CN109438495B - Production method and production system of high-purity ethyl silicate - Google Patents
Production method and production system of high-purity ethyl silicate Download PDFInfo
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Abstract
The invention provides a production method of high-purity ethyl silicate, which comprises the following steps: s1) adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed; s2) treating the ethyl orthosilicate adsorbing the water by a metal ion modified material to obtain treated ethyl orthosilicate; and S3) distilling the treated ethyl orthosilicate to obtain high-purity ethyl silicate. Compared with the prior art, the method has the advantages that after the tetraethoxysilane with water removed is treated by the metal ion modified material, phosphorus-containing and/or boron-containing light-component substances in the tetraethoxysilane are converted into heavy-component compounds, and the heavy-component compounds are distilled and condensed to obtain the high-purity tetraethoxysilane.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a production method and a production system of high-purity ethyl silicate.
Background
Methods for forming oxide layers in semiconductor processes mainly include thermal oxidation (for semiconductor materials capable of forming self-stabilizing oxide layers), low Pressure Chemical Vapor Deposition (LPCVD), plasma Enhanced Chemical Vapor Deposition (PECVD), and Atmospheric Pressure Chemical Vapor Deposition (APCVD), among which most semiconductor processes are currently rarely used due to the large gas flow required by APCVD and relatively large number of process generation particles.
When tetraethyl orthosilicate (TEOS) is used for LPCVD, TEOS is evaporated from a liquid state to a gaseous state, and is decomposed at 700-750 ℃ under 300mTOR pressure to deposit a silicon dioxide film on the surface of a silicon wafer, the deposition rate of the silicon dioxide film can reach 50A/min, the thickness uniformity of the film is less than 3%, and the excellent process characteristics and the obvious characteristics thereof in the aspect of use safety gradually become the main process for depositing the silicon dioxide film.
The silicon dioxide is deposited on the surface of the SiC wafer by using the tetraethyl orthosilicate (TEOS) LPCVD technology, so that the defects of too thin SiC oxide layer and too loose PECVD silicon dioxide layer can be overcome to a certain extent. By reasonably applying the TEOS LPCVD technology and the high-temperature oxidation technology, the compactness of an oxide layer medium and the adhesion capability with a SiC wafer are ensured, the electrical performance and the yield of the device are improved, and the defect of long-time high-temperature oxidation for obtaining an oxide layer with a certain thickness is avoided. After the technology is adopted, the direct current yield of the SiC chip is improved, the comparison flow sheet 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 addition efficiency is improved by about 10%.
The Chinese patent with publication No. CN201310747619.4 discloses a preparation method of electronic grade ethyl orthosilicate, which comprises the steps of complexing most metal impurities in raw materials with complexing agents, filtering with a microporous filter of 0.1 micron, sequentially passing through a cation exchange tower, a quartz plate type distillation tower and a sub-boiling distiller, strictly controlling the temperature, removing trace metal impurities, ethanol and other organic impurities and moisture, wherein the complexing agents are easy to introduce new metal ion impurities, and the method of sub-boiling distillation has the advantages of high processing difficulty, high energy consumption and low efficiency, so that the production cost of products is increased, and continuous production is not realized.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a production method and a production system for high purity ethyl silicate which can be continuously produced and has low cost.
The invention provides a production method of high-purity ethyl silicate, which comprises the following steps:
s1) adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed;
s2) treating the water-removed ethyl orthosilicate with a metal ion modified material to obtain treated ethyl orthosilicate;
and S3) distilling the treated ethyl orthosilicate to obtain high-purity ethyl silicate.
Preferably, the moisture adsorbent is selected from 3A molecular sieves.
Preferably, the metal ion modified material is selected from noble metal-loaded modified silica-alumina gel.
Preferably, the S3) is specifically:
carrying out first distillation and condensation on the treated ethyl orthosilicate to obtain ethyl orthosilicate after first distillation;
performing second distillation on the ethyl orthosilicate after the first distillation, and condensing to obtain ethyl orthosilicate after the second distillation;
and (3) carrying out third distillation and condensation on the ethyl orthosilicate subjected to the second distillation to obtain the high-purity ethyl silicate.
Preferably, after distillation, condensing, and after electrostatic adsorption treatment, obtaining the high-purity ethyl silicate.
The invention also provides a production system of the high-purity ethyl silicate, which comprises the following steps:
a moisture adsorbing device; the moisture adsorption device comprises an inlet and an outlet of a crude product of tetraethoxysilane;
a metal ion modifying device; the outlet of the moisture absorbing device is communicated with the metal ion modifying device;
a distillation column; the distillation tower is communicated with the metal ion modification device.
Preferably, the device also comprises a condensing device; the condensing device is communicated with the top of the distillation tower.
Preferably, the device also comprises a secondary distillation tower and a second condensing device; the secondary distillation tower is communicated with the condensing device; the top of the secondary distillation tower is communicated with a second condensing device.
Preferably, the distillation system further comprises a three-stage distillation tower and a third condensing device; the third-stage distillation tower is communicated with the second condensing device; the top of the three-stage distillation tower is communicated with a third condensing device.
Preferably, the condensing device further comprises a metal ion electrostatic adsorption device, and the metal ion electrostatic adsorption device is communicated with the third condensing device.
The invention provides a production method of high-purity ethyl silicate, which comprises the following steps: s1) adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed; s2) treating the ethyl orthosilicate adsorbing the water by a metal ion modified material to obtain treated ethyl orthosilicate; and S3) distilling the treated ethyl orthosilicate to obtain high-purity ethyl silicate. Compared with the prior art, the method has the advantages that after the tetraethoxysilane with water removed is treated by the metal ion modified material, phosphorus-containing and/or boron-containing light-component substances in the tetraethoxysilane are converted into heavy-component compounds, and the heavy-component compounds are distilled and condensed to obtain the high-purity tetraethoxysilane.
Drawings
FIG. 1 is a schematic diagram of a high purity ethyl silicate production system provided by the invention;
fig. 2 is a schematic structural diagram of the high purity ethyl silicate production system provided by the invention.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention provides a production method of high-purity ethyl silicate, which comprises the following steps: s1) adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed; s2) treating the water-removed ethyl orthosilicate with a metal ion modified material to obtain treated ethyl orthosilicate; and S3) distilling the treated ethyl orthosilicate to obtain high-purity ethyl silicate.
Wherein the crude product of ethyl orthosilicate is a crude product of ethyl orthosilicate well known to the person skilled in the art, and the purity of the ethyl orthosilicate is generally 99%, and the impurities contained in the crude product of ethyl orthosilicate are as follows: moisture, ethanol, methanol, propanol, metal ions, and the like.
Adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed; the moisture adsorbent is a moisture adsorbent well known to those skilled in the art, and is not particularly limited, and is preferably a 3A molecular sieve in the present invention, and the pore diameter of the molecular sieve is smaller, which is almost the same as the diameter of water molecules, so that water molecules can be adsorbed; the flow rate of the crude product of ethyl orthosilicate is preferably 1 to 5 m/s, more preferably 3 m/s.
The water-removed ethyl orthosilicate is treated by a metal ion modified material to obtain treated ethyl orthosilicate; the metal ion modified material is preferably a noble metal-loaded modified silica-alumina gel, more preferably a palladium and/or platinum modified silica-alumina gel; wherein the silica-alumina gel comprises silica and aluminum oxide; the mass ratio of the silicon dioxide to the aluminum oxide is preferably (1-2): 1, more preferably 1.5:1; the loading of the noble metal (i.e., the mass of the noble metal is a percentage of the mass of the silica gel) is preferably 0.1% -1%; some group III and V elements, such as phosphorus and boron, form POCl in tetraethylorthosilicate 3 、BOCl 3 、PCl 3 、BCl 3 And the like. These compounds are present as light components during the distillation of TEOS and therefore flow with the stream into the finished tank during distillation, resulting in the inability to remove these impurities. The method firstly utilizes metal ion modified material to treat the dehydrated tetraethoxysilane, and POCl is carried out by the modified material loaded on the molecular sieve filler through adsorption 3 、BOCl 3 、PCl 3 、BCl 3 And (3) an iso-light component compound is modified into a recombinant fraction compound, and then TEOS is distilled, so that impurities are discharged as heavy components, and the TEOS from the light component is purified.
Distilling the treated ethyl orthosilicate; the temperature of the distillation is preferably 165℃to 170 ℃. In order to further improve the quality of the obtained high-purity ethyl silicate, the invention preferably adopts three-stage distillation, and particularly preferably comprises the following steps: carrying out first distillation and condensation on the treated ethyl orthosilicate to obtain ethyl orthosilicate after first distillation; performing second distillation on the ethyl orthosilicate after the first distillation, and condensing to obtain ethyl orthosilicate after the second distillation; performing third distillation and condensation on the ethyl orthosilicate subjected to the second distillation to obtain high-purity ethyl silicate; the temperatures of the first distillation, the second distillation and the third distillation are each independently preferably 165-170 ℃; the condensation method is preferably a method well known to those skilled in the art, and is not particularly limited, and the condensation method is preferably performed by using circulating cooling water; the temperature of the circulating cooling water is preferably 20 to 30 ℃, more preferably 25 ℃.
Through three-stage distillation, metal ion impurities can be removed in a heavy component discharge mode, and in order to further reduce the content of the metal ion impurities, electrostatic adsorption treatment is carried out after condensation is preferred to obtain high-purity ethyl silicate; the electrostatic adsorption voltage is preferably 300-700 v/m, more preferably 400-600 v/m, still more preferably 500 v/m; the positively charged metal ions can be further removed by electrostatic adsorption.
The method is easy to operate, high in automation degree, capable of continuous production, high in working efficiency and high in quality of the obtained product, and meanwhile energy consumption and cost are reduced only by distillation.
The invention also provides a production system of the high-purity ethyl silicate, which comprises the following steps:
a moisture adsorbing device; the moisture adsorption device comprises an inlet and an outlet of a crude product of tetraethoxysilane;
a metal ion modifying device; the outlet of the moisture absorbing device is communicated with the metal ion modifying device;
a distillation column; the distillation tower is communicated with the metal ion modification device.
Referring to fig. 1 and 2, fig. 1 and 2 are schematic structural diagrams of a high purity ethyl silicate production system provided by the invention.
The high-purity ethyl silicate normal production system provided by the invention preferably comprises a raw material tank, wherein the raw material tank is used for storing crude ethyl silicate; the outlet of the raw material tank is communicated with the inlet of the crude ethyl orthosilicate product of the moisture adsorption device.
The moisture adsorption device is preferably internally provided with a molecular sieve, more preferably a 3A molecular sieve; the aspect ratio of the moisture adsorbing device is preferably (5 to 12): 1, more preferably (7 to 12): 1, more preferably 7:1..
The outlet of the moisture adsorption device is communicated with the metal ion modification device; the metal ion modifying device is filled with a metal ion modifying material; the metal ion modified material is preferably a load modified silica-alumina gel; the aspect ratio of the metal ion modifying apparatus is preferably (5 to 12): 1, more preferably (5 to 10): 1, more preferably (7 to 10): 1, most preferably 7:1.
Preferably according to the invention further comprises a back-up metal ion modification means; the standby metal ion modification device is communicated with an outlet of the moisture adsorption device; the standby metal ion modification device is filled with a metal ion modification material; the metal ion modified material is preferably silicon-aluminum gel modified by loading noble metal; the metal ion modified material is the same as described above and will not be described here again. The standby metal ion modifying apparatus and the metal ion modifying apparatus may be used simultaneously or alternately, and the production may be continued with less burden on both.
The metal ion modification device and the standby metal ion modification device are respectively communicated with the distillation tower; distilling the metal ion modified ethyl orthosilicate in a distillation tower; the distillation tower is a distillation tower well known to those skilled in the art, and is not particularly limited, and in the present invention, the distillation tower preferably uses an oil bath as a heating mode, and is provided with a heat conducting oil inlet and a heat conducting oil outlet; the heat conducting oil inlet and the heat conducting oil outlet are communicated with the heating heat conducting oil tank; to facilitate circulation, the heated conduction oil tank is preferably in communication with the conduction oil inlet of the distillation column via a circulation pump.
According to the invention, the production system preferably further comprises condensing means; the condensing device is communicated with the top of the distillation tower; condensing the distilled tetraethoxysilane steam of the distillation tower through a condensing device; the condensing device is preferably provided with a cooling water inlet and a cooling water outlet; the cooling water inlet and the cooling water outlet are communicated with the cooling water tank.
In order to improve the purity of the ethyl orthosilicate, the method preferably further comprises a secondary distillation tower and a second condensing device; the secondary distillation tower is communicated with the condensing device; the top of the secondary distillation tower is communicated with a second condensing device. In order to improve and guarantee the flow rate of the tetraethoxysilane liquid in the secondary distillation tower; the condensing device is preferably communicated with the secondary distillation tower through a first liquid buffer tank; the secondary distillation tower is a distillation tower well known to those skilled in the art, and is not particularly limited, and in the present invention, the secondary distillation tower preferably uses an oil bath as a heating mode, and is provided with a heat conducting oil inlet and a heat conducting oil outlet; the heat conducting oil inlet and the heat conducting oil outlet of the secondary distillation tower are communicated with the heating heat conducting oil tank; in order to facilitate circulation, the heating conduction oil tank is preferably communicated with a conduction oil inlet of the secondary distillation tower through a circulating pump; the second condensing device is preferably provided with a cooling water inlet and a cooling water outlet; and the cooling water inlet and the cooling water outlet of the second condensing device are communicated with the cooling water tank.
The production system provided by the invention preferably further comprises a three-stage distillation tower and a third condensing device; the third-stage distillation tower is communicated with a second condensing device; the top of the three-stage distillation tower is communicated with a third condensing device. In order to improve and ensure the flow rate of the tetraethoxysilane liquid in the three-stage distillation tower; the condensing device is preferably communicated with the three-stage distillation tower through a second liquid buffer tank; the three-stage distillation tower is a distillation tower well known to those skilled in the art, and is not particularly limited, and in the invention, the three-stage distillation tower preferably adopts an oil bath as a heating mode, and is provided with a heat conducting oil inlet and a heat conducting oil outlet; the heat conducting oil inlet and the heat conducting oil outlet of the three-stage distillation tower are communicated with the heating heat conducting oil tank; in order to facilitate circulation, the heating conduction oil tank is preferably communicated with a conduction oil inlet of the three-stage distillation tower through a circulating pump; the third condensing device is preferably provided with a cooling water inlet and a cooling water outlet; and the cooling water inlet and the cooling water outlet of the third condensing device are communicated with the cooling water tank.
The metal ion impurities can be removed by means of discharging the heavy components at the bottoms of the distillation tower, the secondary distillation tower and the tertiary distillation tower, and in order to further remove positively charged metal ions, the production system provided by the invention preferably further comprises a metal ion electrostatic adsorption device; the metal ion electrostatic adsorption device is communicated with the third condensing device, and is preferably communicated with the third condensing device through a third liquid buffer tank in order to ensure the flow rate of the ethyl orthosilicate liquid in the metal ion electrostatic adsorption device; a negative electrode plate is arranged in the metal ion electrostatic adsorption device; the negative electrode plate is connected with the negative electrode of the power supply; the width of the negative electrode plate is preferably 0.1 to 0.5 meter, more preferably 0.2 to 0.3 meter, still more preferably 0.2 meter; the length of the negative electrode plate is preferably 0.5 to 2 meters, more preferably 0.8 to 1.5 meters, still more preferably 1 meter; the specification of the negative electrode plate used in the present invention is preferably 0.2 m×1 m; the positive pole of the power supply is grounded. The ethyl orthosilicate liquid flows through the negative electrode plate to adsorb metal ions with positive charges, so that the high-purity ethyl silicate is obtained.
The production system provided by the invention preferably further comprises a finished product tank; the finished product tank is communicated with the metal ion electrostatic adsorption device and is used for storing high-purity ethyl silicate.
In order to further illustrate the invention, the following embodiment is used for describing the production method and the production system of the high-purity ethyl silicate.
The reagents used in the examples below are all commercially available.
Example 1
The preparation is carried out by adopting the production system shown in fig. 1 and 2, wherein a 3A molecular sieve is arranged in the moisture adsorption device, and the moisture adsorption deviceThe height-to-diameter ratio of (2) is 7:1; the metal ion modifying device is filled with palladium modified silica-alumina gel (40% Al) 2 O 3 +60％SiO 2 Load 0.5%), the height-to-diameter ratio is 7:1; the strength of the metal ion electrostatic adsorption device is 500 v/m, and the specification of the negative electrode plate is 0.2 m 1 m.
The flow rate of the crude product of ethyl orthosilicate is preferably 3 m/s.
The temperatures of the distillation column, the secondary distillation column and the tertiary distillation column were 170 ℃.
And circulating and condensing the condensing device, the second condensing device and the third condensing device through cooling water at 25 ℃.
The impurity components and the contents of the crude ethyl orthosilicate used in example 1 are shown in Table 1; the high purity ethyl silicate obtained in example 1 was tested and the results are shown in table 2.
TABLE 1 impurity components and content of crude ethyl orthosilicate
Table 2 example 1 detection results of electronic pure ethyl silicate
Example 2
The preparation procedure was the same as in example 1, except that the metal ion electrostatic adsorption device had an intensity of 400 v/m.
The high-purity ethyl orthosilicate product obtained in the example 2 is detected, and the detection result is the same as that of the example 1 and meets the requirements.
Example 3
The preparation procedure was the same as in example 1, except that the metal ion modification apparatus was filled with platinum-modified silica-alumina gel (40% Al) 2 O 3 +60％SiO 2 Load 1%), the height-to-diameter ratio is 10:1; the strength of the metal ion electrostatic adsorption device is 500 v/m, and the specification of the negative electrode plate is 0.3 m 1 m.
The high-purity ethyl orthosilicate product obtained in the example 3 is detected, and the detection result is the same as that of the example 1 and meets the requirements.
Claims (8)
1. The production method of the high-purity ethyl silicate is characterized by comprising the following steps of:
s1) adsorbing the crude product of the ethyl orthosilicate by a moisture adsorbent to obtain the ethyl orthosilicate with moisture removed; the moisture adsorbent is a 3A molecular sieve;
s2) treating the water-removed ethyl orthosilicate with a metal ion modified material to obtain treated ethyl orthosilicate; the metal ion modified material is palladium and/or platinum modified silica-alumina gel;
and S3) distilling the treated ethyl orthosilicate to obtain high-purity ethyl silicate.
2. The production method according to claim 1, wherein S3) is specifically:
carrying out first distillation and condensation on the treated ethyl orthosilicate to obtain ethyl orthosilicate after first distillation;
performing second distillation on the ethyl orthosilicate after the first distillation, and condensing to obtain ethyl orthosilicate after the second distillation;
and (3) carrying out third distillation and condensation on the ethyl orthosilicate subjected to the second distillation to obtain the high-purity ethyl silicate.
3. The method according to claim 2, wherein the high purity ethyl silicate is obtained by condensing after distillation and subjecting to electrostatic adsorption treatment.
4. A production system of high purity ethyl silicate, comprising:
a moisture adsorbing device; the moisture adsorption device comprises an inlet and an outlet of a crude product of tetraethoxysilane; a 3A molecular sieve is arranged in the moisture adsorption device;
a metal ion modifying device; the outlet of the moisture absorbing device is communicated with the metal ion modifying device; the metal ion modifying device is filled with a metal ion modifying material; the metal ion modified material is palladium and/or platinum modified silica-alumina gel;
a distillation column; the distillation tower is communicated with the metal ion modification device.
5. The production system of claim 4, further comprising a condensing device; the condensing device is communicated with the top of the distillation tower.
6. The production system of claim 5, further comprising a secondary distillation column and a second condensing device; the secondary distillation tower is communicated with the condensing device; the top of the secondary distillation tower is communicated with a second condensing device.
7. The production system of claim 6, further comprising a tertiary distillation column and a third condensing device; the third-stage distillation tower is communicated with the second condensing device; the top of the three-stage distillation tower is communicated with a third condensing device.
8. The production system of claim 7, further comprising a metal ion electrostatic adsorption device in communication with the third condensing device.
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| CN109734742A (en) * | 2019-03-12 | 2019-05-10 | 大连恒坤新材料有限公司 | A kind of method of purification of ethyl orthosilicate |
| CN112592717A (en) * | 2020-12-18 | 2021-04-02 | 湖南工业大学 | Nano fluorescent carbon dots and preparation method thereof |
| CN114507250B (en) * | 2022-01-12 | 2023-03-21 | 湖北江瀚新材料股份有限公司 | Synthesis process of electronic-grade ethyl orthosilicate and electronic-grade ethyl polysilicate |
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