CN109467091A - A kind of energy saver and method of silicon tetrachloride synthesis - Google Patents
A kind of energy saver and method of silicon tetrachloride synthesis Download PDFInfo
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- CN109467091A CN109467091A CN201811586226.9A CN201811586226A CN109467091A CN 109467091 A CN109467091 A CN 109467091A CN 201811586226 A CN201811586226 A CN 201811586226A CN 109467091 A CN109467091 A CN 109467091A
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- silicon tetrachloride
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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
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
- C01B33/10721—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride
- C01B33/10726—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material with the preferential formation of tetrachloride from silicon
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Abstract
The present invention relates to the energy savers and method of a kind of synthesis of silicon tetrachloride, including the cooling device of reactor, steam generator and silicon tetrachloride；Reactor bottom is equipped with chlorine inlet, lower part is equipped with the import of Si powder, and top is equipped with silicon tetrachloride import, and top is equipped with material and produces mouth, and material produces mouth and connects the import of steam generator thermal material；Steam generator is equipped with thermal material import, material outlet, water inlet, steam (vapor) outlet, thermal material import connection reactor, the cooling device of material outlet connection silicon tetrachloride；Steam generator is added from water inlet in soft water, and steam is produced from steam (vapor) outlet；The cooling device of silicon tetrachloride is equipped with thermal material import and material outlet, and thermal material import connects steam generator, and material outlet connects subsequent dust removal separation apparatus.The device prepares silicon tetrachloride using chlorine and the directly reaction of Si powder, and sprays into liquid silicon as hot refrigerant is taken into reactor, and steam occurs for the heat recovery that silicon tetrachloride is removed, and reaction heat is recycled.
Description
Technical field
It is the present invention relates to a kind of energy saver of silicon tetrachloride synthesis, in particular to a kind of directly to be synthesized with chlorine and Si powder
The energy saver and method of silicon tetrachloride.
Background technique
High purity silicon tetrachloride is colourless transparent liquid, and the slightly lower presentation of purity is micro- yellow or faint yellow, there is stinkpot.
Normal temperature and pressure lower density 1.48, -70 DEG C of fusing point, 57.6 DEG C of boiling point, boiling point increases as pressure increases.The water in humid air
Solution forms silicic acid and hydrogen chloride.Hydrolysis is very fierce when meeting water, also can play intense reaction with alcohols.It is dissolved in carbon tetrachloride, four
Titanium chloride, tin tetrachloride.It is corrosive to skin.For silicate class processed, organic silicon monomer, organic silicone oil, high-temperature insulation paint,
Silicone resin, silicon rubber etc., also serve as screening smoke.Industrial most produce by silicon powder high temperature and hydrogen chloride synthetic reaction and
?.
Chinese patent CN201310360305.9 proposes the synthetic method and its production system of a kind of silicon tetrachloride, the party
Method includes the production stage and rectification step of silicon tetrachloride crude product, and the production stage of the silicon tetrachloride crude product is with silicon powder
Gas-solid direct synthesis is carried out with chlorine and reacts four chlorinations of preparation under the situation for not adding any catalyst for primary raw material
Silicon, reactor are fluidized bed；Controlling reaction temperature is 250-450 DEG C, and the fluidizing gas velocity of pressure 0.05-0.5MPa, chlorine are
0.05~0.15m/s；Silicon tetrachloride selectivity is 95% or more in crude product.
However a large amount of heat is generated since chlorine and Si powder directly react, above-mentioned patent is in order to keep reactor temperature
Spend range, it is necessary to medium is added and takes out the heat of generation, and commonly taking hot mode is that a large amount of nitrogen of addition or chlorine add
The big excessive heat that reaction generation is removed as refrigerant, to generate following problems:
1, nitrogen and chlorine, which do not have transformed band to walk corresponding heat, needs excess very big, and equipment manufacturing cost is caused to increase；
2, take away corresponding heat using nitrogen, nitrogen can not be recycled in subsequent technique, and nitrogen is caused to waste, increase it is economical at
This；
3, corresponding heat is taken away using chlorine, since outlet temperature is 250-450 DEG C, temperature is higher, chlorine corrosion pole
By force, the corrosivity for needing to cope with chlorine using the high material of cost, not only increases economic cost, and have biggish safety
Hidden danger；
4, the heat of reaction process generation is taken away using nitrogen or chlorine, which can not recycle, and cause energy unrestrained
Take.
Summary of the invention
In order to solve problems in the prior art, the invention proposes a kind of energy savers of silicon tetrachloride synthesis；Using chlorine
Gas and the directly reaction of Si powder prepare silicon tetrachloride, and spray into liquid silicon as refrigerant into reactor, pass through liquid four
The heat that reaction generates is taken away in silicon chloride gasification, has the heat compared with GOOD TASTE after silicon tetrachloride gasification, therefore increases steam hair
Generating apparatus, the heat recovery that silicon tetrachloride is removed occur steam, reaction heat are sufficiently recycled, energy consumption has been saved.Due to
Silicon tetrachloride is reaction product, which not only reduces the additional amount of refrigerant, and avoids the recycling difficult problem of refrigerant；
Since silicon tetrachloride corrosivity is lower, also avoid that equipment material is more demanding and safety problem.Apparatus of the present invention are simple, are easy to
It realizes, substantially increases the economic benefit and social benefit of enterprise.
The technical solution adopted by the invention is as follows:
A kind of energy saver of silicon tetrachloride synthesis, including the cooling device of reactor, steam generator and silicon tetrachloride；Reaction
Device bottom is equipped with chlorine inlet, lower part is equipped with the import of Si powder, and top is equipped with silicon tetrachloride import, and top is equipped with material and produces mouth,
Wherein material extraction mouth connects the import of steam generator thermal material；Steam generator is equipped with thermal material import, material outlet, water
Import, steam (vapor) outlet, wherein thermal material import connects reactor, and material outlet connects the cooling device of silicon tetrachloride；Soft water is from water
Steam generator is added in import, and steam is produced from steam (vapor) outlet；The cooling device of silicon tetrachloride is equipped with thermal material import and thermal material goes out
Mouthful, wherein thermal material import connects steam generator, and material outlet connects subsequent dust removal separation apparatus.
Using the power-economizing method of the device of the invention synthesis silicon tetrachloride, tetrachloro is prepared using chlorine and the directly reaction of Si powder
SiClx, and liquid silicon is sprayed into as hot refrigerant is taken into reactor, reaction is taken away by liquid silicon gasification and is produced
Raw heat, the heat after silicon tetrachloride gasification enter steam generator, and steam occurs for the heat recovery that silicon tetrachloride is removed,
Reaction heat is recycled.
The hot refrigerant that takes of the reactor is silicon tetrachloride；
Taking hot refrigerant is thick silicon tetrachloride of the silicon tetrachloride after dedusting, one in the product silicon tetrachloride after purification
Kind or mixing.
It with silicon tetrachloride with the molar ratio of silicon tetrachloride for reacting generation is 7:1-10:1 that the reactor, which takes heat,.
It is 0.5-1MPa that steam pressure, which occurs, for the steam generator.
A kind of energy saver of the silicon tetrachloride synthesis, it is characterized in that compared with traditional silicon tetrachloride synthesizer,
Energy consumption 20-40% can be saved.
The present invention prepares silicon tetrachloride using chlorine and the directly reaction of Si powder, and liquid silicon is sprayed into reactor
As refrigerant, the heat that reaction generates is taken away by liquid silicon gasification, major advantage is as follows:
1, since silicon tetrachloride is reaction product, which not only reduces the additional amount of refrigerant, and avoids refrigerant
Recycling difficult problem；
2, since silicon tetrachloride corrosivity is lower, avoid that equipment material is more demanding and safety problem；
3, have the heat compared with GOOD TASTE after silicon tetrachloride gasification, therefore increase steam generation facility, silicon tetrachloride is moved
Steam occurs for the heat recovery walked, and reaction heat is sufficiently recycled, compared with traditional silicon tetrachloride synthesizer, can save energy
Consume 20-40%.
Detailed description of the invention
Fig. 1 is overall structure diagram of the invention；
The cooling device of R101 reactor, E101 steam generator, E102 silicon tetrachloride.
Specific embodiment
The present invention is described in further detail in the following with reference to the drawings and specific embodiments:
It is described as follows according to Fig. 1:
Including reactor R101, steam generator E101, the cooling device E102 of silicon tetrachloride；The bottom reactor R101 is equipped with chlorine
Gas import, lower part are equipped with the import of Si powder, and top is equipped with silicon tetrachloride import, and top is equipped with material and produces mouth, and wherein material produces
Mouth connection steam generator E101 thermal material import；Steam generator E101 be equipped with thermal material import, material outlet, water into
Mouthful, steam (vapor) outlet, wherein thermal material import connects reactor R101, and material outlet connects the cooling device E102 of silicon tetrachloride, soft
Steam generator E101 is added from water inlet in water, and steam is produced from steam (vapor) outlet；The cooling device E102 of silicon tetrachloride is equipped with thermal material
Import and material outlet, wherein thermal material import connects steam generator E101, and material outlet connects subsequent dedusting separation
Device.
Reactor R101 is added in chlorine and Si powder, as reaction carries out, moves from silicon tetrachloride is added into reactor R101
Except the heat that reaction generates, unreacted chlorine, silicon tetrachloride and a small amount of Si powder are produced at the top of reactor R101 and enters steam
Generator E101, soft water needed for steam occurs are added from the bottom steam generator E101, extraction at the top of steam generator E101
Steam, the reactor R101 top extraction material after exchanging heat enter subsequent remove after the cooling device E102 of silicon tetrachloride is cooling
Dust separating device is further processed.
It is reaction product silicon tetrachloride that the reactor R101, which takes hot refrigerant,.Reactor R101 take heat with silicon tetrachloride with
The molar ratio for reacting the silicon tetrachloride generated is 7-10.It is 0.5-1MPa that steam pressure, which occurs, for steam generator E101.
Embodiment 1
Reactor R101 is added in chlorine and Si powder, as reaction carries out, moves from silicon tetrachloride is added into reactor R101
Except the heat that reaction generates, unreacted chlorine, silicon tetrachloride and a small amount of Si powder are produced at the top of reactor R101 and enters steam
Generator E101, soft water needed for steam occurs are added from the bottom steam generator E101, extraction at the top of steam generator E101
Steam, the reactor R101 top extraction material after exchanging heat enter subsequent remove after the cooling device E102 of silicon tetrachloride is cooling
Dust separating device is further processed.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that it is reaction product that reactor R101, which takes hot refrigerant,
Silicon tetrachloride.
The energy saver of described a kind of silicon tetrachloride synthesis, it is characterized in that reactor R101 takes heat silicon tetrachloride and anti-
The molar ratio for the silicon tetrachloride that should be generated is 7.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that steam generator E101 generation steam pressure is
0.5MPa。
A kind of energy saver of the silicon tetrachloride synthesis, it is characterized in that compared with traditional silicon tetrachloride synthesizer,
Energy consumption 40% can be saved.
Embodiment 2
Reactor R101 is added in chlorine and Si powder, as reaction carries out, moves from silicon tetrachloride is added into reactor R101
Except the heat that reaction generates, unreacted chlorine, silicon tetrachloride and a small amount of Si powder are produced at the top of reactor R101 and enters steam
Generator E101, soft water needed for steam occurs are added from the bottom steam generator E101, extraction at the top of steam generator E101
Steam, the reactor R101 top extraction material after exchanging heat enter subsequent remove after the cooling device E102 of silicon tetrachloride is cooling
Dust separating device is further processed.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that it is reaction product that reactor R101, which takes hot refrigerant,
Silicon tetrachloride.
The energy saver of described a kind of silicon tetrachloride synthesis, it is characterized in that reactor R101 takes heat silicon tetrachloride and anti-
The molar ratio for the silicon tetrachloride that should be generated is 10.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that steam generator E101 generation steam pressure is
0.5MPa。
A kind of energy saver of the silicon tetrachloride synthesis, it is characterized in that compared with traditional silicon tetrachloride synthesizer,
Energy consumption 20% can be saved.
Embodiment 3
Reactor R101 is added in chlorine and Si powder, as reaction carries out, moves from silicon tetrachloride is added into reactor R101
Except the heat that reaction generates, unreacted chlorine, silicon tetrachloride and a small amount of Si powder are produced at the top of reactor R101 and enters steam
Generator E101, soft water needed for steam occurs are added from the bottom steam generator E101, extraction at the top of steam generator E101
Steam, the reactor R101 top extraction material after exchanging heat enter subsequent remove after the cooling device E102 of silicon tetrachloride is cooling
Dust separating device is further processed.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that it is reaction product that reactor R101, which takes hot refrigerant,
Silicon tetrachloride.
The energy saver of described a kind of silicon tetrachloride synthesis, it is characterized in that reactor R101 takes heat silicon tetrachloride and anti-
The molar ratio for the silicon tetrachloride that should be generated is 7.
The energy saver of a kind of silicon tetrachloride synthesis, it is characterized in that steam generator E101 generation steam pressure is
1MPa。
A kind of energy saver of the silicon tetrachloride synthesis, it is characterized in that compared with traditional silicon tetrachloride synthesizer,
Energy consumption 36% can be saved.
The present invention prepares silicon tetrachloride using chlorine and the directly reaction of Si powder, and liquid silicon is sprayed into reactor
As refrigerant, the heat that reaction generates is taken away by liquid silicon gasification, is had after silicon tetrachloride gasification compared with GOOD TASTE
Heat, therefore increase steam generation facility, steam occurs for the heat recovery that silicon tetrachloride is removed, and reaction heat is sufficiently recycled benefit
With having saved energy consumption.Since silicon tetrachloride is reaction product, which not only reduces the additional amount of refrigerant, and avoids
The recycling difficult problem of refrigerant；Since silicon tetrachloride corrosivity is lower, also avoid that equipment material is more demanding and safety problem.
Apparatus of the present invention are simple, it is easy to accomplish, substantially increase the economic benefit and social benefit of enterprise.
Claims (6)
1. a kind of energy saver of silicon tetrachloride synthesis, including the cooling device of reactor, steam generator and silicon tetrachloride；Reactor
Bottom is equipped with chlorine inlet, lower part is equipped with the import of Si powder, and top is equipped with silicon tetrachloride import, and top is equipped with material and produces mouth,
Middle material extraction mouth connects the import of steam generator thermal material；Steam generator be equipped with thermal material import, material outlet, water into
Mouthful, steam (vapor) outlet, wherein thermal material import connects reactor, and material outlet connects the cooling device of silicon tetrachloride；Soft water from water into
Mouth addition steam generator, steam are produced from steam (vapor) outlet；The cooling device of silicon tetrachloride is equipped with thermal material import and material outlet,
Wherein thermal material import connects steam generator, and material outlet connects subsequent dust removal separation apparatus.
2. the power-economizing method of the device synthesis silicon tetrachloride using claim 1, it is characterized in that directly anti-using chlorine and Si powder
Silicon tetrachloride should be prepared, and sprays into liquid silicon as hot refrigerant is taken into reactor, is gasified by liquid silicon
The heat that reaction generates is taken away, the heat after silicon tetrachloride gasification enters steam generator, and the heat that silicon tetrachloride is removed returns
Raw steam is received and dispatched, reaction heat is recycled.
3. method according to claim 2, it is characterized in that the hot refrigerant that takes of reactor is reaction product silicon tetrachloride.
4. method according to claim 2 derives from it is characterized in that the hot refrigerant that takes of the reactor is silicon tetrachloride
One of product silicon tetrachloride after thick silicon tetrachloride, purification after dedusting or mixing.
5. method according to claim 2, it is characterized in that reactor takes heat silicon tetrachloride and the silicon tetrachloride for reacting generation
Molar ratio be 7-10:1.
6. method according to claim 2, it is characterized in that it is 0.5-1MPa that steam pressure, which occurs, for the steam generator.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811586226.9A CN109467091A (en) | 2018-12-25 | 2018-12-25 | A kind of energy saver and method of silicon tetrachloride synthesis |
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| CN201811586226.9A CN109467091A (en) | 2018-12-25 | 2018-12-25 | A kind of energy saver and method of silicon tetrachloride synthesis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
| CN115636416A (en) * | 2022-11-11 | 2023-01-24 | 武汉新硅科技潜江有限公司 | Synthetic method of silicon tetrachloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2002173313A (en) * | 2000-12-04 | 2002-06-21 | Denki Kagaku Kogyo Kk | Method for manufacturing silicon tetrachloride |
| TW200902443A (en) * | 2007-04-02 | 2009-01-16 | Norsk Hydro As | Process for production of silicon tetrachloride by reaction of silicon metal and chlorine with internal cooling |
| CN203568858U (en) * | 2013-08-19 | 2014-04-30 | 浙江富士特集团有限公司 | Production system for synthesis of silicon tetrachloride |
| CN105800618A (en) * | 2016-02-29 | 2016-07-27 | 天津大学 | Method and device for producing optical fiber-grade silicon tetrachloride |
| CN106241815A (en) * | 2016-09-13 | 2016-12-21 | 中国恩菲工程技术有限公司 | A kind of reactor preparing Silicon chloride. and application |
-
2018
- 2018-12-25 CN CN201811586226.9A patent/CN109467091A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002173313A (en) * | 2000-12-04 | 2002-06-21 | Denki Kagaku Kogyo Kk | Method for manufacturing silicon tetrachloride |
| TW200902443A (en) * | 2007-04-02 | 2009-01-16 | Norsk Hydro As | Process for production of silicon tetrachloride by reaction of silicon metal and chlorine with internal cooling |
| CN203568858U (en) * | 2013-08-19 | 2014-04-30 | 浙江富士特集团有限公司 | Production system for synthesis of silicon tetrachloride |
| CN105800618A (en) * | 2016-02-29 | 2016-07-27 | 天津大学 | Method and device for producing optical fiber-grade silicon tetrachloride |
| CN106241815A (en) * | 2016-09-13 | 2016-12-21 | 中国恩菲工程技术有限公司 | A kind of reactor preparing Silicon chloride. and application |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
| CN114956021B (en) * | 2021-11-22 | 2024-06-04 | 江西吉翔医药化工有限公司 | Preparation method of phosphorus pentachloride |
| CN115636416A (en) * | 2022-11-11 | 2023-01-24 | 武汉新硅科技潜江有限公司 | Synthetic method of silicon tetrachloride |
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