CN102909006A - Catalyst for catalytic hydrogenation of silicon tetrachloride and preparation method thereof - Google Patents
Catalyst for catalytic hydrogenation of silicon tetrachloride and preparation method thereof Download PDFInfo
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- CN102909006A CN102909006A CN2012104379802A CN201210437980A CN102909006A CN 102909006 A CN102909006 A CN 102909006A CN 2012104379802 A CN2012104379802 A CN 2012104379802A CN 201210437980 A CN201210437980 A CN 201210437980A CN 102909006 A CN102909006 A CN 102909006A
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Abstract
The invention discloses silicon a catalyst for reaction of silicon tetrachloride and hydrogen to prepare trichlorosilane. Nanometer platinum particles are active constituents of the catalyst, and silicon dioxide is a carrier. By the catalyst, the time of reaction of the silicon tetrachloride and the hydrogen to prepare the trichlorosilane can be greatly shortened, a reaction condition becomes more temperate, the conversion rate of the silicon tetrachloride reaches 28 to 35 percent on the condition of temperature of 200 DEG C and pressure of 0.2MPa, so that the production cost and equipment investment on transforming trichlorosilane from the silicon tetrachloride and the hydrogen are greatly reduced.
Description
Technical field
The invention belongs to chemical catalysis field, being specifically related to a kind of is the Catalysts and its preparation method of trichlorosilane with hydrogenation of silicon tetrachloride.
Background technology
At present, polysilicon is mainly by improved Siemens production.But, being subjected to the course of reaction process technology limit, this method produces a large amount of silicon tetrachloride as by-product (1 ton of polysilicon of every production can produce the silicon tetrachloride of 15-18 ton) when producing polysilicon.As with 150,000 tons of calculating of the whole of China, then can produce ten thousand tons of silicon tetrachlorides of 225-270.The huge bottleneck that has been processed into restriction whole world polysilicon enterprise development of the silicon tetrachloride that quantity is huge.In addition, silicon tetrachloride is a kind of poisonous and harmful liquid, does not process and arbitrarily discharging if do not add, silicon tetrachloride will be combined by the steam in atmosphere, produces hydrogen chloride gas, thereby environment is caused severe contamination, also cause the significant wastage of resource, strengthened the production cost of enterprise.Rationally recycle silicon tetrachloride, in environmental contamination reduction, greatly reduce the production cost of enterprise, be conducive to the sustainable development of production of polysilicon enterprise.
The best method of polysilicon business processes silicon tetrachloride is that silicon tetrachloride and hydrogen are converted into trichlorosilane under catalyst action, this process can not only make silicon tetrachloride effectively be processed, trichlorosilane and hydrogen chloride as the production of polysilicon raw material have been obtained simultaneously, the secondary pollution of having avoided processing silicon chloride to bring is simultaneously also so that polysilicon enterprise realizes green closed cycle production truly.
Based on course of reaction and the mechanism of hot hydrogenation technology, German goldschmidt chemical corporation has been developed a kind of new silicon tetrachloride catalytic hydrogenating reduction technique.In this technique, adopt a kind in the chloride calcium chloride, strontium chloride, barium chloride of in II main group alkaline earth elements ca, strontium, the barium a kind and they, be mixed and made into the catalyst activity component, with low aluminium zeolite, alkali-free glass, vitreous silica, active carbon or porous SiO
2Prepare loaded catalyst as carrier.This catalyst has low conversion rate (below 23%), and the catalyst preparation is complicated, and reaction temperature and pressure is shortcomings such as higher (temperature are more than 500 ℃, more than the pressure 2.0MPa) still.
Summary of the invention
The object of the present invention is to provide the catalyst that is used for the silicon tetrachloride catalytic hydrogenation is become trichlorosilane that a kind of conversion ratio is high, reaction condition is gentle.
Another object of the present invention provides the preparation method of above-mentioned catalyst.
The present invention realizes that the technical scheme that above-mentioned purpose adopts is as follows:
A kind of catalyst of catalytic hydrogenation silicon tetrachloride, the active component of this catalyst are the nanometer platinum grain, and carrier is silica.
Further, the particle diameter of described nanometer platinum grain is 3-10nm.
Further, described silica is spherical particle.
Further, the particle diameter of the spherical particle of described silica is 200-800nm.
The method for preparing the catalyst of above-mentioned catalytic hydrogenation silicon tetrachloride: silica supports is scattered in the water, add again chloroplatinic acid or chloroplatinate, exist under isopropyl alcohol and the illumination condition reaction more than 10 hours, after separation, washing, drying, obtain described catalyst temperature 500-550 ℃ of lower calcining again.
Further, every 1g chloroplatinic acid or chloroplatinate use the isopropyl alcohol of 9-11ml.
Further, light application time is 10-20 hour.
Further, light application time is 10-15 hour.
Further, described silica supports is to obtain as follows: be 30-50 ℃ under to mix with the tetraethyl orthosilicate ethanolic solution in temperature with the ammoniacal liquor alcohol mixeding liquid, product is through separating, wash, be drying to obtain silica supports, the mol ratio of ammonia and ethanol is 1:(5-8 in the described ammoniacal liquor alcohol mixeding liquid), the volume ratio of described tetraethyl orthosilicate ethanolic solution mesosilicic acid tetra-ethyl ester and ethanol is 1:(5-10).
Further, the volume ratio of ammoniacal liquor alcohol mixeding liquid and tetraethyl orthosilicate ethanolic solution is (2-3): 1.
The load capacity of nanometer platinum grain can be regulated by consumption or the light application time of regulating chloroplatinic acid or chloroplatinate on the silica supports, light application time is longer, it is more complete that chloroplatinic acid or chloroplatinate decompose, usually, the silica supports of every 100g adds chloroplatinic acid or the chloroplatinate of 1-20g, makes the mass percent of nanometer platinum grain in the catalyst that finally makes reach 0.5-5%.
Preferably, the silica supports of every 100g adds chloroplatinic acid or the chloroplatinate of 7-15g.
More preferably, the silica supports of every 100g adds chloroplatinic acid or the chloroplatinate of 10-12g.
Catalyst of the present invention is carried on Platinum Nanoparticles on the silicon dioxide microsphere, make Platinum Nanoparticles keep good dispersiveness, improve the catalytic activity of platinum, this catalyst can shorten the time of silicon tetrachloride and hydrogen reaction generation trichlorosilane greatly, making reaction condition, more gentle (compare existing reaction condition: temperature is more than 500 ℃, more than the pressure 2.0MPa), under 200 ℃ and 0.2MPa condition, the conversion ratio of silicon tetrachloride reaches 28-35%, is that production cost and the equipment investment of trichlorosilane greatly reduces thereby make the silicon tetrachloride hydro-conversion.
Description of drawings
Fig. 1 particle diameter is the SiO of 200nm
2The transmission electron microscope of carrier (TEM) figure.
Fig. 2 is the HRTEM figure of catalyst.
Fig. 3 particle diameter is the SiO of 400nm
2The TEM figure of carrier.
Fig. 4 particle diameter is the SiO of 800nm
2The TEM figure of carrier.
The specific embodiment
The invention will be further described below in conjunction with drawings and Examples.
Embodiment 1
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 5:1 is total to 500ml, stir 10 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 5:1, solution is mixed, after in 30 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 200nm, as shown in Figure 1;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 3.2 g potassium chloroplatinates and 30ml isopropyl alcohol, illumination is 10 hours under high voltage mercury lamp radiation, then centrifugation, washing, dry, obtain the grey black pressed powder, then this grey black pressed powder is placed on 500 ℃ of calcinings 1 hour, obtain catalyst, be designated as 1#, Fig. 2 is high-resolution-ration transmission electric-lens (HRTEM) figure of gained catalyst, from intergranular apart from finding out that the silica surface load has platinum, nanoparticle platinum size is generally 3~10nm.
Embodiment 2
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 3.2 g chloroplatinic acids and 35 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 520 ℃ of calcinings 1.5 hours, obtains catalyst, be designated as 2#.
Embodiment 3
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 8:1 is total to 500ml, stir 15 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 10:1, solution is mixed, after in 50 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 800nm, as shown in Figure 4;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 3.2 g chloroplatinic acids and 35 ml isopropyl alcohols, illumination is 15 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 550 ℃ of calcinings 2 hours, obtains catalyst, be designated as 3#.
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Embodiment 4
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 0.3g potassium chloroplatinate and 3 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 500 ℃ of calcinings 1 hour, obtains catalyst, be designated as 4#.
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 2.1g chloroplatinic acid and 25 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 520 ℃ of calcinings 1.5 hours, obtains catalyst, be designated as 5#.
Embodiment 6
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 4.5 g chloroplatinic acids and 45 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 550 ℃ of calcinings 2 hours, obtains catalyst, be designated as 6#.
Embodiment 7
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 6 g chloroplatinic acids and 61 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 550 ℃ of calcinings 2 hours, obtains catalyst, be designated as 7#.
Embodiment 8
The adding mol ratio is that absolute ethyl alcohol and the ammoniacal liquor mixed solution of 6:1 is total to 500ml, stir 12 min, solution is mixed, then add absolute ethyl alcohol and tetraethyl orthosilicate 250 ml mixed solutions that volume ratio is 8:1, solution is mixed, after in 40 ℃ of waters bath with thermostatic control, reacting completely, centrifugation goes out the silica white powder, then with the absolute ethyl alcohol cyclic washing until solution is neutral, centrifugation goes out the silica white powder, drying is 180 minutes under 180 ℃, obtains SiO
2White powder, gained SiO
2Be spherical, particle diameter is 400nm, as shown in Figure 3;
Silica white powder 30 g of preparation are dispersed in the 1000 ml high purity waters, add 3 g chlorine platinum sodium and 31 ml isopropyl alcohols, illumination is 12 hours under high voltage mercury lamp radiation, then centrifugation, washing, drying, obtain the grey black pressed powder, then this grey black pressed powder is placed on 550 ℃ of calcinings 2 hours, obtains catalyst, be designated as 8#.
Get respectively 1#, 2#, 3#, 4#, 5#, 6#, 7#, 8# catalyst 100 g are dispersed in the 1500 ml water, are an internal diameter 20 mm, external diameter is 24mm, and length is that the stainless-steel pipe of 1 m is immersed in the water of above-mentioned 1500 ml that are dispersed with 100 g catalyst, slowly rolls, take out drying, again submergence after 30 minutes, dry again, the tubular reactor that repeatedly can obtain being equipped with catalyst for three times like this.The mol ratio of then regulating hydrogen and silicon tetrachloride is 6:1, and the temperature of regulating this tubular reactor is 200 ℃, and pressure is 0.2MPa, obtains table 1
The conversion ratio of shown silicon tetrachloride.
Table 1
Adopting as can be seen from Table 1 the 100g particle diameter is the SiO of 200-800nm spherical particle
2Carrier, the converting silicon tetrachloride rate that obtains with 10-12g chloroplatinic acid or chloroplatinate effect (being 1#, 2#, 3# test) is the highest.
Claims (10)
1. the catalyst of a catalytic hydrogenation silicon tetrachloride, it is characterized in that: the active component of described catalyst is the nanometer platinum grain, carrier is silica.
2. the catalyst of described catalytic hydrogenation silicon tetrachloride according to claim 1, it is characterized in that: the particle diameter of described nanometer platinum grain is 3-10nm.
3. the catalyst of described catalytic hydrogenation silicon tetrachloride according to claim 1, it is characterized in that: described silica is spherical particle.
4. the catalyst of described catalytic hydrogenation silicon tetrachloride according to claim 3, it is characterized in that: the particle diameter of the spherical particle of described silica is 200-800nm.
5. according to claim 1 to the catalyst of 4 arbitrary described catalytic hydrogenation silicon tetrachlorides, it is characterized in that: the mass percent of nanometer platinum grain is 0.5-5% in the described catalyst.
6. the preparation method who prepares the catalyst of the described catalytic hydrogenation silicon tetrachloride of claim 1, it is characterized in that: silica supports is scattered in the water, add again chloroplatinic acid or chloroplatinate, exist under isopropyl alcohol and the illumination condition reaction more than 10 hours, after separation, washing, drying, obtain described catalyst temperature 500-550 ℃ of lower calcining again.
7. preparation method according to claim 6 is characterized in that: the isopropyl alcohol of every 1g chloroplatinic acid or chloroplatinate use 9-11ml.
8. preparation method according to claim 6, it is characterized in that, described silica supports is to obtain as follows: be to mix under 30-50 ℃ the ethanolic solution of ammoniacal liquor alcohol mixeding liquid and tetraethyl orthosilicate in temperature, product is through separating, wash, be drying to obtain silica supports, the mol ratio of ammonia and ethanol is 1:(5-8 in the described ammoniacal liquor alcohol mixeding liquid), the volume ratio of described tetraethyl orthosilicate ethanolic solution mesosilicic acid tetra-ethyl ester and ethanol is 1:(5-10).
9. preparation method according to claim 9 is characterized in that: the volume ratio of ammoniacal liquor alcohol mixeding liquid and tetraethyl orthosilicate ethanolic solution is (2-3): 1.
10. the preparation method of the catalyst of described catalytic hydrogenation silicon tetrachloride according to claim 6, it is characterized in that every 100g silica supports adds 1-20g chloroplatinic acid or chloroplatinate, preferably, every 100g silica supports adds 7-15g chloroplatinic acid or chloroplatinate, more preferably, every 100g silica supports adds 10-12g chloroplatinic acid or chloroplatinate.
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Cited By (3)
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CN108439413A (en) * | 2018-05-16 | 2018-08-24 | 亚洲硅业(青海)有限公司 | A kind of method for hydrogenation of silicon tetrachloride |
CN109957104A (en) * | 2019-04-03 | 2019-07-02 | 杭州硅途新材料科技有限公司 | A method of using the modified trisiloxanes of solid-borne platinum catalyst synthesizing polyether |
CN112007634A (en) * | 2019-05-28 | 2020-12-01 | 新特能源股份有限公司 | Novel catalyst for vinyl trichlorosilane, preparation method thereof and method for preparing vinyl trichlorosilane through catalysis of novel catalyst |
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CN106276917B (en) * | 2015-05-28 | 2019-01-22 | 内蒙古盾安光伏科技有限公司 | Polysilicon production process and system |
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CN102198929A (en) * | 2010-03-22 | 2011-09-28 | 中国科学院理化技术研究所 | Hollow silicon dioxide submicron sphere with nanoscale noble metal and silicon dioxide inner core and preparation method thereof |
CN102633263A (en) * | 2012-04-11 | 2012-08-15 | 洛阳晶辉新能源科技有限公司 | Method for preparing trichlorosilane by hydrogenating silicon tetrachloride |
CN102838120A (en) * | 2012-09-18 | 2012-12-26 | 特变电工新疆硅业有限公司 | Method for catalyzing and hydrogenating silicon tetrachloride by using nano platinum |
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CN101816946A (en) * | 2009-02-27 | 2010-09-01 | 比亚迪股份有限公司 | Preparation method and application of catalyst used in hydrogenation of silicon tetrachloride |
CN102198929A (en) * | 2010-03-22 | 2011-09-28 | 中国科学院理化技术研究所 | Hollow silicon dioxide submicron sphere with nanoscale noble metal and silicon dioxide inner core and preparation method thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108439413A (en) * | 2018-05-16 | 2018-08-24 | 亚洲硅业(青海)有限公司 | A kind of method for hydrogenation of silicon tetrachloride |
CN108439413B (en) * | 2018-05-16 | 2019-10-25 | 亚洲硅业(青海)有限公司 | A kind of method for hydrogenation of silicon tetrachloride |
CN109957104A (en) * | 2019-04-03 | 2019-07-02 | 杭州硅途新材料科技有限公司 | A method of using the modified trisiloxanes of solid-borne platinum catalyst synthesizing polyether |
CN112007634A (en) * | 2019-05-28 | 2020-12-01 | 新特能源股份有限公司 | Novel catalyst for vinyl trichlorosilane, preparation method thereof and method for preparing vinyl trichlorosilane through catalysis of novel catalyst |
CN112007634B (en) * | 2019-05-28 | 2023-08-29 | 新特能源股份有限公司 | Novel vinyl trichlorosilane catalyst, preparation method thereof and method for preparing vinyl trichlorosilane by catalysis of novel vinyl trichlorosilane catalyst |
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