CN102321115A - Purification method for electronic-grade dimethyl diethoxy silane - Google Patents
Purification method for electronic-grade dimethyl diethoxy silane Download PDFInfo
- Publication number
- CN102321115A CN102321115A CN201110340336A CN201110340336A CN102321115A CN 102321115 A CN102321115 A CN 102321115A CN 201110340336 A CN201110340336 A CN 201110340336A CN 201110340336 A CN201110340336 A CN 201110340336A CN 102321115 A CN102321115 A CN 102321115A
- Authority
- CN
- China
- Prior art keywords
- tower
- dimethyldiethoxysilane
- purification
- diethoxy silane
- electronic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a purification method for electronic-grade dimethyl diethoxy silane. In the method, a rectification mode is adopted for purification. The process of the purification method comprises the following steps of: (1) adding dimethyl diethoxy silane with 99 percent content into a solvent removal tower, and removing a small amount of residual solvent tetrahydrofuran on the tower top under normal pressure at the temperature of the tower top of 66 DEG C; and (2) flowing the dimethyl diethoxy silane from which solvent is removed out from the tower bottom to enter a heavy component eliminating rectification tower, wherein the region where the heavy component eliminating rectification tower is positioned is a super-clean room; normal pressure operation is adopted in the tower; the temperature of the top is 114 DEG C; the dimethyl diethoxy silane with content of more than 99.8 percent is received; and residual high-boiling-point impurities are discharged from the tower bottom. The inner wall of the heavy component eliminating rectification tower and a receiving container are both wrapped by polytetrafluoroethylene; and filler of the heavy component eliminating rectification tower is wrapped by the polytetrafluoroethylene.
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, be specifically related to a kind of method of purification of electronic-grade dimethyldiethoxysilane.
Background technology
Dimethyldiethoxysilane, a kind of colourless transparent liquid.Be mainly used in the constitution controller in the Zylox preparation, chainextender and silicone oil synthesis material during organosilicon product is synthetic.
Along with the development that VLSI is made, the interconnection line density in the chip constantly increases, and width and the spacing of interconnection line constantly reduce, so the ghost effect that is produced by interconnection resistance (R) and electric capacity (C) is more and more obvious.Age of Technology when 0.25 micron of development of integrated circuits entering; The signal delay that is caused by traditional aluminium and silicon-dioxide interconnection will postpone above gate pole; Become the important factor that the restriction chip performance promotes; Postpone in order to reduce interconnection RC, adopt the interconnect scheme of low-k (k) medium and copper conductor in the world.Low k/ copper interconnection technology successfully was applied in the chip production in 1998, and the research and development and the production of crucial low-k materials begin to become an important topic in this technology.Wherein dimethyldiethoxysilane can be used as a kind of suitable low k liquid source material, is used for further synthetic relevant low-k materials.
The organosilicon raw material that is used for the unicircuit manufacturing must reach electronic-grade, and general business-like dimethyldiethoxysilane has only 99% through common purification back content, and contains the foreign metal ion, can cause the manufacturing of integrated circuit material to have a strong impact on.
Summary of the invention
The method of purification that the purpose of this invention is to provide a kind of electronic-grade dimethyldiethoxysilane, i.e. the method for the dimethyldiethoxysilane of production purity more than 99.8%.
The method of purification step of a kind of electronic-grade dimethyldiethoxysilane provided by the invention is following:
1. the dimethyldiethoxysilane with 99% content gets into electronic-grade silane refining system desolventizing tower through the silane compressor, and the desolventizing tower adopts atmospheric operation, and it is 66 ℃ that cat head receives the cut temperature, and this is isolated solvents tetrahydrofurane.Recommend to adopt the desolventizing tower that 10～80 theoretical plate numbers are arranged, adopt higher stage number separating not influence.
2. will take off the dimethyldiethoxysilane of solvent and go into to take off heavy rectifying tower from tower bottom flow, and take off heavy rectifying tower and adopt atmospheric operation, cat head receives 114 ℃ cut, obtains the dimethyldiethoxysilane of 99.8% above content.High-boiling-point impurity is emitted at the bottom of through tower.Recommend to adopt and contain the heavy rectifying tower of taking off of ripple packing, 60～100 theoretical plate numbers, but adopt higher stage number separating not influence.
In the method for purification of a kind of electronic-grade dimethyldiethoxysilane provided by the invention, operating environment there is particular requirement, i.e. the taking off heavy rectifying tower and must be placed in the clean room and operate of final step.
In the method for purification of a kind of electronic-grade dimethyldiethoxysilane provided by the invention; Operating equipment there is particular requirement; The inwall and the receiving vessel that take off heavy rectifying tower that are final step all adopt teflon-coated, and the filler that takes off heavy rectifying tower adopts teflon-coated.
The inventive method is easy, and the dimethyldiethoxysilane purity that obtains has reached more than 99.8%, and does not have the foreign metal ion, meets the electronic industry demand, and is a kind of industrial method that is fit to.
Description of drawings
Fig. 1 is the gas chromatograph purity detecting collection of illustrative plates of the dimethyldiethoxysilane after the embodiment of the invention 1 is purified.
Fig. 2 is the gas chromatograph purity detecting collection of illustrative plates of the dimethyldiethoxysilane after the embodiment of the invention 2 is purified.
Fig. 3 is the gas chromatograph purity detecting collection of illustrative plates of the dimethyldiethoxysilane after the embodiment of the invention 3 is purified.
Embodiment
Help to understand the present invention through following examples, but be not limited to content of the present invention.
Among the embodiment, take off heavy rectifying tower and must be placed on clean room, the inwall and the receiving vessel that take off heavy rectifying tower all adopt teflon-coated, and the ripple packing that takes off heavy rectifying tower adopts teflon-coated.
Embodiment 1:
The dimethyldiethoxysilane of 1 ton of 99% (weight) content is got into electronic-grade silane refining system desolventizing tower through the silane compressor; Theoretical plate number is 60; The desolventizing tower adopts atmospheric operation, and column bottom temperature adopts the temperature programming heating, is heated to 114 ℃ gradually from room temperature.It is 66 ℃ that cat head receives the cut temperature, is isolated solvents tetrahydrofurane through detecting.When quantity of distillate is more and more littler, until not going out, this moment, tower top temperature began to rise, and the composition check is solvent-free at the bottom of the tower.
To take off the dimethyldiethoxysilane of solvent and go into to take off heavy rectifying tower from tower bottom flow, the desolventizing tower weight newly begins next batch rectifying.Theoretical plate number is 80 the heavy rectifying tower employing atmospheric operation that takes off, and adopts the temperature programming heating at the bottom of the tower, receives 114 ℃ cut until cat head; Through verifying as the dimethyldiethoxysilane of content more than 99.8%, yield 85.6% steams to fluid very slow; And temperature begins to rise; Product content begins to descend, and stops rectifying immediately, and the high boiling point residue is emitted at the bottom of through tower.
Accompanying drawing 1 display density is that the main peak of 99.8255% content is a dimethyldiethoxysilane, and all the other impurity accumulative total content are 0.1745%, and purity meets the requirements.
Embodiment 2:
The dimethyldiethoxysilane of 99% (weight) content is got into electronic-grade silane refining system desolventizing tower through the silane compressor; Theoretical plate number is 60; The desolventizing tower adopts atmospheric operation, and column bottom temperature adopts the temperature programming heating, is heated to 114 ℃ gradually from room temperature.It is 66 ℃ that cat head receives the cut temperature, is isolated solvents tetrahydrofurane through detecting.When quantity of distillate is more and more littler, until not going out, this moment, tower top temperature began to rise, and the composition check is solvent-free at the bottom of the tower.
To take off the dimethyldiethoxysilane of solvent and go into to take off heavy rectifying tower from tower bottom flow, the desolventizing tower weight newly begins next batch rectifying.Theoretical plate number is that 80 the heavy rectifying tower that takes off adopts atmospheric operation, adopts the temperature programming heating at the bottom of the tower, receives 114 ℃ cut until cat head, continues to receive to rise to 115 ℃ until temperature, stops rectifying.Accompanying drawing 2 display densities are that the main peak of 99.7695% content is a dimethyldiethoxysilane, and all the other impurity accumulative total content are 0.2305%, and purity is undesirable
Embodiment 3:
The dimethyldiethoxysilane of 99% (weight) content is got into electronic-grade silane refining system desolventizing tower through the silane compressor; Theoretical plate number is 60; The desolventizing tower adopts atmospheric operation, and column bottom temperature adopts the temperature programming heating, is heated to 114 ℃ gradually from room temperature.It is 66 ℃ that cat head receives the cut temperature, is isolated solvents tetrahydrofurane through detecting.When quantity of distillate is more and more littler, until not going out, this moment, tower top temperature began to rise, and the composition check is solvent-free at the bottom of the tower.
To take off the dimethyldiethoxysilane of solvent and go into to take off heavy rectifying tower from tower bottom flow, the desolventizing tower weight newly begins next batch rectifying.Theoretical plate number is that 80 the heavy rectifying tower that takes off adopts atmospheric operation, adopts the temperature programming heating at the bottom of the tower, receives 114 ℃ cut until cat head, continues to receive to rise to 116 ℃ until temperature, stops rectifying.Accompanying drawing 3 display densities are that the main peak of 99.7115% content is a dimethyldiethoxysilane, and all the other impurity accumulative total content are 0.2885%, and purity is undesirable.
Claims (4)
1. the method for purification of an electronic-grade dimethyldiethoxysilane is characterized in that comprising the steps:
1) dimethyldiethoxysilane with 99% content gets into the desolventizing tower through the silane compressor, and the desolventizing tower is under normal pressure, and it is 66 ℃ that cat head receives the cut temperature, separates and removes solvents tetrahydrofurane;
The dimethyldiethoxysilane that 2) will take off solvent goes into to take off heavy rectifying tower from tower bottom flow, under normal pressure, receives 114 ℃ cut from cat head, the dimethyldiethoxysilane of the 99.8% above content that obtains; High-boiling-point impurity is emitted at the bottom of through tower; Described inwall, filler and the receiving vessel that takes off heavy rectifying tower adopts teflon-coated.
2. method of purification as claimed in claim 1 is characterized in that the described weight rectifying tower that takes off carries out in clean room.
3. method of purification as claimed in claim 1, the stage number that it is characterized in that described desolventizing tower is 10～80.
4. method of purification as claimed in claim 1 is characterized in that described stage number of taking off heavy rectifying tower is 60～100.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340336A CN102321115A (en) | 2011-11-01 | 2011-11-01 | Purification method for electronic-grade dimethyl diethoxy silane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110340336A CN102321115A (en) | 2011-11-01 | 2011-11-01 | Purification method for electronic-grade dimethyl diethoxy silane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102321115A true CN102321115A (en) | 2012-01-18 |
Family
ID=45448972
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110340336A Pending CN102321115A (en) | 2011-11-01 | 2011-11-01 | Purification method for electronic-grade dimethyl diethoxy silane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102321115A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060052569A1 (en) * | 2002-06-21 | 2006-03-09 | Lehmann Lutz U | Silyl alkyl esters of anthracene-and phenanthrene carboxylic acids |
| CN102070663A (en) * | 2010-12-27 | 2011-05-25 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation technology for dimethyl diethoxy silane |
| CN102079754A (en) * | 2010-12-27 | 2011-06-01 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of methyltriethoxysilane |
-
2011
- 2011-11-01 CN CN201110340336A patent/CN102321115A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060052569A1 (en) * | 2002-06-21 | 2006-03-09 | Lehmann Lutz U | Silyl alkyl esters of anthracene-and phenanthrene carboxylic acids |
| CN102070663A (en) * | 2010-12-27 | 2011-05-25 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation technology for dimethyl diethoxy silane |
| CN102079754A (en) * | 2010-12-27 | 2011-06-01 | 蓝星化工新材料股份有限公司江西星火有机硅厂 | Preparation process of methyltriethoxysilane |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101492391B (en) | Process for separating ethane nitrile wastewater with combination of abstraction and distillation | |
| CN102580338B (en) | Method for continuously rectifying 3-chloropropyl triethoxysilane | |
| CN103833551A (en) | Separation equipment and separation method of methyl methacrylate (MMA) | |
| CN103086822B (en) | A kind of separation method of m-pentadiene | |
| CN102583393A (en) | Double-heat-pump rectification device for trichlorosilane extraction and operation method | |
| CN106008186B (en) | A kind of separation method of isopropanol, acetone and water mixed solution | |
| CN101429211B (en) | Separation process for methyl mix monomer in organosilicon production | |
| CN110642828B (en) | Method for purifying vinylene carbonate kettle residues | |
| CN103788124B (en) | A kind of method of purification of electron level octamethylcy-clotetrasiloxane | |
| CN102807223B (en) | Method for refining trichlorosilane | |
| CN204017409U (en) | A kind of device of rectification and purification 3-NCO propyl-triethoxysilicane | |
| CN102321115A (en) | Purification method for electronic-grade dimethyl diethoxy silane | |
| CN105480981B (en) | The recovery method and device of a kind of dichlorosilane in tail gas in polycrystalline reduction production | |
| CN103588658B (en) | A kind of DMF recovery technology | |
| CN1974502A (en) | Method for producing beta-methylnaphthalene | |
| CN202499719U (en) | Dual-heat-pump rectifying device for purifying trichlorosilane | |
| CN108467042A (en) | The preparation method of electronic-grade polycrystalline silicon | |
| CN102616789A (en) | Heat pump rectification dividing wall tower device for separating ultrapure trichlorosilane and operation method | |
| CN102617627B (en) | Method for continuously separating silicon tetrachloride, propyl trichlorosilane and 3-chloropropyltrichlorosilane | |
| CN103288584B (en) | Reformed arene C 10the processing method of middle extraction high-purity beta-methylnaphthalene | |
| CN102424691A (en) | Purification method of electronic-grade methyl phenyl diethoxy silane | |
| CN103351276B (en) | Batch extractive distillation and separation method for ethanol-benzene azeotrope | |
| CN104262384B (en) | A kind of devices and methods therefor of rectification and purification 3-NCO propyl-triethoxysilicane | |
| CN104418734B (en) | From the industrial by-product of terephthalic acid (TPA), directly extract the method for high-purity methyl acetate | |
| CN115028656A (en) | Method and reaction system for continuously producing high-purity trimethylsilane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120118 |