CN106904617B - Device for preparing electronic-grade dichlorosilane - Google Patents
Device for preparing electronic-grade dichlorosilane Download PDFInfo
- Publication number
- CN106904617B CN106904617B CN201710226794.7A CN201710226794A CN106904617B CN 106904617 B CN106904617 B CN 106904617B CN 201710226794 A CN201710226794 A CN 201710226794A CN 106904617 B CN106904617 B CN 106904617B
- Authority
- CN
- China
- Prior art keywords
- tower
- dichlorosilane
- heavy
- removal tower
- purification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10778—Purification
- C01B33/10784—Purification by adsorption
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a device for preparing electronic-grade dichlorosilane. Wherein, the device includes: the reactor is used for reacting aromatic aldehyde or derivatives of the aromatic aldehyde with the raw material dichlorosilane; the purifying tower is used for removing partial heavy components, light components and residual heavy components of reaction products in the reactor to obtain electronic-grade dichlorosilane; and the adsorption purification unit is used for further removing impurities from the dichlorosilane to obtain the electronic-grade dichlorosilane.
Description
Technical Field
The invention relates to the field of chemical industry, and particularly relates to a device for preparing electronic-grade dichlorosilane.
Background
The electronic-grade dichlorosilane belongs to silicon source electronic special gas, is mainly used for silicon source gas of silicon epitaxial wafers, and is mainly used for oriented overgrowth of crystalline silicon, preparation of silicon nitride and preparation of polycrystalline silicon in large-scale integrated circuits at present. At present, the electronic information industry develops rapidly, dichlorosilane electronic gas is used as a raw material, the market demand of the dichlorosilane electronic gas is continuously increased, but the yield of dichlorosilane with electronic grade above China is insufficient, and the high-purity dichlorosilane electronic gas is seriously dependent on overseas markets.
The market demand scale of the dichlorosilane electronic gas is continuously increased, but the electronic-grade dichlorosilane yield in China is basically not high, and the market is totally dependent on overseas markets. At present, the high-purity dichlorosilane is produced mainly by using a traditional purification mode of purification towers, the purification is realized by connecting a plurality of towers in series, the energy consumption is high, the process is not easy to control, and the impurities exist in a complex compound form, have a boiling point close to that of dichlorosilane, are not easy to purify and can only be purified to the solar grade. Therefore, a new process needs to be developed, on one hand, the production of electronic-grade dichlorosilane is realized, on the other hand, the number of purification towers is reduced, and the energy consumption of purification operation is reduced.
Disclosure of Invention
The invention aims to provide a device for preparing electronic-grade dichlorosilane, which aims to solve the technical problems of high energy consumption and unstable product quality in the prior art for preparing electronic-grade dichlorosilane.
In order to achieve the above object, according to one aspect of the present invention, an apparatus for preparing electronic-grade dichlorosilane is provided. The device includes: the reactor is used for reacting aromatic aldehyde or derivatives of the aromatic aldehyde with the raw material dichlorosilane; the purifying tower is used for removing partial heavy components, light components and residual heavy components of reaction products in the reactor to obtain electronic-grade dichlorosilane; and the adsorption purification unit is used for further removing impurities from the dichlorosilane to obtain the electronic-grade dichlorosilane.
And further, the purification tower comprises a first heavy-duty removal tower, a light-duty removal tower and a second heavy-duty removal tower which are sequentially communicated with the reactor, wherein the light-duty removal tower and the second heavy-duty removal tower are thermally coupled by differential pressure, the top gas phase of the second heavy-duty removal tower is used as a reboiler heat source of the light-duty removal tower and then returns to the second heavy-duty removal tower, and partial products are extracted into an adsorption purification unit after condensation.
Further, the operating pressure range of the light component removal tower is 0.05-0.3 MPa, the operating pressure range of the second heavy component removal tower is 0.25-0.8 MPa, and the pressure difference range of the light component removal tower and the second heavy component removal tower is 0.2-0.5 MPa; the average temperature of the heating medium in the reboiler of the lightness-removing column is 20-70 ℃ higher than the average temperature of the cooling medium.
Furthermore, the purification tower is a packed tower or a sieve plate tower, the material of the purification tower is 316L stainless steel, the inner wall of the purification tower is subjected to electrolytic polishing, the surface roughness is 0.1-0.5 mu m, a pipeline in contact with the materials is an electrolytic polishing pipeline made of 316L stainless steel, and a valve is a diaphragm valve.
Further, the reactor has the functions of temperature control, pressure control and stirring; and the reactor is magnetically sealed and is provided with more than two layers of stirring paddles.
Furthermore, the adsorption purification unit comprises one or more adsorption columns, and the packing in the adsorption columns is polymeric resin or activated carbon which is complexed with corresponding functional groups, wherein the polymeric resin is used for adsorbing B, P and metal impurities according to the functional groups, and the metal impurities comprise Al, Fe, Cr or Ni.
Furthermore, the height-diameter ratio of the adsorption column is between 2 and 10, the temperature is between 20 and 70 ℃, the pressure is between 0.2 and 1.0Mpa, the material of the adsorption column is 316L stainless steel, the inner wall is electropolished, and the surface roughness is between 0.1 and 0.5 mu m.
The technical scheme includes that a chemical reagent aromatic aldehyde or an aromatic aldehyde derivative is adopted to react with impurities in dichlorosilane, groups in the reaction reagent are chlorinated and subjected to addition reaction to generate a high molecular polymer, the polymer is combined with impurities such as boron, phosphorus and the like in chlorosilane in a covalent bond mode or physically adsorbed to enable the boiling point to be far higher than that of the chlorosilane, then the polymer is purified by three subsequent towers, part of heavy components are removed, light components and the rest of the heavy components are removed to obtain a purified product, the purified product is sent to an adsorption purification unit, impurities are further removed, and electronic-grade dichlorosilane is obtained. The reaction product is subjected to partial heavy component removal, and then the light component and the residual heavy component removal process can adopt a two-tower differential pressure thermal coupling technology, and a gas-phase material at the top of the second heavy component removal tower is used as a heating medium of a reboiler of the light component removal tower, so that the heating energy loss of the reboiler at the tower bottom of the light component removal tower can be saved, the energy consumption of a condenser at the top of the second heavy component removal tower can be saved, the purification energy consumption is greatly reduced, and the low-cost production of electronic-grade dichlorosilane can be realized. Meanwhile, in order to reduce the fluctuation of the product quality and ensure the stability of the system, the adsorption and purification unit is arranged, so that the influence of the fluctuation of the rectifying tower on the product quality can be reduced, and the product quality is further improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 shows a schematic flow diagram for preparing electronic-grade dichlorosilane according to an embodiment of the present invention; and
fig. 2 shows a schematic structural diagram of an apparatus for preparing electronic-grade dichlorosilane according to an embodiment of the invention.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In a typical embodiment of the invention, the method for preparing electronic-grade dichlorosilane comprises the following steps: s1, reacting aromatic aldehyde or derivatives of the aromatic aldehyde with raw material dichlorosilane to obtain reaction products; s2, removing part of heavy components from the reaction product, wherein the heavy components contain a large amount of chemical reagents and can be returned to the chemical reactor for reuse, so that the material consumption is reduced, and then removing the light components and the rest heavy components to obtain a purified product; and S3, feeding the purified product into an adsorption purification unit, and further removing impurities to obtain the electronic-grade dichlorosilane.
By applying the technical scheme of the invention, as shown in figure 1, firstly, a chemical reagent aromatic aldehyde or a derivative of the aromatic aldehyde is adopted to react with dichlorosilane, namely, a reaction process, groups in the reaction reagent are chlorinated and subjected to addition reaction to generate a high molecular polymer, the polymer and impurities such as boron, phosphorus and the like in chlorosilane can be bonded through valence bonds or physically adsorbed, so that the boiling point is far higher than that of the chlorosilane, and then the polymer is purified by two subsequent towers, namely, a purification process, and a purified product is obtained through weight removal, light weight removal and weight removal; and (4) feeding the purified product into an adsorption purification unit, and further removing impurities to obtain the electronic-grade dichlorosilane. Wherein, partial heavy components are firstly removed from the reaction product, and then a two-tower differential pressure thermal coupling technology can be adopted in the process of removing the light components and the residual heavy components, so that the purification energy consumption is greatly reduced, and the low-cost production of the electronic-grade dichlorosilane is realized. Meanwhile, in order to reduce the fluctuation of the product quality, an adsorption and purification unit is arranged, so that the influence of the fluctuation of the rectifying tower on the product quality is reduced, and the product quality is further improved. Compared with the prior art, the boiling point difference between the chemical reaction reagent and impurities, and between the produced high-boiling-point substance and dichlorosilane is increased, the separation is easier, the original rectification of more than six towers is reduced to the existing three-tower rectification, the flow is greatly shortened, and meanwhile, the two towers adopt the thermal coupling technology, so that the cold quantity and the heat quantity of the purification tower can be saved, and the equipment investment and the operation energy consumption are reduced.
Preferably, the mass percentage of the dichlorosilane in the raw material dichlorosilane is 98-99%.
Preferably, the aromatic aldehyde or the derivative of the aromatic aldehyde is one or more selected from the group consisting of benzaldehyde, 3, 4-dimethylbenzaldehyde, 4-methylbenzaldehyde, o-phthalaldehyde, p-nitrobenzaldehyde, p-methoxybenzaldehyde, cinnamaldehyde, α -methylcinnamaldehyde, α -pentylcinnamaldehyde, α -hexylcinnamaldehyde.
When the amount of the aromatic aldehyde or the aromatic aldehyde derivative added is small, impurities tend to remain, and when the amount is too large, it is uneconomical. Preferably, in S1, the molar ratio of the aromatic aldehyde and/or the derivative of the aromatic aldehyde to the impurities in the raw material dichlorosilane is 100-10000: 1.
In S1, when the temperature is lower than 0 ℃, the conversion efficiency is low, when the temperature is higher than 100 ℃, the chemical reagent can generate byproducts, the formed high boiling point substance can be decomposed, preferably, the reaction pressure is controlled to be 0-8 bar, the reaction temperature is controlled to be 0-170 ℃, and the reaction time is 20 min-48 hours.
To enhance the reaction and improve the efficiency, S1 includes stirring the reactants during the reaction.
In a typical embodiment of the present invention, the chemical reaction of S1 and the purification in the purification tower of S2 may be performed continuously and cyclically, wherein the purification in the tower is the main step of impurity removal and chlorosilane separation, the tower may be a packing or sieve plate tower, and three towers may be used for purification, and the purification in the tower sequentially comprises one heavy component removal (first heavy component removal tower), one light component removal (light component removal tower), one heavy component removal (second heavy component removal tower), and the product is electronic-grade dichlorosilane. The high boiling residue in the first heavy component removal tower contains a large amount of chemical reagents, and can be simply separated and then returned to the chemical reaction step for reuse. The light component removal tower and the second heavy component removal tower adopt a differential pressure thermal coupling technology, and the gas phase at the top of the second heavy component removal tower is used as a heat source of a reboiler of the light component removal tower, so that the purification energy consumption can be greatly reduced.
According to a typical embodiment of the invention, an apparatus for preparing electronic-grade dichlorosilane is provided, as shown in fig. 2, the apparatus comprises a reactor 10 for reacting aromatic aldehyde or aromatic aldehyde derivatives with raw dichlorosilane, an adsorption purification unit for removing a part of heavy components from reaction products in the reactor, and then removing light components and residual heavy components, and an adsorption purification unit for further removing impurities from the purified products, preferably, the purification tower comprises a first heavy component removal tower 21, a light component removal tower 22 and a second heavy component removal tower 23 which are sequentially communicated with the reactor, the purification tower can be a packed tower or a sieve plate tower, the material of the purification tower is 316 stainless steel, the inner wall of the purification tower is electrolytically polished, the surface roughness is 0.05-0.5 μm, a pipeline in contact with the material is an electrolytic polishing pipeline made of 316L stainless steel, valves are selected, the reactor 10 is a reactor with temperature control, pressure control and stirring functions, the aromatic aldehyde or aromatic aldehyde derivatives and the raw dichlorosilane derivatives enter a first heavy component removal column, a second component removal column, a heavy component removal column 21, a heavy component removal column, a heavy component removal purification column, a heavy component removal column, a metal removal column, a heavy component removal column, a metal removal column, a metal removal column, a membrane removal column, a metal removal column, a.
According to a typical embodiment of the invention, the purification tower consists of two towers, namely a light component removal tower and two heavy component removal towers, wherein the first heavy component removal tower removes heavy components, the light component removal tower removes low-boiling products, the second heavy component removal tower removes products and high-boiling products, each tower is provided with a reboiler and a condenser, the light component removal tower and the second heavy component removal tower are thermally coupled by differential pressure, the gas phase at the top of the second heavy component removal tower is used as a heat source of the reboiler of the light component removal tower, the gas phase returns to the second heavy component removal tower after heat exchange, and part of the gas phase is extracted into an adsorption device. Preferably, the operating pressure range of the light component removal tower is 0.05-0.3 MPa, the operating pressure range of the second heavy component removal tower is 0.25-0.8 MPa, and the pressure difference range of the two towers is 0.2-0.5 MPa; the average temperature of the heating medium in the reboiler of the light component removal tower is 20-70 ℃ higher than the average temperature of the cooling medium.
The parameters of tower diameter, tower height, tower tray number, internals, packing and the like of the tower, and the feeding, reflux and height of the three towers are set through simulation calculation and purification operation experienceThe low-boiling discharge amount needs to be in a specified range, the materials of the tower and the internal parts are 316L, meanwhile, the inner wall of the tower and the internal parts are subjected to electrolytic polishing, the method is adopted for the first time in the field of polysilicon purification, in order to better control the process, nitrogen of the system needs to be provided with a purifier, and the purified nitrogen H2O，O2The content is less than 1ppb, high-purity nitrogen is replaced before the system operates to ensure that the contents of oxygen, water and the like in the equipment are within the required range, the material pipeline is a 316L electrolytic polishing pipe, a diaphragm valve is adopted as a valve, the reactor is a reactor with temperature control, pressure control and stirring functions, the material is 316L, the internal electrolytic polishing is realized, stepless speed change is adopted, the stirring speed is convenient to control, magnetic sealing is adopted, the sealing effect is good, and no leakage is ensured during operation.
Preferably, chlorosilane and aromatic aldehyde or derivatives of aromatic aldehyde are controlled to enter a reactor in a certain proportion, and then enter a subsequent purification tower after full reaction in the reactor, so that parameters such as temperature, pressure, reaction time and the like of the reaction are ensured to be within a required range, the situation that impurities cannot react fully can be prevented, the concentration of a chemical reagent is increased, the conversion speed of the impurities is also increased, and when the concentration is too high, the recovery of excessive compounds needs to be considered, so that the material consumption is reduced. The chlorosilane entering the purification step contains excessive chemical reagents and high boiling point substances formed by impurity molecules, the purified chlorosilane can reach an electronic grade and can be used as a raw material for producing semiconductor polycrystalline silicon, the discharge of a tower kettle contains chlorosilane, the chemical reagents and the high boiling point impurities, the high boiling point substances can be separated, and the chlorosilane and the chemical reagents are returned to the impurity conversion step for reuse.
The following examples are provided to further illustrate the advantageous effects of the present invention.
Example 1
The flow shown in FIG. 1 was used, the apparatus shown in FIG. 2 was used, and the specific test parameters are shown in Table 1.
TABLE 1
Under the conditions, the purity of the dichlorosilane product reaches 9N, the impurity content of B is 0.06ppb, the impurity content of P is 0.08ppb, and the impurity content of Al is 0.06 ppb.
Example 2
The flow shown in FIG. 1 was used, the apparatus shown in FIG. 2 was used, and the specific test parameters are shown in Table 2.
TABLE 2
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.02ppb, and the content of P impurities is 0.04ppb and Al impurities is 0.04 ppb.
Example 3
The procedure shown in FIG. 1 was followed using the apparatus shown in FIG. 2, and the experimental parameters are shown in Table 3.
TABLE 3
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.01ppb, and the content of P impurities is 0.03ppb, and the content of Al impurities is 0.03 ppb.
Example 4
The procedure shown in FIG. 1 was followed using the apparatus shown in FIG. 2, and the experimental parameters are shown in Table 4.
TABLE 4
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.02ppb, and the content of P impurities is 0.05ppb, and the content of Al impurities is 0.05 ppb.
Example 5
The procedure shown in FIG. 1 was followed using the apparatus shown in FIG. 2, and the experimental parameters are shown in Table 5.
TABLE 5
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.03ppb, and the content of P impurities is 0.06ppb, and the content of Al impurities is 0.04 ppb.
Example 6
The procedure shown in FIG. 1 was followed using the apparatus shown in FIG. 2, and the experimental parameters are shown in Table 6.
TABLE 6
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.08ppb, and the content of P impurities is 0.07ppb, and the content of Al impurities is 0.09 ppb.
Example 7
The procedure shown in FIG. 1 was followed using the apparatus shown in FIG. 2, and the experimental parameters are shown in Table 7.
TABLE 7
Under the conditions, the purity of the dichlorosilane product reaches 9N, the content of B impurities is 0.09ppb, and the content of P impurities is 0.08ppb, and the content of Al impurities is 0.10 ppb.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1) the dichlorosilane is purified by adopting a reaction and rectification mode, the dichlorosilane can be purified to the purity of a semiconductor application level by only adopting one pretreatment tower (a first heavy-removing tower) and two rectification towers (a light-removing tower and a second heavy-removing tower) on the basis of chemical reaction, the number of purification towers is reduced, and meanwhile, the light-removing tower and the second heavy-removing tower adopt a differential pressure thermal coupling technology, so that the consumption of steam and condensed water is greatly reduced;
2) the chemical reaction adopts aromatic aldehyde and derivatives thereof to react with impurities in the aromatic aldehyde to produce high boiling point substances, so that the aromatic aldehyde and derivatives thereof can be removed more easily;
3) the pretreatment tower is adopted to separate redundant chemical reagents and return the chemical reagents to the chemical reaction step for reuse, so that the generation amount of waste and the consumption amount of the reagents are reduced;
4) the purifying tower adopts internal electrolytic polishing, controls high cleanliness and belongs to the field of polysilicon purification for the first time;
5) the method is different from reactive distillation, a reaction and distillation mode is adopted, the reaction and the distillation belong to two independent units, and the reaction time, the temperature and the proportion of reagents, and the mixing and the replacement of chemical reagents are easier to realize;
6) the distillation tower adopts low-temperature low-pressure distillation, so that the dichlorosilane and the impurity compound are easier to separate, and the product quality can be further ensured by matching with chemical reaction;
7) the adsorption purification unit is arranged, the adsorption columns can realize parallel or serial operation as required, and the filler in the adsorption columns is complex polymer resin or active carbon which can selectively adsorb B, P and metal impurities, so that the product quality is further ensured.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (1)
1. A device for preparing electronic-grade dichlorosilane is characterized by comprising the following components:
the reactor is used for reacting aromatic aldehyde or derivatives of the aromatic aldehyde with the raw material dichlorosilane;
the purification tower is used for removing part of heavy components, light components and the rest heavy components of the reaction product in the reactor to obtain a purified product; and
the adsorption and purification unit is used for further removing impurities from the purified product to obtain electronic-grade dichlorosilane;
the purification tower comprises a first heavy-duty removal tower, a light-duty removal tower and a second heavy-duty removal tower which are sequentially communicated with the reactor, wherein the light-duty removal tower and the second heavy-duty removal tower are thermally coupled by differential pressure, the top gas phase of the second heavy-duty removal tower is used as a reboiler heat source of the light-duty removal tower and then returns to the second heavy-duty removal tower, partial products are collected into the adsorption and purification unit after condensation, the operating pressure range of the light-duty removal tower is 0.05-0.3 MPa, the operating pressure range of the second heavy-duty removal tower is 0.25-0.8 MPa, the differential pressure range of the light-duty removal tower and the second heavy-duty removal tower is 0.2-0.5 MPa, the average temperature of a heating medium in the reboiler of the light-duty removal tower is 20-70 ℃ higher than that of a cooling medium, the purification tower is a filler tower or a sieve plate tower, the purification tower is made of 35316 stainless steel, the inner wall of the purification tower is subjected to electrolytic polishing, the surface roughness of 0.1-0.5 mu m, the surface roughness of a diaphragm valve is in contact with a magnetic force of a material, the adsorption column is used for the adsorption of a metal, the adsorption column, the adsorption unit is used for the adsorption of a high-0.5 mu m, the adsorption column, the adsorption unit is used for the high-0.2-0.3-0.5 mu m metal, the high-0.5-0.3-0.5-0.3-mm metal complex reaction of the metal, the high-0-0.3-0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710226794.7A CN106904617B (en) | 2017-04-06 | 2017-04-06 | Device for preparing electronic-grade dichlorosilane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710226794.7A CN106904617B (en) | 2017-04-06 | 2017-04-06 | Device for preparing electronic-grade dichlorosilane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106904617A CN106904617A (en) | 2017-06-30 |
| CN106904617B true CN106904617B (en) | 2020-07-21 |
Family
ID=59194395
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710226794.7A Active CN106904617B (en) | 2017-04-06 | 2017-04-06 | Device for preparing electronic-grade dichlorosilane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106904617B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107572535A (en) * | 2017-09-22 | 2018-01-12 | 洛阳中硅高科技有限公司 | Prepare the device of dichlororosilane eiectronic grade |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102661654A (en) * | 2012-05-02 | 2012-09-12 | 北京华宇同方化工科技开发有限公司 | Method and system for preparing high purity gas by rectification method |
| CN102701216A (en) * | 2012-06-19 | 2012-10-03 | 中国恩菲工程技术有限公司 | Impurity removing method for dichlorosilane |
| CN202924742U (en) * | 2012-08-08 | 2013-05-08 | 中国恩菲工程技术有限公司 | Dichlorosilane impurity removing equipment |
| CN103201218A (en) * | 2010-10-27 | 2013-07-10 | 信越化学工业株式会社 | Method for purifying chlorosilanes |
| CN206624653U (en) * | 2017-04-06 | 2017-11-10 | 洛阳中硅高科技有限公司 | A kind of device for preparing dichlororosilane eiectronic grade |
-
2017
- 2017-04-06 CN CN201710226794.7A patent/CN106904617B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103201218A (en) * | 2010-10-27 | 2013-07-10 | 信越化学工业株式会社 | Method for purifying chlorosilanes |
| CN102661654A (en) * | 2012-05-02 | 2012-09-12 | 北京华宇同方化工科技开发有限公司 | Method and system for preparing high purity gas by rectification method |
| CN102661654B (en) * | 2012-05-02 | 2014-04-30 | 北京华宇同方化工科技开发有限公司 | Method and system for preparing high purity gas by rectification method |
| CN102701216A (en) * | 2012-06-19 | 2012-10-03 | 中国恩菲工程技术有限公司 | Impurity removing method for dichlorosilane |
| CN102701216B (en) * | 2012-06-19 | 2015-06-03 | 中国恩菲工程技术有限公司 | Impurity removing method for dichlorosilane |
| CN202924742U (en) * | 2012-08-08 | 2013-05-08 | 中国恩菲工程技术有限公司 | Dichlorosilane impurity removing equipment |
| CN206624653U (en) * | 2017-04-06 | 2017-11-10 | 洛阳中硅高科技有限公司 | A kind of device for preparing dichlororosilane eiectronic grade |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106904617A (en) | 2017-06-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106927468A (en) | A kind of device for preparing electron level trichlorosilane | |
| KR101292545B1 (en) | Apparatus for purifying trichlorosilane and method of purifying trichlorosilane | |
| CN101249312A (en) | Separation apparatus and method of high precision rectification purify trichlorosilane | |
| CN105502295A (en) | Electronic grade hydrogen chloride purification method | |
| CN107055550B (en) | Method for preparing electronic-grade dichlorosilane | |
| CN113247908B (en) | Separation method and separation device for chlorosilane in polysilicon production | |
| US20240042343A1 (en) | Production system, production method and application of general-purpose high-purity chemicals | |
| CN104030293B (en) | A kind of silicon tetrachloride purifying technique and system | |
| CN102923714A (en) | Next-door thermal coupling distillation method and equipment for producing polycrystalline silicon | |
| CN110642229A (en) | Mixed analysis purification process and mixed analysis purification device for siloxane-containing hydrochloric acid and organic matter-containing sulfuric acid | |
| CN106904617B (en) | Device for preparing electronic-grade dichlorosilane | |
| CN110078024B (en) | Method and device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas as byproduct of organochlorosilane alcoholysis as raw material | |
| CN109279611B (en) | Method and device for removing impurities in chlorosilane | |
| CN107648976B (en) | Method for preparing ultra-high-purity gas through low-temperature separation and low-temperature separation system | |
| CN115105850B (en) | Electronic grade trichlorosilane purifying device and method | |
| CN111269079B (en) | Preparation system and preparation method of perfluoro 1, 3-butadiene | |
| CN103153420A (en) | Processes and systems for purifying silane | |
| CN100374184C (en) | A process and apparatus for purifying hydrogen bromide | |
| CN206624653U (en) | A kind of device for preparing dichlororosilane eiectronic grade | |
| CN207596482U (en) | A kind of rectifying device for purifying trichlorosilane | |
| CN206624652U (en) | A kind of device for preparing electron level trichlorosilane | |
| CN102502701A (en) | Production process and preparation method of ultrapure ammonia | |
| CN112744787B (en) | FTrPSA separation and purification method for deeply defluorinating and drying HCl gas containing high-concentration HF | |
| CN107055549A (en) | A kind of method for preparing electron level trichlorosilane | |
| KR102012535B1 (en) | Processes and systems for purifying silane |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Liu Jianhua Inventor after: Yan Dazhou Inventor after: Zhao Xiong Inventor after: Wan Ye Inventor after: Guo Shuhu Inventor after: Jiang Lixia Inventor after: Wang Fang Inventor after: Yang Yongliang Inventor after: Du Junping Inventor after: Tang Chuanbin Inventor before: Liu Jianhua Inventor before: Yan Dazhou Inventor before: Zhao Xiong Inventor before: Wan Ye Inventor before: Guo Shuhu Inventor before: Jiang Lixia Inventor before: Wang Fang Inventor before: Yang Yongliang Inventor before: Du Junping Inventor before: Tang Chuanbin |
|
| GR01 | Patent grant | ||
| GR01 | Patent grant |