CN109912636B - Production method of high-purity ethyl orthosilicate - Google Patents
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Abstract
The invention provides a production method of high-purity tetraethoxysilane, which comprises the following steps: s1) carrying out lightness-removing rectification on the crude product of the tetraethoxysilane to obtain a product after lightness-removing rectification; s2) treating the product after light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber; s3) carrying out de-weighting rectification on the treated product to obtain the high-purity ethyl orthosilicate. Compared with the prior art, the method has the advantages that a certain amount of metal ions are removed by adsorption through treatment of an adsorber before heavy rectification, spherical activated carbon is used as a first-stage adsorption material, then a plurality of metal ions are removed by exchange with sodium ions through a second-stage cation exchange resin, and then the material enters a three-stage titanium dioxide nanotube to remove the sodium ions by adsorption, so that the defects of a continuous rectification process are overcome.
Description
Technical Field
The invention belongs to the technical field of semiconductors, and particularly relates to a production method of high-purity tetraethoxysilane.
Background
The integrated circuit industry is one of the most rapidly developed high and new technology industries at present, various chips produced by the integrated circuit industry are widely applied to industrial equipment and machinery and electrical equipment used in daily life, the matched ultra-high purity electronic chemicals belong to the field of fine chemical engineering in the chemical industry, the most typical technical characteristics of the ultra-high purity electronic chemicals are high product purity and stable quality, the integrated circuit industry is a high and new technology industry with high technical content, high investment and high added value, and the integrated circuit industry is one of the most rapidly developed and most active industries in the chemical industry.
The ultra-high purity electronic chemical industry in China develops rapidly, the annual growth rate of the ultra-high purity electronic chemical manufacturing industry exceeds 20 percent in recent years, the ultra-high purity electronic chemical is one of important supporting materials in the semiconductor integrated circuit industry, and the quality of the ultra-high purity electronic chemical directly influences the quality of a semiconductor integrated electric chip.
Tetraethoxysilane (TEOS) is an important one of ultra-high-purity electronic chemicals and is mainly used for an LPCVD (low pressure chemical vapor deposition) process in the manufacturing process of semiconductor integrated circuit chips, specifically, TEOS is firstly evaporated from a liquid state to a gas state, then is decomposed at 700-750 ℃ and under the pressure of 50Pa to deposit a silicon dioxide film on the surface of a silicon wafer, 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 the 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 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.
Trace metal doping of the silicon dioxide film changes its semiconductor properties and affects the performance of the final chip. Therefore, in the production of semiconductor integrated circuits, the metal ions in the raw material TEOS are strictly controlled.
At present, the domestic and foreign purification process for removing metal ions in TEOS mainly utilizes a rectification mode, the rectification mode can effectively remove impurity components with large boiling point difference, and the effect of removing the metal ions is not ideal.
Chinese patent with application number CN201310747619.4 discloses a preparation method of electronic grade ethyl orthosilicate, which comprises the steps of complexing most of metal impurities in raw materials by a complexing agent, and filtering by a 0.1-micron microporous filter; removing trace metal impurities, ethanol and organic impurities thereof and water by a cation exchange tower, a quartz plate distillation tower and a sub-boiling distiller under strict temperature control. However, the method needs a complexing agent, new metal ion impurities are introduced, and the preparation equipment adopting a sub-boiling distillation mode has the disadvantages of high processing difficulty, high energy consumption and low efficiency, so that the production cost of the product is increased, and the continuous production cannot be realized.
Disclosure of Invention
In view of the above, the present invention provides a method for producing high-purity tetraethoxysilane, which can effectively remove metal ions and can be used for continuous production.
The invention provides a production method of high-purity tetraethoxysilane, which comprises the following steps:
s1) carrying out lightness-removing rectification on the crude product of the tetraethoxysilane to obtain a product after lightness-removing rectification;
s2) treating the product after light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber; the volume ratio of the spherical activated carbon to the cation exchange resin to the titanium dioxide nanotube is (0.5-2): (0.5-2): (0.5 to 2);
s3) carrying out de-weighting rectification on the treated product to obtain the high-purity ethyl orthosilicate.
Preferably, the temperature of the light component removal rectification in the step S1) is 160-190 ℃; and the reflux ratio of the light component removal rectification is 8-25.
Preferably, the cation exchange resin is a gel type cation exchange resin.
Preferably, the cation exchange resin is a strong-acid styrene cation exchange resin, and the pore diameter is 0.5-5 nm.
Preferably, the volume ratio of the spherical activated carbon to the cation exchange resin to the titanium dioxide nanotube is 1:1: 1.
preferably, the temperature of the de-heavy distillation is 160-190 ℃; the reflux ratio of the de-heavy rectification is 8-25.
Preferably, the number of theoretical plates of a rectifying tower used for the light component removal rectification is 50-150.
Preferably, the number of theoretical plates of a rectifying tower used for the de-heavy rectification is 50-150.
Preferably, the flow rate of the product after the light component removal and rectification in the step S2) is 0.1-1 m/S.
The invention provides a production method of high-purity tetraethoxysilane, which comprises the following steps: s1) carrying out lightness-removing rectification on the crude product of the tetraethoxysilane to obtain a product after lightness-removing rectification; s2) treating the product after light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber; s3) carrying out de-weighting rectification on the treated product to obtain the high-purity ethyl orthosilicate. Compared with the prior art, the method has the advantages that before the heavy component removal rectification, the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotubes are treated by the absorber, the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotubes are sequentially arranged in the absorber, the spherical activated carbon is used as a first-stage adsorption material to adsorb and remove a certain amount of metal ions, then the material enters the second-stage cation exchange resin to exchange and remove a plurality of metal ions and sodium ions, and then the material enters the third-stage titanium dioxide nanotubes to adsorb and remove sodium ions in the titanium dioxide nanotubes, so that the defects of a continuous rectification process are overcome, the load of the absorber is lightened by the light component removal rectification, the service cycle is prolonged, and meanwhile, the method provided by the invention has the advantages of simple equipment.
Drawings
FIG. 1 is a schematic structural diagram of a production method of high-purity tetraethoxysilane provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a production method of high-purity tetraethoxysilane, which comprises the following steps:
s1) carrying out lightness-removing rectification on the crude product of the tetraethoxysilane to obtain a product after lightness-removing rectification;
s2) treating the product after light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber;
s3) carrying out de-weighting rectification on the treated product to obtain the high-purity ethyl orthosilicate.
Referring to fig. 1, fig. 1 is a schematic flow chart of a production method of high-purity tetraethoxysilane provided by the invention.
The invention has no special reality on the sources of all raw materials, and can be sold in the market.
The crude product of the tetraethoxysilane is the crude product of the tetraethoxysilane known by the technical personnel in the field, namely a tetraethoxysilane monomer, also called tetraethoxysilane-28, and the content of industrial products is generally 99.5 percent Wt.
And (3) performing light component removal rectification on the crude ethyl orthosilicate product to obtain a light component removal rectified product. The light component removal rectification is preferably carried out in a light component removal rectification tower; feeding the crude product of tetraethoxysilane from the middle upper part of a light component removal rectifying tower preferably; the temperature of the dehydrogenation rectification is preferably 160-190 ℃, and more preferably 165-180 ℃; the pressure of the light component removal rectification is preferably-0.1-0.3 bar, more preferably-0.05-0.2 bar, still more preferably 0-0.1 bar, and most preferably 0-0.05 bar; the temperature of the light component removal rectification condensation is preferably 120-150 ℃, more preferably 120-140 ℃, and further preferably 120-130 ℃; the reflux ratio of the light component removal rectification is preferably 8-25, more preferably 10-20, and further preferably 15-19; light components such as ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and the like in the ethyl orthosilicate can be removed through light component removal rectification; the mass of the light components removed during the light component removal rectification is preferably 1/5-1/12 of the mass of the crude product of ethyl orthosilicate, and more preferably 1/8-1/12.
Treating the product after the light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber; the particle size of the spherical activated carbon is preferably 2-5 mm, and more preferably 3-5 mm; the cation exchange resin is preferably gel type cation exchange resin, and more preferably strong acid styrene cation exchange resin; the pore diameter of the cation exchange resin is preferably 0.5-5 nm, and more preferably 1-4 nm; the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotube are sequentially arranged along the flowing direction of the product after light component removal rectification, and the volume ratio of the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotube is preferably (0.5-2): (0.5-2): (0.5-2), more preferably (0.5-1.5): (0.5-1.5): (0.5 to 1.5), and preferably 1:1: 1; the layer heights of the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotube are respectively 0.5-3 m, and more preferably 1-2 m. The flow velocity of the product after the light component removal rectification in the adsorber is preferably 0.1-1 m/s, more preferably 0.3-1 m/s, and still more preferably 0.5-0.7 m/s.
And performing heavy-duty rectification on the treated product to obtain high-purity ethyl orthosilicate. The heavy component removal rectification is preferably carried out in a heavy component removal rectification tower; during the heavy component removal and rectification, the product treated by the adsorber is preferably fed at the middle lower part of the heavy component removal and rectification tower; the temperature of the de-heavy distillation is preferably 160-190 ℃, more preferably 168-180 ℃, and further preferably 168-170 ℃; the pressure of the de-heavy rectification is preferably-0.1-0.3 bar, more preferably-0.05-0.2 bar, still more preferably 0-0.1 bar, and most preferably 0-0.05 bar; the condensation temperature at the top of the tower during the heavy component removal rectification is preferably 120-150 ℃, more preferably 120-140 ℃, and further preferably 123-135 ℃; the reflux ratio of the heavy component removal rectification is preferably 8-25, more preferably 10-20, and further preferably 13-18; heavy components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate can be removed through heavy component removal and rectification, and the heavy components can be recovered; during the heavy component removal and rectification, the mass of the removed heavy components is preferably 1/4-1/12, more preferably 1/6-1/12 and even more preferably 1/9-1/11 of the mass of the treated product; the tetraethoxysilane obtained at the tower top after the heavy component removal and rectification is preferably condensed to obtain high-purity tetraethoxysilane, the component purity can reach more than 5N, and the indexes of metal ions and the like can reach 9N.
The method comprises the steps of treating the materials by an absorber before heavy rectification, arranging spherical activated carbon, cation exchange resin and titanium dioxide nanotubes in the absorber in sequence, adsorbing and removing a certain amount of metal ions by taking the spherical activated carbon as a first-stage adsorption material, then introducing the materials into a second-stage cation exchange resin, exchanging and removing various metal ions and sodium ions, introducing the materials into a third-stage titanium dioxide nanotube, and adsorbing and removing the sodium ions in the titanium dioxide nanotube, so that the defects of a continuous rectification process are overcome, the load of the absorber is reduced by light rectification firstly, and the service cycle of the absorber is prolonged.
In order to further illustrate the present invention, the following will describe the production method of high purity tetraethoxysilane provided by the present invention in detail with reference to the examples.
The reagents used in the following examples are all commercially available.
Example 1
The flow rate of the crude tetraethoxysilane is 0.7m/s, the crude tetraethoxysilane is fed from a crude tetraethoxysilane storage tank through a feeding conveying pump, the crude tetraethoxysilane is fed from the middle upper part of a tetraethoxysilane lightness-removing rectifying tower T01 tower, and the rectifying temperature is 180 ℃; the pressure was 0.05 bar; the condensation temperature at the top of the tower during the light component removal rectification is 130 ℃; the reflux ratio of the light component removal rectification is 10; removing unreacted ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and other light components in the ethyl orthosilicate by light-component removal rectification; the mass of the removed light components is 1/8 of the mass of the crude tetraethoxysilane.
Conveying the product subjected to light component removal rectification to an adsorber at a flow rate of 0.7m/s by a discharge pump of a tetraethoxysilane light component removal rectification tower, wherein spherical active carbon (with the granularity of 3mm), strong-acid styrene cation exchange resin (with the aperture of 4nm) and titanium dioxide nanotubes are sequentially filled in the flow direction of salt tetraethoxysilane in the adsorber, the volume ratio of the spherical active carbon to the salt tetraethoxysilane in the adsorber is 1:1:1, and the layer height of the spherical active carbon to the salt tetraethoxysilane in the adsorber is 2m, so as to obtain the product subjected to adsorption treatment.
The product after adsorption treatment enters an ethyl orthosilicate de-heavy rectification tower T02 through a delivery pump at the flow velocity of 0.7m/s, and is fed from the middle lower part of the tower, and the rectification temperature is 170 ℃; the pressure is 0 bar; the condensation temperature of the tower top during the heavy component removal rectification is 135 ℃; the reflux ratio of the heavy component removal rectification is 13; removing the weight components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate, wherein the mass of the removed weight components is 1/9 of the mass of the product after adsorption treatment; condensing the tower top by a condenser to obtain high-purity ethyl orthosilicate, wherein the purity of the components can reach more than 5N, and the indexes of metal ions and the like reach 9N.
The yield of the high pure ethyl silicate is 76%.
The crude tetraethoxysilane used in example 1 and the obtained highly pure tetraethoxysilane were examined and the results are shown in tables 1 and 2.
TABLE 1 detection results of crude tetraethoxysilane
Table 2 detection results of high purity tetraethoxysilane obtained in example 1
Example 2
The flow rate of the crude tetraethoxysilane is 0.5m/s, the crude tetraethoxysilane is fed from a crude tetraethoxysilane storage tank through a feeding conveying pump, the crude tetraethoxysilane is fed from the middle upper part of a tetraethoxysilane lightness-removing rectifying tower T01 tower, and the rectifying temperature is 165 ℃; the pressure is 0 bar; the condensation temperature at the top of the tower is 120 ℃ during the light component removal rectification; the reflux ratio of the light component removal rectification is 20; removing unreacted ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and other light components in the ethyl orthosilicate by light-component removal rectification; the mass of the removed light components is 1/12 of the mass of the crude tetraethoxysilane.
Conveying the product subjected to light component removal rectification to an adsorber at a flow rate of 0.5m/s by a discharge pump of a tetraethoxysilane light component removal rectification tower, wherein spherical active carbon (with the granularity of 5mm), strong-acid styrene cation exchange resin (with the aperture of 1nm) and titanium dioxide nanotubes are sequentially filled in the flow direction of salt tetraethoxysilane in the adsorber, the volume ratio of the spherical active carbon to the salt tetraethoxysilane in the adsorber is 1:1:1, and the layer heights of the spherical active carbon to the salt tetraethoxysilane in the adsorber are all 1m, so as to obtain the product subjected to adsorption treatment.
The product after adsorption treatment enters an ethyl orthosilicate de-heavy rectification tower T02 through a delivery pump at the flow velocity of 0.5m/s, and is fed from the middle lower part of the tower, and the rectification temperature is 168 ℃; the pressure is 0 bar; the condensation temperature of the tower top during the heavy component removal rectification is 123 ℃; the reflux ratio of the heavy component removal rectification is 18; removing the weight components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate, wherein the mass of the removed weight components is 1/11 of the mass of the product after adsorption treatment; condensing the tower top by a condenser to obtain high-purity ethyl orthosilicate, wherein the purity of the components can reach more than 5N, and the indexes of metal ions and the like reach 9N.
Comparative example 1
The flow rate of the crude tetraethoxysilane is 0.7m/s, the crude tetraethoxysilane is fed from a crude tetraethoxysilane storage tank through a feeding conveying pump, the crude tetraethoxysilane is fed from the middle upper part of a tetraethoxysilane lightness-removing rectifying tower T01 tower, and the rectifying temperature is 140 ℃; the pressure is-0.5 bar; the condensation temperature at the top of the tower is 100 ℃ during the light component removal rectification; the reflux ratio of the light component removal rectification is 6; removing unreacted ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and other light components in the ethyl orthosilicate by light-component removal rectification; the mass of the removed light components is 1/4 of the mass of the crude tetraethoxysilane.
Conveying the product subjected to light component removal rectification to an adsorber at a flow rate of 0.7m/s by a discharge pump of a tetraethoxysilane light component removal rectification tower, wherein the adsorber is sequentially filled with strong-acid styrene cation exchange resin (the aperture is 3nm) and titanium dioxide nanotubes in the flowing direction of tetraethoxysilane, the volume ratio of the strong-acid styrene cation exchange resin to the titanium dioxide nanotubes is 1:1, and the layer height of the titanium dioxide nanotubes is 2m, so as to obtain the product subjected to adsorption treatment.
The product after adsorption treatment enters an ethyl orthosilicate de-heavy rectification tower T02 through a delivery pump at the flow velocity of 0.7m/s, and is fed from the middle lower part of the tower, and the rectification temperature is 120 ℃; the pressure was-0.8 bar; the condensation temperature of the tower top during the heavy component removal and rectification is 80 ℃; the reflux ratio of the heavy component removal rectification is 7; removing the weight components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate, wherein the mass of the removed weight components is 1/5 of the mass of the product after adsorption treatment; condensing the tower top by a condenser to obtain the de-heavy rectified tetraethoxysilane.
The results of detection of the ethyl orthosilicate obtained in comparative example 1 after the heavy distillation are shown in the following table.
Detection result of ethyl orthosilicate after heavy distillation obtained in comparative example 1
Comparative example 2
The flow rate of the crude tetraethoxysilane is 1.3m/s, the crude tetraethoxysilane is fed from a crude tetraethoxysilane storage tank through a feeding conveying pump, the crude tetraethoxysilane is fed from the middle upper part of a tetraethoxysilane lightness-removing rectifying tower T01 tower, and the rectifying temperature is 195 ℃; the pressure was 0.3 bar; the condensation temperature at the top of the tower during the light component removal rectification is 140 ℃; the reflux ratio of the light component removal rectification is 13; removing unreacted ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and other light components in the ethyl orthosilicate by light-component removal rectification; the mass of the removed light components is 1/9 of the mass of the crude tetraethoxysilane.
And (3) conveying the product subjected to light component removal rectification to an adsorber at a flow speed of 1.3m/s by using a discharge pump of a tetraethoxysilane light component removal rectification tower, wherein spherical activated carbon (with the granularity of 4mm) and titanium dioxide nanotubes are sequentially filled in the flow direction of the tetraethoxysilane in the adsorber, the volume ratio of the spherical activated carbon to the titanium dioxide nanotubes is 1:1, and the layer height of the spherical activated carbon to the titanium dioxide nanotubes is 2m, so as to obtain the product subjected to adsorption treatment.
The product after adsorption treatment enters an ethyl orthosilicate de-heavy rectification tower T02 through a delivery pump at the flow velocity of 1.3m/s, and is fed from the middle lower part of the tower, and the rectification temperature is 190 ℃; the pressure was 0.3 bar; the condensation temperature of the tower top during the heavy component removal rectification is 135 ℃; the reflux ratio of the heavy component removal rectification is 15; removing the weight components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate, wherein the mass of the removed weight components is 1/10 of the mass of the product after adsorption treatment; condensing the tower top by a condenser to obtain the de-heavy rectified tetraethoxysilane.
The results of detection of the ethyl orthosilicate obtained in comparative example 2 after the heavy distillation are shown in the following table.
Detection result of ethyl orthosilicate after heavy distillation obtained in comparative example 2
Comparative example 3
The flow rate of the crude tetraethoxysilane is 1m/s, the crude tetraethoxysilane is fed from a crude tetraethoxysilane storage tank through a feeding conveying pump, the crude tetraethoxysilane is fed from the middle upper part of a tetraethoxysilane lightness-removing rectifying tower T01 tower, and the rectifying temperature is 178 ℃; the pressure was 0.1 bar; the condensation temperature at the top of the tower is 110 ℃ during the light component removal rectification; the reflux ratio of the light component removal rectification is 17; removing unreacted ethanol, triethoxysilane, methyltriethoxysilane, methoxytriethoxysilane and other light components in the ethyl orthosilicate by light-component removal rectification; the mass of the removed light components is 1/13 of the mass of the crude tetraethoxysilane.
Conveying the product subjected to light component removal rectification to an adsorber at a flow rate of 1m/s by a discharge pump of a tetraethoxysilane light component removal rectification tower, wherein spherical active carbon (with the granularity of 2mm) and strong-acid styrene cation exchange resin (with the aperture of 0.5nm) are sequentially filled in the flow direction of tetraethoxysilane in the adsorber, the volume ratio of the spherical active carbon to the strong-acid styrene cation exchange resin is 1:1, and the layer height of the spherical active carbon to the layer height of the strong-acid styrene cation exchange resin is 1.3, so as to obtain the product subjected to adsorption treatment.
The product after adsorption treatment enters an ethyl orthosilicate de-heavy rectifying tower T02 through a delivery pump at the flow velocity of 1m/s, and is fed from the middle lower part of the tower, and the rectifying temperature is 172 ℃; the pressure is 0 bar; the condensation temperature at the top of the tower is 120 ℃ during the heavy component removal and rectification; the reflux ratio of the heavy component removal rectification is 13; removing the weight components such as propyltriethoxysilane, ethyl orthosilicate dimer, ethyl orthosilicate trimer and the like in the ethyl orthosilicate, wherein the mass of the removed weight components is 1/15 of the mass of the product after adsorption treatment; condensing the tower top by a condenser to obtain the de-heavy rectified tetraethoxysilane.
The results of detection of the ethyl orthosilicate obtained in comparative example 3 after the heavy distillation are shown in the following table.
Detection result of ethyl orthosilicate after heavy distillation obtained in comparative example 3
Claims (5)
1. A method for producing tetraethoxysilane is characterized by comprising the following steps:
s1) carrying out lightness-removing rectification on the crude product of the tetraethoxysilane to obtain a product after lightness-removing rectification; the temperature of light component removal rectification is 160-190 ℃; the reflux ratio of the light component removal rectification is 8-25;
s2) treating the product after light component removal and rectification by an adsorber to obtain a treated product; spherical activated carbon, cation exchange resin and titanium dioxide nanotubes are sequentially filled in the adsorber; the volume ratio of the spherical activated carbon to the cation exchange resin to the titanium dioxide nanotube is (0.5-2): (0.5-2): (0.5 to 2); the cation exchange resin is strong-acid styrene cation exchange resin, and the aperture is 0.5-5 nm;
s3) carrying out de-weighting rectification on the treated product to obtain tetraethoxysilane; the temperature of the de-heavy distillation is 160-190 ℃; the reflux ratio of the de-heavy rectification is 8-25.
2. The production method according to claim 1, wherein the volume ratio of the spherical activated carbon, the cation exchange resin and the titanium dioxide nanotubes is 1:1: 1.
3. the production method according to claim 1, wherein the number of theoretical plates of a rectifying tower used for the light component removal rectification is 50-150.
4. The production method according to claim 1, wherein the number of theoretical plates of a rectifying column used for the de-heavy distillation is 50 to 150.
5. The production method according to claim 1, wherein the flow rate of the product after the light ends removal and rectification in the step S2) is 0.1-1 m/S.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
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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. |