CN117820350A - Alkyl aminosilane and preparation method thereof - Google Patents
Alkyl aminosilane and preparation method thereof Download PDFInfo
- Publication number
- CN117820350A CN117820350A CN202311846582.0A CN202311846582A CN117820350A CN 117820350 A CN117820350 A CN 117820350A CN 202311846582 A CN202311846582 A CN 202311846582A CN 117820350 A CN117820350 A CN 117820350A
- Authority
- CN
- China
- Prior art keywords
- catalyst
- alkylaminosilane
- phase catalyst
- filler
- silane
- 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.)
- Withdrawn
Links
- -1 Alkyl aminosilane Chemical compound 0.000 title claims description 4
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 120
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000000945 filler Substances 0.000 claims abstract description 36
- 239000007791 liquid phase Substances 0.000 claims abstract description 31
- 239000007790 solid phase Substances 0.000 claims abstract description 31
- 229910000077 silane Inorganic materials 0.000 claims abstract description 23
- 150000001412 amines Chemical class 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims description 14
- 239000010935 stainless steel Substances 0.000 claims description 14
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 11
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 11
- PZPGRFITIJYNEJ-UHFFFAOYSA-N disilane Chemical compound [SiH3][SiH3] PZPGRFITIJYNEJ-UHFFFAOYSA-N 0.000 claims description 9
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 6
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 6
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 abstract description 8
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 239000012299 nitrogen atmosphere Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 12
- 238000000227 grinding Methods 0.000 description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 11
- 239000012159 carrier gas Substances 0.000 description 10
- 238000001816 cooling Methods 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 10
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910052786 argon Inorganic materials 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 description 4
- VYIRVGYSUZPNLF-UHFFFAOYSA-N n-(tert-butylamino)silyl-2-methylpropan-2-amine Chemical compound CC(C)(C)N[SiH2]NC(C)(C)C VYIRVGYSUZPNLF-UHFFFAOYSA-N 0.000 description 4
- DZMHLJIUUXHYMI-UHFFFAOYSA-N N-[(tert-butylamino)-silylsilyl]-2-methylpropan-2-amine Chemical compound CC(C)(C)N[SiH]([SiH3])NC(C)(C)C DZMHLJIUUXHYMI-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- 239000005046 Chlorosilane Substances 0.000 description 2
- WLSVLQJPKZNQJC-UHFFFAOYSA-N N-propan-2-ylpropan-2-amine silane Chemical compound [SiH4].C(C)(C)NC(C)C WLSVLQJPKZNQJC-UHFFFAOYSA-N 0.000 description 2
- CQJXZWXDVFJKTL-UHFFFAOYSA-N [SiH3][SiH3].C(C)(C)NC(C)C Chemical compound [SiH3][SiH3].C(C)(C)NC(C)C CQJXZWXDVFJKTL-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000005576 amination reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 125000005265 dialkylamine group Chemical group 0.000 description 1
- WZUCGJVWOLJJAN-UHFFFAOYSA-N diethylaminosilicon Chemical compound CCN([Si])CC WZUCGJVWOLJJAN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- OWKFQWAGPHVFRF-UHFFFAOYSA-N n-(diethylaminosilyl)-n-ethylethanamine Chemical compound CCN(CC)[SiH2]N(CC)CC OWKFQWAGPHVFRF-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/025—Silicon compounds without C-silicon linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses an alkylaminosilane and a preparation method thereof, wherein the alkylaminosilane is obtained by introducing silane A and an organic amine source B into a fluidized bed reactor filled with a catalyst C for reaction, the catalyst C is prepared by a solid phase catalyst A, a liquid phase catalyst B and a filler, and the solid phase catalyst A and the liquid phase catalyst B are uniformly attached to the filler. According to the alkylaminosilane and the preparation method thereof, the silane A and the organic amine source B in the fluidized bed reactor are in gas state, the unreacted silane A and the unreacted organic amine source B can participate in the reaction again after being cooled and collected at low temperature, so that the material utilization rate is improved, the resource waste is reduced, the catalyst C is prepared by the solid phase catalyst A, the liquid phase catalyst B and the filler, the reaction of the silane A and the organic amine source B can be efficiently catalyzed, the alkylaminosilane is synthesized by a one-step method, the preparation process is simple, the reaction yield is high, and the method is suitable for mass production of the alkylaminosilane.
Description
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to an alkylaminosilane and a preparation method thereof.
Background
High purity aminosilanes are a very important class of silicon-based precursor materials. Such materials are widely used in the manufacture of semiconductor materials, including chemical vapor deposition (MOCVD) and Atomic Layer Deposition (ALD) techniques, for the manufacture of silicon-based semiconductor thin film materials such as high purity silicon oxide thin films, silicon nitride and silicon carbide thin films, substrate materials, and the like. These high purity thin film materials are widely used in the leading edge fields of manufacturing semiconductor memory devices, light emitting diodes, solar thin film batteries, quantum dot illumination, and the like.
Traditional chlorosilane amination reactions for preparing aminosilanes, such as the patent of publication No. JPWO2016152226A1, disclose the preparation of aminosilanes by direct reaction of dialkylamine with chlorosilane, but this preparation method produces a large amount of byproduct hydrochloride in addition to the target product, requiring an additional liquid-solid separation step to filter out the hydrochloride byproduct, increasing process complexity and being unfavorable for mass production. In addition, the product of the preparation method easily contains high-content chloride ion impurities, the process for removing the chloride ion impurities is complex, and the cost of the product is increased.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention aims to provide an alkylaminosilane and a preparation method thereof.
In order to achieve the above purpose and achieve the above technical effects, the invention adopts the following technical scheme:
an alkylaminosilane is obtained by introducing silane A and an organic amine source B into a fluidized bed reactor filled with a catalyst C for reaction, wherein the catalyst C is prepared by a solid phase catalyst A, a liquid phase catalyst B and a filler, and the solid phase catalyst A and the liquid phase catalyst B are uniformly attached to the filler.
The invention also discloses a preparation method of the alkylaminosilane, which comprises the following steps:
introducing silane A and organic amine source B into a fluidized bed reactor filled with catalyst C, and reacting at 40-180 ℃ and 1-16 bar pressure to obtain the required alkylaminosilane.
Further, the molar ratio of silane a to organic amine source B is 1:0.9 to 2.2.
Further, the silane A is selected from any one of monosilane and disilane; the organic amine source B is selected from any one of ethylamine, n-propylamine, isopropylamine, n-butylamine and tert-butylamine.
Further, the catalyst C is prepared from a solid phase catalyst A, a liquid phase catalyst B and a filler, wherein the solid phase catalyst A and the liquid phase catalyst B are uniformly attached to the filler.
Further, the mole ratio of the solid phase catalyst A to the liquid phase catalyst B is 3-6: 1.
further, the solid phase catalyst A is ZnCl 2 、ZnBr 2 、ZnI 2 One or a combination of several of them.
Further, the liquid phase catalyst B is Zn (CH) 3 ) 2 、Zn(C 2 H 5 ) 2 、Mg(C 4 H 9 ) 2 One or a combination of several of them.
Further, the filler is selected from ceramic or metal fillers, and is in a shape of a sheet, a sphere or a rod.
Further, the filler is spherical stainless steel filler.
Compared with the prior art, the invention has the beneficial effects that:
the invention discloses an alkylaminosilane and a preparation method thereof, wherein the alkylaminosilane is obtained by introducing silane A and an organic amine source B into a fluidized bed reactor filled with a catalyst C for reaction, the silane A and the organic amine source B are both in a gaseous state in the fluidized bed reactor, unreacted silane A and organic amine source B can participate in the reaction again after being cooled and collected at a low temperature, the material utilization rate is improved, the resource waste is reduced, the catalyst C is prepared by a solid phase catalyst A, a liquid phase catalyst B and a filler, the reaction of the silane A and the organic amine source B can be efficiently catalyzed, the one-step synthesis of the alkylaminosilane is realized, the preparation process is simple, the reaction yield is high, the raw materials can be recycled, no extra liquid-solid separation step is needed to filter out hydrochloride byproducts, the problems existing in the prior art are solved, and the method is suitable for mass production of the alkylaminosilane.
Detailed Description
The present invention is described in detail below so that advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and unambiguous the scope of the present invention.
The following presents a simplified summary of one or more aspects in order to provide a basic understanding of such aspects. This summary is not an extensive overview of all contemplated aspects, and is intended to neither identify key or critical elements of all aspects nor delineate the scope of any or all aspects. Its sole purpose is to present some concepts of one or more aspects in a simplified form as a prelude to the more detailed description that is presented later.
In one aspect, the present invention discloses an alkylaminosilane obtained by reacting silane A and organoamine source B in a fluidized bed reactor containing catalyst C at a reaction temperature of 40 to 180 ℃, preferably 60 to 160 ℃, more preferably 80 to 130 ℃, at a reaction pressure of 1 to 16bar, preferably 2 to 10bar, more preferably 4 to 8bar.
On the other hand, the invention also discloses a preparation method of the alkylaminosilane, which comprises the following steps:
introducing silane A and organic amine source B into a fluidized bed reactor filled with catalyst C, and reacting in an inert gas (nitrogen or argon) atmosphere at 40-180 ℃ and under the pressure of 1-16 bar to obtain the required alkylaminosilane.
The molar ratio of silane a to organic amine source B was 1:0.9 to 2.2, preferably 1:1 to 2, more preferably 1:1.4 to 1.8.
The silane A is selected from any one of monosilane and disilane.
The organic amine source B is selected from any one of ethylamine, n-propylamine, isopropylamine, n-butylamine and tert-butylamine.
The catalyst C is prepared from a solid phase catalyst A, a liquid phase catalyst B and a filler, and comprises the following specific steps:
in an inert gas (nitrogen or argon) atmosphere, a solid phase catalyst A and a liquid phase catalyst B are mixed according to a molar ratio of 3-6: 1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to the filler.
The solid phase catalyst A is ZnCl 2 、ZnBr 2 、ZnI 2 One or a combination of several of them.
The liquid phase catalyst B is Zn (CH) 3 ) 2 、Zn(C 2 H 5 ) 2 、Mg(C 4 H 9 ) 2 One or a combination of several of them.
The filler is selected from ceramic or metal filler, preferably stainless steel filler, and has a plate-like, spherical or rod-like shape, preferably spherical shape.
Example 1
Under nitrogen atmosphere, the solid phase catalyst methyl ZnCl 2 With liquid phase catalyst B Mg (C) 4 H 9 ) 2 According to the mole ratio of 3:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min with a nitrogen carrier gas to bring in tert-butylamine with a molar ratio of tert-butylamine to monosilane of 1.8:1, controlling the reaction temperature to 115 ℃, controlling the reaction pressure to 5.5bar, cooling at low temperature after the reaction is finished, collecting the output, and calculating to obtain the required bis (tertiary butyl amino) silane, wherein the product yield is 85.7%.
Example 2
Under nitrogen atmosphere, the solid phase catalyst methyl ZnCl 2 With liquid phase catalyst B Mg (C) 4 H 9 ) 2 According to the mole ratio of 5:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min and introduction of isopropylamine with argon carrier gas at a molar ratio of isopropylamine to monosilane of 2:1, controlling the reaction temperature to 115 ℃, controlling the reaction pressure to 4bar, cooling at low temperature after the reaction is finished, collecting the output, and calculating to obtain the required diisopropylamine silane, wherein the product yield is 80.21%.
Example 3
In nitrogen atmosphere, the solid phase catalyst methyl ZnBr 2 With liquid phase catalyst B Mg (C) 4 H 9 ) 2 According to the mole ratio of 6:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of disilane at a rate of 2L/min with isopropylamine carried with argon carrier gas at a molar ratio of isopropylamine to disilane of 1.2:1, controlling the reaction temperature to 90 ℃ and the reaction pressure to 8bar, cooling at low temperature after the reaction is finished, and collecting the output, thus obtaining the required diisopropylamine disilane.
Example 4
Under nitrogen atmosphere, the solid phase catalyst methyl ZnI 2 With liquid phase catalyst B Mg (C) 4 H 9 ) 2 According to the mole ratio of 5:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min and introduction of diethylamine with a nitrogen carrier gas at a molar ratio of diethylamine to monosilane of 2:1, controlling the reaction temperature to be 95 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, collecting the output, and calculating to obtain the required bis (diethylamino) silane.
Example 5
Under nitrogen atmosphere, the solid phase catalyst methyl ZnI 2 With liquid phase catalyst B Zn (CH) 3 ) 2 According to the mole ratio of 5:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min with a nitrogen carrier gas to bring in tert-butylamine with a molar ratio of tert-butylamine to disilane of 2:1, controlling the reaction temperature to be 115 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, collecting the output, and calculating to obtain the required bis (tertiary butyl amino) disilane.
Example 6
Under nitrogen atmosphere, the solid phase catalyst methyl ZnCl 2 With liquid phase catalyst B Zn (CH) 3 ) 2 According to the mole ratio of 3:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel fillerObtaining a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min with a nitrogen carrier gas to bring in tert-butylamine with a molar ratio of tert-butylamine to disilane of 1.8:1, controlling the reaction temperature to be 115 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, collecting the output, and calculating to obtain the required bis (tertiary butyl amino) disilane.
Example 7
Under nitrogen atmosphere, the solid phase catalyst methyl ZnCl 2 With liquid phase catalyst B Zn (C) 2 H 5 ) 2 According to the mole ratio of 5:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min and introduction of diethylamine with a nitrogen carrier gas at a molar ratio of diethylamine to monosilane of 2:1, controlling the reaction temperature to be 95 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, collecting the output, and calculating to obtain the required diethylaminosilane.
Example 8
Under nitrogen atmosphere, the solid phase catalyst methyl ZnI 2 With liquid phase catalyst B Zn (C) 2 H 5 ) 2 According to the mole ratio of 5:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min with a nitrogen carrier gas to bring in tert-butylamine with a molar ratio of tert-butylamine to disilane of 2:1, controlling the reaction temperature to be 115 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, collecting the output, and calculating to obtain the required bis (tertiary butyl amino) disilane.
Example 9
In nitrogen atmosphere, the solid phase catalyst methyl ZnBr 2 With liquid phase catalyst B Zn (C) 2 H 5 ) 2 According to the mole ratio of 3:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min with isopropylamine carried with a nitrogen carrier gas at a molar ratio of isopropylamine to monosilane of 1.8:1, controlling the reaction temperature to be 125 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, and collecting the output, thus obtaining the required diisopropylamine silane.
Example 10
In nitrogen atmosphere, the solid phase catalyst methyl ZnBr 2 With liquid phase catalyst B Zn (CH) 3 ) 2 According to the mole ratio of 6:1, adding the catalyst mixture into a planetary grinder for grinding and dispersing, and uniformly attaching the dispersed catalyst mixture to spherical stainless steel filler to obtain a catalyst C;
1000g of catalyst C was charged into a fluidized bed reactor under nitrogen atmosphere, followed by introduction of monosilane at a rate of 2L/min and introduction of isopropylamine with a nitrogen carrier gas at a molar ratio of isopropylamine to disilane of 2:1, controlling the reaction temperature to be 125 ℃, controlling the reaction pressure to be 5.5bar, cooling at a low temperature after the reaction is finished, and collecting the output, thus obtaining the required diisopropylamine disilane.
Comparative example 1
The comparative example differs from example 1 in that the liquid phase catalyst ethylmg (C 4 H 9 ) 2 As a result of the other operations in example 1, the yield of bis (t-butylamino) silane obtained in this comparative example was 42.6% which is far lower than that in example 1.
Comparative example 2
The difference between this comparative example and example 1 is that this comparative example does not add the solid phase catalyst methyl ZnCl 2 As a result of the other operations in example 1, the yield of bis (t-butylamino) silane obtained in this comparative example was 43.5%, which is far lower than that in example 1.
Comparative example 3
The difference between this comparative example and example 1 is that this comparative example does not use spherical stainless steel filler, and the rest is the same as example 1, and as a result, the yield of bis (t-butylamino) silane obtained in this comparative example is 40.6% which is far lower than that of example 1.
Examples 1-10 and comparative examples 1-3 show that the required high-yield alkylaminosilane can be prepared only by adopting the solid-phase catalyst A, the liquid-phase catalyst B and the filler disclosed by the invention to be compounded and then combining the silane A and the organic amine source B, no additional liquid-solid separation step is needed to filter out hydrochloride byproducts, the problems in the prior art are solved, and the industrialized mass production of the preparation route has obvious advantages.
Parts or structures of the present invention, which are not specifically described, may be existing technologies or existing products, and are not described herein.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.
Claims (10)
1. The alkylaminosilane is characterized in that the alkylaminosilane is obtained by introducing silane A and an organic amine source B into a fluidized bed reactor filled with a catalyst C for reaction, wherein the catalyst C is prepared by a solid-phase catalyst A, a liquid-phase catalyst B and a filler, and the solid-phase catalyst A and the liquid-phase catalyst B are uniformly attached to the filler.
2. A method for preparing an alkylaminosilane, comprising the steps of:
introducing silane A and organic amine source B into a fluidized bed reactor filled with catalyst C, and reacting at 40-180 ℃ and 1-16 bar pressure to obtain the required alkylaminosilane.
3. The process for preparing an alkylaminosilane according to claim 2, wherein the molar ratio of silane a to organoamine source B is 1:0.9 to 2.2.
4. The method for preparing alkylaminosilane according to claim 2, wherein silane a is selected from any one of monosilane and disilane; the organic amine source B is selected from any one of ethylamine, n-propylamine, isopropylamine, n-butylamine and tert-butylamine.
5. The method for preparing alkylaminosilane according to claim 2, wherein the catalyst C is prepared by a solid phase catalyst a, a liquid phase catalyst b and a filler, and the solid phase catalyst a and the liquid phase catalyst b are uniformly adhered to the filler.
6. The method for preparing an alkylamino silane according to claim 5, wherein the molar ratio of the solid phase catalyst a to the liquid phase catalyst b is 3-6: 1.
7. the method for preparing an alkylamino silane according to claim 5, wherein the solid phase catalyst A is ZnCl 2 、ZnBr 2 、ZnI 2 One or a combination of several of them.
8. The method for preparing an alkylaminosilane according to claim 5, wherein the liquid phase catalyst B is Zn (CH) 3 ) 2 、Zn(C 2 H 5 ) 2 、Mg(C 4 H 9 ) 2 One or a combination of several of them.
9. The process for preparing an alkylaminosilane according to claim 5, wherein the filler is selected from ceramic and metal fillers and is in the form of a sheet, sphere or rod.
10. The method for preparing an alkylaminosilane according to claim 9, wherein said filler is spherical stainless steel filler.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311846582.0A CN117820350A (en) | 2023-12-29 | 2023-12-29 | Alkyl aminosilane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311846582.0A CN117820350A (en) | 2023-12-29 | 2023-12-29 | Alkyl aminosilane and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117820350A true CN117820350A (en) | 2024-04-05 |
Family
ID=90520296
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311846582.0A Withdrawn CN117820350A (en) | 2023-12-29 | 2023-12-29 | Alkyl aminosilane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117820350A (en) |
-
2023
- 2023-12-29 CN CN202311846582.0A patent/CN117820350A/en not_active Withdrawn
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9487405B2 (en) | Method for manufacturing SiC powders with high purity | |
| US7238596B2 (en) | Method for preparing Ge1-x-ySnxEy (E=P, As, Sb) semiconductors and related Si-Ge-Sn-E and Si-Ge-E analogs | |
| USRE45839E1 (en) | Pentakis(dimethylamino) disilane precursor comprising compound and method for the preparation thereof | |
| JP6165160B2 (en) | Method for preparing trialkylgallium compound | |
| US4318942A (en) | Process for producing polycrystalline silicon | |
| JPS6228083B2 (en) | ||
| US10030038B2 (en) | Monoaminosilane compounds | |
| JP2017524728A (en) | Diaminosilane compound | |
| JP5972999B2 (en) | Preparation of trialkylgallium compounds or trialkylindium compounds | |
| CN117820350A (en) | Alkyl aminosilane and preparation method thereof | |
| WO2014093419A1 (en) | Production of tri-alkyl compounds of group 3a metals | |
| US7030260B2 (en) | Preparation of mixed-halogen halo-silanes | |
| WO2017036899A1 (en) | Process for the preparation of trimethyl metal compounds | |
| KR20170025030A (en) | Preparation of alkylaminosilane by reaction of chlorosilane with alkylamine mixture | |
| WO2014078263A1 (en) | Methods of producing trimethylgallium | |
| CN115417413B (en) | Preparation method and application of neopentasilane intermediate | |
| US11827522B2 (en) | Partially hydrogenated chlorosilanes and methods for preparing same by selective hydrogenation | |
| TWI682052B (en) | System for producing crystalline silicon and method for producing crystalline silicon | |
| KR20170005305A (en) | Process for the preparation of trisalkylaminosilane | |
| JP2001019419A (en) | Production of monosilane and tetraalkoxysilane | |
| KR20250014292A (en) | Silicon precursor compounds and method for manufacturing the same, and method of forming silicon-containing films | |
| CN117383567A (en) | Method for preparing diiodosilane by iodination of silane | |
| CN115536687A (en) | Process for preparing trialkylaminosilanes and use thereof | |
| CN118320750A (en) | Trimethyl silicon-based dialkylamine synthesis device system and preparation method | |
| FR2989074A1 (en) | Preparing mixture of silane and germane compounds, involves reacting mixture of alloy containing silicon alloy in the form of powder and germanium alloy in the form of powder with hydrochloric acid that is pre-dissolved in aqueous solution |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20240405 |