CN103772424B - A kind of preparation method of electronic-grade tetraethyl orthosilicate - Google Patents
A kind of preparation method of electronic-grade tetraethyl orthosilicate Download PDFInfo
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- CN103772424B CN103772424B CN201310747619.4A CN201310747619A CN103772424B CN 103772424 B CN103772424 B CN 103772424B CN 201310747619 A CN201310747619 A CN 201310747619A CN 103772424 B CN103772424 B CN 103772424B
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- tetraethyl orthosilicate
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000004821 distillation Methods 0.000 claims abstract description 34
- 239000012535 impurity Substances 0.000 claims abstract description 31
- 238000009835 boiling Methods 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 32
- 239000000706 filtrate Substances 0.000 claims description 15
- 125000002091 cationic group Chemical group 0.000 claims description 9
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000011049 filling Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910021654 trace metal Inorganic materials 0.000 abstract description 3
- 238000000746 purification Methods 0.000 abstract description 2
- 238000005341 cation exchange Methods 0.000 abstract 1
- 239000008139 complexing agent Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 5
- 238000012423 maintenance Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 3
- 238000010959 commercial synthesis reaction Methods 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052744 lithium Inorganic materials 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 230000003000 nontoxic effect Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 238000007740 vapor deposition Methods 0.000 description 3
- 238000000207 volumetry Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910000103 lithium hydride Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The present invention relates to a kind of preparation method of electronic-grade tetraethyl orthosilicate, particularly relate to a kind of preparation method for semicon industry chemical vapour deposition electronic-grade tetraethyl orthosilicate, first use in complexing agent complexes raw material after most of metallic impurity, filter with the millipore filter of 0.1 micron; By cation exchange tower, quartzy plate tower, sub-boiling distillation device, strict temperature control, removes trace metal impurities, ethanol and organic impurity thereof and moisture content.Adopt conventional purification equipment, easy to operate, be beneficial to industrial scale and produce, product cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of electronic-grade tetraethyl orthosilicate, particularly relate to a kind of preparation method for semicon industry chemical vapour deposition electronic-grade tetraethyl orthosilicate.
Background technology
In the manufacture of semiconductor electronic component, must by element encases in glass, or with glass as interlayer insulating film.Usually, glass coating is with chemical vapor deposition (CVD) method making SiO on a surface of a wafer
2layer.
Use the inflammable silane of severe toxicity as vapor deposition source at first, along with the update of electronic material and technology, people are pursuing the high-performance of product simultaneously, more focus on the features such as its nontoxic, green, environmental friendliness.The relative silane toxicity of tetraethyl orthosilicate reduces greatly, is liquid at normal temperatures, operates more easy.And greatly improve than the density of forming silane film, thus decrease the possibility of leaking electricity between layers of multilayer circuit board and layer.
Industrial tetraethyl orthosilicate can reach 99% by content after general preparation, but still contains the impurity up to 1%, and wherein metal ion is electrically active impurity, can reduce and be deposited on semiconducter device SiO
2thin film layer insulating property, can cause micron-sized circuit mutually to be connected, thus cause circuit card to be scrapped; Electrically inactive impurity wherein such as moisture content, organism can affect even film layer and the planarization of deposition.
Gas-chromatography is used to prepare tetraethyl orthosilicate in US Patent No. 5840953, and remove water impurity with lithium hydride, product (in the metallic impurity) purity obtained is not less than the tetraethyl orthosilicate of 99.999999%, water content is less than 2PPM, because gas chromatograph is mainly used in the analyzing and testing of trace element, and gas chromatograph apparatus expensive, improve production cost.
Summary of the invention
The object of the invention is to the defect overcoming prior art; there is provided a kind of and be not less than 99.999999%(w/w in its purity of metallic impurity) preparation method of electronic-grade tetraethyl orthosilicate; the content of organic impurity (with alcohol meter) is lower than 1ppm; water content is lower than 0.3ppm; adopt conventional Preparation equipment, easy to operate, be beneficial to industrial scale and produce; product cost is low, and quality can meet the requirement of semicon industry vapor deposition source.
The present invention is achieved the above object by following measures:
(1) the present invention is first with most of metallic impurity in analytically pure EDTA complex agent complexing raw material, through fully mixing, stirring, filters with the millipore filter of 0.1 micron;
(2) by the filtrate of collecting through cationic exchange column device, collect product, remove trace metal impurities further.
(3) the present invention adopts quartzy plate tower, by efficient distillation, strict control device extraction cut temperature, treat that cut temperature controls within the scope of 159.0 ~ 166.0 DEG C, after total reflux 7 ~ 16h hour, extraction fraction from tower top, ethanol and organic impurity content thereof are less than 1ppm, and metallic impurity total content is less than 5ppm.
(4) distilled through sub-boiling distillation device by the fraction collected, strict control distillation temperature 90 ~ 100 DEG C, remove moisture, other inorganic phase impurity in material further, the water content in product is to below 0.3ppm.
In whole production process, product does not contact the external world, and wherein said strainer, cationic exchange coloum and pipe material adopt tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
A kind of preparation method for semicon industry chemical vapor deposition (CVD) source electronic-grade tetraethyl orthosilicate of the present invention.Realized by following steps:
(1) in technical grade tetraethyl orthosilicate raw material, add the agent of analytical pure EDTA complex, fully mixing, stirring 30-60 minute, the millipore filter entering 0.1 micron filters; (2) by the filtrate of collecting through cationic exchange column device, collect product, remove trace metal impurities further; (3) filtration gained filtrate is added distillation tower to distill, after total reflux 7 ~ 16h hour, gather fraction 159.0 ~ 166.0 DEG C from tower top; (4) distilled through sub-boiling distillation device by the fraction collected, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature, at 90 ~ 100 DEG C, collects 90 ~ 100 DEG C of distillation product; (5) products obtained therefrom is not more than thousand grades in entirety, local is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Preparation method of the present invention, the wherein said analytical pure EDTA complex agent quality added is the 3-10% of raw material tetraethyl orthosilicate quality, and the mix and blend time is preferably 40-50 minute.
Preparation method of the present invention, wherein said millipore filter filter membrane is using tetrafluoroethylene as mould material.
Preparation method of the present invention, wherein said distillation tower adopts quartzy plate tower, and tower top gathers fraction and is preferably 164 ~ 166.0 DEG C.
Preparation method of the present invention, wherein said sub-boiling distillation temperature remains on 95 ~ 98 DEG C.
Preparation method of the present invention, wherein said strainer, cationic exchange coloum and pipe material adopt tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
Preparation method of the present invention, is characterized in that the tetraethyl orthosilicate product purity obtained with aforesaid method is not less than 99.999999%(w/w), the content < 1ppm of organic impurity (with alcohol meter); Water-content < 0.3ppm.
Effect of the present invention: the present invention adopts millipore filtration, column plate distillation, sub-boiling distillation to combine; adopt conventional purification equipment; easy to operate; can effectively remove solid impurity in raw material, metallic impurity, low-boiling-point substance, micro-moisture; product purity (in metallic impurity) is not less than 99.999999%(w/w); and our bright preparation method is beneficial to industrial scale production, product cost is low, and quality can meet the requirement of semicon industry vapor deposition source.
The advantages such as it is high that product of the present invention has purity, safe, nontoxic, difficult combustion, environmental pollution is little.
Product of the present invention adopts quartz source bottle packaging, and client is easy to use.
Product of the present invention can be semicon industry, unicircuit, semiconductor separation part provide that high-efficiency environment friendly is nontoxic, low cost silicon depositing source, promotes semicon industry sustainable and stable development.
Embodiment
In order to the present invention is described, provide following case study on implementation.But be interpreted as claim of the present invention not by the restriction of following embodiment.
Embodiment 1:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the tetraethyl orthosilicate crude product 12kg of commercial synthesis in the polytetrafluoroethylcontainer container of 20L, add the agent of 0.36kg analytical pure EDTA complex, abundant mixing, stirring 30 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate of collecting through cationic exchange column device, remove metallic impurity further, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower to distill, after total reflux 7 hours, gather fraction 163 DEG C from tower top; (4) distilled through sub-boiling distillation device by the fraction collected, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature is at 95 DEG C, and collect 95 DEG C of distillation product, sampling detects; (5) products obtained therefrom is not more than thousand grades in entirety, local is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Product detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein with icp ms (ICP-MS), detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), detect water-content by Ka Er-Fei Xiu (KF) volumetry.
Detected result sees attached list.
Embodiment 2:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the tetraethyl orthosilicate crude product 12kg of commercial synthesis in the polytetrafluoroethylcontainer container of 20L, add the agent of 0.72kg analytical pure EDTA complex, abundant mixing, stirring 45 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate of collecting through cationic exchange column device, remove metallic impurity further, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower to distill, after total reflux 10 hours, gather fraction 165 DEG C from tower top; (4) distilled through sub-boiling distillation device by the fraction collected, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature is at 98 DEG C, and collect 98 DEG C of distillation product, sampling detects; (5) products obtained therefrom is not more than thousand grades in entirety, local is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Product detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein with icp ms (ICP-MS), detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), detect water-content by Ka Er-Fei Xiu (KF) volumetry.
Detected result sees attached list.
Embodiment 3:
A kind of preparation method of electronic-grade tetraethyl orthosilicate: (1) gets the tetraethyl orthosilicate crude product 12kg of commercial synthesis in the polytetrafluoroethylcontainer container of 20L, add the agent of 1.2kg analytical pure EDTA complex, abundant mixing, stirring 60 minutes, then filter with the millipore filter of 0.1 micron; (2) by the filtrate of collecting through cationic exchange column device, remove metallic impurity further, collect filtrate; (3) filtrate of collection is added board-like quartzy distillation tower to distill, after total reflux 15 hours, gather fraction 163 DEG C from tower top; (4) distilled through sub-boiling distillation device by the fraction collected, regulate sub-boiling distillation device heating unit voltage, maintenance medium surface temperature is at 90 DEG C, and collect 90 DEG C of distillation product, sampling detects; (5) products obtained therefrom is not more than thousand grades in entirety, local is not more than the clean room of hundred grades, adopts quartz source bottle to carry out filling, obtains electronic-grade tetraethyl orthosilicate product.
Product detects conventional 17 kinds of metals content impurities such as Li, Na, Mg, Al wherein with icp ms (ICP-MS), detect the organic impurity contents such as ethanol with gas chromatograph-mass spectrometer (GC-MS), detect water-content by Ka Er-Fei Xiu (KF) volumetry.
Detected result sees attached list.
Subordinate list
Ppm, ppb of the present invention refer to mass concentration unit, 1ppm=1000ppb.
Claims (7)
1. a preparation method for electronic-grade tetraethyl orthosilicate, is characterized in that comprising the steps:
(1) in technical grade tetraethyl orthosilicate raw material, add the agent of analytical pure EDTA complex, fully mixing, stirring 30-60 minute, the millipore filter entering 0.1 micron filters;
(2) gained filtrate will be filtered through cationic exchange column device, collect filtrate;
(3) filtrate of collection is added distillation tower to distill, after total reflux 7 ~ 16 hours, from tower top collecting fractions 159 ~ 166 DEG C;
(4) fraction collected is distilled through sub-boiling distillation device, regulate sub-boiling distillation device heating unit voltage, keep liquid level temperature at 90 ~ 100 DEG C, collect 90 ~ 100 DEG C of distillation product;
(5) the distillation product collected are not more than thousand grades in entirety, local is not more than the clean room of hundred grades, carry out filling with quartz source bottle, obtain electronic-grade tetraethyl orthosilicate product.
2. preparation method according to claim 1, the wherein said analytical pure EDTA complex agent quality added is the 3-10% of raw material tetraethyl orthosilicate quality, and the mix and blend time is preferably 40-50 minute.
3. preparation method according to claim 1, wherein said millipore filter filter membrane is using tetrafluoroethylene as mould material.
4. preparation method according to claim 1, wherein said distillation tower adopts quartzy plate tower, and tower top gathers fraction and is preferably 164 ~ 166.0 DEG C.
5. preparation method according to claim 1, wherein said sub-boiling distillation temperature maintains 95 ~ 98 DEG C.
6., according to the preparation method one of claim 1-5 Suo Shu, the pipe material of wherein said strainer, cationic exchange coloum adopts tetrafluoroethylene, and plate tower, sub-boiling distillation equipment matter adopt quartz.
7. according to the preparation method one of claim 1-5 Suo Shu, it is characterized in that the tetraethyl orthosilicate product obtained with aforesaid method is not less than 99.999999%w/w in metallic impurity purity, organic impurity is with the content < 1ppm of alcohol meter; Water-content < 0.3ppm.
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| CN201310747619.4A CN103772424B (en) | 2013-12-31 | 2013-12-31 | A kind of preparation method of electronic-grade tetraethyl orthosilicate |
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| CN201310747619.4A CN103772424B (en) | 2013-12-31 | 2013-12-31 | A kind of preparation method of electronic-grade tetraethyl orthosilicate |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109438495B (en) * | 2018-12-25 | 2023-05-26 | 金宏气体股份有限公司 | Production method and production system of high-purity ethyl silicate |
| CN109459539B (en) * | 2018-12-29 | 2024-03-22 | 金宏气体股份有限公司 | Method and system for detecting trace moisture in high-purity ethyl silicate |
| CN109705153B (en) * | 2019-02-02 | 2020-04-07 | 苏州金宏气体股份有限公司 | Purifying method of ethyl orthosilicate |
| CN115304632B (en) * | 2022-07-21 | 2023-08-29 | 湖北新蓝天新材料股份有限公司 | Preparation method and application of electronic-grade tetraalkoxysilane |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5840953A (en) * | 1995-11-16 | 1998-11-24 | Eagle-Picher Industries, Inc. | Purified tetraethoxysilane and method of purifying |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5902893A (en) * | 1997-05-20 | 1999-05-11 | Air Products And Chemicals, Inc. | Purification of organosilanes of group 13 (IIIA) and 15 (VA) impurities |
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- 2013-12-31 CN CN201310747619.4A patent/CN103772424B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5840953A (en) * | 1995-11-16 | 1998-11-24 | Eagle-Picher Industries, Inc. | Purified tetraethoxysilane and method of purifying |
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