CN117263970A - Method for synthesizing electronic grade alkoxy silane by direct method - Google Patents
Method for synthesizing electronic grade alkoxy silane by direct method Download PDFInfo
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- CN117263970A CN117263970A CN202311232000.XA CN202311232000A CN117263970A CN 117263970 A CN117263970 A CN 117263970A CN 202311232000 A CN202311232000 A CN 202311232000A CN 117263970 A CN117263970 A CN 117263970A
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- copper
- alkoxy silane
- electronic grade
- methanol
- silicon powder
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- 238000000034 method Methods 0.000 title claims abstract description 54
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 47
- -1 alkoxy silane Chemical compound 0.000 title claims abstract description 46
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 208
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 60
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 claims abstract description 58
- 239000003054 catalyst Substances 0.000 claims abstract description 56
- 239000012043 crude product Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 36
- 238000003756 stirring Methods 0.000 claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000005749 Copper compound Substances 0.000 claims abstract description 18
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007789 gas Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000004064 recycling Methods 0.000 claims abstract description 10
- 230000000536 complexating effect Effects 0.000 claims abstract description 9
- 238000009833 condensation Methods 0.000 claims abstract description 8
- 230000005494 condensation Effects 0.000 claims abstract description 8
- 150000001880 copper compounds Chemical class 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims description 50
- 239000000375 suspending agent Substances 0.000 claims description 39
- 239000007788 liquid Substances 0.000 claims description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 28
- 239000001257 hydrogen Substances 0.000 claims description 28
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 239000011261 inert gas Substances 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 20
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 claims description 16
- 230000015572 biosynthetic process Effects 0.000 claims description 16
- 238000012856 packing Methods 0.000 claims description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 14
- 239000000706 filtrate Substances 0.000 claims description 14
- 230000007062 hydrolysis Effects 0.000 claims description 14
- 238000006460 hydrolysis reaction Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 13
- 239000005751 Copper oxide Substances 0.000 claims description 13
- 150000004996 alkyl benzenes Chemical class 0.000 claims description 13
- 229910000431 copper oxide Inorganic materials 0.000 claims description 13
- 238000010668 complexation reaction Methods 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 10
- 239000006227 byproduct Substances 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 9
- 239000011343 solid material Substances 0.000 claims description 8
- 239000006200 vaporizer Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 230000007246 mechanism Effects 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- YOPUATYREUZXIO-UHFFFAOYSA-N copper;methanol Chemical compound [Cu].OC YOPUATYREUZXIO-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 229940116318 copper carbonate Drugs 0.000 claims description 4
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- 229920002545 silicone oil Polymers 0.000 claims description 4
- 238000005273 aeration Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 3
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 3
- 229940112669 cuprous oxide Drugs 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 2
- 229910000009 copper(II) carbonate Inorganic materials 0.000 claims 1
- 229940076286 cupric acetate Drugs 0.000 claims 1
- 235000019854 cupric carbonate Nutrition 0.000 claims 1
- 239000011646 cupric carbonate Substances 0.000 claims 1
- 238000005507 spraying Methods 0.000 claims 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 abstract description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052802 copper Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 16
- 239000007795 chemical reaction product Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000005750 Copper hydroxide Substances 0.000 description 7
- 229910001956 copper hydroxide Inorganic materials 0.000 description 7
- 230000008016 vaporization Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 3
- 239000005052 trichlorosilane Substances 0.000 description 3
- 229910003910 SiCl4 Inorganic materials 0.000 description 2
- 238000006136 alcoholysis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 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
- C07F7/04—Esters of silicic acids
-
- 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 a method for synthesizing electronic grade alkoxy silane by a direct method, which belongs to the technical field of organic fine chemicals and comprises the following steps: s1: preparing a material; s2: metering high-purity silicon powder, a copper-silicon catalyst and a solvent, sequentially placing the high-purity silicon powder, the copper-silicon catalyst and the solvent into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, and performing two-stage condensation to form a crude product; s3: complexing; s4: separating at normal pressure to form electronic grade alkoxy silane; s5: tail gas recycling treatment; s6: recycling and treating materials; the invention prepares the chlorine-free copper compound into the polyvalent copper catalyst, the catalyst can be stored and placed for a long time in an oxygen-free environment, when in use, the catalyst can be directly added into a synthesis reaction kettle to catalyze silanol to react directly, the silicon powder has high utilization rate and good selectivity, the metal ions of alkoxy silane and chloride ions are produced, and the purity can reach the electronic grade.
Description
Technical Field
The invention belongs to the technical field of organic fine chemicals, and particularly relates to a method for synthesizing electronic grade alkoxy silane by a direct method.
Background
Alkoxysilanes are an important silane intermediate in silicon-functional organosilanes and can be used as chemical base materials.
The conventional alkoxysilane production process generally adopts silicon to react with hydrogen chloride to generate trichlorosilane, and then adopts methanol (or ethanol) alcoholysis of the trichlorosilane to prepare the alkoxysilane, wherein the reaction formula is as follows:
the first step: si+HCl- & gtHSiCl3+SiCl4+H2 ≡plus other by-products of the chlorosilicane hospital;
and a second step of: hsicl3+3roh→hsi (OR) 3+3hcl +.r=me, et, etc
SiCl4+4ROH→Si(OR)4+4HCl↑；
The two-step method for producing the alkoxy silane has long process flow and large material loss, and simultaneously, the byproduct HCl can cause equipment corrosion and environmental pollution.
Based on the improvement of the method, the method for synthesizing the alkoxy silane by adopting silanol direct reaction is provided, compared with the method for preparing the alkoxy silane by using the alcoholysis reaction of trichlorosilane, the method has the advantages of simple process and one-step completion of the synthesis of the alkoxy silane, and the reaction formula is as follows:
si, +CH3OH→HSi (OR) 3+Si (OR) 4+H2 +.h+other by-products
Alkyl groups such as r=ch3, CH2CH3, etc.;
from the above equation, the advantage of direct synthesis is that the production process to obtain the target product is short and no corrosive gas HCl is generated.
Although the prior direct synthesis method synthesizes alkoxy silane such as trimethoxy silane, the selectivity of the trialkoxy silane is not ideal, the selectivity of the trialkoxy silane can reach about 80 percent only in a period of time in the whole reaction process, which indicates that the catalyst or the catalytic silicon/alcohol has poor stability in direct reaction; in addition, the silicon powder has not high utilization rate, the methanol content in the reaction product is high, azeotrope formed by the silicon powder and trimethoxysilane is not easy to separate, and pure trimethoxysilane with high yield is difficult to obtain.
In view of this, a direct method for synthesizing electronic grade alkoxysilane is designed to solve the above problems.
Disclosure of Invention
To solve the problems set forth in the background art. The invention provides a method for synthesizing electronic grade alkoxy silane by a direct method, which has the characteristics of high utilization rate, good selectivity and high purity reaching electronic grade.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, a copper silicon catalyst, a solvent and vaporized methanol required by synthesis;
s2: metering high-purity silicon powder, a copper-silicon catalyst and a solvent, sequentially placing the high-purity silicon powder, the copper-silicon catalyst and the solvent into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation through a vapor/liquid separation cyclone separator, enabling a suspension agent and solid materials carried by primary recovered gas to return to the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to form electronic grade alkoxy silane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
Further, in the step S1, the content of the high-purity silicon powder is more than 99.99 percent, the metal impurity is less than 200ppm, and the particle size is 80-800 meshes.
Further, in the step S1, the preparation method of the copper-silicon catalyst is as follows: placing a copper compound and 200-400 mesh high-purity silicon powder into a mixer for mixing, uniformly distributing the copper compound on the surface of the high-purity silicon powder, introducing inert gas into the mixer for removing oxygen, heating the mixer to 300-700 ℃, introducing hydrogen and carbon monoxide into the mixer for reduction treatment to form a multivalent silicon-copper compound, namely a copper-silicon catalyst, introducing inert gas into the mixer for removing hydrogen and carbon monoxide, cooling the mixer to 50 ℃, and metering and placing the mixture into a reactor under the protection of the inert gas.
Further, in the step S1, the copper compound is one or more of copper oxide, copper hydroxide, copper carbonate, copper acetate and methoxy copper.
Further, in the step S1, the solvent is one or more of alkylbenzene, high-temperature heat-conducting oil and silicone oil.
Further, in the step S1, the preparation method of the vaporized methanol is as follows: placing methanol into an adsorption tower, treating the methanol by the adsorption tower, passing the methanol through a methanol vaporizer in a liquid state, entering a distributor through a pipeline, and entering a reactor through the distributor.
Further, in the step S1, the content of methanol is more than 99.99%, the metal ion is less than 10ppm, the chloride ion is less than 10ppm, and the water content is less than 50ppm.
Further, in the step S2, the addition amount of the copper-silicon catalyst is 2% -5% of the addition amount of the high-purity silicon powder, and the addition weight ratio of the solvent to the high-purity silicon powder is 1:1-1:5.
Further, in the step S2, the aeration rate of the vaporized methanol is initially at a rate of 40ml/h, and during the reaction, the alcohol inlet rate is adjusted by analyzing the alcohol content in the effluent product, wherein the alcohol content in the effluent product is controlled to be 2wt%.
In step S5, the spray absorption liquid is alcohol, suspending agent, crude product, and high boiling residue after product rectification.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention prepares the chlorine-free copper compound into the polyvalent copper catalyst, the catalyst can be stored and placed for a long time in an oxygen-free environment, when in use, the catalyst can be directly added into a synthesis reaction kettle to catalyze silanol to react directly, the silicon powder has high utilization rate and good selectivity, the metal ions of alkoxy silane and chloride ions are produced, and the purity can reach the electronic grade.
2. According to the invention, methanol passes through the adsorption tower, the alcohol is changed into steam through the alcohol evaporator and then is introduced into the reaction kettle, so that metal ions and chloride ions carried in raw materials are reduced through the operation, and the substances in the product can be reduced.
3. The invention adopts an intermittent process, namely, materials required by production are sequentially put into a reaction kettle according to the amount, after the reaction is normally carried out, the consumption of silicon powder is estimated through alcohol inlet metering, and when the silicon powder is consumed for about 90wt% in the reaction, the selectivity and activity of the catalyst are obviously reduced and stopped, the silicon powder utilization rate in the intermittent operation process can reach more than 95%.
4. The product of the invention is that the air flow firstly passes through the air flow/liquid separation cyclone separator to recycle the suspending agent and solid materials carried by the air flow into the reaction kettle, then the crude product is obtained by collection, and the crude product is purified by the rectifying tower after complexing treatment of the packing tower, thereby being beneficial to the purification of the product and reducing the impurity carried by the reaction.
5. The invention adopts a method of recycling and repeatedly using the solvent, reduces the consumption of the solvent and reduces the production cost.
Drawings
FIG. 1 is a flow chart of a method for synthesizing electronic grade alkoxy silane by a direct method.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
Referring to fig. 1, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, copper-silicon catalyst A, alkylbenzene and vaporized methanol required by synthesis;
s2: sequentially placing 350g of high-purity silicon powder, 7g of copper-silicon catalyst A and 350ml of alkylbenzene into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation by a vapor/liquid separation cyclone separator, returning a suspending agent and solid materials carried by primary recovered gas into the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to obtain the crude product: 850g of trimethoxysilane and 480g of tetraalkoxysilane with the content of 99.99% respectively to form electronic grade alkoxysilane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
The preparation method of the copper-silicon catalyst A comprises the following steps: 100 parts of copper oxide, 50 parts of cuprous hydroxide and 50 parts of 200-400 mesh high-purity silicon powder are placed into a mixer for mixing according to parts by mass, so that the copper oxide and the cuprous hydroxide are uniformly distributed on the surface of the high-purity silicon powder, inert gas is introduced into the mixer for removing oxygen, the mixer is heated to 300-700 ℃, hydrogen and carbon monoxide are introduced into the mixer for reduction treatment for 20 hours, a multivalent silicon-copper compound, which is a copper-silicon catalyst, inert gas is introduced into the mixer for removing hydrogen and carbon monoxide, the mixer is cooled to 50 ℃, and the mixture is metered into a reactor under the protection of the inert gas.
Example 2
Referring to fig. 1, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, a copper silicon catalyst B, alkylbenzene and vaporized methanol required by synthesis;
s2: sequentially placing 350g of high-purity silicon powder, 7g of copper-silicon catalyst B and 500ml of alkylbenzene into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation by a vapor/liquid separation cyclone separator, returning a suspending agent and solid materials carried by primary recovered gas into the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to obtain the crude product: 650g of trimethoxysilane and 700g of tetraalkoxysilane, wherein the content of the trimethoxysilane and the tetraalkoxysilane is 99.99% respectively, so as to form electronic grade alkoxysilane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
The preparation method of the copper-silicon catalyst B comprises the following steps: 50 parts of copper oxide, 50 parts of cuprous hydroxide, 50 parts of copper acetate and 150 parts of 200-400 mesh high-purity silicon powder are placed into a mixer for mixing according to parts by mass, so that the copper oxide, the cuprous hydroxide and the copper acetate are uniformly distributed on the surface of the high-purity silicon powder, inert gas is introduced into the mixer for removing oxygen, the mixer is heated to 300-700 ℃, hydrogen and carbon monoxide are introduced into the mixer for reduction treatment for 20 hours, a multivalent silicon-copper compound is formed, the multivalent silicon-copper compound is a copper-silicon catalyst, the inert gas is introduced into the mixer for removing the hydrogen and the carbon monoxide, the mixer is cooled to 50 ℃, and the material is placed into a reactor in a metering way through the protection of the inert gas.
Example 3
Referring to fig. 1, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, a copper-silicon catalyst C, high-temperature heat conduction oil and vaporized methanol required by synthesis;
s2: sequentially placing 350g of high-purity silicon powder, 7g of copper-silicon catalyst C and 500ml of high-temperature heat-conducting oil into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation through a vapor/liquid separation cyclone separator, returning a suspending agent and solid materials carried by primary recovered gas into the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to obtain the crude product: 350g of trimethoxysilane and 400g of tetraalkoxysilane, wherein the content of the trimethoxysilane and the tetraalkoxysilane is 99.99% respectively, so as to form electronic grade alkoxysilane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
The preparation method of the copper-silicon catalyst C comprises the following steps: placing 70 parts of copper oxide, 30 parts of cuprous oxide, 50 parts of cuprous hydroxide and 150 parts of 200-400 mesh high-purity silicon powder into a mixer for mixing according to parts by mass, uniformly distributing the copper oxide, the cuprous oxide and the cuprous hydroxide on the surface of the high-purity silicon powder, introducing inert gas into the mixer for removing oxygen, heating the mixer to 300-700 ℃, introducing hydrogen and carbon monoxide into the mixer for reduction treatment for 20h to form a multivalent silicon-copper compound, namely a copper-silicon catalyst, introducing the inert gas into the mixer for removing the hydrogen and the carbon monoxide, cooling the mixer to 50 ℃, and metering and placing the mixture into a reactor under the protection of the inert gas.
Example 4
Referring to fig. 1, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, a copper silicon catalyst D, silicone oil and vaporized methanol required by synthesis;
s2: sequentially placing 350g of high-purity silicon powder, 7g of copper silicon catalyst D and 500ml of silicone oil into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation by a vapor/liquid separation cyclone separator, returning a suspending agent and solid materials carried by primary recovered gas into the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to obtain the crude product: 650g of trimethoxysilane and 500g of tetraalkoxysilane, the content of which is 99.99% respectively, to form electronic grade alkoxysilane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
The preparation method of the copper-silicon catalyst D comprises the following steps: according to the mass parts, 70 parts of copper hydroxide, 30 parts of copper carbonate, 20 parts of copper acetate, 30 parts of methoxy copper and 150 parts of 200-400 mesh high-purity silicon powder are placed into a mixer to be mixed, so that the copper hydroxide, the copper carbonate, the copper acetate and the methoxy copper are uniformly distributed on the surface of the high-purity silicon powder, inert gas is introduced into the mixer to remove oxygen, the mixer is heated to 300-700 ℃, hydrogen and carbon monoxide are introduced into the mixer to carry out reduction treatment for 20 hours, a multivalent silicon-copper compound is formed, the multivalent silicon-copper compound is a copper-silicon catalyst, the inert gas is introduced into the mixer to remove hydrogen and carbon monoxide, the mixer is cooled to 50 ℃, and the material is metered and placed into a reactor through the protection of the inert gas.
Example 5
Referring to fig. 1, the present invention provides the following technical solutions: a method for synthesizing electronic grade alkoxy silane by a direct method comprises the following steps:
s1: preparing high-purity silicon powder, a copper silicon catalyst E, alkylbenzene and vaporized methanol required by synthesis;
s2: sequentially placing 350g of high-purity silicon powder, 7g of copper-silicon catalyst E and 1750ml of alkylbenzene into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation by a vapor/liquid separation cyclone separator, returning a suspending agent and solid materials carried by primary recovered gas into the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to obtain the crude product: 1050g of trimethoxysilane and 300g of tetraalkoxysilane with the content of 99.99 percent respectively to form electronic grade alkoxysilane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
The preparation method of the copper-silicon catalyst E comprises the following steps: according to the mass parts, 30 parts of copper oxide, 70 parts of copper hydroxide, 20 parts of copper acetate, 30 parts of methoxy copper and 150 parts of 200-400 mesh high-purity silicon powder are placed into a mixer to be mixed, so that the copper oxide, the copper hydroxide, the copper acetate and the methoxy copper are uniformly distributed on the surface of the high-purity silicon powder, inert gas is introduced into the mixer to remove oxygen, the mixer is heated to 300-700 ℃, hydrogen and carbon monoxide are introduced into the mixer to carry out reduction treatment for 20 hours, a multivalent silicon-copper compound is formed, the multivalent silicon-copper compound is a copper-silicon catalyst, the inert gas is introduced into the mixer to remove hydrogen and carbon monoxide, the mixer is cooled to 50 ℃, and the material is metered and placed into a reactor through the protection of the inert gas.
In the above embodiment:
the content of the high-purity silicon powder is more than 99.99 percent, the metal impurity is less than 200ppm, and the grain diameter is 80-800 meshes;
the preparation method of the vaporized methanol comprises the following steps: placing methanol into an adsorption tower, treating the methanol by the adsorption tower, passing the methanol through a methanol vaporizer in a liquid state, entering a distributor through a pipeline, and entering a reactor through the distributor;
the content of methanol is more than 99.99 percent, the metal ion is less than 10ppm, the chloride ion is less than 10ppm, and the water content is less than 50ppm;
the aeration rate of the vaporized methanol is initially 40ml/h, and during the reaction, the alcohol inlet rate is adjusted by analyzing the alcohol content in the effluent product, wherein the alcohol content in the effluent product is controlled to be 2wt%;
the spray absorption liquid is alcohol, suspending agent, crude product and high-boiling residue after rectification.
Production example 1
Adding 1500L of alkylbenzene into a 3000L special reaction kettle, adding 1000KG of high-purity silicon powder and 20KG of copper-silicon catalyst A under the condition of stirring, heating the reaction kettle, when the temperature is raised to 180-300 ℃, starting a methanol vaporizer to introduce methanol, controlling the content of methanol in the vaporized reaction product by adjusting the speed of vaporizing the methanol, controlling the content of methanol in the vaporized reaction product to be lower than 2wt%, controlling the alcohol introducing speed to be between 40 and 60L per hour, stopping the reaction when the alcohol content is raised to 40%, then co-introducing 3.5T of methanol, and obtaining about 4.5T of crude product after the reaction time is about 60 hours in the whole process, and after the post-complexation treatment, obtaining about 2.76T of trimethoxysilane, 99.99 percent of chloride ion, 50ppb of metal ion, 1.56T of tetraalkoxysilane, 99.99 percent of chloride ion and 90ppb of metal ion after the separation in a continuous rectifying tower.
Production example 2
Adding 1500L of alkylbenzene into a 3000L special reaction kettle, adding 1000KG of high-purity silicon powder and 20KG of copper-silicon catalyst B under the condition of stirring, heating the reaction kettle, when the temperature is raised to 180-300 ℃, starting a methanol vaporizer to introduce methanol, controlling the content of methanol in the vaporized reaction product by adjusting the speed of vaporizing the methanol, controlling the content of methanol in the vaporized reaction product to be lower than 2wt%, controlling the alcohol introducing speed to be between 40 and 60L per hour, stopping the reaction when the alcohol content is raised to 40%, then co-introducing 3.5T of methanol, and separating the mixture by a continuous rectifying tower for about 60 hours to obtain crude product of about 4.3T, wherein after the post-complexation treatment, the trimethoxysilane is obtained after separation by the continuous rectifying tower, the content of about 3.21T, the content of chloride ion of 99.99 ppb, the content of metal ion of 70ppb, the tetraalkoxysilane of 0.92T, the content of the tetraethoxysilane of 99.99%, the content of chlorine ion of 8ppb and the content of the metal ion of 90ppb.
Production example 3
Adding 1500L of alkylbenzene into a 3000L special reaction kettle, adding 1000KG of high-purity silicon powder and 20KG of copper-silicon catalyst C under the condition of stirring, heating the reaction kettle, when the temperature is raised to 180-300 ℃, starting a methanol vaporizer to introduce methanol, controlling the content of methanol in the vaporized reaction product by adjusting the speed of vaporizing the methanol, controlling the content of methanol in the vaporized reaction product to be lower than 2wt%, controlling the alcohol introducing speed to be between 40 and 60L per hour, stopping the reaction when the alcohol content is raised to 40%, then co-introducing 3.5T of methanol, and separating the mixture by a continuous rectifying tower for about 60 hours to obtain crude product of about 4.5T, wherein after the post-complexation treatment, the trimethoxysilane is obtained after separation by the continuous rectifying tower, the content of about 3.5T, the content of chloride ion of 99.99 ppb, the content of metal ion of 30ppb, the tetraalkoxysilane of 0.80T, the content of the chloride ion of 99.99 ppb, and the content of the metal ion of 50ppb.
Production example 4
Adding 1500L of alkylbenzene into a 3000L special reaction kettle, adding 1000KG of high-purity silicon powder and 20KG of copper-silicon catalyst D under the condition of stirring, heating the reaction kettle, when the temperature is raised to 180-300 ℃, starting a methanol vaporizer to introduce methanol, controlling the content of methanol in the vaporized reaction product by adjusting the speed of vaporizing the methanol, controlling the content of methanol in the vaporized reaction product to be lower than 2wt%, controlling the alcohol introducing speed to be between 40 and 60L per hour, stopping the reaction when the alcohol content is raised to 40%, then co-introducing 3.5T of methanol, and obtaining crude product of about 4.6T after the reaction time is about 60 hours, and after the post-complexation treatment, obtaining trimethoxysilane of about 3.25T, the content of 99.99%, the content of chloride ion of 4ppb, the content of metal ion of 50ppb, the content of tetraalkoxysilane of 0.97T, the content of 99.99%, the content of chloride ion of 7ppb and the content of metal ion of 60ppb after the separation by a continuous rectifying tower.
Production example 5
Adding 1500L of alkylbenzene into a 3000L special reaction kettle, adding 1000KG of high-purity silicon powder and 20KG of copper-silicon catalyst E under the condition of stirring, heating the reaction kettle, when the temperature is raised to 180-300 ℃, starting a methanol vaporizer to introduce methanol, controlling the content of methanol in the vaporized reaction product by adjusting the speed of vaporizing the methanol, controlling the content of methanol in the vaporized reaction product to be lower than 2wt%, controlling the alcohol introducing speed to be between 40 and 60L per hour, stopping the reaction when the alcohol content is raised to 40%, then co-introducing 3.5T of methanol, and separating the mixture by a continuous rectifying tower for about 60 hours to obtain crude product of about 4.4T, wherein after the post-complexation treatment, trimethoxysilane is obtained after separation by the continuous rectifying tower, the content of about 3.21T, the content of chlorine ion is 99.99%, the content of chlorine ion is 5ppb, the content of the tetraalkoxysilane is 1.25T, the content of the chlorine ion is 6ppb, and the content of the metal ion is 50ppb.
TABLE 1
From the experimental data in the above table, it is known that electronic grade alkoxysilane is synthesized directly by the copper silicon catalyst C made of 70 parts of copper oxide, 30 parts of copper oxide, 50 parts of copper hydroxide and 150 parts of 200-400 mesh high purity silicon powder, the trimethoxysilane output is highest, electronic grade alkoxysilane is synthesized directly by the copper silicon catalyst a made of 100 parts of copper oxide, 50 parts of copper hydroxide and 50 parts of 200-400 mesh high purity silicon powder, the tetraalkoxysilane output is highest, and the purity of alkoxysilane metal ions and chloride ions produced by the direct synthesis method of the present invention can reach electronic grade.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The method for synthesizing the electronic grade alkoxy silane by the direct method is characterized by comprising the following steps of:
s1: preparing high-purity silicon powder, a copper silicon catalyst, a solvent and vaporized methanol required by synthesis;
s2: metering high-purity silicon powder, a copper-silicon catalyst and a solvent, sequentially placing the high-purity silicon powder, the copper-silicon catalyst and the solvent into a reactor, introducing nitrogen, stirring, heating to 180-300 ℃, preserving heat for 1h, introducing vaporized methanol, reacting for 40h, performing two-stage condensation through a vapor/liquid separation cyclone separator, enabling a suspension agent and solid materials carried by primary recovered gas to return to the reactor, and collecting secondary liquid into a receiving tank to form a crude product;
s3: placing the crude product into a packed tower for complexation treatment;
s4: placing the crude product subjected to the complexing treatment into a rectifying tower for normal pressure separation treatment to form electronic grade alkoxy silane;
s5: the reaction byproduct hydrogen flow entrains the reaction material and enters a packing tower, the absorption liquid is sprayed through the top end of the packing tower to absorb the low boiling point material in the tail gas, the absorbed material enters a rectifying tower to be separated, and electronic grade alkoxy silane is formed, and the hydrogen is treated and recycled through a recycling mechanism;
s6: after the reaction, solid residues comprising high-purity silicon powder and copper-silicon catalyst and suspending agent are filtered by a first-stage filter, filtrate enters a suspending agent treatment kettle, water and auxiliary agents are added, stirring is carried out until the solid residues are completely hydrolyzed, hydrolysis liquid is filtered by a second-stage filter to remove hydrolysis materials, filtrate enters a centrifuge, suspending agent is recovered, and the suspending agent can be used for electronic-grade alkoxy silane and synthesis after being distilled and dried.
2. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S1, the content of the high-purity silicon powder is more than 99.99 percent, the metal impurity is less than 200ppm, and the particle size is 80-800 meshes.
3. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S1, the preparation method of the copper-silicon catalyst is as follows: placing a copper compound and 200-400 mesh high-purity silicon powder into a mixer for mixing, uniformly distributing the copper compound on the surface of the high-purity silicon powder, introducing inert gas into the mixer for removing oxygen, heating the mixer to 300-700 ℃, introducing hydrogen and carbon monoxide into the mixer for reduction treatment to form a multivalent silicon-copper compound, namely a copper-silicon catalyst, introducing inert gas into the mixer for removing hydrogen and carbon monoxide, cooling the mixer to 50 ℃, and metering and placing the mixture into a reactor under the protection of the inert gas.
4. A method for synthesizing electronic grade alkoxysilane by direct process according to claim 3, wherein: in the step S1, the copper compound is one or more of copper oxide, cuprous oxide, cupric hydroxide, cuprous hydroxide, cupric carbonate, cupric acetate and methoxy copper.
5. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S1, the solvent is one or more of alkylbenzene, high-temperature heat-conducting oil and silicone oil.
6. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S1, the preparation method of the vaporized methanol comprises the following steps: placing methanol into an adsorption tower, treating the methanol by the adsorption tower, passing the methanol through a methanol vaporizer in a liquid state, entering a distributor through a pipeline, and entering a reactor through the distributor.
7. The method for synthesizing electronic grade alkoxysilane according to claim 6, wherein: in the step S1, the content of methanol is more than 99.99 percent, the metal ion is less than 10ppm, the chloride ion is less than 10ppm, and the water content is less than 50ppm.
8. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S2, the addition amount of the copper-silicon catalyst is 2% -5% of the addition amount of the high-purity silicon powder, and the addition weight ratio of the solvent to the high-purity silicon powder is 1:1-1:5.
9. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S2, the aeration rate of the vaporized methanol is initially 40ml/h, and the alcohol inlet rate is adjusted by analyzing the alcohol content in the effluent product during the reaction, wherein the alcohol content in the effluent product is controlled to be 2wt%.
10. The method for synthesizing electronic grade alkoxy silane according to claim 1, wherein the method comprises the following steps: in the step S5, the spraying absorption liquid is alcohol, suspending agent, crude product and high-boiling residue after rectification.
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