CN109912636A - A kind of production method of high-purity ethyl orthosilicate - Google Patents
A kind of production method of high-purity ethyl orthosilicate Download PDFInfo
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Abstract
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising: S1) ethyl orthosilicate crude product is carried out to take off light rectifying, it obtains taking off the product after light rectifying；S2) by the product taken off after light rectifying after absorber is handled, the product that obtains that treated；Spherical activated charcoal, cation exchange resin and titania nanotube have been sequentially filled in the absorber；S3) by treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.Compared with prior art, for the present invention by handling before de- rectifying again through absorber, spherical activated charcoal is adsorbed and removed a certain number of metal ions as one section of adsorbent material, then through two sections of cation exchange resins, various metals ion and sodium ion exchange are removed, then material enters in three sections of titania nanotubes, is adsorbed and removed sodium ion, to overcome the weakness of continuous rectificating technique, this method is simple using equipment simultaneously, and low energy consumption, production process continuous-stable.
Description
Technical field
The invention belongs to technical field of semiconductors more particularly to a kind of production methods of high-purity ethyl orthosilicate.
Background technique
IC industry is one of new high-tech industry with the fastest developing speed at present, and the various chips of output are extensive
Applied to the ultra-pure electronic chemical product in industrial equipment and mechanical and electrical equipment used in daily life, to match therewith
Belong to the field of fine chemical in chemical industry, it is high skill that product purity is high, stay in grade is its technical characterstic the most typical
Art content, high investment, high added value new high-tech industry, will become chemical industry in it is with the fastest developing speed, most active
One of industry.
The ultra-pure electronic chemical product industrial development development in China is swift and violent, in recent years the year of ultra-pure electronic chemical product manufacturing industry
Equal growth rate has been more than 20%, and ultra-pure electronic chemical product is important one of the backing material of semiconductor IC industry,
The quality of quality will directly affect the quality of semiconductor integrated power chips.
Ethyl orthosilicate (TEOS) is mainly used for the integrated electricity of semiconductor as one kind important in ultra-pure electronic chemical product
TEOS is specially flashed to gaseous state from liquid first, then 700 DEG C~750 by the LPCVD technique in the chip manufacturing proces of road
DEG C, it is decomposed under 50Pa pressure and deposits generation silica membrane in silicon chip surface, the rate of silica membrane deposition can reach
To 50 à/min, the thickness uniformity of film is less than 3%, these excellent operational characteristiies and its showing in terms of safety in utilization
Work feature has gradually become the prevailing technology of cvd silicon dioxide film.
Realize that silica in the deposit on SiC wafer surface, can make up to a certain extent using TEOS LPCVD technology
SiC oxide layer is excessively thin and the excessively loose drawback of PECVD silicon dioxide layer.Using TEOS LPCVD technology and high-temperature oxydation technology
Reasonable utilization, not only ensure that the compactness of oxide layer medium and the adhesive capacity with SiC wafer, but also improve the electrical property of device
Energy and yield rate, while avoiding to obtain the deficiency of certain thickness oxide layer long-time high-temperature oxydation.
The minim metal doped of silica membrane will change its semiconducting behavior, just will affect the property of final chip
Energy.It therefore, be to the metal ion strict control in raw material TEOS in semiconductor integrated circuit production process.
The purifying process that metal ion in TEOS is removed both at home and abroad at present, mainly in the way of rectifying, and rectifying
Mode can effectively remove the biggish impurity composition of boiling point difference, and undesirable to metal ion removal effect.
Application No. is the Chinese patents of CN201310747619.4 to disclose a kind of preparation side of electron level ethyl orthosilicate
Method, this method first with after most of metal impurities in complexing agent complexing raw material, are filtered with 0.1 μm of millipore filter；Pass through sun
Ion exchange tower, quartzy plate tower, sub-boiling distillation device, strict temperature control remove trace metal impurities, ethyl alcohol and its have
Machine impurity and moisture content.But this method needs complexing agent, can introduce new impurity metal ion, and the system by way of sub-boiling distillation
Standby equipment difficulty of processing is big, high energy consumption and efficiency is low, so that the production cost increases for product, and is unable to continuous production.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is that provide a kind of production method of high-purity ethyl orthosilicate,
This method can effectively remove metal ion and can continuous production.
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising:
S1) ethyl orthosilicate crude product is carried out to take off light rectifying, obtains taking off the product after light rectifying；
S2) by the product taken off after light rectifying after absorber is handled, the product that obtains that treated；In the absorber
It has been sequentially filled spherical activated charcoal, cation exchange resin and titania nanotube；The spherical activated charcoal, cation exchange
The volume ratio of resin and titania nanotube is (0.5~2): (0.5~2): (0.5~2)；
S3) by treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.
Preferably, the step S1) in take off light rectifying temperature be 160 DEG C~190 DEG C；The reflux ratio for taking off light rectifying
It is 8~25.
Preferably, the cation exchange resin is gel-network precipitation method.
Preferably, the cation exchange resin is strongly acidic styrene type cation exchange resin, aperture 0.5~
Between 5nm.
Preferably, the volume ratio of the spherical activated charcoal, cation exchange resin and titania nanotube is 1:1:1.
Preferably, the temperature of the de- rectifying again is 160 DEG C~190 DEG C；The reflux ratio of the de- rectifying again is 8~25.
Preferably, the number of theoretical plate for taking off rectifying column used in light rectifying is 50~150.
Preferably, the number of theoretical plate of rectifying column used in the de- rectifying again is 50~150.
Preferably, the step S2) in take off the product after light rectifying flow velocity be 0.1~1m/s.
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising: S1) ethyl orthosilicate crude product is carried out
Light rectifying is taken off, obtains taking off the product after light rectifying；S2) product taken off after light rectifying is obtained everywhere after absorber is handled
Product after reason；Spherical activated charcoal, cation exchange resin and titania nanotube have been sequentially filled in the absorber；
S3) by treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.Compared with prior art, the present invention is logical
It crosses and is handled before de- rectifying again through absorber, spherical activated charcoal, cation exchange resin and titania nanotube in absorber
Three is arranged successively, and spherical activated charcoal is adsorbed and removed a certain number of metal ions as one section of adsorbent material, then material into
Enter in two sections of cation exchange resins, various metals ion and sodium ion exchange are removed, then material enters three sections of titanium dioxides
In titanium nanotube, sodium ion is adsorbed and removed in titania nanotube, to overcome the weakness of continuous rectificating technique, and first
Light rectifying is taken off, the load of absorber is alleviated, service life extends, while method provided by the invention is simple using equipment,
Low energy consumption, production process continuous-stable.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of high-purity ethyl orthosilicate production method provided by the invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
The present invention provides a kind of production methods of high-purity ethyl orthosilicate, comprising:
S1) ethyl orthosilicate crude product is carried out to take off light rectifying, obtains taking off the product after light rectifying；
S2) by the product taken off after light rectifying after absorber is handled, the product that obtains that treated；In the absorber
It has been sequentially filled spherical activated charcoal, cation exchange resin and titania nanotube；
S3) by treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.
Referring to Fig. 1, Fig. 1 is the flow diagram of high-purity ethyl orthosilicate production method provided by the invention.
The present invention has no special reality to the source of all raw materials, is commercially available.
The ethyl orthosilicate crude product is ethyl orthosilicate crude product well known to those skilled in the art, i.e., positive silicic acid second
Ester monomer, also known as ethyl orthosilicate -28, industrial goods content are generally 99.5%Wt.
Ethyl orthosilicate crude product is carried out to take off light rectifying, obtains taking off the product after light rectifying.It is described to take off light rectifying and preferably exist
It is carried out in de-light rectification column；It is preferably fed from the middle and upper part of de-light rectification column through ethyl orthosilicate crude product；The dehydrogenation rectifying
Temperature is preferably 160 DEG C~190 DEG C, more preferably 165 DEG C~180 DEG C；The pressure for taking off light rectifying preferably -0.1~
0.3bar, more preferably -0.05~0.2bar are further preferably 0~0.1bar, most preferably 0~0.05bar；The de- light essence
The temperature for evaporating condensation is preferably 120 DEG C~150 DEG C, and more preferably 120 DEG C~140 DEG C, be further preferably 120 DEG C~130 DEG C；It is described
The reflux ratio for taking off light rectifying is preferably 8~25, and more preferably 10~20, it is further preferably 15~19；It can be removed by taking off light rectifying
The light components such as ethyl alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane in ethyl orthosilicate；
The quality that light component is removed when taking off light rectifying is preferably the 1/5~1/12 of ethyl orthosilicate crude product quality, more preferably 1/8
~1/12.
By the product taken off after light rectifying after absorber is handled, the product that obtains that treated；In the absorber according to
It is secondary to be filled with spherical activated charcoal, cation exchange resin and titania nanotube；The partial size of the spherical activated charcoal is preferably 2
~5mm, more preferably 3~5mm；The cation exchange resin is preferably gel-network precipitation method, more preferably by force
Acid styrene type cation exchange resin；The aperture of the cation exchange resin is preferably 0.5~5nm, more preferably 1~
4nm；The direction of the product flowing of the spherical activated charcoal, cation exchange resin and titania nanotube after taking off light rectifying
It is arranged successively, the volume ratio of three is preferably (0.5~2): (0.5~2): (0.5~2), more preferably (0.5~1.5): (0.5
~1.5): (0.5~1.5) is further preferably 1:1:1；The spherical activated charcoal, cation exchange resin and titania nanotube
Layer height be each independently 0.5~3m, more preferably 1~2m.Flow velocity of the product taken off after light rectifying in absorber
Preferably 0.1~1m/s, more preferably 0.3~1m/s are further preferably 0.5~0.7m/s.
By treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.The de- rectifying again preferably exists
It is carried out in de- heavy distillation column；When de- rectifying again, through absorber, treated that product is preferably fed in the middle and lower part of de- heavy distillation column；
The temperature of the de- rectifying again is preferably 160 DEG C~190 DEG C, and more preferably 168 DEG C~180 DEG C, be further preferably 168 DEG C~170
℃；The pressure of the de- rectifying again is preferably -0.1~0.3bar, more preferably -0.05~0.2bar, further preferably for 0~
0.1bar, most preferably 0~0.05bar；The temperature of overhead condensation is preferably 120 DEG C~150 DEG C when the de- rectifying again, more excellent
120 DEG C~140 DEG C are selected as, is further preferably 123 DEG C~135 DEG C；The reflux ratio of de- rectifying again is preferably 8~25, and more preferably 10
~20, it is further preferably 13~18；Propyl-triethoxysilicane in ethyl orthosilicate, positive silicic acid second can be removed by de- rectifying again
The heavy constituents such as ester dimer, ethyl orthosilicate tripolymer, these heavy constituents may be recovered；When the de- rectifying again, removing weight
Preferably treated the 1/4~1/12 of product quality, more preferably 1/6~1/12 for the quality of component, is further preferably 1/9~1/
11；The ethyl orthosilicate that tower top obtains after de- rectifying again preferably also obtains high-purity ethyl orthosilicate after condensation, and component is pure
Degree may be up to 5N or more, and the indexs such as metal ion reach 9N.
The present invention before de- rectifying again through absorber by handling, spherical activated charcoal, cation exchange resin in absorber
Three is arranged successively with titania nanotube, and spherical activated charcoal is adsorbed and removed a certain number of gold as one section of adsorbent material
Belong to ion, then material enters in two sections of cation exchange resins, various metals ion and sodium ion exchange is removed, then object
Material enters in three sections of titania nanotubes, sodium ion is adsorbed and removed in titania nanotube, to overcome continuous fine
The weakness of technique is evaporated, and is first taken off light rectifying, alleviates the load of absorber, extends the service life of absorber, while this
The method that invention provides is simple using equipment, and low energy consumption, production process continuous-stable.
In order to further illustrate the present invention, with reference to embodiments to a kind of high-purity ethyl orthosilicate provided by the invention
Production method is described in detail.
Reagent used in following embodiment is commercially available.
Embodiment 1
Thick ethyl orthosilicate flow velocity be 0.7m/s from thick ethyl orthosilicate storage tank through feeding delivery pump, it is de- from ethyl orthosilicate
The middle and upper part of light rectifying column T01 tower is fed to it, and the temperature of rectifying is 180 DEG C；Pressure is 0.05bar；It is described when taking off light rectifying
The temperature of overhead condensation is 130 DEG C；Take off the reflux ratio 10 of light rectifying；By taking off the unreacted in light rectifying removing ethyl orthosilicate
The light components such as ethyl alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane；Remove light component
Quality is the 1/8 of ethyl orthosilicate crude product quality.
The product after light rectifying will be taken off to convey through ethyl orthosilicate de-light rectification column discharging pump with the flow velocity of 0.7m/s to inhaling
In adnexa, the direction that salt ethyl orthosilicate flows in the absorber has been sequentially filled spherical activated charcoal (granularity 3mm), highly acid
Styrene type cation exchange resin (aperture 4nm) and titania nanotube, the volume ratio of three are 1:1:1, three's
Layer height is 2m, the product after obtaining adsorption treatment.
Product after the adsorption treatment is entered into ethyl orthosilicate through delivery pump with the flow velocity of 0.7m/s and takes off heavy distillation column
The middle and lower part of T02, Jing Congta are fed, and the temperature of rectifying is 170 DEG C；Pressure is 0bar；The condensation temperature of tower top when de- rectifying again
It is 135 DEG C；The reflux ratio of de- rectifying again is 13；Remove propyl-triethoxysilicane, the ethyl orthosilicate two in ethyl orthosilicate
The heavy components such as aggressiveness, ethyl orthosilicate tripolymer remove the quality of heavy constituent as 1/9 of product quality after adsorption treatment；Tower top
It condenses to obtain high-purity ethyl orthosilicate through condenser, component purity may be up to 5N or more, and the indexs such as metal ion reach 9N.
The yield of high-purity ethyl orthosilicate is 76%.
It to ethyl orthosilicate crude product used in embodiment 1 and obtains high-purity ethyl orthosilicate and detects, obtain result
It is shown in Table 1 and table 2.
1 ethyl orthosilicate crude product testing result of table
The testing result of high-purity ethyl orthosilicate obtained in 2 embodiment 1 of table
Embodiment 2
Thick ethyl orthosilicate flow velocity be 0.5m/s from thick ethyl orthosilicate storage tank through feeding delivery pump, it is de- from ethyl orthosilicate
The middle and upper part of light rectifying column T01 tower is fed to it, and the temperature of rectifying is 165 DEG C；Pressure is 0bar；Tower top when taking off light rectifying
The temperature of condensation is 120 DEG C；Take off the reflux ratio 20 of light rectifying；By taking off the unreacted second in light rectifying removing ethyl orthosilicate
The light components such as alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane；Remove the quality of light component
It is the 1/12 of ethyl orthosilicate crude product quality.
The product after light rectifying will be taken off to convey through ethyl orthosilicate de-light rectification column discharging pump with the flow velocity of 0.5m/s to inhaling
In adnexa, the direction that salt ethyl orthosilicate flows in the absorber has been sequentially filled spherical activated charcoal (granularity 5mm), highly acid
Styrene type cation exchange resin (aperture 1nm) and titania nanotube, the volume ratio of three are 1:1:1, three's
Layer height is 1m, the product after obtaining adsorption treatment.
Product after the adsorption treatment is entered into ethyl orthosilicate through delivery pump with the flow velocity of 0.5m/s and takes off heavy distillation column
The middle and lower part of T02, Jing Congta are fed, and the temperature of rectifying is 168 DEG C；Pressure is 0bar；The condensation temperature of tower top when de- rectifying again
It is 123 DEG C；The reflux ratio of de- rectifying again is 18；Remove propyl-triethoxysilicane, the ethyl orthosilicate two in ethyl orthosilicate
The heavy components such as aggressiveness, ethyl orthosilicate tripolymer remove the quality of heavy constituent as 1/11 of product quality after adsorption treatment；Tower top
It condenses to obtain high-purity ethyl orthosilicate through condenser, component purity may be up to 5N or more, and the indexs such as metal ion reach 9N.
Comparative example 1
Thick ethyl orthosilicate flow velocity be 0.7m/s from thick ethyl orthosilicate storage tank through feeding delivery pump, it is de- from ethyl orthosilicate
The middle and upper part of light rectifying column T01 tower is fed to it, and the temperature of rectifying is 140 DEG C；Pressure is -0.5bar；It is described when taking off light rectifying
The temperature of overhead condensation is 100 DEG C；Take off the reflux ratio 6 of light rectifying；By taking off the unreacted in light rectifying removing ethyl orthosilicate
The light components such as ethyl alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane；Remove light component
Quality is the 1/4 of ethyl orthosilicate crude product quality.
The product after light rectifying will be taken off to convey through ethyl orthosilicate de-light rectification column discharging pump with the flow velocity of 0.7m/s to inhaling
In adnexa, the direction that salt ethyl orthosilicate flows in the absorber has been sequentially filled strongly acidic styrene's cation exchange tree
The volume ratio of rouge (aperture 3nm) and titania nanotube, the two is 1:1, and the layer height of the two is 2m, obtains adsorption treatment
Product afterwards.
Product after the adsorption treatment is entered into ethyl orthosilicate through delivery pump with the flow velocity of 0.7m/s and takes off heavy distillation column
The middle and lower part of T02, Jing Congta are fed, and the temperature of rectifying is 120 DEG C；Pressure is -0.8bar；The condensation temperature of tower top when de- rectifying again
Degree is 80 DEG C；The reflux ratio of de- rectifying again is 7；Remove propyl-triethoxysilicane, the ethyl orthosilicate two in ethyl orthosilicate
The heavy components such as aggressiveness, ethyl orthosilicate tripolymer remove the quality of heavy constituent as 1/5 of product quality after adsorption treatment；Tower top
Ethyl orthosilicate after condenser condenses to obtain de- rectifying again.
Ethyl orthosilicate after de- rectifying again obtained in comparative example 1 is detected, obtaining result see the table below.
The testing result of the ethyl orthosilicate after rectifying again is taken off obtained in comparative example 1
Comparative example 2
Thick ethyl orthosilicate flow velocity be 1.3m/s from thick ethyl orthosilicate storage tank through feeding delivery pump, it is de- from ethyl orthosilicate
The middle and upper part of light rectifying column T01 tower is fed to it, and the temperature of rectifying is 195 DEG C；Pressure is 0.3bar；Tower when taking off light rectifying
The temperature of top condensation is 140 DEG C；Take off the reflux ratio 13 of light rectifying；It is unreacted in light rectifying removing ethyl orthosilicate by taking off
The light components such as ethyl alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane；Remove the matter of light component
Amount is the 1/9 of ethyl orthosilicate crude product quality.
The product after light rectifying will be taken off to convey through ethyl orthosilicate de-light rectification column discharging pump with the flow velocity of 1.3m/s to inhaling
In adnexa, the direction that salt ethyl orthosilicate flows in the absorber has been sequentially filled spherical activated charcoal (granularity 4mm) and dioxy
Change titanium nanotube, the volume ratio of the two is 1:1, and the layer height of the two is 2m, the product after obtaining adsorption treatment.
Product after the adsorption treatment is entered into ethyl orthosilicate through delivery pump with the flow velocity of 1.3m/s and takes off heavy distillation column
The middle and lower part of T02, Jing Congta are fed, and the temperature of rectifying is 190 DEG C；Pressure is 0.3bar；The condensation temperature of tower top when de- rectifying again
Degree is 135 DEG C；The reflux ratio of de- rectifying again is 15；Remove propyl-triethoxysilicane, the ethyl orthosilicate in ethyl orthosilicate
The heavy components such as dimer, ethyl orthosilicate tripolymer remove the quality of heavy constituent as 1/10 of product quality after adsorption treatment；Tower
Push up the ethyl orthosilicate after condenser condenses to obtain de- rectifying again.
Ethyl orthosilicate after de- rectifying again obtained in comparative example 2 is detected, obtaining result see the table below.
The testing result of the ethyl orthosilicate after rectifying again is taken off obtained in comparative example 2
Comparative example 3
Thick ethyl orthosilicate flow velocity be 1m/s from thick ethyl orthosilicate storage tank through feeding delivery pump, it is de- light from ethyl orthosilicate
The middle and upper part of rectifying column T01 tower is fed to it, and the temperature of rectifying is 178 DEG C；Pressure is 0.1bar；Tower top when taking off light rectifying
The temperature of condensation is 110 DEG C；Take off the reflux ratio 17 of light rectifying；By taking off the unreacted second in light rectifying removing ethyl orthosilicate
The light components such as alcohol, triethoxysilane, methyltriethoxysilane, methoxyl group triethoxysilane；Remove the quality of light component
It is the 1/13 of ethyl orthosilicate crude product quality.
The product after light rectifying will be taken off to convey through ethyl orthosilicate de-light rectification column discharging pump with the flow velocity of 1m/s to adsorbing
In device, the direction that salt ethyl orthosilicate flows in the absorber has been sequentially filled spherical activated charcoal (granularity 2mm) and highly acid
The volume ratio of styrene type cation exchange resin (aperture 0.5nm), the two is 1:1, and the layer height of the two is 1.3, is obtained
Product after adsorption treatment.
Product after the adsorption treatment is entered into ethyl orthosilicate through delivery pump with the flow velocity of 1m/s and takes off heavy distillation column
The middle and lower part of T02, Jing Congta are fed, and the temperature of rectifying is 172 DEG C；Pressure is 0bar；The condensation temperature of tower top when de- rectifying again
It is 120 DEG C；The reflux ratio of de- rectifying again is 13；Remove propyl-triethoxysilicane, the ethyl orthosilicate two in ethyl orthosilicate
The heavy components such as aggressiveness, ethyl orthosilicate tripolymer remove the quality of heavy constituent as 1/15 of product quality after adsorption treatment；Tower top
Ethyl orthosilicate after condenser condenses to obtain de- rectifying again.
Ethyl orthosilicate after de- rectifying again obtained in comparative example 3 is detected, obtaining result see the table below.
The testing result of the ethyl orthosilicate after rectifying again is taken off obtained in comparative example 3
Claims (9)
1. a kind of production method of high-purity ethyl orthosilicate characterized by comprising
S1) ethyl orthosilicate crude product is carried out to take off light rectifying, obtains taking off the product after light rectifying；
S2) by the product taken off after light rectifying after absorber is handled, the product that obtains that treated；In the absorber successively
Filled with spherical activated charcoal, cation exchange resin and titania nanotube；The spherical activated charcoal, cation exchange resin
Volume ratio with titania nanotube is (0.5~2): (0.5~2): (0.5~2)；
S3) by treated product the carries out de- rectifying again, high-purity ethyl orthosilicate is obtained.
2. production method according to claim 1, which is characterized in that the step S1) in take off light rectifying temperature be 160
DEG C~190 DEG C；The reflux ratio for taking off light rectifying is 8~25.
3. production method according to claim 1, which is characterized in that the cation exchange resin is gel type cation
Exchanger resin.
4. production method according to claim 1, which is characterized in that the cation exchange resin is strongly acidic styrene
Cation exchanger resin, aperture is between 0.5~5nm.
5. production method according to claim 1, which is characterized in that the spherical activated charcoal, cation exchange resin with
The volume ratio of titania nanotube is 1:1:1.
6. production method according to claim 1, which is characterized in that the temperature of the de- rectifying again is 160 DEG C~190
℃；The reflux ratio of the de- rectifying again is 8~25.
7. production method according to claim 1, which is characterized in that the theoretical plate for taking off rectifying column used in light rectifying
Number is 50~150.
8. production method according to claim 1, which is characterized in that the theoretical plate of rectifying column used in the de- rectifying again
Number is 50~150.
9. production method according to claim 1, which is characterized in that the step S2) in take off the product after light rectifying
Flow velocity is 0.1~1m/s.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022247166A1 (en) * | 2021-05-26 | 2022-12-01 | 苏州金宏气体股份有限公司 | Purification method and purification system for electronic grade tetraethyl orthosilicate |
| CN116903653A (en) * | 2023-07-11 | 2023-10-20 | 大连恒坤新材料有限公司 | Preparation method and production system of high-purity ethyl silicate |
| CN116903653B (en) * | 2023-07-11 | 2024-05-24 | 大连恒坤新材料有限公司 | Preparation method and production system of high-purity ethyl silicate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080287700A1 (en) * | 2004-06-16 | 2008-11-20 | Kamel Ramdani | Method for Preparing an Omega-Haloalkyl Dialkylhalosilane |
| CN104558015A (en) * | 2015-01-22 | 2015-04-29 | 中国科学院上海有机化学研究所 | Preparation method of high-purity organosilicone monomer |
| CN109400637A (en) * | 2018-09-29 | 2019-03-01 | 苏州金宏气体股份有限公司 | A kind of production method and production system of high-purity ethyl orthosilicate |
| CN208617730U (en) * | 2018-09-29 | 2019-03-19 | 苏州金宏气体股份有限公司 | A kind of production system of high-purity ethyl orthosilicate |
| CN208617729U (en) * | 2018-09-29 | 2019-03-19 | 苏州金宏气体股份有限公司 | A kind of production system of high-purity ethyl orthosilicate |
-
2019
- 2019-04-11 CN CN201910289723.0A patent/CN109912636B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080287700A1 (en) * | 2004-06-16 | 2008-11-20 | Kamel Ramdani | Method for Preparing an Omega-Haloalkyl Dialkylhalosilane |
| CN104558015A (en) * | 2015-01-22 | 2015-04-29 | 中国科学院上海有机化学研究所 | Preparation method of high-purity organosilicone monomer |
| CN109400637A (en) * | 2018-09-29 | 2019-03-01 | 苏州金宏气体股份有限公司 | A kind of production method and production system of high-purity ethyl orthosilicate |
| CN208617730U (en) * | 2018-09-29 | 2019-03-19 | 苏州金宏气体股份有限公司 | A kind of production system of high-purity ethyl orthosilicate |
| CN208617729U (en) * | 2018-09-29 | 2019-03-19 | 苏州金宏气体股份有限公司 | A kind of production system of high-purity ethyl orthosilicate |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022247166A1 (en) * | 2021-05-26 | 2022-12-01 | 苏州金宏气体股份有限公司 | Purification method and purification system for electronic grade tetraethyl orthosilicate |
| CN116903653A (en) * | 2023-07-11 | 2023-10-20 | 大连恒坤新材料有限公司 | Preparation method and production system of high-purity ethyl silicate |
| CN116903653B (en) * | 2023-07-11 | 2024-05-24 | 大连恒坤新材料有限公司 | Preparation method and production system of high-purity ethyl silicate |
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