CN100425313C - Technology for separating and enrichment recovering silicon tetrachloride - Google Patents
Technology for separating and enrichment recovering silicon tetrachloride Download PDFInfo
- Publication number
- CN100425313C CN100425313C CNB2005100030811A CN200510003081A CN100425313C CN 100425313 C CN100425313 C CN 100425313C CN B2005100030811 A CNB2005100030811 A CN B2005100030811A CN 200510003081 A CN200510003081 A CN 200510003081A CN 100425313 C CN100425313 C CN 100425313C
- Authority
- CN
- China
- Prior art keywords
- silicon tetrachloride
- tetrachloride
- technology
- enrichment
- recovering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Abstract
The present invention relates to a technology for separating, enriching and recovering silicon tetrachloride from crude low-boiling point titanium tetrachloride mixtures which are generated from refined titanium tetrachloride and contain various impurities, such as titanium tetrachloride, silicon tetrachloride, chlorides of carbon and sulfur, etc. An asymmetrical fractionation technology which uses titanium tetrachloride / silicon tetrachloride as a key component, and a cutting fractionation technology of an intermediate key component are adopted to control the temperature of a tower body and a tower top; the low-boiling point mixture whose silicon tetrachloride content is from 0.3 to 20% can be separated, enriched and recovered to obtain the silicon tetrachloride whose content is more than 90%; meanwhile, the pollution problem of discharge of the silicon tetrachloride in the process of production of the refined titanium tetrachloride is solved.
Description
Technical field
The invention belongs to branch gold-plating technical field, be specifically related to separate a kind of low boiling crude titanic chloride mixture of the numerous impurity such as chloride that contain titanium tetrachloride, silicon tetrachloride and carbon, sulphur that produce from refining titanic chloride and the technology of enrichment recovering silicon tetrachloride.
Technical background
In titanium sponge was produced, a kind of process route was to utilize rich titanium material, and high titanium slag during for example ilmenite is smelted is made crude titanic chloride with chlorine through high-temp chlorination, after the crude titanic chloride rectification and purification, obtained the titanium sponge product with magnesium-reduced vacuum distillation.In the titanium-riched material chlorination process, impurity components such as the silicon that contains in the raw materials such as reducing agent petroleum coke, sulphur carry out side reaction, produce numerous impurity compounds such as silicon tetrachloride, carbon tetrachloride, carbon disulfide, sulfur dichloride, sulfur monochloride, dichloro sulphur carbon, tetrachloro oxygen two sulphur.Partly silicon tetrachloride is not with coagulating the exhaust emissions except that lacking, and all the other silicon tetrachlorides enter in the crude titanic chloride.According to the quality requirement that titanium sponge is produced, the silicon tetrachloride impurity content that enters the titanium tetrachloride of reduction distillation technology need be controlled at≤0.01% level, and titanium tetrachloride purity need reach more than 99.9%, so crude titanic chloride must carry out rectifying desiliconization processing.In the refining production process of titanium tetrachloride, produce the titanium tetrachloride seminal fluid and by the low boiling mixture of numerous impurity such as titanium tetrachloride, silicon tetrachloride, carbon tetrachloride, carbon disulfide, sulfur dichloride, sulfur monochloride, dichloro sulphur carbon, tetrachloro oxygen two sulphur.In the current technology, in order to reclaim titanium tetrachloride, low boiling mixture is returned refining system, when reclaiming titanium tetrachloride, low boiling chloride impurities such as silicon tetrachloride repeatedly enter in the atmosphere after the circulation in refining production system, this repeatedly circulating effect the operation control and the purification efficiency of valve tower.Silicon tetrachloride is a harmful substance, enters the hydrogen chloride gas that can be converted into nanometer grade silica aerosol and highly corrosive in the atmosphere, has both polluted environment, causes the waste of resource again.
Produce in the titanium white technology in chloridising, be rich in the low boiling mixture of compositions such as titanium tetrachloride, silicon tetrachloride, carbon tetrachloride and sulfur monochloride in the crude titanic chloride too.When titanium tetrachloride hydrolysis generated titanium dioxide, the silicon tetrachloride of not removing generated silica impurity and enters in the product, has both influenced the quality of titanium dioxide, has wasted the silicon tetrachloride resource again.
Summary of the invention
The invention provides a kind of from the low boiling mixture that refining titanic chloride produces, the separation and the technology of enrichment recovering silicon tetrachloride.
The raw materials used low boiling mixture that contains numerous impurity such as silicon tetrachloride, carbon tetrachloride, carbon disulfide, sulfur dichloride of the present invention for the refining titanic chloride generation, silicon tetrachloride content is 0.3～20% in the low boiling mixture, and adopting with titanium tetrachloride/silicon tetrachloride is the asymmetric fractionation and the middle key component cutting technique fractionating technology of key component system.Because the boiling point of titanium tetrachloride is 136.4 ℃, the boiling point of silicon tetrachloride is 56.8 ℃, technological parameter is controlled to be in the asymmetric fractional distillation process: reflux ratio is 3～25: 1; The distillation temperature in the kettle is 110～136 ℃, and fractionating column control temperature is 32～56 ℃, and the condenser condenses coolant-temperature gage is lower than 15 ℃, and the cooling water temperature of tail condenser is lower than 5 ℃.In condenser, obtain silicon tetrachloride liquid respectively and in distillation still, obtain titanium tetrachloride liquid through fractionation.The silicon tetrachloride content that reclaims enrichment is more than 90%.
Adopting technology of the present invention, can will be the thick silicon tetrachloride product of high-load from the low content silicon tetrachloride enrichment the low boiling mixture that refining titanic chloride produces.This technology simultaneously also enrichment the titanium tetrachloride in the low boiling mixed liquor, improved the utilization rate of resource and the purification efficiency of titanium tetrachloride, reduced production cost, the environmental pollution that silicon tetrachloride causes to airborne release when having eliminated former refining titanic chloride.
The specific embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1, is 15% low boiling mixture with valve tower intermittent fractionation silicon tetrachloride content, and distillation still adopts the valve tower distillation still of Φ 1200 * 1500mm, and fractionating column adopts the valve tower of Φ 270 * 8910mm, and condenser adopts 25m
2Condenser.The temperature of distillation still is controlled at 110 ℃～132 ℃, and the tower top temperature of valve tower is 35 ℃～56 ℃, and the condensate temperature of condenser is 8～12 ℃, the condensate temperature of tail condenser-2～2 ℃, and reflux ratio is 3～16: 1.The silicon tetrachloride content that reclaims is 90%.
Embodiment 2, it with valve tower intermittent fractionation silicon tetrachloride content 0.5% low boiling mixture, equipment and flow process are identical with embodiment one, the tower top temperature of valve tower is 32 ℃～56 ℃, the condensate temperature of condenser is 6～10 ℃, the condensate temperature of tail condenser-4～0 ℃, reflux ratio is 15～25: 1.The temperature of distillation still is controlled at 134 ℃～136 ℃.The silicon tetrachloride pregnant solution content that reclaims is 91%.
Embodiment 3, it with the continuous fractionation silicon tetrachloride of valve tower content 15% low boiling mixture, equipment and flow process are identical with embodiment one, the tower top temperature of valve tower is 32 ℃～56 ℃, the condensate temperature of condenser is 12～15 ℃, 2～5 ℃ of the condensate temperatures of tail condenser, reflux ratio are 15～20: 1.The temperature of distillation still is controlled at 130 ℃～136 ℃.The silicon tetrachloride pregnant solution content that reclaims is 93%.
Claims (2)
1, the technology of a kind of separation and enrichment recovering silicon tetrachloride, it is characterized in that the raw materials used low boiling mixture that contains silicon tetrachloride, carbon tetrachloride, carbon disulfide and the numerous impurity of sulfur dichloride for the refining titanic chloride generation, adopting titanium tetrachloride/silicon tetrachloride is the asymmetric fractionation and the middle key component cutting fractionation process of key component system, and technological parameter is controlled to be: reflux ratio is 3～25: 1; The distillation temperature in the kettle is 110～136 ℃, and fractionating column control temperature is 32～56 ℃, and the condenser condenses coolant-temperature gage is lower than 15 ℃, and the cooling water temperature of tail condenser is lower than 5 ℃.
2, the technology of a kind of separation according to claim 1 and enrichment recovering silicon tetrachloride, it is characterized in that silicon tetrachloride content is 0.3～20% in the low boiling mixture that contains silicon tetrachloride, carbon tetrachloride, carbon disulfide and the numerous impurity of sulfur dichloride that used refining titanic chloride produces, the silicon tetrachloride content of enriching and recovering is more than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100030811A CN100425313C (en) | 2005-05-26 | 2005-05-26 | Technology for separating and enrichment recovering silicon tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100030811A CN100425313C (en) | 2005-05-26 | 2005-05-26 | Technology for separating and enrichment recovering silicon tetrachloride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1868875A CN1868875A (en) | 2006-11-29 |
| CN100425313C true CN100425313C (en) | 2008-10-15 |
Family
ID=37442682
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100030811A Expired - Fee Related CN100425313C (en) | 2005-05-26 | 2005-05-26 | Technology for separating and enrichment recovering silicon tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100425313C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113912107B (en) * | 2021-11-08 | 2023-03-28 | 贵州威顿晶磷电子材料股份有限公司 | High-purity titanium tetrachloride purification manufacturing process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4385964A (en) * | 1979-05-21 | 1983-05-31 | Aluminum Company Of America | Method for preventing the undesirable condensation of aluminum chloride in a fractional distillation column |
| US5242549A (en) * | 1991-12-06 | 1993-09-07 | Shell Oil Company | Distillation separation process of titanium tetrachloride and halohydrocarbon |
| CN1232043A (en) * | 1998-04-15 | 1999-10-20 | 北京有色金属研究总院 | Method for removing large amount of organic impurities from titanium tetrachloride |
-
2005
- 2005-05-26 CN CNB2005100030811A patent/CN100425313C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4385964A (en) * | 1979-05-21 | 1983-05-31 | Aluminum Company Of America | Method for preventing the undesirable condensation of aluminum chloride in a fractional distillation column |
| US5242549A (en) * | 1991-12-06 | 1993-09-07 | Shell Oil Company | Distillation separation process of titanium tetrachloride and halohydrocarbon |
| CN1232043A (en) * | 1998-04-15 | 1999-10-20 | 北京有色金属研究总院 | Method for removing large amount of organic impurities from titanium tetrachloride |
Non-Patent Citations (1)
| Title |
|---|
| 浮阀塔精制四氯化钛工艺参数的选择. 张常武等.钛工业进展，第6期. 1997 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1868875A (en) | 2006-11-29 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3635664A (en) | REGENERATION OF HYDROCHLORIC ACID PICKLING WASTE BY H{11 SO{11 {0 ADDITION, DISTILLATION AND FeSO{11 {0 Precipitation | |
| US3966458A (en) | Separation of zirconium and hafnium | |
| CN102153053B (en) | Methods for purifying and comprehensively utilizing hydrogen sulfide byproduct during production of carbon disulfide by methane method | |
| CA1115492A (en) | Production of chlorine | |
| CN1209282C (en) | Method for producing concentrated nitric acid and installation for carrying out a method of this type | |
| CN1295969A (en) | Process for separation and recovery hydrogen chloride from water | |
| CN100425313C (en) | Technology for separating and enrichment recovering silicon tetrachloride | |
| EP2995702A1 (en) | Zinc production method | |
| CN103936047B (en) | A kind of preparation method of anhydrous Aluminum chloride | |
| CN105129799A (en) | Refining purification of product carbon disulfide in methane-method carbon disulfide production process | |
| EP0234894A2 (en) | Process for the production of sulfur | |
| CA1073634A (en) | Recovery of sulfur values from spent sulfuric acid | |
| EP0016290A1 (en) | Continuous process for the removal of sulphur dioxide from waste gases, and hydrogen and sulphuric acid produced thereby | |
| CN101955413B (en) | Method for separating acidic dichloroethane mixture | |
| CA1143694A (en) | Method of winning aluminum metal from aluminous ore | |
| US4547353A (en) | Apparatus and processes for the concentration of sulphuric acid | |
| CN114671405A (en) | Process for preparing high-purity hydrogen chloride from by-product hydrochloric acid in methane chloride process | |
| CN103539711B (en) | A kind of technique being continuously separated pure compound from refinery's mercaptan removal waste liquid | |
| CN101219943A (en) | Method for purifying and using chloroethanoic acid tail gas | |
| CN107285350A (en) | A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon | |
| JP2011178586A (en) | Method for refining polycrystalline silicon | |
| JP3247420B2 (en) | Method for producing titanium tetrachloride | |
| CN106187676B (en) | The recovery method of distillation residual liquid in a kind of production of tetrachloro-ethylene | |
| CN109956452A (en) | A kind of preparation method and its device of reagent hydrochloric acid | |
| CN116161622B (en) | Method for preparing bromine by using carnallite mother liquor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20081015 Termination date: 20150526 |
|
| EXPY | Termination of patent right or utility model |