CN1291912C - Large-scale apparatus for synthesis of trichlorosilane and synthesis method thereof - Google Patents
Large-scale apparatus for synthesis of trichlorosilane and synthesis method thereof Download PDFInfo
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- CN1291912C CN1291912C CN 200510200333 CN200510200333A CN1291912C CN 1291912 C CN1291912 C CN 1291912C CN 200510200333 CN200510200333 CN 200510200333 CN 200510200333 A CN200510200333 A CN 200510200333A CN 1291912 C CN1291912 C CN 1291912C
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Abstract
The present invention relates to a large-scale apparatus for synthesizing trichlorosilane, which is in the structure of a barrel shape. A barrel diameter enlarging part at the upper part is a gas-solid separating section which is provided with a discharge opening, a straight barrel section at the middle part is a reaction section wrapped by a heater, a silicon powder feeding hole is arranged on the upper part of the heater, and the bottom is connected with a lower sealing head on which a hydrogen chloride inlet port and a slag discharging port are arranged. A gas distributing board is arranged above the hydrogen chloride inlet port at the bottom of the barrel reaction section, and gas holes are distributed in the gas distributing board. An inner heat exchange casing tube is arranged in the barrel body, and the inner heat exchange casing tube is communicated with a heat medium inlet pipe and a heat medium outlet pipe outside the barrel body. The large-scale apparatus solves the problem of large-scale trichlorosilane production and has the characteristics of convenient disassembly, high capability of synthesis, stable reaction, high utilization rate or conversion rate of raw material, and high trichlorosilane content in products. The large-scale apparatus is mainly used for fields of non-ferrous metallurgy, electronic material, chemical industry, etc.
Description
(1) technical field
The present invention relates to a kind of synthesizer and synthetic method of Chemicals, particularly a kind of trichlorosilane synthesizer and synthetic method.
(2) background technology
At present, minor diameter trichlorosilane synthesizer (diameter 400mm is following) is mainly adopted in the production of trichlorosilane.Silica flour is interrupted and adds the trichlorosilane synthesizer, and hydrogenchloride enters trichlorosilane synthetic furnace after measuring, and silica flour, hydrogenchloride react in the reaction in furnace district, produce trichlorosilane and silicon tetrachloride, and a spot of dichloro-dihydro silicon.The chlorosilane (trichlorosilane, silicon tetrachloride, a spot of dichloro-dihydro silicon and other silicon high boiling compound) that produces enters chlorosilane cooling, condenser system then through gas solid separation.In reaction process, the heat of generation is taken out of outside the stove by low-pressure steam or warm water, keeps the constant of reaction in furnace temperature by given steam (or warm water) amount.Silicon powder layer height, temperature of reaction are two important parameters that speed, trichlorosilane synthetic ratio height are carried out in reaction.At present, above-mentioned two parameters mainly lean on knowhow by manually controlling.
Existing trichlorosilane synthesizer is a tubular construction, top barrel diameter expansion section s is the gas solid separation section, this section is provided with discharge port, the direct tube section at middle part is a conversion zone, conversion zone outsourcing well heater, top is provided with the silica flour opening for feed, and the bottom connects lower cover, have the hydrogenchloride inlet mouth on the lower cover, the shortcoming of existence is:
1, the little (Φ≤400mm) of stove tube diameter, conversion zone length is unreasonable with cooperating of diameter, gas-solid is short duration of contact, react insufficient, production equipment elasticity is little, synthesis capability is little, and seriously restricting with the trichlorosilane is the downstream Chemicals of raw material and the industrial scale of electronic product, simultaneously, influence the research and development of derived product, influence the development of whole silicon industrial chain.
2, the temperature of reaction of conversion zone is inhomogeneous, fluctuation is big, and the heat and mass instability causes reaction too fast or slow excessively, influences the productive rate of synthetic product chlorosilane; Simultaneously, because temperature is too high, cause the generation of a large amount of contour compounds that boil of silicon tetrachloride as by-product in the building-up process sometimes, synthetic middle trichlorosilane content is low; In addition, temperature is too high in the reaction process, influences the work-ing life of device.
3, the silica flour amount and the hydrogen chloride gas scale of construction do not match, and bed depth is wayward, cause that the silica flour transformation efficiency is low, the hydrogenchloride utilization ratio is low, the yield in unit time instability; Simultaneously, because the silica flour transformation efficiency is low, the quantity of slag increases, and once with short production cycle, deslagging labour intensity is big.
4, gas solid separation is insufficient, cause sintetics chlorosilane (trichlorosilane, silicon tetrachloride, a spot of dichloro-dihydro silicon and other silicon high boiling compound) impure easily, in the sintetics chlorosilane fine silica powder is arranged, influence sintetics purity, increase the back operation simultaneously and separate the purification difficulty.
5, furnace bottom does not have slag-drip opening, need dismantle lower cover during deslagging, deslagging inconvenience, and the deslagging treatment time is long, and labour intensity is big, and production environment is poor.
(3) summary of the invention
The object of the present invention is to provide a kind of large-scale trichlorosilane synthesizer and synthetic method; solve the problem of large-scale production trichlorosilane, and solve that the synthesis capability that exists in the present synthesizer is little, reaction is unstable, raw material availability or transformation efficiency is low, problems such as trichlorosilane content is low in the product.
Technical scheme of the present invention: this large-scale trichlorosilane synthesizer, be tubular construction, top barrel diameter expansion section s is the gas solid separation section, this section is provided with discharge port, the direct tube section at middle part is a conversion zone, conversion zone outsourcing well heater, the well heater top is provided with the silica flour opening for feed, the bottom connects lower cover, has the hydrogenchloride inlet mouth on the lower cover, and it is characterized in that: lower cover has slag-drip opening, the hydrogenchloride inlet mouth top of the conversion zone bottom of cylindrical shell is provided with gas distribution grid, be distributed with pore on the gas distribution grid, cylindrical shell is built-in with interior heat exchange clutch, and interior heat exchange clutch is communicated with cylindrical shell heat medium enter hose and heat medium produce hose outward.
The taper gas cap is housed on the pore of above-mentioned gas grid distributor.
Above-mentioned conversion zone, gas solid separation section, lower cover section and gas distribution grid bracing frame are absolute construction, and parts connect by flange each other.
The diameter of above-mentioned gas solid separation section is 1.5～3.5m.
The diameter of above-mentioned conversion zone is 0.45～2.8m.
The ratio of above-mentioned conversion zone height and conversion zone diameter is 3-10.
Above-mentioned interior heat exchange clutch bottom is 10～150mm from the distance of the pore taper gas cap of gas distribution grid.
Above-mentioned silica flour opening for feed is 1.6～10.7m apart from the distance of conversion zone bottom.
Above-mentioned well heater upper edge is 1.5～10m apart from the distance of conversion zone bottom.
The trichlorosilane synthesis method of this employing claim 1 synthesizer, it is characterized in that following steps are arranged: before reaction, at first silica flour is joined in the synthesizer, start the outer well heater of synthesizer, furnace body temperature is heated to 250-350 ℃, feed hydrogen chloride gas simultaneously, after treating that silica flour and hydrogen chloride gas begin reaction, stop outer heater heats, reaction in furnace is undertaken by reaction self heat release constant temperature, and 7-10 days deslagginves once.
The present invention has following significant effect:
(1), the ratio of conversion zone height and conversion zone diameter is 3-10, increased gas-solid duration of contact, making gas-solid duration of contact is 10S～55S, makes reaction more abundant, helps improving the quality of products.
(2), the interior heat exchange clutch arrangement increased the homogeneity of temperature of reaction, helps improving the gas-solid contact, enhancing mass and heat transfer.
(3), the setting of gas distribution grid, hydrogen chloride gas is evenly entered in the conversion zone, make reaction more even; The position of gas distribution grid is reasonable, and shutdown maintenance can not destroy thermal insulation layer, reduces labour intensity.
(4), the diameter of gas solid separation section be straight tube conversion zone 1.5-3.5 doubly, help gas solid separation.
(5), slag-drip opening is set, adopt nitrogen purging, vacuum sucking-off mode deslagging need not dismantled lower cover during deslagging at lower cover.
The invention solves the problem of large-scale production trichlorosilane, can determine the diameter of synthesizer conversion zone according to ultimate production, diameter range is 0.45-2.8m, is suitable for the factory of 1000 ~ 15000 tons of trichlorosilanes of annual production.The present invention uses the trichlorosilane synthesizer to produce trichlorosilane, and stable reaction is produced trichlorosilane per year more than 2000 tons, trichlorosilane and solid impurity separator well, quality product height.Realize extensive trichlorosilane production and production of polysilicon, guarantee the development of silicon industrial chain.Be mainly used in fields such as nonferrous metallurgy, electronic material and chemical industry.
(4) description of drawings
Fig. 1 is a structural representation of the present invention.
1-gas solid separation section, 2-conversion zone, 3-well heater, 4-heat medium produce hose, 5-heat medium enter hose, 6-interior heat exchange clutch, 7-lower cover, 8-discharge port, 9-silica flour opening for feed, 10-hydrogenchloride inlet mouth, 11-gas distribution grid, 12-taper gas cap, 13-slag-drip opening, 14-pressure tap.
(5) embodiment
Embodiment is referring to Fig. 1, and the large-scale trichlorosilane synthesizer of the present invention is a tubular construction, and top barrel diameter expansion section s is a gas solid separation section 1, the neck of gas solid separation section 1 is a reverse frustoconic, this section is provided with discharge port 8, and the opening of discharge port 8 is tilted to down, helps discharging.
The direct tube section at middle part is a conversion zone 2, conversion zone outsourcing well heater 3, and the well heater top is provided with silica flour opening for feed 9, and the opening of silica flour opening for feed 9 is tilted to, and helps charging.
The bottom connects lower cover 7, has hydrogenchloride inlet mouth 10 and slag-drip opening 13 on the lower cover, whenever necessary, can also offer pressure tap 14.
The hydrogenchloride inlet mouth top of the conversion zone bottom of its cylindrical shell is provided with gas distribution grid 11, is distributed with pore on the gas distribution grid, for increasing the distribution effect, taper gas cap 12 is housed on the pore of above-mentioned gas grid distributor 11.
Cylindrical shell is built-in with interior heat exchange clutch 6, and interior heat exchange clutch is communicated with cylindrical shell heat medium enter hose 5 and heat medium produce hose 4 outward.
Above-mentioned gas solid separation section 1, conversion zone 2, lower cover 7 connect by flange each other, are convenient to loading and unloading and maintenance.
The diameter of above-mentioned gas solid separation section 1 is 1.5～3.5m.The direct tube section at middle part is that the barrel dliameter of conversion zone 2 is 0.45～2.8m.
Conversion zone 2 height are 3-10 with the ratio of conversion zone diameter.
Above-mentioned silica flour opening for feed 9 is 1.6～10.7m apart from the distance of conversion zone bottom.Above-mentioned well heater 3 upper edges are 1.5～10m apart from the distance of conversion zone bottom.Above-mentioned heat transfer tube bottom is 10～150mm from the distance of the pore taper gas cap of gas distribution grid 11.
Adopt the synthetic method of above-mentioned large-scale trichlorosilane synthesizer, following concrete steps are arranged: before reaction, at first silica flour is joined 1.5～10m height in the synthesizer, start the outer well heater of synthesizer, furnace body temperature is heated to 250-350 ℃, feed hydrogen chloride gas simultaneously, after treating that silica flour and hydrogen chloride gas begin reaction, stop outer heater heats, reaction in furnace is undertaken by reaction self heat release constant temperature, and 7-10 days deslagginves once.
Claims (7)
1. one kind large-scale trichlorosilane synthesizer, be tubular construction, top barrel diameter expansion section s is the gas solid separation section, this section is provided with discharge port, the direct tube section at middle part is a conversion zone, conversion zone outsourcing well heater, the well heater top is provided with the silica flour opening for feed, the bottom connects lower cover, has the hydrogenchloride inlet mouth on the lower cover, and it is characterized in that: lower cover has slag-drip opening, the hydrogenchloride inlet mouth top of the conversion zone bottom of cylindrical shell is provided with gas distribution grid, be distributed with pore on the gas distribution grid, cylindrical shell is built-in with interior heat exchange clutch, and interior heat exchange clutch is communicated with cylindrical shell heat medium enter hose and heat medium produce hose outward;
The diameter of above-mentioned gas solid separation section is 1.5～3.5m;
The diameter of above-mentioned conversion zone is 0.45～2.8m;
The ratio of above-mentioned conversion zone height and conversion zone diameter is 3-10.
2. large-scale trichlorosilane synthesizer according to claim 1 is characterized in that: the taper gas cap is housed on the pore of above-mentioned gas grid distributor.
3. large-scale trichlorosilane synthesizer according to claim 1 is characterized in that: above-mentioned conversion zone, gas solid separation section, lower cover section and gas distribution grid bracing frame are absolute construction, and parts connect by flange each other.
4. large-scale trichlorosilane synthesizer according to claim 2 is characterized in that: above-mentioned interior heat exchange clutch bottom is 10～150mm from the distance of the pore taper gas cap of gas distribution grid.
5. large-scale trichlorosilane synthesizer according to claim 1 is characterized in that: above-mentioned silica flour opening for feed is 1.6～10.7m apart from the distance of conversion zone bottom.
6. large-scale trichlorosilane synthesizer according to claim 1 is characterized in that: above-mentioned well heater upper edge is 1.5～10m apart from the distance of conversion zone bottom.
7. trichlorosilane synthesis method that adopts claim 1 synthesizer, it is characterized in that following steps are arranged: before reaction, at first silica flour is joined in the synthesizer, start the outer well heater of synthesizer, furnace body temperature is heated to 250～350 ℃, feed hydrogen chloride gas simultaneously, after treating that silica flour and hydrogen chloride gas begin reaction, stop outer heater heats, reaction in furnace is undertaken by reaction self heat release constant temperature, and 7-10 days deslagginves once.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510200333 CN1291912C (en) | 2005-06-16 | 2005-06-16 | Large-scale apparatus for synthesis of trichlorosilane and synthesis method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510200333 CN1291912C (en) | 2005-06-16 | 2005-06-16 | Large-scale apparatus for synthesis of trichlorosilane and synthesis method thereof |
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| CN1699162A CN1699162A (en) | 2005-11-23 |
| CN1291912C true CN1291912C (en) | 2006-12-27 |
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5428146B2 (en) * | 2006-10-31 | 2014-02-26 | 三菱マテリアル株式会社 | Trichlorosilane production equipment |
| CN101143723B (en) * | 2007-08-08 | 2010-09-01 | 徐州东南多晶硅材料研发有限公司 | Modified method and device for preparing trichlorosilane and multicrystal silicon |
| US20090060819A1 (en) * | 2007-08-29 | 2009-03-05 | Bill Jr Jon M | Process for producing trichlorosilane |
| JP5359082B2 (en) * | 2007-10-23 | 2013-12-04 | 三菱マテリアル株式会社 | Trichlorosilane production apparatus and trichlorosilane production method |
| CN102040223B (en) * | 2010-12-23 | 2011-08-31 | 江西嘉柏新材料有限公司 | Method for producing trichlorosilane by continuously adding silicon powder |
| CN102745691B (en) * | 2012-07-16 | 2014-07-09 | 新特能源股份有限公司 | Method and device for recovering waste silicon powder from trichlorosilane synthetic furnace |
| KR101644239B1 (en) * | 2013-09-30 | 2016-07-29 | 주식회사 엘지화학 | Process for producing trichlorosilane |
| CN108607476B (en) * | 2016-12-09 | 2021-02-09 | 中国石油化工股份有限公司 | Fluidized bed reactor, application thereof and method for adsorbing and desulfurizing hydrocarbon oil |
| CN107619051A (en) * | 2017-09-20 | 2018-01-23 | 河南尚宇新能源股份有限公司 | A kind of method of trichlorosilane synthetic furnace and its volume increase consumption reduction |
| CN109607549A (en) * | 2019-01-31 | 2019-04-12 | 内蒙古通威高纯晶硅有限公司 | Furnace method is opened in a kind of trichlorosilane production technology in production of polysilicon |
| CN109879289A (en) * | 2019-04-12 | 2019-06-14 | 四川永祥多晶硅有限公司 | A kind of low value silicon powder recycling system |
| CN110817884A (en) * | 2019-12-10 | 2020-02-21 | 唐山三孚硅业股份有限公司 | Silicon tetrachloride synthetic furnace of high conversion |
| CN112279256A (en) * | 2020-10-23 | 2021-01-29 | 淮阴工学院 | Trichlorosilane fluidized bed reactor |
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Owner name: CHINA YOUSE ENGINEERING CO., LTD. Free format text: FORMER NAME: CHINA NONFERROUS ENGINEERING RESEARCH INSTITUTE |
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Address after: No. 12 Fuxing Road, Beijing, Beijing, Haidian District Patentee after: China Nonferrous Metals Engineering Company Limited Address before: No. 12 Fuxing Road, Beijing, Beijing, Haidian District Patentee before: China Non-ferrous Engineering Design General Inst. |
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Assignee: Luoyang Zhonggui High-tech Co., Ltd. Assignor: China Nonferrous Metals Engineering Company Limited Contract record no.: 2011410000011 Denomination of invention: Large-scale apparatus for synthesis of trichlorosilane and synthesis method thereof Granted publication date: 20061227 License type: Exclusive License Open date: 20051123 Record date: 20110322 |