CN113292588A - Purification method and purification system of electronic grade ethyl orthosilicate - Google Patents
Purification method and purification system of electronic grade ethyl orthosilicate Download PDFInfo
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- CN113292588A CN113292588A CN202110577902.1A CN202110577902A CN113292588A CN 113292588 A CN113292588 A CN 113292588A CN 202110577902 A CN202110577902 A CN 202110577902A CN 113292588 A CN113292588 A CN 113292588A
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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 74
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000000746 purification Methods 0.000 title claims abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000012535 impurity Substances 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims description 45
- 238000011084 recovery Methods 0.000 claims description 36
- 238000010992 reflux Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 10
- 238000004891 communication Methods 0.000 claims description 6
- 238000009835 boiling Methods 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000005049 silicon tetrachloride Substances 0.000 abstract description 3
- QYBKVVRRGQSGDC-UHFFFAOYSA-N triethyl methyl silicate Chemical compound CCO[Si](OC)(OCC)OCC QYBKVVRRGQSGDC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 239000007788 liquid Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000000623 plasma-assisted chemical vapour deposition Methods 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 239000008234 soft water Substances 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/04—Esters of silicic acids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a purification method and a purification system of electronic grade ethyl orthosilicate, which comprises the following steps: s100) filling nitrogen; s200) carrying out adsorption operation on the crude tetraethoxysilane to obtain a product with the impurities removed preliminarily; s300) carrying out multi-tower continuous rectification on the product with the impurities removed primarily to obtain electronic grade ethyl orthosilicate; the invention adopts an adsorption column and a multi-tower continuous rectification process to separate component impurities such as silicon tetrachloride, ethanol, diethyl ether, methoxy triethoxy silicon and the like and remove various metal impurities to obtain an electronic grade tetraethoxysilane product; in the method, the adsorption column is arranged at the front section of the rectifying tower, so that part of metal ions can be removed, the separation load of the rectifying tower is greatly reduced, and the complexity of the system is reduced.
Description
Technical Field
The invention relates to the technical field of semiconductors, in particular to a method and a system for purifying electronic-grade ethyl orthosilicate.
Background
The method for forming an oxide layer in a semiconductor process mainly includes thermal oxidation (for a semiconductor material capable of forming a self-stabilizing oxide layer), Low Pressure Chemical Vapor Deposition (LPCVD), Plasma Enhanced Chemical Vapor Deposition (PECVD), and Atmospheric Pressure Chemical Vapor Deposition (APCVD), wherein, due to the large gas flow rate required by APCVD and the relatively large amount of particles generated by the process, most of the semiconductor processes are rarely used at present.
When Tetraethoxysilane (TEOS) is used for LPCVD, TEOS is evaporated from a liquid state to a gas state, the TEOS is decomposed at 700-750 ℃ and 300mTOR pressure and is deposited on the surface of a silicon wafer to form a silicon dioxide film, the deposition rate of the silicon dioxide film can reach 50 a/min, the thickness uniformity of the film is less than 3%, and the excellent process characteristics and the obvious characteristics of the film in the aspect of use safety gradually become a mainstream process for depositing the silicon dioxide film.
The deposition of silicon dioxide on the surface of the SiC wafer is realized by applying the tetraethyl orthosilicate (TEOS) LPCVD technology, and the defects that the SiC oxide layer is too thin and the PECVD silicon dioxide layer is too loose can be overcome to a certain extent. By adopting the reasonable application of the TEOSLPCVD technology and the high-temperature oxidation technology, the compactness of an oxide layer medium and the adhesive capacity with a SiC wafer are ensured, the electrical property and the yield of a device are improved, and the defect of long-time high-temperature oxidation of the oxide layer with a certain thickness is avoided. After the technology is adopted, the direct current yield of the SiC chip is improved, the comparative slide result of the microwave power device shows that the microwave performance is also obviously improved, the power gain is improved by about 1.5dB compared with the original technology, and the power additional efficiency is improved by nearly 10%.
However, the existing purification method of electronic grade ethyl orthosilicate has overlarge energy consumption and high production cost of products, and continuous production cannot be realized.
Disclosure of Invention
The invention aims to provide a method and a system for purifying electronic grade ethyl orthosilicate.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: a method for purifying electronic grade ethyl orthosilicate comprises the following steps:
s100) filling nitrogen;
s200) carrying out adsorption operation on the crude tetraethoxysilane to obtain a product with the impurities removed preliminarily;
s300) carrying out multi-tower continuous rectification on the product with the impurities removed primarily to obtain the electronic grade ethyl orthosilicate.
Preferably, the nitrogen filling in step S100) is performed by opening a communication valve inside the system, closing a communication valve connecting the system and the outside, performing nitrogen filling and pressure relief operations in the system, and repeating the operations at least three times.
Preferably, the adsorption operation in step S200) is specifically that the crude tetraethoxysilane is pumped and then enters an adsorption column to remove a part of metal ions, so as to obtain a product with the impurities primarily removed.
Preferably, the multi-tower continuous rectification process in the step S300) is specifically,
s310) carrying out primary rectification on the product with the impurities removed preliminarily to obtain TEOS containing low-boiling-point substances and a first rectification substance;
s320) carrying out secondary rectification on the first rectification substance to obtain TEOS containing a high-boiling-point substance and a second rectification substance;
s330) carrying out third rectification on the second rectification substance to obtain TEOS containing low-boiling-point substances and a third rectification substance;
s340) carrying out fourth rectification on the third rectification product to obtain TEOS containing high-boiling-point substances and electronic-grade ethyl orthosilicate.
Preferably, the tower top temperature of the second rectification, the third rectification and the fourth rectification is higher than that of the first rectification.
Preferably, the reflux ratio of the first rectification to the second rectification is 1: 1.5-2; the reflux ratio of the third rectification to the fourth rectification is 1: 1.5-2.
The invention also claims a purification system of electronic grade ethyl orthosilicate, which comprises,
the raw material tank is used for storing and outputting tetraethoxysilane;
the adsorption column is communicated with the discharge end of the raw material tank;
the first rectifying tower is communicated with the discharge end of the adsorption column;
the second rectifying tower is communicated with the tower bottom of the first rectifying tower;
the third rectifying tower is communicated with the tower top of the second rectifying tower;
and the fourth rectifying tower is communicated with the tower bottom of the second rectifying tower.
Preferably, the device also comprises a first recovery tank, wherein the feed end of the first recovery tank is connected with the top of the first rectifying tower and the bottom of the second rectifying tower; and the feed end of the second recovery tank is connected with the tower top of the third rectifying tower and the tower bottom of the fourth rectifying tower.
Preferably, the device also comprises a low-boiling-point substance recovery tank, and the feeding end of the low-boiling-point substance recovery tank is connected with the top of the first rectifying tower and the top of the third rectifying tower; and the feed end of the high-boiling-point substance recovery tank is connected with the tower bottom of the second rectifying tower and the tower bottom of the fourth rectifying tower.
Preferably, the discharge end of the second recovery tank is connected with the raw material tank.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the purification method adopts an adsorption column and a multi-tower continuous rectification process to separate component impurities such as silicon tetrachloride, ethanol, ether, methoxy triethoxy silicon and the like and remove various metal impurities to obtain an electronic grade ethyl orthosilicate product; in the method, the adsorption column is arranged at the front section of the rectifying tower, so that part of metal ions can be removed, the separation load of the rectifying tower is greatly reduced, and the complexity of the system is reduced;
2. the method can be used together with other systems, fully ensures that the product purity meets the production requirement of high-quality electronic grade ethyl orthosilicate, and can also meet the production requirement of industrial grade ethyl orthosilicate;
3. the four rectifying towers are arranged for switching use, so that high-purity TEOS product cache can be provided for subsequent filling, and each batch of high-purity TEOS products can be conveniently detected; the production method is easy to operate, high in automation degree, capable of carrying out continuous production, high in working efficiency and high in quality of obtained products.
4. The method is simple and easy to implement, has low cost and is suitable for popularization and application.
Drawings
FIG. 1 is a schematic flow chart of example 3 of the present invention;
FIG. 2 is a schematic structural view of embodiment 1 of the present invention;
fig. 3 is a schematic structural diagram of embodiment 2 of the present invention.
Detailed Description
The invention is further described with reference to the following figures and examples:
example 1
Referring to fig. 1, an electronic grade system for purifying tetraethoxysilane comprises a raw material tank for storing and outputting tetraethoxysilane; the adsorption column is communicated with the discharge end of the raw material tank; the first rectifying tower is communicated with the discharge end of the adsorption column; the second rectifying tower is communicated with the tower bottom of the first rectifying tower; the third rectifying tower is communicated with the tower top of the second rectifying tower; and the fourth rectifying tower is communicated with the tower bottom of the second rectifying tower.
The feed end of the first recovery tank is connected with the top of the first rectifying tower and the bottom of the second rectifying tower; a feed end of the second recovery tank is connected with the tower top of the third rectifying tower and the tower bottom of the fourth rectifying tower; the discharge end of the second recovery tank is connected with the raw material tank and is also used for producing electronic-grade ethyl orthosilicate, and the first recovery tank can be used for producing industrial-grade ethyl orthosilicate.
Example 2
This embodiment is performed based on embodiment 1, and the same parts as those in the above embodiment are not repeated.
Referring to fig. 2, the first recovery tank and the second recovery tank are replaced by a low-boiling-point substance recovery tank and a high-boiling-point substance recovery tank; the feed end of the low-boiling-point substance recovery tank is connected with the top of the first rectifying tower and the top of the third rectifying tower; the feed end of the high-boiling-point substance recovery tank is connected with the tower bottom of the second rectifying tower and the tower bottom of the fourth rectifying tower; the low-boiling-point substance recovery tank and the high-boiling-point substance recovery tank are respectively connected with a spray guiding system; part of tetraethoxysilane, water vapor, ethanol, ether and the like are recycled in the low-boiling-point substance recycling tank; part of tetraethoxysilane, high silicon tetrachloride, methoxy triethoxy silicon, metal ions and the like are recovered in the high-boiling-point substance recovery tank.
Example 3
This example mainly introduces a method for purifying electronic grade ethyl orthosilicate, which comprises the following steps:
s100) filling nitrogen;
the nitrogen filling in the step S100) is specifically performed by opening a communication valve inside the system, closing a communication valve connecting the system and the outside, performing nitrogen filling and pressure relief operations in the system, and repeating the operations at least three times;
more specifically, the temperature and pressure of a heating medium, the pressure of circulating soft water, the flow rate, the pressure of nitrogen, the pressure of an instrument, the input condition of a tail gas environment-friendly treatment device, pipeline inspection and the like are firstly inspected, and all pneumatic valves in the system are determined to be debugged normally and consistent with the display of a computer; and opening a communicating valve in the system, closing the communicating valve connected with the system and the outside, filling nitrogen to 0.08MPa, controlling each valve in the system to release pressure to micro positive pressure after maintaining for 3 minutes, repeating the steps for three times, and finishing the operation after checking that the content of the nitrogen meets the requirement.
S200) carrying out adsorption operation on the crude tetraethoxysilane to obtain a product with the impurities removed preliminarily;
the adsorption operation in the step S200) is specifically that the crude tetraethoxysilane is pressurized by a pump and then enters an adsorption column to remove part of metal ions, so that a product with the impurities removed primarily is obtained;
more specifically, the internal filling of the adsorbent is completed for two adsorption columns, the two adsorption columns are switched to be used, and the adsorption operation is performed on the crude tetraethoxysilane, so that part of impurities such as boron, metal and the like in the crude tetraethoxysilane can be removed, and a product with the impurities removed primarily is obtained;
the operation pressure of the adsorption column is 500-650kPa, and the adsorption temperature is 20-80 ℃; the preferred operating pressure is 580-610kPa, and the adsorption temperature is 25-40 ℃; more preferably, the operation pressure is 590-600kPa, and the adsorption temperature is 28-35 ℃.
S300) carrying out multi-tower continuous rectification on the product with the impurities removed primarily to obtain electronic grade ethyl orthosilicate; wherein the operating pressure of each rectifying tower is preferably 1-150kPa (a) independently, more preferably 100 kPa (a) independently, and most preferably 110kPa (a);
wherein the multi-tower continuous rectification process in the step S300) is specifically,
s310) carrying out primary rectification on the product with the impurities removed preliminarily to obtain TEOS containing low-boiling-point substances and a first rectification substance; the tower top temperature of the first rectifying tower is preferably 120-140 ℃, and the tower bottom temperature of the first rectifying tower is preferably 170-175 ℃;
s320) carrying out secondary rectification on the first rectification substance to obtain TEOS containing a high-boiling-point substance and a second rectification substance; the tower top temperature and the tower bottom temperature of the second rectifying tower are respectively independent, preferably 170-175 ℃;
s330) carrying out third rectification on the second rectification substance to obtain TEOS containing low-boiling-point substances and a third rectification substance; the tower top temperature and the tower bottom temperature of the third rectifying tower are respectively independent, preferably 170-175 ℃;
s340) carrying out fourth rectification on the third rectification product to obtain TEOS containing high-boiling-point substances and electronic-grade ethyl orthosilicate; the tower top temperature and the tower bottom temperature of the fourth rectifying tower are respectively independent, preferably 170-175 ℃;
more specifically, step S310) includes,
s311) opening a feeding valve of the first rectifying tower, and feeding into the tower; stopping feeding the rectifying tower when the liquid level in the tower kettle is higher than 90%;
s312) starting a reboiler for preheating;
s313) heating the first rectifying tower with the opening of the steam regulating valve increased;
s314) adjusting the reflux tank to full reflux operation, maintaining the liquid level of the tower kettle at 70 percent, and the reflux amount reaches 0.7m3The heat-conducting oil amount is about 10.6 t/h; the stable total reflux operation is kept for more than 8 hours in the state.
S315) finishing reflux operation, wherein materials extracted from the tower top enter a first recovery tank or a low-boiling-point substance recovery tank, materials extracted from the tower bottom enter a second rectifying tower to open the second rectifying tower for padding,
the liquid level of the reflux tank is gradually increased, which proves that the protective gas N2 in the tower is basically exhausted, the tower kettle of the first rectifying tower is continuously heated, and tail gas is not frequently exhausted any more; in the adjusting process, if the liquid level of the tower bottom of the first rectifying tower is reduced to 30 percent, the feeding is recovered,maintaining the liquid level of the tower kettle at 70%; when the liquid level of the reflux tank reaches 50%, a reflux pump is started, a reflux control valve is manually adjusted, the reflux temperature is controlled at a set value by adjusting a circulating soft water adjusting valve of the condenser, and the heating quantity of the reboiler is adjusted simultaneously, so that the upper liquid level and the lower liquid level are kept stable, the feeding valve is closed, and feeding is stopped. Adjusting the operation to full reflux with reflux amount of 0.7m3The quantity of the heat transfer oil is about 10.6 t/h.
Step S320) and step S310) are performed under the same standard, and the same parts are not described again, except that the reflux amount reaches 1.2m3The heat transfer oil amount is about 17.2 t/h; wherein the material extracted from the tower top enters a third rectifying tower to perform padding for the opening of the third rectifying tower, and the material extracted from the tower kettle enters a first recovery tank or a high-boiling residue recovery tank;
step S330) and step S310) are carried out under the same standard, and the description of the same parts is omitted, except that the reflux amount reaches 0.7m3The heat-conducting oil amount is about 9.5 t/h; wherein the material extracted from the tower top enters a second recovery tank or a low-boiling-point substance recovery tank, and the material extracted from the tower bottom enters a fourth rectifying tower to open the tower for padding;
step S340) and step S310) are carried out under the same standard, and the same parts are not described again, except that the reflux amount reaches 1.2m3The quantity of the heat-conducting oil is about 16.8 t/h; wherein the material extracted from the tower top is electronic grade ethyl orthosilicate and is sent to an intermediate product tank, and the material extracted from the tower bottom enters a second recovery tank or a high-boiling-point substance recovery tank.
On the basis of embodiment 1, the method for purifying electronic grade tetraethoxysilane further comprises the following steps: s400) connecting the liquid outlet end of the second recovery tank with the feed end of the raw material tank.
On the basis of embodiment 2, the method for purifying electronic grade tetraethoxysilane further comprises the following steps: s400) conducting and sprinkling operation is respectively carried out on the low-boiling-point substance recovery tank and the high-boiling-point substance recovery tank.
Example 4
The purification operation was carried out on crude tetraethoxysilane by the purification method of example 3, and the process conditions and results are shown in Table 1.
Table 1 shows the process conditions and purification results of electronic grade ethyl orthosilicate
| Tower name | C01A/B | T01 | T02 | T03 | T04 | |
| Operating pressure | kPa(a) | 590 | 110 | 110 | 110 | 110 |
| Temperature at the top of the column | ℃ | 30 | 135.7 | 170.9 | 170.9 | 170.9 |
| Temperature of the column bottom | ℃ | 30 | 172.7 | 172.8 | 172.6 | 172.6 |
| Amount of feed | kg/h | 180 | 180 | 160 | 145 | 135 |
| Overhead withdrawal | kg/h | — | 20 | 145 | 10 | 125 |
| Tower bottom extraction | kg/h | — | 160 | 15 | 135 | 10 |
| Amount of reflux | kg/h | — | 580 | 1000 | 580 | 1000 |
Example 5
The fuel power consumption estimation required for the purification process of example 3 is shown in table 2.
TABLE 2 is the energy consumption (equivalent value) conversion statistical table
The project energy consumption structure mainly takes electric power as a main part, accords with the local energy supply condition, and is reasonable; the adsorption column is arranged at the front section of the rectifying tower, so that part of metal ions can be removed, the separation load of the rectifying tower is greatly reduced, and the energy consumption is reduced.
Example 6
The electronic grade ethyl orthosilicate obtained in example 3 was examined, and the results are shown in table 3.
Table 3 shows the detection results of electronic grade ethyl orthosilicate in example 3
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to the above-described embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for purifying electronic grade ethyl orthosilicate is characterized by comprising the following steps:
s100) filling nitrogen;
s200) carrying out adsorption operation on the crude tetraethoxysilane to obtain a product with the impurities removed preliminarily;
s300) carrying out multi-tower continuous rectification on the product with the impurities removed primarily to obtain the electronic grade ethyl orthosilicate.
2. The method for purifying electronic grade tetraethoxysilane as claimed in claim 1, wherein:
the nitrogen filling in the step S100) is specifically performed by opening a communication valve inside the system, closing a communication valve connecting the system and the outside, performing nitrogen filling and pressure relief operations in the system, and repeating the operations at least three times.
3. The method for purifying electronic grade tetraethoxysilane as claimed in claim 1, wherein: the adsorption operation in the step S200) is specifically that the crude tetraethoxysilane is pressurized by a pump and then enters an adsorption column to remove a part of metal ions, so as to obtain a product with the impurities primarily removed.
4. The method for purifying electronic grade tetraethoxysilane as claimed in claim 1, wherein: the multi-tower continuous rectification process in the step S300) is specifically,
s310) carrying out primary rectification on the product with the impurities removed preliminarily to obtain TEOS containing low-boiling-point substances and a first rectification substance;
s320) carrying out secondary rectification on the first rectification substance to obtain TEOS containing a high-boiling-point substance and a second rectification substance;
s330) carrying out third rectification on the second rectification substance to obtain TEOS containing low-boiling-point substances and a third rectification substance;
s340) carrying out fourth rectification on the third rectification product to obtain TEOS containing high-boiling-point substances and electronic-grade ethyl orthosilicate.
5. The method for purifying electronic grade tetraethoxysilane as claimed in claim 4, wherein: the tower top temperature of the second rectification, the third rectification and the fourth rectification is higher than that of the first rectification.
6. The method for purifying electronic grade tetraethoxysilane as claimed in claim 4, wherein: the reflux ratio of the first rectification to the second rectification is 1: 1.5-2; the reflux ratio of the third rectification to the fourth rectification is 1: 1.5-2.
7. A purification system of electronic grade ethyl orthosilicate is characterized by comprising,
the raw material tank is used for storing and outputting tetraethoxysilane;
the adsorption column is communicated with the discharge end of the raw material tank;
the first rectifying tower is communicated with the discharge end of the adsorption column;
the second rectifying tower is communicated with the tower bottom of the first rectifying tower;
the third rectifying tower is communicated with the tower top of the second rectifying tower;
and the fourth rectifying tower is communicated with the tower bottom of the second rectifying tower.
8. The system for purifying electronic grade tetraethoxysilane as claimed in claim 7, further comprising a first recovery tank, a feed end of which is connected with the top of the first rectifying tower and the bottom of the second rectifying tower; and the feed end of the second recovery tank is connected with the tower top of the third rectifying tower and the tower bottom of the fourth rectifying tower.
9. The purification system of electronic grade tetraethoxysilane, as recited in claim 7, further comprising a low-boiling substance recovery tank, a feed end of which is connected to the top of the first rectification column and the top of the third rectification column; and the feed end of the high-boiling-point substance recovery tank is connected with the tower bottom of the second rectifying tower and the tower bottom of the fourth rectifying tower.
10. The system for purifying electronic-grade tetraethoxysilane as claimed in claim 8, wherein a discharge end of said second recovery tank is connected with said raw material tank.
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| PCT/CN2021/131413 WO2022247166A1 (en) | 2021-05-26 | 2021-11-18 | Purification method and purification system for electronic grade tetraethyl orthosilicate |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114920767A (en) * | 2022-05-26 | 2022-08-19 | 苏州金宏气体股份有限公司 | Production system and process of high-purity ethyl orthosilicate |
| 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 |
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| WO2022247166A1 (en) | 2022-12-01 |
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