CN101306818A - Method for preparing magnesium silicide and device - Google Patents
Method for preparing magnesium silicide and device Download PDFInfo
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- CN101306818A CN101306818A CNA2008100627366A CN200810062736A CN101306818A CN 101306818 A CN101306818 A CN 101306818A CN A2008100627366 A CNA2008100627366 A CN A2008100627366A CN 200810062736 A CN200810062736 A CN 200810062736A CN 101306818 A CN101306818 A CN 101306818A
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Abstract
The invention discloses a preparation method of magnesium silicide and a device thereof. In the preparation method, equivalently mixed magnesium powder and silicon powder are used as raw materials, continuously fed into a vertical cylindrical reactor from the top under vacuum or gas protection, and continuously stirred, so as to allow uniform and complete reaction and prevent excessive heat generation from the reaction and magnesium vapor escape. The inventive device is mainly the vertical cylindrical reactor instead of a horizontal reactor, and a reducer at the top of the rector is used for driving a spiral stirrer to stir the raw materials; a heater is arranged on the upper part of the outer wall of the reactor for heating, a cooling water jacket is arranged on the lower part of the reactor for cooling, a scraper and a perforated plate are arranged at the bottom of the reactor for pulverizing the generated magnesium silicide from the reaction, the upper part of the reactor is connected with a feeding device, and the lower part of the reactor is connected with a discharge device. After the reaction is completed, the continuous product is made into magnesium silicide powder with fine particle size, uniform composition and equivalent weight through pulverization by the scraper and the perforated plate. The inventive preparation method can realize continuous production of magnesium silicide, improve conversion rate of raw materials, reduce magnesium consumption, and reduce energy consumption.
Description
Technical field
The present invention relates to a kind of preparation method and device of magnesium silicide.
Background technology
Magnesium silicide is a kind of important industrial raw material, be widely used in preparing silane gas, polysilicon, amorphous silicon membrane, stupalith and siliceous nanometer powder etc., semi-conductor microelectronics production, solar cell production, material coating processing industry and advanced ceramics are had more and more important effect.Exploitation is efficient, the industrial synthesis of high quality and less energy-consumption is the developing direction of magnesium silicide technology.
The synthetic method of tradition magnesium silicide is that silica flour and magnesium powder are mixed in proportion, and is being heated to about 500～650 ℃ under nitrogen atmosphere or the vacuum, and it is reacted, and generates the magnesium silicide powder, and reaction formula is:
2Mg+Si→Mg
2Si+77.4kJ
Because it is thermopositive reaction that the reaction of synthesizing magnesium silicide is one, in large-scale fixed bed device, during synthesizing magnesium silicide, will run into a serious problem, i.e. material reaction heat release causes high temperature, material can be warmed up to 650～800 ℃ automatically.At this moment the product of Sheng Chenging is the bonding bulk, forms and departs from Mg
2Si.Thereby the yield that causes departing from this composition feedstock production silane is on the low side.Simultaneously, large-scale fixed bed device generally is the mode of production of interval type, and promptly it needs to feed, heat, be incubated, cool off and get processes such as material, and production efficiency is lower, and energy consumption is bigger, and the product caking is serious, difficult treatment, and the labour protection condition is poor.
The relative gap mode of production, the magnesium silicide continuous synthesis has more advantage.German Patent 1143190 has proposed the method for continuously synthesizing magnesium silicide.A scheme is that horizontal spiral advances reactor, and compound is fed forward by the spiral propeller of rotation in the reaction tubes of level, passes through the heating zone while stir.Another scheme is to prolong elbow type, and reaction tubes tilts slightly, and material rotates by reacting pipe, and one side is mixed and stirred one side and passed through the heating zone.Silicon magnesium compound is by the hot-zone in continuous oven, and heat transfer and mass transfer are more even, is eased because of reaction heat causes the superheated problem, thereby the yield of producing silane is improved.But because above two schemes have all been used the reaction tubes of level substantially, reaction tubes top does not have material to fill, thereby causes that magnesium vapor leaks, and causes the loss of magnesium.Material proportion in this type of horizontal reactor, magnesium is essential excessive 3～10%, not only cause the waste of magnesium, and the crystallization meeting on reaction tubes inner part surface of the magnesium of evaporation hinders the normal operation of mechanism.Therefore, the output of device and quality product are restricted.
Summary of the invention
In order to overcome the problem that background technology exists, the object of the present invention is to provide a kind of preparation method and device of magnesium silicide.
The applicant when magnesium silicide synthesizes, at first is the distillation of magnesium according to discovering for many years, gasiform magnesium and the effect of silica flour solid then, and magnesium atom to internal divergence, forms magnesium silicide by silicon powder surface at last.Because thermopositive reaction raises temperature of charge suddenly, under the high temperature under magnesium silicide instability and the high temperature magnesium evaporate easily, make building-up process complicated.The actual temperature of material has very material impact to the magnesium silicide quality when synthetic.Actual building-up reactions has following possible reversing process:
2Mg+Si→Mg
2Si (2)
Mg
2Si→MgSi+Mg (3)
2MgSi→Mg
2Si+Si (4)
MgSi→Mg+Si (5)
500 ℃ begin the reaction begin to be undertaken with obvious speed by (2) formula, product is Mg
2Si.Evaporate because of magnesium when being higher than 700 ℃, the decomposition course of (3) formula begins to preponderate.Temperature is higher, and heat-up time is longer, divides to solve the more.The intermediate compound MgSi instability that generates below 700 ℃ the time, as (4), changes into Mg
2Si separates out silicon simultaneously.Further be decomposed into silicon and magnesium by (5) formula when being higher than 1100 ℃.So under the high temperature in the synthetic magnesium silicide, Mg
2The content of Si is few, and free magnesium, the free silica of separating out are more.And at present the preparation facilities of magnesium silicide can't solve the problem that problems of excessive heat and magnesium steam escape in the building-up process.
The technical scheme that the present invention solves its technical problem employing is:
One, a kind of preparation method of magnesium silicide:
1) with silica flour and magnesium powder mixed according to mass ratio 1: 1.5～2.3, add transition hopper after, vacuumize or charge into shielding gas, put it into elevating hopper again;
2) give vertical and cylindrical reactor continuous charging by spiral propeller;
3) the flight agitator of raw material by the vertical and cylindrical reactor stirs, and allows its thermal field through reactor top, and the temperature range of this thermal field control is 500～650 ℃, and this moment, silica flour and the magnesium powder generation magnesium silicide that reacts was emitted heat simultaneously;
4) magnesium silicide of harsh one-tenth enters the cold water jacket cooling of reactor lower part under action of gravity, and it is overheated to prevent to react;
5), after powder ground, send into recovering hopper, and take out final product by discharge bucket at last by scraper and orifice plate.
Described shielding gas is hydrogen or argon gas.
Two, a kind of preparation facilities of magnesium silicide:
The present invention includes vertical and cylindrical reactor, flight agitator, two step-down gears, well heater, cold water jacket, scraper, orifice plate, recovering hopper, spiral propeller, discharge bucket, elevating hopper, transition hopper, three dust filter units, two oil-sealed rotary pumps, nine valves, visor and nitrogengas cylinders; The outlet of transition hopper connects hopper through first valve, and the outlet of elevating hopper connects spiral propeller; The external cylindrical surface upper end of vertical and cylindrical reactor coats well heater, and the lower end coats cold water jacket, and inside is furnished with flight agitator, scraper and orifice plate, and the top is furnished with visor; Flight agitator and spiral propeller adopt step-down gear to drive respectively; The vertical and cylindrical reactor links to each other with first oil-sealed rotary pump by second dust filter unit and the 7th valve; The vertical and cylindrical reactor bottom links to each other with recovering hopper with orifice plate by scraper, and recovering hopper links to each other by second valve with discharge bucket; Discharge bucket links to each other with nitrogengas cylinder with the 8th valve by the 3rd dust filter unit; Transition hopper links to each other with second oil-sealed rotary pump with the 6th valve by first dust filter unit, and connects the 3rd dust filter unit through the 4th valve, on recovering hopper, elevating hopper and the transition hopper, is connected to the 3rd valve, the 5th valve and the 5th valve respectively.
The present invention compares with background technology, and the beneficial effect that has is as follows:
(1) the serialization production of steps such as can reality reinforced, reaction of the present invention and rewinding, need not magnesium silicide interval type working system charging, heating, insulation, cool off and get process such as material, production efficiency improves, energy consumption reduces.
(2) compare with horizontal reactor or nearly horizontal reactor, the vertical and cylindrical reactor that the present invention adopts, can effectively prevent escaping of magnesium steam, effectively save the consumption of magnesium, avoid the crystallization meeting on reaction tubes inner part surface of the magnesium that evaporates to hinder the normal operation of mechanism simultaneously.
(3) the vertical and cylindrical reactor of the present invention's employing, the heating zone on top and the cooling zone of bottom have been designed, the heat that reaction is produced is brought into the cooling zone cooling of bottom along with magnesium silicide, effectively prevent because of reacting thermogenetic problems of excessive heat, avoid the generation of product caking and side reaction, thereby ensure the quality of products.
Description of drawings
Fig. 1 is a structural representation of the present invention.
Fig. 2 is the XRD figure spectrum of embodiment 1 gained magnesium silicide product.
Among the figure: 1. vertical and cylindrical reactor, 2. flight agitator, 3a, 3b. step-down gear, 4. well heater, 5. cold water jacket, 6. scraper, 7. orifice plate, 8. recovering hopper, 9. spiral propeller, 10. discharge bucket, 11. elevating hoppers, 12. transition hopper, 13a～13c. dust filter unit, 14a, 14b. oil-sealed rotary pump, 15a～15i. valve, 16. visor, 17. nitrogengas cylinders
Embodiment
As shown in Figure 1, the present invention includes vertical and cylindrical reactor 1, flight agitator 2, two step-down gear 3a, 3b, well heater 4, cold water jacket 5, scraper 6, orifice plate 7, recovering hopper 8, spiral propeller 9, discharge bucket 10, elevating hopper 11, transition hopper 12, three dust filter unit 13a～13c, two oil-sealed rotary pump 14a, 14b, nine valve 15a～15i, visor 16 and nitrogengas cylinder 17; The outlet of transition hopper 12 connects hopper 11 through the first valve 15a, and the outlet of elevating hopper 11 connects spiral propeller 9; The external cylindrical surface upper end of vertical and cylindrical reactor 1 coats well heater 4, and the lower end coats cold water jacket 5, and inside is furnished with flight agitator 2, scraper 6 and orifice plate 7, and the top is furnished with visor 16; Flight agitator 2 and spiral propeller 9 adopt step-down gear 3a, 3b to drive respectively; Vertical and cylindrical reactor 1 links to each other with the first oil-sealed rotary pump 14a by the second dust filter unit 13b and the 7th valve 15g; Vertical and cylindrical reactor 1 bottom links to each other with recovering hopper 8 with orifice plate 7 by scraper 6, and recovering hopper 8 links to each other by the second valve 15b with discharge bucket 10; Discharge bucket 10 links to each other with nitrogengas cylinder 17 with the 8th valve 15h by the 3rd dust filter unit 13c; Transition hopper 12 links to each other with the second oil-sealed rotary pump 14b with the 6th valve 15f by the first dust filter unit 13a, and meet the 3rd dust filter unit 13c through the 4th valve 15d, on recovering hopper 8, elevating hopper 11 and the transition hopper 12, be connected to the 3rd valve 15c, the 5th valve 15e and the 5th valve 15i respectively.
The concrete implementation step of the present invention is as follows:
(1) with silica flour and magnesium powder mixed according to the rules, stirs;
(2) to total system through nitrogen purging repeatedly with vacuumize, finally keep vacuum state, hydrogen or argon shield if desired after vacuumizing, charges into hydrogen or argon gas;
(3) begin well heater 4 is begun heating, and, open the step-down gear 3a at vertical and cylindrical reactor 1 top, the flight of the flight agitator 2 of vertical and cylindrical reactor 1 is upwards promoted cold water jacket 5 logical water coolants;
(4) valve-off 15a, above-mentioned raw materials put into transition hopper 12 after, sealing;
(5) open vacuum pump 14b and valve 15f, begin transition hopper 12 is vacuumized, exhaust vacuum after, valve-off 15f;
(6) open valve 15a, raw material is put into elevating hopper 11 after, open the step-down gear 3b of spiral propeller 9, it is reinforced to begin vertical barrel type reactor 1;
(7) raw material generates magnesium silicide in the thermal field district reaction of well heater 4 generations of vertical and cylindrical reactor 1, enters the cooling of cold water jacket 5 cooling zones;
(8) observe vertical and cylindrical reactor 1 by visor 16, treat that the vertical and cylindrical reactor is full, stop step-down gear 3b earlier, continue reaction.
(9) stop step-down gear 3a after, and allow its counter-rotating, the beginning rewinding.
Embodiment 1:
Silica flour and magnesium powder are after 1: 1.7 the mixed, to pour in the preparation facilities of the present invention according to mass ratio, and the temperature of vertical and cylindrical reactor heating zone is controlled at 550 ℃.Finally having obtained the magnesium silicide product, is its XRD figure spectrum as shown in Figure 2, and all XRD diffraction peaks are all identical with the standard card 35-0773 of magnesium silicide in this collection of illustrative plates, illustrate that product is the higher magnesium silicide of purity.
Embodiment 2:
Silica flour and magnesium powder are after 1: 1.5 the mixed, to pour in the preparation facilities of the present invention according to mass ratio, and the temperature of vertical and cylindrical reactor heating zone is controlled at 650 ℃.Finally obtained the magnesium silicide product.
Embodiment 3:
Silica flour and magnesium powder are after 1: 2.3 the mixed, to pour in the preparation facilities of the present invention according to mass ratio, and the temperature of vertical and cylindrical reactor heating zone is controlled at 500 ℃.Finally obtained the magnesium silicide product.
Claims (3)
1, a kind of preparation method of magnesium silicide is characterized in that:
1) with silica flour and magnesium powder mixed according to mass ratio 1: 1.5～2.3, add transition hopper after, vacuumize or charge into shielding gas, put it into elevating hopper again;
2) give vertical and cylindrical reactor continuous charging by spiral propeller;
3) the flight agitator of raw material by the vertical and cylindrical reactor stirs, and allows its thermal field through reactor top, and the temperature range of this thermal field control is 500～650 ℃, and this moment, silica flour and the magnesium powder generation magnesium silicide that reacts was emitted heat simultaneously;
4) magnesium silicide of harsh one-tenth enters the cold water jacket cooling of reactor lower part under action of gravity, and it is overheated to prevent to react;
5), after powder ground, send into recovering hopper, and take out final product by discharge bucket at last by scraper and orifice plate.
2. the preparation method of a kind of magnesium silicide according to claim 1, it is characterized in that: described shielding gas is hydrogen or argon gas.
3. the preparation facilities of a magnesium silicide is characterized in that: comprise vertical and cylindrical reactor (1), flight agitator (2), two step-down gears (3a, 3b), well heater (4), cold water jacket (5), scraper (6), orifice plate (7), recovering hopper (8), spiral propeller (9), discharge bucket (10), elevating hopper (11), transition hopper (12), three dust filter units (13a～13c), two oil-sealed rotary pumps (14a, 14b), nine valves (15a～15i), visor (16) and nitrogengas cylinder (17); The outlet of transition hopper (12) connects hopper (11) through first valve (15a), and the outlet of elevating hopper (11) connects spiral propeller (9); The external cylindrical surface upper end of vertical and cylindrical reactor (1) coats well heater (4), and the lower end coats cold water jacket (5), and inside is furnished with flight agitator (2), scraper (6) and orifice plate (7), and the top is furnished with visor (16); Flight agitator (2) and spiral propeller (9) adopt step-down gear (3a, 3b) to drive respectively; Vertical and cylindrical reactor (1) is by second dust filter unit (13b) and the 7th valve (15g), and (14a) links to each other with first oil-sealed rotary pump; Vertical and cylindrical reactor (1) bottom links to each other with recovering hopper (8) with orifice plate (7) by scraper (6), and recovering hopper (8) links to each other by second valve (15b) with discharge bucket (10); Discharge bucket (10) links to each other with nitrogengas cylinder (17) with the 8th valve (15h) by the 3rd dust filter unit (13c); Transition hopper (12) links to each other with second oil-sealed rotary pump (14b) with the 6th valve (15f) by first dust filter unit (13a), and connect the 3rd dust filter unit (13c) through the 4th valve (15d), on recovering hopper (8), elevating hopper (11) and the transition hopper (12), be connected to the 3rd valve (15c), the 5th valve (15e) and the 5th valve (15i) respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008100627366A CN101306818B (en) | 2008-07-01 | 2008-07-01 | Method for preparing magnesium silicide and device |
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|---|---|---|---|
| CN2008100627366A CN101306818B (en) | 2008-07-01 | 2008-07-01 | Method for preparing magnesium silicide and device |
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| CN101306818A true CN101306818A (en) | 2008-11-19 |
| CN101306818B CN101306818B (en) | 2010-06-09 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928006A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Equipment and method for producing magnesium silicide |
| CN101928005A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Reaction device for continuously synthesizing magnesium silicide |
| CN101928007A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Magnesium-silicide spiral cooling device |
| CN101928004A (en) * | 2010-03-31 | 2010-12-29 | 清华大学 | Method for preparing Mg2Si crystal and fluidized bed reactor |
| CN102452653A (en) * | 2011-05-10 | 2012-05-16 | 浙江仪和岚新能源科技有限公司 | Method and device for producing magnesium silicide |
| CN102874818A (en) * | 2011-07-11 | 2013-01-16 | 浙江仪和岚新能源科技有限公司 | Method for preparing magnesium silicide powder |
| CN106495159A (en) * | 2016-12-07 | 2017-03-15 | 武汉化工新材料工业技术研究院有限责任公司 | Continous way Self-propagating Reaction Synthesis device and its synthetic method |
| CN106913582A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院上海硅酸盐研究所 | A kind of magnesium silicide nano material and its preparation method and application |
| CN107032356A (en) * | 2017-04-26 | 2017-08-11 | 许昌学院 | A kind of preparation method of porous nano silicon |
| CN107597025A (en) * | 2017-09-26 | 2018-01-19 | 中天储能科技有限公司 | A kind of silicon monoxide quantity-produced apparatus |
| CN112479211A (en) * | 2020-12-17 | 2021-03-12 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1027439C (en) * | 1991-12-14 | 1995-01-18 | 浙江大学 | Making method of magnesium silicide |
| CN1291048C (en) * | 2002-02-15 | 2006-12-20 | 株式会社东京大学Tlo | Magnesium base composite material and method for production thereof |
-
2008
- 2008-07-01 CN CN2008100627366A patent/CN101306818B/en not_active Expired - Fee Related
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928004A (en) * | 2010-03-31 | 2010-12-29 | 清华大学 | Method for preparing Mg2Si crystal and fluidized bed reactor |
| CN101928004B (en) * | 2010-03-31 | 2013-02-20 | 清华大学 | Method for preparing Mg2Si crystal and fluidized bed reactor |
| CN101928007B (en) * | 2010-09-13 | 2013-04-17 | 中国化学赛鼎宁波工程有限公司 | Magnesium-silicide spiral cooling device |
| CN101928005A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Reaction device for continuously synthesizing magnesium silicide |
| CN101928007A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Magnesium-silicide spiral cooling device |
| CN101928005B (en) * | 2010-09-13 | 2012-07-11 | 化学工业第二设计院宁波工程有限公司 | Reaction device for continuously synthesizing magnesium silicide |
| CN101928006A (en) * | 2010-09-13 | 2010-12-29 | 化学工业第二设计院宁波工程有限公司 | Equipment and method for producing magnesium silicide |
| CN102452653A (en) * | 2011-05-10 | 2012-05-16 | 浙江仪和岚新能源科技有限公司 | Method and device for producing magnesium silicide |
| CN102874818A (en) * | 2011-07-11 | 2013-01-16 | 浙江仪和岚新能源科技有限公司 | Method for preparing magnesium silicide powder |
| CN106913582A (en) * | 2015-12-28 | 2017-07-04 | 中国科学院上海硅酸盐研究所 | A kind of magnesium silicide nano material and its preparation method and application |
| CN106495159A (en) * | 2016-12-07 | 2017-03-15 | 武汉化工新材料工业技术研究院有限责任公司 | Continous way Self-propagating Reaction Synthesis device and its synthetic method |
| CN107032356A (en) * | 2017-04-26 | 2017-08-11 | 许昌学院 | A kind of preparation method of porous nano silicon |
| CN107032356B (en) * | 2017-04-26 | 2019-02-19 | 许昌学院 | A kind of preparation method of porous nano silicon |
| CN107597025A (en) * | 2017-09-26 | 2018-01-19 | 中天储能科技有限公司 | A kind of silicon monoxide quantity-produced apparatus |
| CN112479211A (en) * | 2020-12-17 | 2021-03-12 | 烟台万华电子材料有限公司 | Method for continuously producing disilane |
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