CN209816001U - Production system of high-purity tetraethoxysilane - Google Patents
Production system of high-purity tetraethoxysilane Download PDFInfo
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Abstract
The utility model provides a production system of high-purity tetraethoxysilane, include: a vaporizer; a first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the inlet of the first adsorption device is communicated with the gas outlet of the vaporizer; a drying device; the inlet of the drying device is communicated with the outlet of the first adsorption device; a second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the inlet of the second adsorption device is communicated with the outlet of the drying device; a condensing unit. Compared with the prior art, the utility model discloses earlier vaporize tetraethoxysilane crude product, then utilize ethanol, methyl alcohol, propanol, moisture and metal ion among the adsorption removal gaseous state tetraethoxysilane, can obtain high-purity tetraethoxysilane after the condensation, produce easily operation, degree of automation is high, can carry out continuous production, only need once vaporize simultaneously and also reduced the energy consumption, and energy saving reduces originally.
Description
Technical Field
The utility model belongs to the technical field of the semiconductor, especially, relate to a production system of high-purity tetraethoxysilane.
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 TEOS LPCVD 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%.
Chinese patent publication No. CN201310747619.4 discloses a method for preparing electronic grade ethyl orthosilicate, which comprises complexing most of the metal impurities in the raw material with a complexing agent, filtering with a 0.1 micron microporous filter, passing through a cation exchange column, a quartz plate distillation column, and a sub-boiling distiller in sequence, strictly controlling the temperature, removing trace metal impurities, ethanol, other organic impurities, and moisture, but using a complexing agent to introduce new metal ion impurities easily, and processing difficulty by a sub-boiling distillation method is high, energy consumption is high, and efficiency is low, so that the production cost of the product is increased, and continuous production cannot be achieved.
SUMMERY OF THE UTILITY MODEL
In view of this, the technical problem to be solved by the present invention is to provide a production system of high purity ethyl silicate capable of continuous production and with low cost.
The utility model also provides a production system of high-purity tetraethoxysilane, include:
a vaporizer; the vaporizer is provided with an inlet and a gas outlet of a crude product of tetraethoxysilane;
a first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the inlet of the first adsorption device is communicated with the gas outlet of the vaporizer;
a drying device; the inlet of the drying device is communicated with the outlet of the first adsorption device;
a second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the inlet of the second adsorption device is communicated with the outlet of the drying device;
a condensing unit; and the inlet of the condensing device is communicated with the outlet of the second adsorption device.
Preferably, a particle filter is also included; the gas outlet of the vaporizer is in communication with the inlet of the first adsorption means through a particulate filter.
Preferably, the particulate filter is sintered polytetrafluoroethylene.
Preferably, the device further comprises a third adsorption device; and the outlet of the first adsorption device is communicated with the drying device through a third adsorption device.
Preferably, an electrode is arranged outside the first adsorption device and/or the third adsorption device.
Preferably, the inlets of the first adsorption device, the second adsorption device and the third adsorption device are arranged at the bottom of the device, and the outlets of the first adsorption device, the second adsorption device and the third adsorption device are arranged at the top of the device.
Preferably, the height-diameter ratio of the first adsorption device, the second adsorption device and the third adsorption device is (5-12): 1.
preferably, the device also comprises a product tank; the inlet of the product tank is communicated with the outlet of the condensing device
The utility model provides a production system of high-purity tetraethoxysilane, include: a vaporizer; the vaporizer is provided with an inlet and a gas outlet of a crude product of tetraethoxysilane; a first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the inlet of the first adsorption device is communicated with the gas outlet of the vaporizer; a drying device; the inlet of the drying device is communicated with the outlet of the first adsorption device; a second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the inlet of the second adsorption device is communicated with the outlet of the drying device; a condensing unit; and the inlet of the condensing device is communicated with the outlet of the second adsorption device. Compared with the prior art, the utility model discloses earlier vaporize tetraethoxysilane crude product, then utilize ethanol, methyl alcohol, propanol, moisture and metal ion among the adsorption removal gaseous state tetraethoxysilane, can obtain high-purity tetraethoxysilane after the condensation, production method easily operates, and degree of automation is high, can carry out continuous production, and the product quality that work efficiency is high and obtain is also higher, only needs vaporization once simultaneously also to reduce the energy consumption, and is energy-conserving this reduction.
Drawings
FIG. 1 is a schematic view of a process for preparing high-purity tetraethoxysilane provided by the present invention;
FIG. 2 is a structural diagram of a high-purity tetraethoxysilane production system provided by the utility model;
fig. 3 is a schematic structural diagram of a high-purity tetraethoxysilane production system provided by the utility model.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
The utility model provides a production method of high-purity ethyl orthosilicate, comprising the following steps:
heating the crude product of tetraethoxysilane to obtain gaseous tetraethoxysilane;
removing ethanol and diethyl ether from the gaseous tetraethoxysilane by an adsorption method, drying, and removing metal ions by the adsorption method to obtain adsorbed gaseous tetraethoxysilane;
and condensing the adsorbed gaseous tetraethoxysilane to obtain the high-purity tetraethoxysilane.
Wherein the crude tetraethoxysilane is a crude tetraethoxysilane known to those skilled in the art, and the purity of the tetraethoxysilane is usually 99%, and the crude tetraethoxysilane comprises the following impurities: water, ethanol, methanol, propanol, metal ions, and the like.
Heating the crude product of tetraethoxysilane to obtain gaseous tetraethoxysilane; the heating temperature is preferably greater than the boiling point of ethyl orthosilicate, more preferably from 170 ℃ to 175 ℃.
Removing alcohol impurities and ether impurities from the gaseous tetraethoxysilane by an adsorption method; the adsorbent used for removing the alcohol impurities and the ether impurities by the adsorption method is preferably a 4A molecular sieve and/or a 5A molecular sieve. The molecular sieve has larger pore diameter, larger diameters of ethanol and ether molecules, and matched pore diameter with the molecular diameter, and can adsorb ethanol and ether; the flow velocity of the gaseous tetraethoxysilane is preferably 0.5-2 m/s, more preferably 1-1.5 m/s, and further preferably 1 m/s; the pressure of the gaseous ethyl orthosilicate in the adsorption process is preferably 0.05-0.1 MPa, more preferably 0.07-0.09 MPa, and still more preferably 0.08 MPa.
Because the ethanol, the methanol and the propanol are difficult to adsorb, in order to prevent the alcohol impurities and the ether impurities from remaining, the ethanol and the ether are preferably removed by two times of adsorption; the adsorbent used for removing ethanol and diethyl ether by the second adsorption is preferably a 4A molecular sieve and/or a 5A molecular sieve.
The molecular sieve is a strong polar adsorbent, and the mechanism of the molecular sieve for adsorbing impurities is that when impurity molecules pass through micropores of the molecular sieve, the strong polarity of the molecular sieve attracts the impurity molecules with polarity, so that the impurity molecules are adsorbed on the surface of the molecular sieve, the impurity removal effect is influenced by the polarity of the impurities, and the larger the polarity of the impurity molecules is, the adsorption is also facilitated. In the impurities of the crude product of the ethyl orthosilicate, the polarity is 4.3 parts of ethanol, 6.6 parts of methanol, 4 parts of propanol and the water content is 10.2 parts. Therefore, the moisture is very easily adsorbed and removed, and the other three impurities are relatively difficult to remove. In order to improve the adsorption efficiency of the alcohol impurities, the alcohol impurities and ether impurities are preferably removed by adsorption in the presence of an electric field; the strength of the electric field is preferably 1000-2000V/m; the polarity of molecules such as ethanol, methanol, propanol and the like is increased in an electric field, and the molecules are more easily adsorbed on the molecular sieve.
Adsorbing to remove ethanol and diethyl ether, and drying; the drying is preferably carried out by using a molecular sieve; the molecular sieve is preferably a 3A molecular sieve, and the molecular sieve has small pore size which is almost the same as the diameter of water molecules, so that the molecular sieve can adsorb the water molecules.
After drying, removing metal ions by adsorption; the adsorbent for adsorbing and removing the metal ions is preferably silicon-aluminum gel modified by loading metal oxides; wherein the silica-alumina gel comprises silicon dioxide 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 supported metal oxide is preferably manganese oxide and/or molybdenum oxide; the loading amount of the metal oxide (namely, the mass of the noble metal is the percentage of the mass of the silica gel) is preferably 1 to 5 percent; in the present invention, the adsorbent for adsorbing and removing metal ions is most preferably a silica-alumina gel of model SA-S01, pure technologies and technologies, Inc., available in Tianjin.
The utility model discloses earlier utilize 4A molecular sieve and/or 5A molecular sieve to adsorb ethanol, methyl alcohol, propanol, because the diameter of ethanol, methyl alcohol, propanol is great, can cause the jam to the micropore of the 3A molecular sieve of adsorbed moisture for the molecular sieve loses activity, consequently need adsorb ethanol, methyl alcohol, propanol earlier, adsorbs the back, then recycles the 3A molecular sieve and adsorbs the drying to the hydrone of minor diameter.
And finally, adsorbing and removing metal ions, wherein the metal ion adsorption is finally carried out because the metal ion adsorption is carried out by adopting the silicon-aluminum gel modified by the loaded metal oxide, and the ethanol, the methanol, the propanol and the moisture can make the modified material loaded on the silicon-aluminum gel lose activity, so that the metal ion adsorption is not carried out.
The utility model discloses earlier vaporize tetraethoxysilane crude product, then utilize and adsorb ethanol, methyl alcohol, propanol, moisture and metal ion in the detached gaseous state tetraethoxysilane, can obtain high-purity tetraethoxysilane after the condensation, production method easily operates, and degree of automation is high, can carry out continuous production, and the product quality that work efficiency is high and obtain is also higher, only needs vaporization once simultaneously also to reduce the energy consumption, and energy saving reduces originally.
The utility model also provides a production system of high-purity tetraethoxysilane, include:
a vaporizer; the vaporizer is provided with an inlet and a gas outlet of a crude product of tetraethoxysilane;
a first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the inlet of the first adsorption device is communicated with the gas outlet of the vaporizer;
a drying device; the inlet of the drying device is communicated with the outlet of the first adsorption device;
a second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the inlet of the second adsorption device is communicated with the outlet of the drying device;
a condensing unit; and the inlet of the condensing device is communicated with the outlet of the second adsorption device.
Referring to fig. 3, fig. 3 is a schematic structural diagram of a high-purity tetraethoxysilane production system provided by the present invention.
The utility model discloses in, preferred still include the head tank, the head tank is linked together with the import of the tetraethoxysilane crude of vaporizer.
The vaporizer is preferably provided with heating means; the heating device is a heating device known to those skilled in the art, and is not particularly limited, and an electric heating device is preferred in the present invention; and vaporizing the crude product of the tetraethoxysilane in the vaporizer by an electric heating device to obtain the gaseous tetraethoxysilane.
In order to improve the production efficiency of the high-purity tetraethoxysilane, a second vaporizer is preferably further included; the second vaporizer is provided with an inlet and a gas outlet of a crude product of tetraethoxysilane; an outlet of the crude product of the ethyl orthosilicate of the second vaporizer is communicated with the raw material tank; the gas outlet of the second vaporizer is communicated with the first adsorption device; and the second vaporizer is not communicated with the vaporizer to form a state that the two vaporizers are used as one for one.
The production system provided by the utility model preferably also comprises a particle filter; the gas outlet of the vaporizer is communicated with the first adsorption device through a particle filter; the gas outlet of the second vaporizer is preferably also in communication with the first adsorption means via a particulate filter; the particle filter is a particle filter known to those skilled in the art, and is not particularly limited, but is preferably sintered polytetrafluoroethylene; the pore size of the sintered polytetrafluoroethylene is preferably 0.01 μm.
To control the flow rate of the gas, the particulate filter is preferably in communication with the first adsorption means by a pressure gauge; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the adsorbent for adsorbing the alcohol impurities and the ether impurities is preferably a 4A molecular sieve and/or a 5A molecular sieve; the height-diameter ratio of the first adsorption device is preferably (5-12): 1, more preferably (7-12): 1, more preferably 7: 1.
in order to prevent alcohol impurities and ether impurities from remaining in the gas, a third adsorption device is preferably further included; the third adsorption device is communicated with the first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the third adsorption device; the adsorbent for adsorbing the alcohol impurities and the ether impurities is preferably a 4A molecular sieve and/or a 5A molecular sieve; the height-diameter ratio of the third adsorption device is preferably (5-12): 1, more preferably (7-12): 1, more preferably 7: 1.
in order to be more beneficial to removing impurities such as ethanol, methanol, propanol and the like, electrodes are preferably arranged outside the first adsorption device and/or the third adsorption device, and an electric field can be formed to act on the first adsorption device and/or the third adsorption device.
The gas outlet of the third adsorption device is communicated with the drying device; a moisture adsorbent is preferably arranged in the drying device; the moisture adsorbent is preferably a 3A molecular sieve; the height-diameter ratio of the drying device is preferably (5-12): 1, more preferably (7-12): 1, more preferably 7: 1.
the outlet of the drying device is communicated with the second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the adsorbent for adsorbing metal ions is preferably metal oxide modified silicon-aluminum gel; wherein the silica-alumina gel comprises silicon dioxide 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 supported metal oxide is preferably manganese oxide and/or molybdenum oxide; the loading amount of the metal oxide (namely, the mass of the noble metal is the percentage of the mass of the silica gel) is preferably 1 to 5 percent; in the present invention, the adsorbent for adsorbing and removing metal ions is most preferably a silica-alumina gel of type SA-S01, pure technologies ltd, tianjin; the height-diameter ratio of the second adsorption device is preferably (5-12): 1, more preferably (7-12): 1, more preferably 7: 1. the utility model discloses in, must carry out metal ion's absorption at last, this is because metal ion adsorbs the modified silicon-aluminum gel for the load that adopts, and ethanol, methyl alcohol, propanol and moisture can make the modified material of load on the silicon-aluminum gel lose activity, and then do not play the effect of adsorbing metal ion.
In order to improve the adsorption efficiency, the utility model discloses the entry of stating first adsorption equipment, second adsorption equipment and third adsorption equipment sets up in the device bottom, and the export sets up in the device top.
In order to improve the production efficiency of the high-purity ethyl orthosilicate, the high-purity ethyl orthosilicate adsorption equipment preferably further comprises a standby first adsorption device, a standby second adsorption device and a standby third adsorption device; the standby first adsorption device is communicated with the vaporizer; the standby third adsorption device is communicated with the standby first adsorption device; the standby second adsorption device is communicated with the standby third adsorption device to form a standby state.
The outlet of the second adsorption device is communicated with a condenser, and the gaseous tetraethoxysilane is condensed into liquid high-purity tetraethoxysilane in the condenser; a cooling water circulation system is preferably arranged outside the condenser, and condensation is carried out through the cooling water circulation system; the cooling water circulation system preferably comprises a shield pump, and cooling water is transported and circulated through the shield pump.
In order to improve the cooling efficiency, a second condenser is preferably further included; the second condenser is linked together with second adsorption equipment's export, just the second condenser does not communicate with the condenser to form the state that one of condenser was equipped with one, simultaneously the utility model provides a condenser and second condenser also can regard as the product jar, need fill dress when filling the dress steel bottle, and two condensers can fill dress by one, and another receives the finished product, alternate use.
In order to further illustrate the present invention, the following detailed description is made on a production system of high purity tetraethoxysilane provided by the present invention with reference to the examples.
The reagents used in the following examples are all commercially available.
Example 1
The preparation is carried out according to the flow shown in figure 1 and the production system shown in figure 2, wherein the height-diameter ratio of the first adsorption device is 7: 1; the height-diameter ratio of the third adsorption device is 7: 1; the height-diameter ratio of the drying device is 7: 1; the height-diameter ratio of the second adsorption device is 7: 1; the strength of the electric field is 1000 v/m.
Heating the crude product of the tetraethoxysilane to 170 ℃ to obtain gaseous tetraethoxysilane.
And (2) adsorbing the gaseous tetraethoxysilane with the flow rate of 1 m/S and the pressure of 0.08MPa twice by using a 5A molecular sieve, drying by using a 3A molecular sieve, and finally adsorbing the dried gaseous tetraethoxysilane by using silicon-aluminum gel (model: SA-S01, pure technologies and technologies Co., Ltd., Tianjin) to obtain the adsorbed gaseous tetraethoxysilane.
And circularly condensing the adsorbed gaseous tetraethoxysilane by cooling water at 25 ℃ to obtain the high-purity tetraethoxysilane.
The impurity components and contents of the crude tetraethoxysilane used in example 1 are shown in table 1; the high purity tetraethoxysilane obtained in example 1 was examined, and the results are shown in table 2.
Table 1 example 1 impurity components and contents of crude ethyl orthosilicate
Table 2 example 1 detection results of electronically pure ethyl silicate
Example 2
The preparation process is the same as that of example 1, except that the pressure of the gaseous tetraethoxysilane is 0.05MPa, and the height-diameter ratio of the first adsorption device, the second adsorption device and the third adsorption device is 10: 1; the electric field strength was 2000 v/m.
The high-purity tetraethoxysilane product obtained in the example 2 is detected, and the detection result is the same as that of the example 1 and meets the requirement.
Example 3
The preparation process is the same as that of example 1, except that the pressure of the gaseous tetraethoxysilane is 0.1MPa, and the height-diameter ratio of the first adsorption device, the second adsorption device and the third adsorption device is 12: 1.
The high-purity tetraethoxysilane product obtained in the embodiment 3 is detected, and the detection result is the same as that of the embodiment 1 and meets the requirement.
Claims (8)
1. A production system of high-purity tetraethoxysilane is characterized by comprising:
a vaporizer; the vaporizer is provided with an inlet and a gas outlet of a crude product of tetraethoxysilane;
a first adsorption device; an adsorbent for adsorbing alcohol impurities and ether impurities is arranged in the first adsorption device; the inlet of the first adsorption device is communicated with the gas outlet of the vaporizer;
a drying device; the inlet of the drying device is communicated with the outlet of the first adsorption device;
a second adsorption device; an adsorbent for adsorbing metal ions is arranged in the second adsorption device; the inlet of the second adsorption device is communicated with the outlet of the drying device;
a condensing unit; and the inlet of the condensing device is communicated with the outlet of the second adsorption device.
2. The production system of claim 1, further comprising a particulate filter; the gas outlet of the vaporizer is in communication with the inlet of the first adsorption means through a particulate filter.
3. The production system of claim 2, wherein the particulate filter is sintered polytetrafluoroethylene.
4. The production system of claim 1, further comprising a third adsorption device; and the outlet of the first adsorption device is communicated with the drying device through a third adsorption device.
5. The production system according to claim 4, wherein an electrode is arranged outside the first adsorption device and/or the third adsorption device.
6. The production system of claim 4, wherein the inlets of the first adsorption device, the second adsorption device and the third adsorption device are arranged at the bottom of the device, and the outlets are arranged at the top of the device.
7. The production system according to claim 4, wherein the aspect ratio of the first adsorption device, the second adsorption device and the third adsorption device is (5-12): 1.
8. the production system of claim 1, further comprising a product tank; the inlet of the product tank is communicated with the outlet of the condensing device.
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| CN201822192267.1U CN209816001U (en) | 2018-12-25 | 2018-12-25 | Production system of high-purity tetraethoxysilane |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215152 No. 6 Anmin Road, Panyang Industrial Park, Huangdi Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |