CN116284096B - Synthesis method of tri (tert-butoxy) silanol with ultralow chloride ion content - Google Patents
Synthesis method of tri (tert-butoxy) silanol with ultralow chloride ion content Download PDFInfo
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- CN116284096B CN116284096B CN202310567060.0A CN202310567060A CN116284096B CN 116284096 B CN116284096 B CN 116284096B CN 202310567060 A CN202310567060 A CN 202310567060A CN 116284096 B CN116284096 B CN 116284096B
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- HLDBBQREZCVBMA-UHFFFAOYSA-N hydroxy-tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[Si](O)(OC(C)(C)C)OC(C)(C)C HLDBBQREZCVBMA-UHFFFAOYSA-N 0.000 title claims abstract description 37
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 29
- 238000001308 synthesis method Methods 0.000 title abstract description 4
- FVBYRRMYZCJOAC-UHFFFAOYSA-N chloro-tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[Si](Cl)(OC(C)(C)C)OC(C)(C)C FVBYRRMYZCJOAC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003960 organic solvent Substances 0.000 claims abstract description 11
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical group CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 230000002194 synthesizing effect Effects 0.000 claims description 10
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- 239000012043 crude product Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052987 metal hydride Inorganic materials 0.000 claims description 6
- 150000004681 metal hydrides Chemical class 0.000 claims description 6
- 239000012074 organic phase Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 238000006722 reduction reaction Methods 0.000 claims description 5
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical group [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- 229910000103 lithium hydride Inorganic materials 0.000 claims description 4
- SIAPCJWMELPYOE-UHFFFAOYSA-N lithium hydride Chemical compound [LiH] SIAPCJWMELPYOE-UHFFFAOYSA-N 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000013557 residual solvent Substances 0.000 claims description 4
- 229910000104 sodium hydride Inorganic materials 0.000 claims description 4
- 239000012312 sodium hydride Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- QCKKBOHAYRLMQP-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]silane Chemical compound CC(C)(C)O[SiH](OC(C)(C)C)OC(C)(C)C QCKKBOHAYRLMQP-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000102 alkali metal hydride Inorganic materials 0.000 abstract description 3
- 150000008046 alkali metal hydrides Chemical class 0.000 abstract description 3
- 238000007796 conventional method Methods 0.000 abstract description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 33
- 239000000047 product Substances 0.000 description 15
- 150000002500 ions Chemical class 0.000 description 8
- AOJFQRQNPXYVLM-UHFFFAOYSA-N pyridin-1-ium;chloride Chemical compound [Cl-].C1=CC=[NH+]C=C1 AOJFQRQNPXYVLM-UHFFFAOYSA-N 0.000 description 8
- 238000004821 distillation Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000007867 post-reaction treatment Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 125000001309 chloro group Chemical group Cl* 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydroxyl hydrogen Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 229910052914 metal silicate Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 238000007740 vapor deposition 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
- C07F7/025—Silicon compounds without C-silicon linkages
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/55—Design of synthesis routes, e.g. reducing the use of auxiliary or protecting groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The embodiment of the invention discloses a synthesis method of tri (tert-butoxy) silanol with low chloride ion content. The invention can effectively separate tri (tert-butoxy) silanol by reducing tri (tert-butoxy) silane which is obtained by a conventional method into tri (tert-butoxy) silane by reducing tri-tert-butoxy chlorosilane with alkali metal hydride in the presence of an organic solvent, thereby eliminating residual trace chloride ions in the product and obtaining tri (tert-butoxy) silanol high-purity product.
Description
Technical Field
The embodiment of the invention relates to the technical field of fine chemical engineering, in particular to a method for synthesizing tri (tert-butoxy) silanol with ultralow chloride ion content.
Background
Tri (t-butoxy) silanol has weakly acidic hydroxyl hydrogen, has similar chemical properties as most silanol, and can undergo ligand replacement reaction with alkylamine-coordinated metal compounds to form metal alkylsilicon esters, which can be used as precursors for vapor deposition of metal silicates. It is also an ideal precursor for silicon dioxide deposition, and when a semiconductor device such as a low-k dielectric mask layer is manufactured, salt precipitation is easy to generate, and chlorine residues are easy to generate in a film, so that the performance of the semiconductor device is influenced.
The conventional synthesis method of tri (tert-butoxy) silanol is that tri-tert-butoxy chlorosilane reacts with water in the presence of acid-binding agent pyridine to generate a product, diethyl ether is used as a solvent to generate a target product and pyridine hydrochloride byproducts, and after repeated water washing, the organic phase is subjected to desolventizing and vacuum rectification treatment successively, the yield of the obtained product is about 80%, the gas phase purity can reach 99%, and the chloride ion content is more than 500ppm.
CN 115490719a discloses a method for purifying alkoxysilane composition, adding ethanol into crude alkoxysilane, converting organic chloride into hydrogen chloride under reflux condition, introducing inert gas to exchange hydrogen chloride, and finally distilling to obtain pure product. The content of chloride ions in the pure product obtained by the method is less than 1ppm, and ethanol is remained at 5-20ppm, and the method can influence the performance of semiconductor devices.
Disclosure of Invention
Therefore, the embodiment of the invention provides a method for synthesizing tri (tert-butoxy) silanol with ultralow chloride ion content.
In order to achieve the above object, the embodiment of the present invention provides the following technical solutions:
a method of synthesizing tris (t-butoxy) silanol having an ultra-low chloride ion content, the method comprising:
taking tri-tert-butoxy chlorosilane and water as raw materials, pyridine as an acid-attaching agent, carrying out hydrolysis reaction in the presence of a first organic solvent, repeatedly washing with water, collecting an organic phase, removing residual solvent, and carrying out first reduced pressure rectification to obtain a tri (tert-butoxy) silanol crude product;
and (3) carrying out reduction reaction on the crude tri (tert-butoxy) silanol and metal hydride in the presence of a second organic solvent, filtering, removing residual solvent, and carrying out second vacuum rectification to obtain tri (tert-butoxy) silanol with ultralow chloride ion content.
Further, the first organic solvent is diethyl ether, methyl tertiary butyl ether, dibutyl ether, tetrahydrofuran, toluene or methylene chloride, preferably dibutyl ether; the second organic solvent is diethyl ether, dimethyl ether, dibutyl ether or 1, 4-dioxane, preferably dibutyl ether.
The research shows that when the first organic solvent/the second organic solvent is dibutyl ether, the raw material has higher reactivity, the tri-tert-butoxy chlorosilane has more thorough reaction, the yield and the product purity are improved, and the reduction of the chloride ion content is facilitated.
Further, the hydrolysis reaction is carried out at a temperature of 20 to 50 ℃ for 3 to 12 hours.
Further, the reduction reaction is carried out under reflux conditions for 8 to 20 hours.
Further, the mass ratio of the tri-tert-butoxychlorosilane to water is 1:5-15, wherein the mole ratio of the tri-tert-butoxychlorosilane to the pyridine is 1:2-4.
Further, the metal hydride is sodium hydride or lithium hydride, and the molar ratio of the metal hydride to the tri-tert-butoxychlorosilane is 1-3:1.
further, the conditions of the first reduced pressure rectification are as follows: vacuum degree is 5-10mmHg and temperature is 50-80 ℃.
Further, the conditions of the second reduced pressure rectification are as follows: vacuum degree is 5-10mmHg, and temperature is 70-83 ℃.
The embodiment of the invention has the following advantages:
in the crude tri (t-butoxy) silanol obtained by the conventional method, the tri (t-butoxy) silanol is not completely separated by the way of vacuum distillation because the boiling point of the tri (t-butoxy) silanol is close to that of the raw material tri (t-butoxy) chlorosilane, so that the crude tri (t-butoxy) silanol still contains a small amount of tri (t-butoxy) chlorosilane.
The invention can effectively separate tri (tert-butoxy) silanol by reducing tri (tert-butoxy) silane which is obtained by a conventional method into tri (tert-butoxy) silane by reducing tri-tert-butoxy chlorosilane by alkali metal hydride and alkali metal hydride under reflux, thereby eliminating trace chloride ions remained in the crude product and obtaining tri (tert-butoxy) silanol high-purity product.
Detailed Description
Other advantages and advantages of the present invention will become apparent to those skilled in the art from the following detailed description, which, by way of illustration, is to be read in connection with certain specific embodiments, 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
This example provides a method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content:
step 1: 100g of tri-tert-butoxychlorosilane was weighed out and dissolved in 1.2L of diethyl ether and 0.8L of water, and 87g of pyridine was added thereto to react at 40℃for 12 hours. The post-reaction treatment is to remove pyridine hydrochloride by repeated water washing, collect an organic phase, remove diethyl ether by reduced pressure distillation, and perform reduced pressure rectification under the vacuum degree of 10mmHg and the temperature of 77-79 ℃ to obtain 85g of crude tri (tert-butoxy) silanol, and the content of chloride ions is 518.7ppm by using an ion chromatograph.
Step 2: dissolving the crude product in 1L diethyl ether, adding 17g of sodium hydride, heating and refluxing for 12 hours, filtering, distilling under reduced pressure to remove diethyl ether, distilling a small amount of first fraction at the vacuum degree of 5mmHg and the temperature of 52-54 ℃, and distilling a large amount of product at the temperature of 70-72 ℃ to obtain 75g of tri (tert-butoxy) silanol pure product, wherein the yield is 81%, and the content of chloride ions is 22.3ppm by using an ion chromatograph.
Example 2
This example provides a method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content:
step 1: 100g of tri-tert-butoxychlorosilane were weighed out and dissolved in 1.2L of dibutyl ether and 0.8L of water, and 87g of pyridine was added thereto to react at 40℃for 12 hours. The post-reaction treatment is to remove the solvent by repeated water elution, and to carry out vacuum rectification at the vacuum degree of 10mmHg and the temperature of 77-79 ℃ to obtain 85g of crude tri (tert-butoxy) silanol, and to detect the content of chloride ions to be 140.6ppm by using an ion chromatograph.
Step 2: dissolving the crude product in 1L dibutyl ether, adding 17g of sodium hydride, heating and refluxing for 12 hours, filtering, removing dibutyl ether by reduced pressure distillation, rectifying under reduced pressure, distilling off a small amount of first fraction at 52-53 ℃ under the vacuum degree of 5mmHg, distilling off a large amount of products at 70-71 ℃ to obtain 83g of tri (tert-butoxy) silanol pure product, and detecting the content of chloride ions to be 0.5ppm by using an ion chromatograph after the detection.
Example 3
This example provides a method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content:
step 1: 100g of tri-tert-butoxychlorosilane was weighed out and dissolved in 1.2L of diethyl ether and 0.8L of water, and 87g of pyridine was added thereto to react at 40℃for 12 hours. The post-reaction treatment is to remove pyridine hydrochloride by repeated water washing, collect an organic phase, remove diethyl ether by reduced pressure distillation, and perform reduced pressure rectification under the vacuum degree of 9mmHg and the temperature of 79-80 ℃ to obtain 85g of crude tri (tert-butoxy) silanol, and the content of chloride ions is 443.5ppm by using an ion chromatograph.
Step 2: dissolving the crude product in 1L diethyl ether, adding 5.7g of lithium hydride, heating and refluxing for 12 hours, filtering, distilling under reduced pressure to remove diethyl ether, distilling under reduced pressure and 6mmHg vacuum degree to obtain a small amount of first fraction at 51-53 ℃, and distilling a large amount of product at 71-72 ℃ to obtain 77g of tri (tert-butoxy) silanol pure product, wherein the yield is 83%, and the content of chloride ions is detected to be 12.1ppm by using an ion chromatograph.
Example 4
This example provides a method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content:
step 1: 100g of tri-tert-butoxychlorosilane were weighed out and dissolved in 1.2L of dibutyl ether and 0.8L of water, and 87g of pyridine was added thereto to react at 40℃for 12 hours. The post-reaction treatment is to remove pyridine hydrochloride by repeated water washing, collect organic phase, remove dibutyl ether by reduced pressure distillation, and carry out reduced pressure rectification under the vacuum degree of 10mmHg and the temperature of 79-80 ℃ to obtain 85g of crude tri (tert-butoxy) silanol, and the content of chloride ions is detected to be about 130.8ppm by an ion chromatograph.
Step 2: dissolving the crude product in 1L dibutyl ether, adding 5.7g of lithium hydride, heating and refluxing for 12 hours, filtering, removing dibutyl ether by reduced pressure distillation, distilling a small amount of first fraction at 52-53 ℃ under the vacuum degree of reduced pressure distillation, and distilling a large amount of products at about 70-71 ℃ to obtain 84g of tri (tert-butoxy) silanol pure product, wherein the yield is 90%, and detecting the chloride ion content to be 0.8ppm by using an ion chromatograph.
While the invention has been described in detail in the foregoing general description and specific examples, it will be apparent to those skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (3)
1. A method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content, comprising:
taking tri-tert-butoxy chlorosilane and water as raw materials, pyridine as an acid-attaching agent, carrying out hydrolysis reaction in the presence of a first organic solvent, repeatedly washing with water, collecting an organic phase, removing residual solvent, and carrying out first reduced pressure rectification to obtain a tri (tert-butoxy) silanol crude product;
carrying out reduction reaction on the crude tri (tert-butoxy) silanol and metal hydride in the presence of a second organic solvent, filtering to remove residual solvent, and carrying out second vacuum rectification to obtain tri (tert-butoxy) silanol with ultralow chloride ion content;
the first organic solvent is dibutyl ether; the second organic solvent is dibutyl ether;
the reduction reaction is carried out for 8-20 hours under the reflux condition;
the metal hydride is sodium hydride or lithium hydride, and the molar ratio of the metal hydride to the tri-tert-butoxychlorosilane is 1-3:1, a step of;
the conditions of the first reduced pressure rectification are as follows: vacuum degree is 5-10mmHg, and temperature is 50-80 ℃;
the conditions of the second reduced pressure rectification are as follows: vacuum degree is 5-10mmHg, and temperature is 70-83 ℃.
2. The method for synthesizing tri (t-butoxy) silanol having ultra-low chloride ion content as claimed in claim 1, wherein the hydrolysis reaction is carried out at a temperature of 20-50 ℃ for 3-12 hours.
3. The method for synthesizing tri (t-butoxy) silanol with ultra-low chloride ion content as claimed in claim 1, wherein the mass ratio of tri-t-butoxy chlorosilane to water is 1:5-15, wherein the mole ratio of the tri-tert-butoxychlorosilane to the pyridine is 1:2-4.
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| CN1821251A (en) * | 2004-12-09 | 2006-08-23 | 气体产品与化学公司 | Precursors for silica or metal silicate films |
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| CN113845507A (en) * | 2021-08-26 | 2021-12-28 | 珠海理文新材料有限公司 | Method for removing water and chloride ions in fluoroethylene carbonate |
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