
In production of polysilicon and organic silicon production process, considerable amount of chlorosilane raffinate can be generated, ingredient includes containing 1
The solid impurities such as chlorosilane, the silicon powder of a silicon atom, high polymer (being commonly called as " high-boiling components ").Pass through the hands such as filtering, separation, rectifying
Section can recycle the most chlorosilane for containing 1 silicon atom, and the solid impurities such as silicon powder can also carry out integrated treatment, but high
Boiling object, structure is complicated, and ingredient is uncertain, cannot achieve trans-utilization by simple organic separation.The continuous product of high-boiling components
The problems such as gathering or overstocked, will cause enterprise's production cost increase and environmental pollution, hamper the hair of polysilicon and organosilicon industry
Exhibition.
Patent CN101659672A has invented a kind of cracking processing of the waste residue slurry formed in organic silicon monomer synthesis process
Method, the liquid-solid mixture for being 20% by organic silicon waste residue slurry solid content are added the high-boiling components of phase homogenous quantities, are made into cracking stock
Liquid；Catalyst is tri-n-butylamine, and cracking reaction temperature is 80~160 DEG C, is passed through HCl gas, and hydrogen chloride charging rate is mixed with raw material
Closing liquor ratio is 1: 1.05~1: 1.12；The present invention is used cooperatively the slurry of solid content 20% with high-boiling components, in cracking process
It is directly separated the alkane that product contains 1 silicon atom, for conversion ratio 70% or more, dimethyldichlorosilane is selectively greater than 35%, one
Methylhydrosiloxane is selectively greater than 40%, and the screenings after cracking has certain mobility, can be further processed.
At present since existing catalyst and polysilane system are immiscible, lead to slurry or reaction system flowing after cracking
Property it is bad, lead to the problem that catalysis reaction is uneven, transformation efficiency is low, and patent CN103553056A is passed through using ionic liquid
Temperature control phase inversion means realize silicon tetrachloride and the efficient quick separating of trichlorosilane, and this method is based on ionic liquid in different temperatures
Under to the difference of silicon tetrachloride and trichlorosilane solubility, by the mixed chlorosilane of different quality ratio be added to lower temperature from
In sub- liquid, so that chlorosilane is sufficiently dissolved and is distributed in ionic liquid, upper layer and lower layer are divided into after standing；Again by two layers of liquid phase point
After opening, then two liquid phase layers are evaporated and are condensed at different temperatures respectively, i.e., height that is separable, recycling one-component
Purity chlorosilane shows that ionic liquid has preferable solubility for chlorosilane system.
Therefore, the current situation of the prior art is that method that is a kind of simple and effectively handling silicon polymer is still required,
The silicon polymers such as polysilicon high-boiling components and organosilicon high-boiling product treating capacity can improved simultaneously, reduce cost, reduce catalyst
Environmental pollution is eliminated in loss.The present invention uses ionic liquid for catalyst, by using the method for ionic-liquid catalyst, benefit
With the good feature of chlorosilane system dissolubility of the ionic liquid to silicon-containing polymer, the chlorosilane of silicon-containing polymer will be handled by realizing
System solvation and the purpose for not being re-introduced into other impurities are reacted in ionic liquid-silicon-containing polymer chlorosilane of solvation
In system, silicon polymer and anhydrous hydrogen chloride are reacted, generate trichlorosilane, dichlorosilane, silicon tetrachloride or methyl chloride silicon
The chlorosilane cpd containing only 1 silicon atom such as alkane.
Summary of the invention
The method for effectively handling silicon polymer technical problem to be solved by the invention is to provide a kind of simple, solves
Introducing is not friendly to environment when the problem that processing polysilicon cannot dissolve each other with organosilicon by-product higher boiling silicon polymer and catalyst
The good catalyst containing benzene causes to lead to the problem of new environmentally friendly risk, is improving polysilicon high-boiling components and organosilicon high-boiling product etc.
Silicon polymer treating capacity simultaneously, reduces cost, reduces catalyst attrition, eliminates environmental pollution.
Inventors discovered through research that ionic liquid can not only carry out the disproportionated reaction of chlorosilane, it can also be in difference
Reaction condition and differential responses system under be catalyzed polysilicon and organosilicon by-product silicon polymer cracking reaction, having silicon polymerization
Addition is using cation as quaternary ammonium salt, anion CF in the mixed solution of object3SO3 -、CF3COO-、PF6 -、N(CF3SO2)2 -、C
(CF3SO2)3 -、N(CN)2 -、Cl-Ionic liquid, it is good using chlorosilane system dissolubility of the ionic liquid to silicon-containing polymer
Feature can be with ionic liquid by being passed through anhydrous hydrogen chloride, under conditions of 30 DEG C -180 DEG C, 0.02MPa-1.2MPa
Catalyst generates the chlorosilane cpd containing only 1 silicon atom, thus effectively by being reacted with anhydrous hydrogen chloride and silicon polymer
Realize the object of the invention.
The technical solution adopted by the invention is as follows:
As shown in Figure 1, silicon polymer is added by feed pipe 4 and contains 1 silicon atom in silicon polymer treatment reactor 2
Anhydrous HCl is added in silicon polymer treatment reactor 2 by pipeline 12 through gas distributor 6 mixture of chlorosilane, and silicon is poly-
The flow for closing object and the mixture containing 1 silicon atom chlorosilane can be controlled by the valve 3, and anhydrous hydrogen chloride flow can
To control uninterrupted by valve 13, silicon polymer and the mixture containing 1 silicon atom chlorosilane are reacted with catalyst formation
Mixture 5.Reaction product contains the mixture of 1 silicon atom chlorosilane and the complete anhydrous hydrogen chloride of unreacted is taken by pipeline 11
Out, the mixture after condensing containing 1 silicon atom chlorosilane goes rectifying to separate, and unreacted anhydrous hydrogen chloride is after condensing and separating
It is recycled by being returned after compressor compresses, the cleavage reaction pressure of silicon polymer can be controlled by valve 10.?
Silicon polymer handles preceding or silicon polymer after treatment, can be purged by pipeline 8 and valve 7 into nitrogen, tail
Gas is discharged after lye absorbs by pipeline 1 and the discharge of valve 9.
In the above scheme, the polymer that the silicon polymer is formed with silicon-silicon key pattern.
In the above scheme, the silicon polymer can be expressed as Ra—SiHbClc- (SiHeClfRg-SiHiCljRk)n—
SiHxClyRzForm, wherein one of a, b, c, x, y, z 0,1,2,3, one of e, f, g, i, j, k 0,1,2, and a+b+c=3, e+
F+g=2, i+j+k=2, x+y+z=3；N is the integer of nonnegative number；R=H, Cl, alkyl, the alkyl etc. containing benzene.
In the above scheme, the catalyst used is ionic-liquid catalyst, but the preferred ionic liquid is quaternary ammonium
Salt ion liquid.
In the above scheme, the ionic liquid anion of the addition is CF3SO3 -、CF3COO-、PF6 -、N(CF3SO2)2 -、C
(CF3SO2)3 -、N(CN)2 -、Cl-One of or it is several.
In the above scheme, the chlorosilane product for containing 1 silicon atom can be expressed as Rm—SiHnClp, R=H, Cl,
Alkyl, the alkyl etc. containing benzene, one of m, n, p 0,1,2,3,4, and m+n+p=4.
In the above scheme, the silicon polymer preferably refers to what silicon polymer and the chlorosilane containing 1 silicon atom were formed
Mixture.
In the above scheme, the silicon polymer preferably refers to polysilicon by-product high-boiling components containing silicon polymer and organic
Silicon by-product high-boiling components.
In the above scheme, catalyst can be added in reactor 2 by pipeline 4 and valve 3, catalyst can be with
Silicon polymer is added together with the mixture containing 1 silicon atom chlorosilane, can also be previously added, and silicon polymerization can also be added
It is added after object and the mixture containing 1 silicon atom chlorosilane, charging can also be suspended during processing and pass through pipeline 4 and valve
Supplement catalyst is added in door 3.
In the above scheme, reactor 2 between 0.02MPa to 1.2MPa, between preferably 0.05MPa to 0.5MPa,
More preferably between 0.1MPa to 0.45MPa.Silicon polymer treatment temperature between 30-180 DEG C, preferably 50-150 DEG C it
Between, more preferably between 70-130 DEG C.
In the above scheme, anhydrous hydrogen chloride polymerize with silicon polymer and containing the silicon in 1 silicon atom chlorosilane mixture
The molar ratio of object is between 0.5-30:1, preferably between 1-10:1, more preferably between 3-6:1.
In the above scheme, can be into the material of reactor 2 it is not concentrated, but it is preferable that into reactor 2
Material is by concentration in advance, and the concentration of silicon polymer is between 10%-80%, between preferably 30-60%.
In the above scheme, into catalyst and silicon polymer mole or mass ratio between 1:1-200, but preferably
, between 1:9-99.
In the above scheme, can be into the material of reactor 2 it is untreated, but it is preferable that into reactor 2
Material removes silicon powder therein and oversaturated metallic compound impurity by pre-processing.
In the above scheme, reactor 2 shown in Fig. 1 and pipeline, valve preferably pass through jacket heat-preservation or heat tracing pipeline is protected
Temperature or heat supply.
Detailed description of the invention
Fig. 1 is the schematic diagram of processing silicon polymer technique of the present invention.
Wherein, 1 pipeline, 2 reactors, 3 valves, 4 pipelines, 5 reaction mixtures, 6 gas distributors, 7 valves, 8 pipelines, 9
Valve, 10, valve, 11 pipelines, 12, pipeline, 13 valves.
Specific embodiment
According to the present invention, the material into reactor 2 can be it is not concentrated, but it is preferable that enter reaction
The material of device 2 is by concentration in advance, and the concentration of silicon polymer is between 10%-80%, between preferably 30-60%, and by filtering out
Remove silicon powder and oversaturated metallic compound.
For convenience's sake, expansion explanation is carried out to silicon polymer processing method of the invention taking the example shown in figure 1.But it needs
It is noted that processing method of the invention is not limited to certain specific structure.For known to those skilled in the art, the processing
Feed entrance point, nozzle position and the feed pipe quantity of device can be with simple changes.
According to the present invention, the ionic liquid cation of the addition is quaternary ammonium salt, ionic liquid anion CF3SO3 -、
CF3COO-、PF6 -、N(CF3SO2)2 -、C(CF3SO2)3 -、N(CN)2 -、Cl-One of class is several, and following embodiment is pair
Further explanation of the invention, rather than limit the present invention.
Embodiment 1:
Using reactor as shown in Figure 1, in reactor 2, silicon polymer is added by feed pipe 4 and valve 3 and contains 1
Anhydrous hydrogen chloride is added chlorosilane, the catalyst of silicon atom by pipeline 12 and valve 13, and reaction product passes through 11 He of pipeline
Valve 10 produces, and separates hydrogen chloride and chlorosilane after condensing.
In the above scheme, for the ionic liquid cation used for hexyl triethyl ammonium ion, anion is N (CN)2 -, from
The additional amount of sub- liquid is every 1800 kilograms of silicon polymers with containing 1 144 kilograms of silicon atom chlorosilane mixture addition, and silicon polymerize
Object with containing 1 silicon atom chlorosilane mixture concentration 30%.The pressure of reactor is controlled in 0.25MPaG, reaction temperature is 90
DEG C, for the molar ratio of anhydrous hydrogen chloride and polysilane in 3:1, the conversion ratio of silicon polymer is 90%.
Embodiment 2:
Using reactor as shown in Figure 1, in reactor 2, silicon polymer is added by feed pipe 4 and valve 3 and contains 1
Anhydrous hydrogen chloride is added chlorosilane, the catalyst of silicon atom by pipeline 12 and valve 13, and reaction product passes through 11 He of pipeline
Valve 10 produces, and separates hydrogen chloride and chlorosilane after condensing.
In the above scheme, for the ionic liquid cation used for hexyl triethyl ammonium ion, anion is N (CN)2 -, from
The additional amount of sub- liquid is every 1800 kilograms of silicon polymers with containing 1 200 kilograms of silicon atom chlorosilane mixture addition, and silicon polymerize
Object with containing 1 silicon atom chlorosilane mixture concentration 30%.The pressure of reactor is controlled in 0.3MPaG, reaction temperature is 100
DEG C, for the molar ratio of anhydrous hydrogen chloride and polysilane in 3:1, the conversion ratio of silicon polymer is 91%.
Although above with reference to attached drawing, the detailed description and description of the specific embodiments of the present invention are given, should refer to
Bright, those skilled in the art can carry out various equivalent changes to above embodiment according to the concept of the present invention and repair
Change, it, should all be within protection scope of the present invention when the spirit that generated function is still covered without departing from specification.
Claims (12)
1. it is by anti-as raw material and anhydrous hydrogen chloride using silicon polymer the present invention relates to a kind of method of silicon polymer processing
The method that the chlorosilane containing 1 silicon atom should be prepared, it is characterised in that using ionic liquid as catalyst, silicon polymer and anhydrous
Hydrogen chloride is reacted under conditions of 30-180 DEG C, 0.02-1.2MPa in the reactor, obtains the chlorine silicon containing 1 silicon atom
Alkane product, used ionic liquid cation are quaternary ammonium salt, and the ionic liquid anion of addition is CF3SO3 -、CF3COO-、
PF6 -、N(CF3SO2)2 -、C(CF3SO2)3 -、N(CN)2 -、Cl-Class.
2. silicon polymer according to claim 1, which is characterized in that the polymerization that polymer is formed with silicon-silicon key pattern
Object.
3. silicon polymer according to claim 2, which is characterized in that silicon polymer can be expressed as Ra—SiHbClc—
(SiHeClfRg-SiHiCljRk)n—SiHxClyRzForm, wherein one of a, b, c, x, y, z 0,1,2,3, e, f, g, i, j, k are
0, one of 1,2, and a+b+c=3, e+f+g=2, i+j+k=2, x+y+z=3；N is the integer of nonnegative number；R=H, Cl, alkyl contain benzene
Alkyl etc..
4. according to the method described in claim 1, the catalyst used is ion liquid of quaternaries.
5. according to the method described in claim 4, it is characterized in that, the ionic liquid anion of the addition is CF3SO3 -、
CF3COO-、PF6 -、N(CF3SO2)2 -、C(CF3SO2)3 -、N(CN)2 -、Cl-One of or it is several.
6. according to the method described in claim 1, the chlorosilane product for containing 1 silicon atom can be expressed as Rm—
SiHnClp, R=H, Cl, alkyl, the alkyl etc. containing benzene, one of m, n, p 0,1,2,3,4, and m+n+p=4.
7. according to the method described in claim 2, the silicon polymer preferably refers to silicon polymer and the chlorine silicon containing 1 silicon atom
The mixture that alkane is formed.
8. according to the method described in claim 2, the silicon polymer preferably refers to that the polysilicon by-product containing silicon polymer is high
Boil object and organosilicon by-product high-boiling components.
9. according to the method described in claim 1, the silicon polymer and anhydrous hydrogen chloride reaction temperature are at 30 DEG C -180 DEG C.
10. according to the method described in claim 1, the silicon polymer and anhydrous hydrogen chloride reaction pressure are preferably in 0.02-
1.2MPa。
11. according to the method described in claim 1, the amount molar ratio of anhydrous hydrogen chloride and silicon polymer is between 0.5-30:1.
12. according to the method described in claim 1, catalyst and silicon polymer mole or mass ratio between 1:1-200.
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| CN201811525561.8A CN109384233B (en) | 2018-12-13 | 2018-12-13 | Method for treating silicon polymers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113772677A (en) * | 2021-09-30 | 2021-12-10 | 四川永祥新能源有限公司 | Cracking reaction column and cracking process for byproduct chlorosilane high-boiling-point substances in polycrystalline silicon production |
| CN114288697A (en) * | 2022-01-11 | 2022-04-08 | 中国科学院过程工程研究所 | Cracking process method for reactive distillation of chlorosilane slag slurry |
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| CN109384233B (en) | 2023-10-20 |
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