CN106220772A - A kind of preparation method of Trichlorosilane purification adsorbent - Google Patents
A kind of preparation method of Trichlorosilane purification adsorbent Download PDFInfo
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- CN106220772A CN106220772A CN201610691202.4A CN201610691202A CN106220772A CN 106220772 A CN106220772 A CN 106220772A CN 201610691202 A CN201610691202 A CN 201610691202A CN 106220772 A CN106220772 A CN 106220772A
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- Prior art keywords
- trichlorosilane
- purification adsorbent
- triolefin
- adsorbent
- titanium
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- C01B33/10778—Purification
- C01B33/10784—Purification by adsorption
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Analytical Chemistry (AREA)
Abstract
The invention provides the preparation method of a kind of Trichlorosilane purification adsorbent: be distributed in water by a certain amount of styrene, it is proportionally added into 5 cyclohexylidene 2 norborene, double (cyclopentadienyl group) titanium of dicarbapentaborane, potassium peroxydisulfate and dodecylbenzene sodium sulfonate, 1 [1 [2 (7, 10 dioxa dicyclo [4.4.0] last of the ten Heavenly stems 1, 3, 5 triolefin 9 bases) 2 hydroxyethyls] 4 piperidyls] 3H benzimidazole 2 ketone, octadecyl vinyl ether, heat up, react under preference temperature, after reaction terminates, product filters, dry, i.e. obtain Trichlorosilane purification adsorbent.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the preparation method of a kind of Trichlorosilane purification adsorbent.
Background technology
Trichlorosilane is the raw material manufacturing polysilicon, and polysilicon has semiconductor property, is particularly important excellent partly lead
Body material, is widely used in manufacture transistor radio, recorder, electric refrigerator, colour TV, videocorder, electronics calculating in electronics industry
The basic material of machine etc..Be the present age artificial intelligence, automatically control, information processing, the e-mail of the semiconductor device such as opto-electronic conversion
Breath basic material.But the impurity of trace is the biggest for the impact of trichlorosilane products quality.
CN104003402A discloses the method for purification of a kind of trichlorosilane.The method comprises the following steps: by trichlorine hydrogen
The thick liquid of silicon is heated by heating system, is heated to predetermined temperature；The thick liquid of trichlorosilane after heating is passed through exhaust tank, de-
Go out fixed gas；The thick liquid of trichlorosilane of abjection fixed gas is passed through purification tower system purify, obtains trichlorosilane products；Its
In, predetermined temperature is less than or equal to the saturation temperature under the first rectifying column feedboard pressure of purification tower system.The method is by three
The thick liquid of chlorine hydrogen silicon enters before purifying tower system and heats it, it is possible to make the dissolubility of fixed gas in thick liquid decline, Jin Eryou
The fixed gas being beneficial in thick liquid is separated.Then the thick liquid after heating is passed through exhaust tank, it is possible to by fixed gas therein
Discharge.
CN104071791A discloses the method for purification of a kind of trichlorosilane.The method includes leading to thick for trichlorosilane liquid
Entering to purify the step of tower system, the step that thick for trichlorosilane liquid is passed through purification tower system includes: is passed through by thick for trichlorosilane liquid and includes
The weight-removing column group of at least two weight-removing column carries out taking off heavily processing successively, heavily processes, through de-, the low-boiling-point substance obtained to obtain；Will be through de-
Heavily process the low-boiling-point substance feeding obtained and include that the lightness-removing column group of at least one lightness-removing column carries out de-light process successively, to obtain trichlorine
Hydrogen silicon.In the method, thick for trichlorosilane liquid is first passed through weight-removing column group again by lightness-removing column group, thick liquid can be made to carry out de-heavy industry
De-light industry sequence is carried out again after sequence.
Existing Trichlorosilane purification technology, has and needs repeatedly to purify, and operating procedure is complicated, and production cost is high, removing
The shortcoming of impurity poor effect, product purity needs to improve.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of Trichlorosilane purification adsorbent, it can apply to three
In chlorine hydrogen silicon purification, adsorption rate is fast, and adsorbing contaminant amount is big, easy and simple to handle during application, apply that this adsorbent produces three
Chlorine hydrogen silicon product purity is high.It is characterized in that preparation process includes:
Being distributed in water by a certain amount of styrene, add 5-cyclohexylidene-2-norborene in following ratio, dicarbapentaborane is double
(cyclopentadienyl group) titanium, potassium peroxydisulfate and dodecylbenzene sodium sulfonate, 1-[1-[2-(7,10-dioxa dicyclo [4.4.0] decyl-
1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole, octadecyl vinyl ether, rise
Temperature, at 80-110 DEG C, reacts 10-15 hour, and product filters, and dries, i.e. obtains Trichlorosilane purification adsorbent.
Ingredients weight parts
Styrene 100
5-ethylidene-2-norbornene 2-5
Double (cyclopentadienyl group) the titanium 0.1-1 of dicarbapentaborane
Potassium peroxydisulfate 0.2-0.8
Dodecylbenzene sodium sulfonate 0.5-1.5
1-[1-[2-(7,10-dioxa dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidines
Base]-3H-2-ketone benzimidaozole, 0.01-0.05
Octadecyl vinyl ether 0.5-2
Water 1000
Double (cyclopentadienyl group) titanium of described dicarbapentaborane is commercially available prod, the product produced such as AlfaAesar Chemical Co., Ltd.；5-
Ethylidene-2-norborene is commercially available prod, the product that as above Shanghai's style Er Ke chemical materials limited company produces；Dodecane
Base benzene sulfonic acid sodium salt is commercially available prod, the product produced such as Yan Sheng bio tech ltd, Shanghai；1-[1-[2-(7,10-dioxy
Miscellaneous dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole, for city
Sell product, the product produced such as Hubei Ju Sheng Science and Technology Ltd.；Octadecyl vinyl ether is commercially available prod, sun as big in Hangzhou
The product that Chemical Co., Ltd. produces.
The product of the present invention has the advantages that
Introduce 5-ethylidene-2-norbornene, double (cyclopentadienyl group) titanium of dicarbapentaborane, 1-[1-[2-(7,10-dioxa dicyclos
[4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole, single as polymerization
Body, makes the chemical stability of adsorbent product and heat stability be greatly enhanced.This adsorbent product adsorption rate is fast, adsorbing contaminant
Amount is big, put into production trichlorosilane time imurity-removal effective, the trichlorosilane products purity of output is high.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
1000Kg water, 100Kg styrene, 3Kg5-ethylidene-2-norborene, 0.5Kg bis-carbonyl is added in 2000L reactor
Double (cyclopentadienyl group) titanium of base, 0.5Kg potassium peroxydisulfate, 1Kg dodecylbenzene sodium sulfonate, 0.03Kg1-[1-[2-(7,10-dioxies
Miscellaneous dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole, 1Kg
Octadecyl vinyl ether, is warming up to 100 DEG C, reacts 12h, and product filters, and dries, and i.e. obtains Trichlorosilane purification absorption
Agent.
Embodiment 2
1000Kg water, 100Kg styrene, 1Kg5-ethylidene-2-norborene, 0.1Kg bis-carbonyl is added in 2000L reactor
Double (cyclopentadienyl group) titanium of base, 0.2Kg potassium peroxydisulfate, 0.5Kg dodecylbenzene sodium sulfonate, 0.01Kg1.5Kg1-[1-[2-(7,
10-dioxa dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-benzimidazolyl-2 radicals-
Ketone, 0.5Kg octadecyl vinyl ether, it is warming up to 80 DEG C, reacts 10h, product filters, and dries, i.e. obtains Trichlorosilane purification
Use adsorbent.
Embodiment 3
1000Kg water, 100Kg styrene, 5Kg5-ethylidene-2-norborene, 1Kg dicarbapentaborane is added in 2000L reactor
Double (cyclopentadienyl group) titanium, 0.8Kg potassium peroxydisulfate, 1.5Kg dodecylbenzene sodium sulfonate, 0.05Kg1.5Kg1-[1-[2-(7,
10-dioxa dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-benzimidazolyl-2 radicals-
Ketone, 2Kg octadecyl vinyl ether, it is warming up to 110 DEG C, reacts 15h, product filters, and dries, and i.e. obtains Trichlorosilane purification and uses
Adsorbent.
Comparative example 1
Being added without 5-ethylidene-2-norbornene, other conditions are with embodiment 1.
Comparative example 2
Being added without double (cyclopentadienyl group) titanium of dicarbapentaborane, other conditions are with embodiment 1.
Comparative example 3
It is added without 1.5Kg1-[1-[2-(7,10-dioxa dicyclo [4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxyl-second
Base]-4-piperidyl]-3H-2-ketone benzimidaozole, other conditions are with embodiment 1.
Comparative example 4
Being added without octadecyl vinyl ether, other conditions are with embodiment 1.
Embodiment 4
500g weight/mass percentage composition is about the trichlorosilane crude product of 99.5%, is passed through equipped with this patent embodiment 1-3 and contrast
The 1000ml exchange column of adsorbent 500g prepared by example 1-4, at 50 DEG C, under the conditions of flow velocity 0.5BV/h, absorption purifies, and uses gas phase color
The weight/mass percentage composition of spectrum detection effluent, is shown in Table 1.
Table 1: the trichlorosilane products purity after the adsorbent product absorption purification that different process is produced.
| Numbering | Purity of trichlorosilane (%) |
| Embodiment 1 | 99.99 |
| Embodiment 2 | 99.99 |
| Embodiment 3 | 99.99 |
| Comparative example 1 | 99.91 |
| Comparative example 2 | 99.93 |
| Comparative example 3 | 99.94 |
| Comparative example 4 | 99.89 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (2)
1. the preparation method of a Trichlorosilane purification adsorbent, it is characterised in that comprise the following steps:
A certain amount of styrene is distributed in water, is proportionally added into 5-cyclohexylidene-2-norborene, the double (ring penta of dicarbapentaborane
Dialkylene) titanium, potassium peroxydisulfate and dodecylbenzene sodium sulfonate, 1-[1-[2-(7,10-dioxa dicyclo [4.4.0] decyl-1,3,
5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole, octadecyl vinyl ether, heat up,
80-110 DEG C, reacting 10-15 hour, product filters, and dries, i.e. obtains Trichlorosilane purification adsorbent.
Trichlorosilane purification adsorbent the most according to claim 1, it is characterised in that: the ratio of raw material components is for by weight
Amount part meter styrene 100 parts, 1000 parts of water, 5-cyclohexylidene-2-norborene 2-5 part, double (cyclopentadienyl group) titanium of dicarbapentaborane
0.1-1 part, potassium peroxydisulfate 0.2-0.8 part, dodecylbenzene sodium sulfonate 0.5-1.5 part, 1-[1-[2-(7,10-dioxa dicyclos
[4.4.0] decyl-1,3,5-triolefin-9-base)-2-hydroxy-ethyl]-4-piperidyl]-3H-2-ketone benzimidaozole 0.01-0.05
Part, octadecyl vinyl ether 0.5-2 part.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691202.4A CN106220772A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of Trichlorosilane purification adsorbent |
| CN201710310094.6A CN107082835A (en) | 2016-08-21 | 2017-05-05 | A kind of preparation method of Trichlorosilane purification purification aids |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610691202.4A CN106220772A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of Trichlorosilane purification adsorbent |
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| CN106220772A true CN106220772A (en) | 2016-12-14 |
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| CN201610691202.4A Withdrawn CN106220772A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of Trichlorosilane purification adsorbent |
| CN201710310094.6A Withdrawn CN107082835A (en) | 2016-08-21 | 2017-05-05 | A kind of preparation method of Trichlorosilane purification purification aids |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201710310094.6A Withdrawn CN107082835A (en) | 2016-08-21 | 2017-05-05 | A kind of preparation method of Trichlorosilane purification purification aids |
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| US20230097766A1 (en) * | 2020-11-05 | 2023-03-30 | Wacker Chemie Ag | Process for removing an impurity from a chlorosilane mixture |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101244377B (en) * | 2008-03-18 | 2011-04-13 | 西北大学 | Polymer absorbing agent and preparation thereof |
| CN101444721B (en) * | 2008-12-17 | 2012-07-04 | 凯瑞化工股份有限公司 | Nanometer-material-modified micron-level nonpolar adsorption resin with high specific surface area and preparation method thereof |
| CN101992068A (en) * | 2009-08-09 | 2011-03-30 | 中国科学院兰州化学物理研究所 | Nitrogen and phosphorus absorbing agent |
| CN105294910B (en) * | 2015-11-30 | 2018-04-03 | 王金明 | A kind of preparation method of adsorbent applied to Pristinamycin separation |
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2016
- 2016-08-21 CN CN201610691202.4A patent/CN106220772A/en not_active Withdrawn
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- 2017-05-05 CN CN201710310094.6A patent/CN107082835A/en not_active Withdrawn
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| CN107082835A (en) | 2017-08-22 |
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Application publication date: 20161214 |