CN105271246B - A kind of method that chloro disilane is prepared using polysilicon by-product - Google Patents
A kind of method that chloro disilane is prepared using polysilicon by-product Download PDFInfo
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- CN105271246B CN105271246B CN201510217057.1A CN201510217057A CN105271246B CN 105271246 B CN105271246 B CN 105271246B CN 201510217057 A CN201510217057 A CN 201510217057A CN 105271246 B CN105271246 B CN 105271246B
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- disilane
- mixed system
- chloro disilane
- chloro
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- FXMNVBZEWMANSQ-UHFFFAOYSA-N chloro(silyl)silane Chemical compound [SiH3][SiH2]Cl FXMNVBZEWMANSQ-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 48
- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims abstract description 39
- 229920005591 polysilicon Polymers 0.000 title claims abstract description 38
- 239000006227 byproduct Substances 0.000 title claims abstract description 33
- 239000013078 crystal Substances 0.000 claims abstract description 40
- 238000009835 boiling Methods 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 18
- 238000004821 distillation Methods 0.000 claims abstract description 13
- 150000001399 aluminium compounds Chemical class 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 39
- 239000010703 silicon Substances 0.000 claims description 39
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 38
- 238000006243 chemical reaction Methods 0.000 claims description 15
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- 229910052801 chlorine Inorganic materials 0.000 claims description 14
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 14
- 239000000460 chlorine Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 13
- -1 acetyl hydroxyl Chemical group 0.000 claims description 10
- 239000013067 intermediate product Substances 0.000 claims description 10
- TZXKOCQBRNJULO-UHFFFAOYSA-N Ferriprox Chemical compound CC1=C(O)C(=O)C=CN1C TZXKOCQBRNJULO-UHFFFAOYSA-N 0.000 claims description 8
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- 125000001309 chloro group Chemical group Cl* 0.000 claims description 7
- 230000003287 optical effect Effects 0.000 claims description 7
- 229910000077 silane Inorganic materials 0.000 claims description 7
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 6
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 125000003368 amide group Chemical group 0.000 claims description 4
- FXDUXBIZVCPXPZ-UHFFFAOYSA-N 2-iodoquinolin-8-ol Chemical compound C1=C(I)N=C2C(O)=CC=CC2=C1 FXDUXBIZVCPXPZ-UHFFFAOYSA-N 0.000 claims description 3
- 241000255964 Pieridae Species 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 claims 2
- 229910001510 metal chloride Inorganic materials 0.000 abstract description 7
- 239000012752 auxiliary agent Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 12
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 12
- 239000002994 raw material Substances 0.000 description 12
- ZOYFEXPFPVDYIS-UHFFFAOYSA-N trichloro(ethyl)silane Chemical compound CC[Si](Cl)(Cl)Cl ZOYFEXPFPVDYIS-UHFFFAOYSA-N 0.000 description 11
- 239000007789 gas Substances 0.000 description 7
- ZBJWWKFMHOAPNS-UHFFFAOYSA-N loretin Chemical compound C1=CN=C2C(O)=C(I)C=C(S(O)(=O)=O)C2=C1 ZBJWWKFMHOAPNS-UHFFFAOYSA-N 0.000 description 7
- 239000005046 Chlorosilane Substances 0.000 description 6
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 241000209094 Oryza Species 0.000 description 5
- 235000007164 Oryza sativa Nutrition 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 235000009566 rice Nutrition 0.000 description 5
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- 239000005049 silicon tetrachloride Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- KAESVJOAVNADME-UHFFFAOYSA-N 1H-pyrrole Natural products C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 description 2
- FNWQKSHFBHPPGU-UHFFFAOYSA-N [Si].ClC=C Chemical compound [Si].ClC=C FNWQKSHFBHPPGU-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Substances C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 2
- 239000005052 trichlorosilane Substances 0.000 description 2
- UUDALWDRIFYZPM-UHFFFAOYSA-N 1h-pyridine-2,4-dione Chemical class O=C1CC(=O)C=CN1 UUDALWDRIFYZPM-UHFFFAOYSA-N 0.000 description 1
- AXKOGJAAENJJFI-UHFFFAOYSA-N 7-iodoquinolin-8-ol Chemical compound C1=CN=C2C(O)=C(I)C=CC2=C1 AXKOGJAAENJJFI-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- 229920004482 WACKER® Polymers 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of method that chloro disilane is prepared using polysilicon by-product, it comprises the following steps：1st, the high-boiling components containing alchlor of by-product in polysilicon production process are incubated to form crystal and isolate crystal；2nd, eliminated into step 1 and auxiliary agent formation mixed system is added in the high-boiling components of crystal；3rd, heating makes the temperature of the mixed system in step 2 rise to 30 DEG C~120 DEG C and be incubated to form the mixed system containing nonvolatile aluminium compound；4th, the mixed system in step 3 is obtained into the mixing chloro disilane without alchlor in the lower distillation of normal pressure or absolute pressure less than 0.2MPa；5th, the mixing chloro disilane rectifying that step 4 obtains is obtained into the chloro disilane of one pack system.The present invention has the following effects that：1st, the metal chloride in high-boiling components is efficiently removed；2nd, from Light chlorimation mode, chlorination is carried out in liquid phase, process can be made safer.
Description
Technical field
The invention belongs to chemical field, is related to a kind of preparation method of chloro disilane, more particularly to one kind utilizes polycrystalline
The method that silicon accessory substance prepares chloro disilane.
Background technology
Chloro disilane especially disilicone hexachloride is the important silicon source material of hyundai electronicses manufacturing field, such as in Tokyo
In the patent CN200480028369 of willpower Kechuang Co., Ltd., the deposition of the silicon-containing film carried out with disilicone hexachloride；SMIS state
IC manufacturing (Beijing) Co., Ltd in border is in its patent CN200810113992, using the mixing comprising disilicone hexachloride
Gas is as silicon source；Canon Co., Ltd uses disilicone hexachloride to lead to as unstrpped gas in its patent CN201210375335
Cross low-pressure chemical vapor deposition method and form silicon nitride film.With the fast development of high-accuracy electronic device, electronic industry pair
The demand of disilicone hexachloride quickly increases.
In the manufacture view of disilicone hexachloride, Mitsubishi Materials Polycrystalline Silicon Corp is in its patent
A kind of method for producing disilicone hexachloride is disclosed in CN01803007.This method is from chlorosilane and hydrogen gas production polysilicon
The waste gas condensation discharged in stove is distilled gained condensate to isolate unreacted chlorosilane and by-product with isolating hydrogen
Thing silicon tetrachloride, then further distill to reclaim disilicone hexachloride and the silicon of four chlorination two, the purity of the disilicone hexachloride of recovery
The purity of conventional products than being produced with metallic silicon is much higher, while is passed through chlorine in this process, is passed through the purpose of chlorine
It is in order that the silicon of four chlorination two or being converted into disilicone hexachloride so as to increase the yield of disilicone hexachloride.This method is actually
Micro disilicone hexachloride in the mixed gas gone out using a series of separation processes recovery polysilicon deposition fire grate, due to polysilicon
Cvd furnace discharge mixed gas in disilicone hexachloride content it is extremely low, therefore the process high energy consumption and efficiency it is low.This method
Advantage be, the metal impurities such as aluminium chloride are not contained in handled process so that using rectificating method purify hexachloroethanc
Silane is possibly realized.The patent illustrated in its background of invention existing method preparation disilicone hexachloride in containing aluminium chloride,
These chlorides of titanium chloride, the boiling point and disilicone hexachloride of aluminium chloride and titanium chloride approach, therefore are generally difficult to the side with rectifying
Method refines disilicone hexachloride.And the patent prepares disilicone hexachloride using the raw material without metal chloride, therefore use essence
Evaporate method and prepare disilicone hexachloride as feasible.
Deuki Kagaku Kogyo Co., Ltd of Japan disclosed in its patent CN200980158582 by silicon tetrachloride and
The recovery method of the disilicone hexachloride generated during hydrogen gas production trichlorosilane as accessory substance, the technological process of this method is to make four
Chlorosilane and hydrogen react at a temperature of 700~1400 DEG C of scopes, react the gas cooling of generation to 30~60 DEG C
Temperature range, so as to obtain the condensate liquid containing disilicone hexachloride, then concentration and recovery contains disilicone hexachloride from condensate liquid
The process of high boiling product.This method is really what the hydrogenation furnace for preparing trichlorosilane using hot hydro-reduction silicon tetrachloride was excluded
Contain the mixed gas of disilicone hexachloride as raw material, obtain disilicone hexachloride by a series of separation processes, it is essential and special
Sharp CN01803007 is consistent, does not contain metal chloride in the raw material utilized equally, therefore can be compared with by the method for rectifying
Readily realize.
Wacker Chemical Stock Co., Ltd discloses one kind in its patent CN200880108573 and includes hexachloroethanc by rectifying
The method that the mixture of silane prepares disilicone hexachloride, it is in polycrystalline that disilicone hexachloride mixture is specify that in its claim
The industrial waste gas obtained in siliceous deposits, that is, used raw material is caused by polysilicon deposition process, and patent
All raw materials of CN01803007 have uniformity, i.e., the raw material is free of metal chloride.
The patent CN201310059040 of University Of Tianjin discloses one kind and hexachloroethanc is reclaimed and purified from chlorosilane raffinate
The intermittently operated method and device of silane.This method and device mainly include just dividing rectifying column and batch fractionating tower.The invention can
The disilicone hexachloride of purity more than 98% is obtained with recovery.
By-product based on silicon tetrachloride and chloro disilane, contains chlorination to polysilicon enterprise of China simultaneously in process of production
The high-boiling components of the metal chlorides such as aluminium.Existing open source information and our practices for many years all have confirmed that, the gold in high-boiling components
Category chloride especially aluminium chloride can separation equipment inwall or touch the surface of chlorosilane medium and form hard solid
Crystal, finally make equipment failure.Therefore, the technology of preparing of existing high-purity disilicone hexachloride is generally using not metal impurities
It is raw material especially without the miscellaneous mixed chlorosilane of alchlor.An object of the present invention is to utilize polysilicon producer of China pair
Production is raw material containing the higher metal chloride especially high-boiling components containing higher alchlor, by removing alchlor reality
Now to the further utilization of high-boiling components.
Prior art merely isolates hexachloroethanc simply by rectificating method from the mixture of chloro disilane mostly
Silane, patent CN01803007 have isolated disilicone hexachloride and four silicon hexachlorides simultaneously, and in distillation process or residual in rectifying
The mode that chlorine is passed through in liquid improves the yield of disilicone hexachloride.
Our research is found, disilicone hexachloride, five chloroethene silicon are contained in high-boiling components caused by polysilicon producer of China
These chloro disilanes of alkane, four silicon hexachlorides, trichloroethyl silane, two silicon hexachlorides.Hydrogeneous chloro disilane can pass through chlorination
It is changed into more molecules containing chlorine atom.But existing knowledge is taught that, hydrogeneous chloro disilane and gaseous oxidizer mix
Credit union forms explosive reaction, and therefore, the behavior in distillation process introducing chlorine described by patent CN01803007 is extremely to endanger
Danger.Special means must be used to eliminate the danger of chlorination process.
The invention is intended to provide a kind of method for preparing chloro disilane, this method can overcome the deficiencies in the prior art, make
Alchlor separates from high-boiling components raffinate, afterwards by safe and efficient chlorination means by hydrogeneous chloro disilane selectivity chlorine
Change, the chloro disilane mixture to be meeted the requirements, the mixture is separated by existing distillation technology one pack system chlorine is made again
For disilane.
The content of the invention
Goal of the invention：The present invention has made improvements in view of the above-mentioned problems of the prior art, i.e., the invention discloses one kind
The method that chloro disilane is prepared using polysilicon by-product.
Technical scheme：A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1), by the high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process at -5 DEG C~-50 DEG C
Lower insulation forms crystal in 10~80 hours, and crystal is isolated by way of secondary filter；
(2) 0.01~0.1 part of N'- [5- [[4- [[5- (second of addition in the high-boiling components of crystal, is eliminated into step (1)
Acyl azanol base) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides (No. CAS
70-51-9) either add 0.01~0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyridone (CAS 30652-11-0) or add
Enter 0.01~0.1 part of 7 iodo 8 hydroxy quinoline 5 sulfonic acid (CAS 547-91-1) and form mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C~120 DEG C, and at 30 DEG C~120 DEG C
Insulation 5~10 hours, form the mixed system containing nonvolatile aluminium compound；
(4), by the mixed system in step (3), in the case where normal pressure or absolute pressure are less than 0.2MPa, distillation obtains 90
~98 parts of mixing chloro disilanes for being free of alchlor；
(5) the mixing chloro disilane rectifying that step (4) obtains, is obtained into the chloro disilane of one pack system.
As a kind of a kind of preferred scheme for the method that chloro disilane is prepared using polysilicon by-product in the present invention：Step
Suddenly the condition of secondary filter is in (1)：The filtering accuracy of accurate filter used is 0.1~10 micron.
As a kind of a kind of preferred scheme for the method that chloro disilane is prepared using polysilicon by-product in the present invention：Step
Suddenly the chloro disilane of (5) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four silicon hexachlorides and trichloroethyl silane.
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1), by the high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process at -5 DEG C~-50 DEG C
Lower insulation forms crystal in 10~80 hours, and crystal is isolated by way of secondary filter；
(2) 0.01~0.1 part of N'- [5- [[4- [[5- (second of addition in the high-boiling components of crystal, is eliminated into step (1)
Acyl azanol base) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides (No. CAS
70-51-9) either add 0.01~0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyridone (CAS 30652-11-0) or add
Enter 0.01~0.1 part of 7 iodo 8 hydroxy quinoline 5 sulfonic acid (CAS 547-91-1) and form mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C~120 DEG C, and at 30 DEG C~120 DEG C
Insulation forms the mixed system containing nonvolatile aluminium compound in 5~10 hours；
(4), by the mixed system in step (3), in the case where normal pressure or absolute pressure are less than 0.2MPa, distillation obtains 90
~98 parts of mixing chloro disilanes for being free of alchlor；
(5) the mixing chloro disilane in step (4), is subjected to chlorination in optical chlorinating reaction device and obtains intermediate product,
The condition of chlorination is：Chlorine is passed into mixing chloro disilane liquid phase, is passed through quality of chlorine gas and is mixed not higher than obtained by step (4)
The 50% of chloro disilane quality, using 254nm light as light source, reaction temperature is controlled at -10 DEG C~0 DEG C；
(6) the intermediate product rectifying that step (5) obtains, is obtained into the chloro disilane of one pack system.
As a kind of a kind of preferred scheme for the method that chloro disilane is prepared using polysilicon by-product in the present invention：Step
Suddenly the chloro disilane of (6) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four silicon hexachlorides and trichloroethyl silane.
As a kind of a kind of preferred scheme for the method that chloro disilane is prepared using polysilicon by-product in the present invention：Step
Suddenly the condition of secondary filter is in (1)：The filtering accuracy of accurate filter used is 0.1~10 micron.
Beneficial effect：The invention discloses it is a kind of using polysilicon by-product prepare chloro disilane method have it is following
Beneficial effect：
1st, the metal chloride in high-boiling components using aluminium chloride as representative is efficiently removed, is provided conveniently for follow-up process；
2nd, using Light chlorimation mode, chlorination is carried out in liquid phase, process can be made safer.
Embodiment：
The embodiment of the present invention is described in detail below.
Specific embodiment 1
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 80 at -5 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) 0.01 part of N'- [5- [[4- [[5- (acetyl hydroxyl of addition in the high-boiling components of crystal, is eliminated into step (1)
Amido) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides (CAS 70-
51-9) form mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C, and is incubated 10 hours at 30 DEG C, is formed
Mixed system containing nonvolatile aluminium compound；
(4), the mixed system in step (3) is distilled in the case of normal pressure and obtains 90 parts of mixing for being free of alchlor
Chloro disilane；
(5) the mixing chloro disilane rectifying that step (4) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 0.1 micro-
Rice.
In the present embodiment, the chloro disilane of step (5) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
Specific embodiment 2
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 10 at -50 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) 0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyrrole of addition in the high-boiling components of crystal, is eliminated into step (1)
Pyridine ketone (CAS 30652-11-0) forms mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 120 DEG C, and is incubated 5 hours at 120 DEG C, shape
Into the mixed system containing nonvolatile aluminium compound；
(4), the mixed system in step (3) is distilled in the case of absolute pressure 0.2MPa and obtains 98 parts and is free of trichlorine
Change the mixing chloro disilane of aluminium；
(5) the mixing chloro disilane rectifying that step (4) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 10 micro-
Rice.
In the present embodiment, the chloro disilane of step (5) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
Specific embodiment 3
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 40 at -25 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) 0.05 part of 7 iodo 8 hydroxy quinoline 5 sulfonic acid of addition in the high-boiling components of crystal, is eliminated into step (1)
(CAS 547-91-1) forms mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 70 DEG C, and is incubated 8 hours at 70 DEG C, is formed
Mixed system containing nonvolatile aluminium compound；
(4), the mixed system in step (3) is distilled in the case of 7 absolute pressure 0.1MPa and obtains 95 parts without three
The mixing chloro disilane of aluminium chloride；
(5) the mixing chloro disilane rectifying that step (4) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 5 microns.
In the present embodiment, the chloro disilane of step (5) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
Specific embodiment 4
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 80 at -5 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) 0.01 part of N'- [5- [[4- [[5- (acetyl hydroxyl of addition in the high-boiling components of crystal, is eliminated into step (1)
Amido) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides (CAS 70-
51-9) form mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C, and is incubated 10 hours at 30 DEG C and is formed
Mixed system containing nonvolatile aluminium compound；
(4), the mixed system in step (3) is distilled at ambient pressure to obtain 90 parts of mixing chloro second for being free of alchlor
Silane；
(5) the mixing chloro disilane in step (4), is subjected to chlorination in optical chlorinating reaction device and obtains intermediate product,
The condition of chlorination is：Chlorine is passed into mixing chloro disilane liquid phase, is passed through quality of chlorine gas mixing chloro obtained by step (4)
The 40% of disilane quality, using 254nm light as light source, reaction temperature is controlled at -10 DEG C；
(6) the intermediate product rectifying that step (5) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the chloro disilane of step (6) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 0.1 micro-
Rice.
Specific embodiment 5
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 10 at -50 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) 0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyrrole of addition in the high-boiling components of crystal, is eliminated into step (1)
Pyridine ketone (CAS 30652-11-0) forms mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 120 DEG C, and is incubated 5 hours at 120 DEG C and is formed
Mixed system containing nonvolatile aluminium compound；
(4) mixed system in step (3), is obtained 98 parts in absolute pressure 0.2MPa lower distillation and is free of alchlor
Mixing chloro disilane；
(5) the mixing chloro disilane in step (4), is subjected to chlorination in optical chlorinating reaction device and obtains intermediate product,
The condition of chlorination is：Chlorine is passed into mixing chloro disilane liquid phase, is passed through quality of chlorine gas mixing chloro obtained by step (4)
The 50% of disilane quality, using 254nm light as light source, reaction temperature is controlled at 0 DEG C；
(6) the intermediate product rectifying that step (5) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the chloro disilane of step (6) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 10 micro-
Rice.
Specific embodiment 6
A kind of method that chloro disilane is prepared using polysilicon by-product, is comprised the following steps：
(1) high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process, are incubated 50 at -30 DEG C
Hour forms crystal, and crystal is isolated by way of secondary filter；
(2) the 5 addition iodo- 8-hydroxyquinoline -5- sulphurs of 0.05 part of 7- in the high-boiling components of crystal, are eliminated into step (1)
Sour (CAS 547-91-1) forms mixed system；
(3), heating makes the temperature of the mixed system in step (2) rise to 60 DEG C, and is incubated 8 hours at 60 DEG C and is formed and contain
There is the mixed system of nonvolatile aluminium compound；
(4) mixed system in step (3), is obtained 95 parts in absolute pressure 0.1MPa lower distillation and is free of alchlor
Mixing chloro disilane；
(5) the mixing chloro disilane in step (4), is subjected to chlorination in optical chlorinating reaction device and obtains intermediate product,
The condition of chlorination is：Chlorine is passed into mixing chloro disilane liquid phase, is passed through quality of chlorine gas mixing chloro obtained by step (4)
The 10% of disilane quality, using 254nm light as light source, reaction temperature is controlled at -5 DEG C；
(6) the intermediate product rectifying that step (5) obtains, is obtained into the chloro disilane of one pack system.
In the present embodiment, the chloro disilane of step (6) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four
Silicon hexachloride and trichloroethyl silane.
In the present embodiment, the condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 5 microns.
Specific embodiment 7
The high-boiling components of polysilicon plant-site by-product, icp analysis alchlor content are 0.5%；Gas-chromatography analysis of components is such as
Under, disilicone hexachloride 35%, five silicon hexachlorides 20%, four silicon hexachlorides 30%, trichloroethyl silane 10%, two silicon hexachlorides 5%.
The 2.1kg high-boiling components are incubated 80 hours at -10 DEG C, and crystal is isolated with 10 microns of filter of filtering accuracy.
2.05g 7 iodo 8 hydroxy quinoline 5 sulfonic acids are added into the 2.05kg high-boiling components for eliminate crystal, are warming up to 30 DEG C,
This temperature 10 hours.Air-distillation obtains 2kg distillates (mixing chloro disilane), is detected through ICP, aluminium content
1.5ppbw.Distillate is passed through 0.9kg chlorine, reaction temperature dimension in optical chlorinating reaction device bottom using 254nm uviol lamps as light source
Hold at 0 DEG C.Reaction product obtains disilicone hexachloride 2.5kg, five silicon hexachloride 0.5kg by rectifying, and remaining is 0.12kg tetrachloros
Disilane.
Specific embodiment 8
Using the raw material 2.1kg used in embodiment 1, the raw material is incubated 10 hours at -35 DEG C, micro- with filtering accuracy 2
The filter of rice isolates crystal.0.21g 1,2- dimethyl -3- is added into the high-boiling components 2.06kg for eliminate crystal
Hydroxyl -4- pyridones, were warming up to 90 DEG C, in this temperature 5 hours.Air-distillation obtains 2kg distillates (mixing chloro second silicon
Alkane), detected through ICP, aluminium content 1.0ppbw.Distillate is passed through using 254nm uviol lamps as light source in optical chlorinating reaction device bottom
0.5kg chlorine, reaction temperature maintain -10 DEG C.Reaction product obtains disilicone hexachloride 0.75kg, five chloroethene silicon by rectifying
The silicon hexachloride of alkane 0.6kg, 0.88kg tetra-.
Specific embodiment 9
Using the raw material 2.1kg used in embodiment 1, the raw material is incubated 12 hours at -45 DEG C, with filtering accuracy 0.1
The filter of micron isolates crystal.1.1g N'- [5- [[4- are added into the 2.05kg high-boiling components for eliminate crystal
The oxygen-butyls of [[5- (acetyl hydroxyl base) amyl group] ammonia] -1,4- two] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimidyl acyls
Amine, 60 DEG C are warming up to, in this temperature 7 hours.Air-distillation obtains 2kg distillates (mixing chloro disilane), is examined through ICP
Survey, aluminium content 0.8ppbw.For distillate without superchlorination, direct rectifying obtains disilicone hexachloride 0.62kg, five silicon hexachlorides
0.32kg, four silicon hexachloride 0.55kg, trichloroethyl silane 0.18kg, two silicon hexachlorides are not collected as front-end volatiles.
Embodiments of the present invention are elaborated above.But the present invention is not limited to above-mentioned embodiment,
In art those of ordinary skill's possessed knowledge, it can also be done on the premise of present inventive concept is not departed from
Go out various change.
Claims (2)
- A kind of 1. method that chloro disilane is prepared using polysilicon by-product, it is characterised in that comprise the following steps：(1), the high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process are protected at -5 DEG C~-50 DEG C Temperature forms crystal in 10~80 hours, and crystal is isolated by way of secondary filter；(2) 0.01~0.1 part of N'- [5- [[4- [[5- (acetyl hydroxyl of addition in the high-boiling components of crystal, is eliminated into step (1) Amido) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides or addition 0.01~0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyridone adds the iodo- 8-hydroxyquinoline -5- sulphurs of 0.01~0.1 part of 7- Acid forms mixed system；(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C~120 DEG C, and is incubated 5 at 30 DEG C~120 DEG C ~10 hours, form the mixed system containing nonvolatile aluminium compound；(4), by the mixed system in step (3), in the case where normal pressure or absolute pressure are less than 0.2MPa, distillation obtains 90~98 Part is free of the mixing chloro disilane of alchlor；(5) the mixing chloro disilane rectifying that step (4) obtains, is obtained into the chloro disilane of one pack system, wherein：The condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 0.1~10 micron；The chloro disilane of step (5) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four silicon hexachlorides and three chloroethenes Silane.
- A kind of 2. method that chloro disilane is prepared using polysilicon by-product, it is characterised in that comprise the following steps：(1), the high-boiling components containing alchlor of by-product in 100 parts of polysilicon production process are protected at -5 DEG C~-50 DEG C Temperature forms crystal in 10~80 hours, and crystal is isolated by way of secondary filter；(2) 0.01~0.1 part of N'- [5- [[4- [[5- (acetyl hydroxyl of addition in the high-boiling components of crystal, is eliminated into step (1) Amido) amyl group] ammonia] two oxygen-butyls of -1,4-] azanol] amyl group]-N- (5- Aminopentyls)-N- hydroxysuccinimides or addition 0.01~0.1 part of 1,2- dimethyl -3- hydroxyl -4- pyridone adds the iodo- 8-hydroxyquinoline -5- sulphurs of 0.01~0.1 part of 7- Acid forms mixed system；(3), heating makes the temperature of the mixed system in step (2) rise to 30 DEG C~120 DEG C, and is incubated 5 at 30 DEG C~120 DEG C Form the mixed system containing nonvolatile aluminium compound within~10 hours；(4), by the mixed system in step (3), in the case where normal pressure or absolute pressure are less than 0.2MPa, distillation obtains 90~98 Part is free of the mixing chloro disilane of alchlor；(5) the mixing chloro disilane in step (4), is subjected to chlorination in optical chlorinating reaction device and obtains intermediate product, chlorination Condition be：Chlorine is passed into mixing chloro disilane liquid phase, is passed through quality of chlorine gas not higher than mixing chloro obtained by step (4) The 50% of disilane quality, using 254nm light as light source, reaction temperature is controlled at -10 DEG C~0 DEG C；(6) the intermediate product rectifying that step (5) obtains, is obtained into the chloro disilane of one pack system, wherein：The chloro disilane of step (6) described one pack system includes disilicone hexachloride, five silicon hexachlorides, four silicon hexachlorides and three chloroethenes Silane；The condition of secondary filter is in step (1)：The filtering accuracy of accurate filter used is 0.1~10 micron.
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| CN106946261A (en) * | 2017-04-06 | 2017-07-14 | 洛阳中硅高科技有限公司 | The retracting device of disilicone hexachloride |
| CN106966397A (en) * | 2017-04-06 | 2017-07-21 | 洛阳中硅高科技有限公司 | The recovery method of disilicone hexachloride |
| CN112479213B (en) * | 2020-12-18 | 2023-09-19 | 武汉新硅科技潜江有限公司 | Method for producing electronic grade hexachlorodisilane by continuous rectification method |
| CN115849384B (en) * | 2022-11-30 | 2023-11-07 | 华陆工程科技有限责任公司 | Cracking treatment method for high-boiling-point substances of polycrystalline silicon |
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