CN114669071A - Vacuum rectification device and method for silicon-based electronic product - Google Patents
Vacuum rectification device and method for silicon-based electronic product Download PDFInfo
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- CN114669071A CN114669071A CN202210355468.7A CN202210355468A CN114669071A CN 114669071 A CN114669071 A CN 114669071A CN 202210355468 A CN202210355468 A CN 202210355468A CN 114669071 A CN114669071 A CN 114669071A
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 75
- 239000010703 silicon Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000002994 raw material Substances 0.000 claims abstract description 91
- 238000009835 boiling Methods 0.000 claims abstract description 63
- 239000000463 material Substances 0.000 claims abstract description 60
- 230000006837 decompression Effects 0.000 claims abstract description 25
- 230000008569 process Effects 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- 239000007789 gas Substances 0.000 claims description 90
- 230000001105 regulatory effect Effects 0.000 claims description 29
- 239000012071 phase Substances 0.000 claims description 26
- 238000012806 monitoring device Methods 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 24
- 239000002826 coolant Substances 0.000 claims description 21
- 239000007791 liquid phase Substances 0.000 claims description 21
- 239000003507 refrigerant Substances 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 17
- 239000011344 liquid material Substances 0.000 claims description 12
- 238000005086 pumping Methods 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 7
- LXEXBJXDGVGRAR-UHFFFAOYSA-N trichloro(trichlorosilyl)silane Chemical compound Cl[Si](Cl)(Cl)[Si](Cl)(Cl)Cl LXEXBJXDGVGRAR-UHFFFAOYSA-N 0.000 claims description 6
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 5
- 239000005049 silicon tetrachloride Substances 0.000 claims description 5
- 239000002912 waste gas Substances 0.000 claims description 5
- 239000005046 Chlorosilane Substances 0.000 claims description 4
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 claims description 4
- 239000003595 mist Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 3
- 239000007792 gaseous phase Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 24
- 239000000126 substance Substances 0.000 description 15
- 238000005292 vacuum distillation Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 150000001263 acyl chlorides Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- 238000003335 Production assurance Methods 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000000275 quality assurance Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000003303 reheating Methods 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
- B01D3/322—Reboiler specifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
- B01D3/4211—Regulation; Control of columns
- B01D3/4216—Head stream
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/04—Esters of silicic acids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a decompression rectification device and a decompression rectification method for a silicon-based electronic product, which comprise a raw material tank, a rectification device, a product tank and a recooling device; the rectifying device comprises a rectifying tower, a tower top condenser and a reboiler; the outlet of the reboiler is connected with a gas phase pipe at the bottom of the rectifying tower; a high-low boiling material outlet of the rectifying tower is connected with a high-low boiling tank; a condensed material outlet of the tower top condenser is respectively connected with a material return port of the rectifying tower and a product inlet of the product tank; the recooling device comprises a cold trap, a buffer tank, a vacuum pump and a deep cooler, wherein the cold trap is respectively connected with a gas circulation port of the raw material tank, an uncondensed gas outlet of the tower top condenser, a tank top gas pipeline of the product tank and a tank top gas pipeline of the high-low boiling tank, the buffer tank is connected with the uncondensed gas outlet of the cold trap, the vacuum pump is connected with the buffer tank, and the deep cooler is connected with the vacuum pump. The invention can solve the problems of higher operation temperature, high consumption of heating medium in the production process, long process of the traditional decompression rectification device, unstable control and the like in the prior art.
Description
Technical Field
The invention relates to the technical field of rectification, in particular to a decompression rectification device and method for a silicon-based electronic product.
Background
Silicon-based electronic products are indispensable raw materials in the manufacturing process of integrated circuits, and the purity of the silicon-based electronic products directly influences the quality of the integrated circuit products. At present, a rectification method is mostly used in a silicon-based electronic product purification method, and impurities are separated by utilizing the difference of the volatility of the impurities and the volatility of the product, so that a high-purity product is obtained. The rectification method for producing silicon-based electronic products is mostly normal pressure or pressurization rectification, for example, the patent No. CN109912636A mentions a production method of high-purity ethyl orthosilicate, which adopts differential pressure coupling rectification combined with adsorption treatment technology, and after treatment by two groups of rectification towers, metal ions are removed by adsorption treatment, and finally, the high-purity ethyl orthosilicate is obtained by two groups of rectification.
However, since some silicon-based electronic products have higher boiling points, such as hexachlorodisilane with a boiling point of 145 ℃ and tetraethoxysilane with a boiling point of 165 ℃ at normal pressure, if the traditional normal pressure or pressure rectification is adopted, the operation temperature is higher, and the consumption of heating media in the production process is high. It is well documented that silicon-based electronic products may decompose at high temperatures, which can affect the purity of the high purity product.
The vacuum rectification mode is adopted, so that the operation temperature can be reduced, and the consumption of the heating medium is reduced. Many devices for providing reduced pressure rectification in the field of chemical industry are provided, for example, a device and a method for improving vacuum degree of acyl chloride vacuum rectification are provided in the patent No. CN107998679A, the device comprises an acyl chloride rectification device, a vacuum buffer tank, an alkali injection device and a vacuum unit, the vacuum degree of a rectification system can be improved, and the quality of a rectification product is improved. For another example, patent No. CN107501100A discloses a vacuum pumping process system of m-phenylenediamine vacuum distillation tower, which comprises a distillation tower, a tower top condenser, a reflux tank, a buffer tank and a vacuum pump, and has the advantages of high heat exchange efficiency, low system energy consumption, long service life of equipment, and improved product yield.
However, the vacuum rectification device in the chemical industry has the disadvantages of long process flow and unstable control, and is not beneficial to the stable production and quality assurance of high-purity silicon-based electronic products, so that the vacuum rectification technology which is suitable for silicon-based electronic products and has short process flow and stable control is urgently needed to be provided.
Disclosure of Invention
In view of the above problems, an object of the present invention is to provide a vacuum distillation apparatus and method for silicon-based electronic products, so as to solve the problems of high operation temperature, high consumption of heating medium during the production process, long process of the conventional vacuum distillation apparatus, unstable control, etc. in the prior art.
The invention provides a decompression rectification device of a silicon-based electronic product, which comprises a raw material tank, a rectification device, a product tank and a recooling device, wherein the raw material tank is connected with the rectification device; wherein,
a raw material output port, a liquid material return port and a gas circulation port are arranged on the raw material tank;
the rectifying device comprises a rectifying tower connected with the raw material output port, an overhead condenser connected with an overhead gas outlet of the rectifying tower and a reboiler connected with a tower bottom liquid phase pipeline of the rectifying tower; the outlet of the reboiler is connected with a tower bottom gas phase pipe of the rectifying tower; a high-low boiling discharge port of the rectifying tower is connected with a high-low boiling tank; a condensed material outlet of the tower top condenser is respectively connected with a material return port of the rectifying tower and a product inlet of the product tank;
the sub-cooling device comprises a cold trap, a buffer tank, a vacuum pump and a deep cooler, wherein the cold trap is respectively connected with a gas flow port of the raw material tank, an uncondensed gas outlet of the tower top condenser, a tank top gas pipeline of the product tank and a tank top gas pipeline of the high-low boiling tank, the buffer tank is connected with the uncondensed gas outlet of the cold trap, the vacuum pump is connected with the buffer tank, and the deep cooler is connected with the vacuum pump;
the condensed material outlet of the cold trap, the liquid material outlet of the buffer tank and the condensed material outlet of the deep cooler are connected with the liquid material return port of the raw material tank, and the non-condensed gas outlet of the deep cooler is connected with an exhaust gas treatment system.
In addition, the preferable scheme is that a pressure gauge is arranged on the buffer tank; the pressure gauge is interlocked with a pumping speed control valve of the vacuum pump.
In addition, it is preferable that a first regulating valve, a second regulating valve, a third regulating valve and a fourth regulating valve are respectively arranged at an uncondensed gas outlet of the overhead condenser, at a gas flow port of the raw material tank, on a tank top gas pipeline of the product tank and on a tank top gas pipeline of the high-low boiling tank;
a first pressure monitoring device, a second pressure monitoring device, a third pressure monitoring device and a fourth pressure monitoring device are respectively arranged on the top of the rectifying tower, the top of the raw material tank, the top of the product tank and the top of the high-low boiling tank;
the first regulating valve and the first pressure monitoring device, the second regulating valve and the second pressure monitoring device, the third regulating valve and the third pressure monitoring device, and the fourth regulating valve and the fourth pressure monitoring device are interlocked respectively.
In addition, it is preferable that the reaction mixture,
the number of the rectifying devices is at least two; the rectification devices are connected in parallel or in series; wherein,
when the rectifying devices are connected in series, a rectifying tower in the first rectifying device in the series is connected with the raw material tank, and a tower bottom liquid phase pipeline of the rectifying tower in the previous rectifying device is connected with a feed inlet of the rectifying tower in the next rectifying device between the adjacent rectifying devices; and a condensed material outlet of the tower top condenser in the last rectifying device in the series is connected with the product tank, the last rectifying device is removed, and condensed material outlets of tower top condensers in other rectifying devices are connected with the high-low boiling tank.
In addition, the preferred scheme is that the rectifying tower is a tower or a packed tower; a tower plate is arranged in the rectifying tower, and a filling material is arranged on the tower plate; the number of the tower plates is 10-100;
and/or the reboiler is a vertical or horizontal heat exchanger; the heating medium of the reboiler is any one of water vapor, hot water and heat conducting oil;
and/or the tower top condenser is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the tower top condenser is circulating water or a refrigerant; the use temperature of a cooling medium of the overhead condenser is-60-50 ℃;
and/or the cold trap is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the cold trap is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃;
and/or the buffer tank is a vertical storage tank or a horizontal storage tank; the volume of the buffer tank is 0.2-2 m 3;
and/or the vacuum pump is any one of a screw vacuum pump, a roots vacuum pump and a reciprocating pump;
and/or the deep cooler is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the deep cooler is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃;
the raw material tank is a vertical storage tank or a horizontal storage tank; the volume of the raw material tank is 1-20 m 3;
and/or the product tank is a vertical storage tank or a horizontal storage tank; the volume of the product tank is 1-20 m 3;
and/or the high-low boiling tank is a vertical storage tank or a horizontal storage tank; the volume of the high-low boiling tank is 1-20 m 3.
In addition, preferably, the feed inlet of the raw material tank is connected with a conveying pipe for raw materials of the silicon-based electronic product.
In addition, it is preferable that the raw material of the silicon-based electronic product includes any one of silicon tetrachloride, hexachlorodisilane, tetraethoxysilane and chlorosilane or at least two of them mixed in any proportion.
In addition, the preferred scheme is that the motor of the vacuum pump is a variable frequency motor; the pumping speed of the vacuum pump is 0-100%.
In addition, the operating pressure of the decompression rectification device of the silicon-based electronic product is preferably lower than the atmospheric pressure.
The invention provides a decompression rectification method of a silicon-based electronic product, which utilizes the decompression rectification device of the silicon-based electronic product to carry out decompression distillation on the raw material of the silicon-based electronic product and comprises the following steps:
conveying the raw material of the silicon-based electronic product in the raw material tank into the rectifying tower, and rectifying the raw material by the rectifying tower to respectively obtain a gas phase and a liquid phase;
for the gas phase, the gas phase enters a tower top condenser through a tower top gas outlet of the rectifying tower, the gas phase is condensed through the tower top condenser, the obtained condensed material returns to the rectifying tower from one part of a condensed material outlet of the tower top condenser, the rectification is continued, and the other part of the condensed material enters the product tank; the liquid phase enters the reboiler through a tower bottom liquid phase pipeline of the rectifying tower, is reboiled by the reboiler and then returns to the rectifying tower in a gas form, and the liquid phase which is not reboiled enters a high-low boiling tank through a high-low boiling discharge hole of the rectifying tower and is gasified by the high-low boiling tank to obtain a gaseous material;
the gas phase that is not condensed in the tower top condenser, gaseous material in the high-low boiling tank, gas in the feed tank and the mist that the gas in the product jar formed all get into in the recooling device, pass through in proper order the cold trap with the deep cooler is right the mist carries out deep cooling, and the liquid material that obtains after the cooling returns the process of continuing circulation rectification in the feed tank again, and the waste gas that deep cooling produced carries out exhaust-gas treatment through exhaust treatment system.
According to the technical scheme, the reduced pressure rectification device and the method for the silicon-based electronic product can realize the reduced pressure rectification of the silicon-based electronic product through the structural design and the mutual connection relationship of the raw material tank, the rectification device, the product tank and the secondary cooling device, and compared with a reduced pressure rectification system in the traditional chemical industry, the reduced pressure rectification device has the advantages of simple process flow, stable and controllable operation pressure in the production process of the silicon-based electronic product, small fluctuation and contribution to ensuring the quality of a high-purity product; the reduced pressure rectification reduces the saturated vapor pressure of the materials in the operation process, the material quantity proportion entering the gas phase is reduced, meanwhile, the unnecessary consumption of the raw materials in the production process of the silicon-based electronic product can be greatly reduced through the design of the secondary cooling device, and compared with a normal pressure and pressurized rectification system, the unnecessary consumption of the raw materials in the production process is reduced.
To the accomplishment of the foregoing and related ends, one or more aspects of the invention comprise the features hereinafter fully described. The following description and the annexed drawings set forth in detail certain illustrative aspects of the invention. These aspects are indicative, however, of but a few of the various ways in which the principles of the invention may be employed. Further, the present invention is intended to include all such aspects and their equivalents.
Drawings
Other objects and results of the present invention will become more apparent and more readily appreciated as the same becomes better understood by reference to the following description taken in conjunction with the accompanying drawings. In the drawings:
FIG. 1 is a schematic diagram of a vacuum distillation apparatus for silicon-based electronic products according to an embodiment of the present invention;
fig. 2 is a process flow diagram of a vacuum rectification method of a silicon-based electronic product according to an embodiment of the invention.
In the attached figure, 1-a raw material tank, 21-a rectifying tower, 22-an overhead condenser, 23-a reboiler, 3-a product tank, 41-a cold trap, 42-a buffer tank, 43-a vacuum pump, 44-a deep cooler, 5-a high-low boiling tank, 61-a first regulating valve, 62-a second regulating valve, 63-a third regulating valve and 64-a fourth regulating valve.
The same reference numbers in all figures indicate similar or corresponding features or functions.
Detailed Description
In the following description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of one or more embodiments. It may be evident, however, that such embodiment(s) may be practiced without these specific details.
Aiming at the problems of higher operating temperature, high consumption of heating medium in the production process, long process of the traditional vacuum rectification device, unstable control and the like in the prior art, the vacuum rectification device and the method for the silicon-based electronic product are provided.
Specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
In order to illustrate the vacuum rectification apparatus and method for silicon-based electronic products provided by the present invention, fig. 1 shows the structure of the vacuum rectification apparatus for silicon-based electronic products according to an embodiment of the present invention; fig. 2 shows a process flow of a vacuum rectification method of a silicon-based electronic product according to an embodiment of the invention.
As shown in the figure 1 and the figure 2 together, the invention provides a silicon-based electronic product vacuum rectification device, which comprises a raw material tank 1, a rectification device, a product tank 3 and a sub-cooling device; wherein, a raw material output port, a liquid material return port and a gas circulation port are arranged on the raw material tank 1; the rectifying device comprises a rectifying tower 21 connected with a raw material output port, a tower top condenser 22 connected with a tower top gas outlet of the rectifying tower 21 and a reboiler 23 connected with a tower bottom liquid phase pipeline of the rectifying tower; the outlet of the reboiler 23 is connected with a tower bottom gas phase pipe of the rectifying tower 21; a high-low boiling discharge port of the rectifying tower 21 is connected with a high-low boiling tank 5; a condensed material outlet of the tower top condenser 22 is respectively connected with a material return port of the rectifying tower 21 and a product inlet of the product tank 3; the re-cooling device comprises a cold trap 41 connected with a gas circulation port of the raw material tank 1, an uncondensed gas outlet of the tower top condenser 22, a tank top gas pipeline of the product tank 3 and a tank top gas pipeline of the high-low boiling tank 5, a buffer tank 42 connected with the uncondensed gas outlet of the cold trap 41, a vacuum pump 43 connected with the buffer tank 42 and a deep cooler 44 connected with the vacuum pump 43; the condensed material outlet of the cold trap 41, the liquid material outlet of the buffer tank 42 and the condensed material outlet of the chiller 44 are all connected with the liquid material return port of the raw material tank 1, and the non-condensed gas outlet of the chiller 44 is connected with an exhaust gas treatment system.
Through the structural design and the mutual connection relationship of the raw material tank 1, the rectifying device, the product tank 3 and the recooling device, the silicon-based electronic product can be rectified under reduced pressure, and compared with a reduced pressure rectifying system in the traditional chemical industry, the process flow is simple, the operating pressure is stable and controllable in the production process of the silicon-based electronic product, the fluctuation is small, and the quality of a high-purity product is guaranteed; the reduced pressure rectification reduces the saturated vapor pressure of the materials in the operation process, the material quantity proportion entering the gas phase is reduced, meanwhile, the unnecessary consumption of the raw materials in the production process of the silicon-based electronic product can be greatly reduced through the design of the secondary cooling device, and compared with a normal pressure and pressurized rectification system, the unnecessary consumption of the raw materials in the production process is reduced.
As a preferred embodiment of the present invention, a pressure gauge is provided on the buffer tank 42; the pressure gauge is interlocked with the pumping speed control valve of the vacuum pump 43. The air pressure in the buffer tank 42 can be detected in real time by arranging the pressure gauge, the pressure gauge and the pumping speed control valve of the vacuum pump 43 are designed in an interlocking mode, the pumping speed of the vacuum pump 43 is adjusted conveniently according to the pressure in the buffer tank 42, and automatic adjustment is achieved.
As a preferred embodiment of the present invention, a first regulating valve 61, a second regulating valve 62, a third regulating valve 63 and a fourth regulating valve 64 are provided at the non-condensed gas outlet of overhead condenser 22, at the gas flow port of raw material tank 1, on the overhead gas pipe of product tank 3 and on the overhead gas pipe of high-low boiling tank 5, respectively;
a first pressure monitoring device, a second pressure monitoring device, a third pressure monitoring device and a fourth pressure monitoring device are respectively arranged on the top of the rectifying tower 21, the top of the raw material tank 1, the top of the product tank 3 and the top of the high-low boiling tank 5;
the first regulating valve 61 and the first pressure monitoring device, the second regulating valve 62 and the second pressure monitoring device, the third regulating valve 63 and the third pressure monitoring device, and the fourth regulating valve 64 and the fourth pressure monitoring device are interlocked with each other.
Through the structural design, the pressure of equipment in the device can be independently controlled without influencing each other, and meanwhile, the automatic control can be realized through interlocking, so that the device is simple to operate, stable and controllable. Particularly, for the production process of silicon-based electronic products, the operation pressure is stable and controllable, the fluctuation is small, and the quality of high-purity products is guaranteed.
As a preferred embodiment of the present invention, the number of the rectifying means is at least two; the rectification devices are connected in parallel or in series; wherein,
when the rectifying devices are connected in series, the rectifying tower 21 in the first rectifying device in the series is connected with the raw material tank 1, and a tower bottom liquid phase pipeline of the rectifying tower 21 in the previous rectifying device is connected with a feed inlet of the rectifying tower 21 in the next rectifying device between the adjacent rectifying devices; the condensed material outlet of the tower top condenser 22 in the last rectifying device in the series is connected with the product tank 3, the last rectifying device is removed, and the condensed material outlet of the tower top condenser 22 in other rectifying devices is connected with the high-low boiling tank 5. The product purity of rectification can be better through the structural design of a plurality of rectification devices connected in series, and the rectification efficiency can be improved through a plurality of rectification devices connected in parallel.
As a preferred embodiment of the present invention, the rectifying tower 21 is a tower column or a packed tower; a column plate is arranged in the rectifying tower, and a filler is arranged on the column plate; the number of the tower plates is 10-100; the filling material comprises one or more of a plurality of kinds of filling absorbent, catalyst and complexing agent which are mixed in any proportion.
And/or reboiler 23 is a vertical or horizontal heat exchanger; the heating medium of the reboiler 23 is any one of water vapor, hot water and heat conducting oil; the method is mainly used for reheating the liquid phase in the rectifying tower 21, gasifying part of the liquid phase into gas phase, returning the gas phase to the rectifying tower 21, and rectifying.
And/or, the overhead condenser 22 is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the tower top condenser 22 is circulating water or a refrigerant; the use temperature of the cooling medium of the overhead condenser 22 is-60-50 ℃; the method is mainly used for condensing the gas phase to obtain a rectified product, wherein the temperature of the cooling medium is lower than that of the gas phase material.
And/or the cold trap 41 is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the cold trap 41 is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃.
And/or the buffer tank 42 is a vertical storage tank or a horizontal storage tank; the volume of the buffer tank is 0.2-2 m3；
And/or the vacuum pump 43 is any one of a screw vacuum pump, a roots vacuum pump and a reciprocating pump;
and/or, the chiller 44 is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the chiller 44 is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃.
And/or the raw material tank 1 is a vertical storage tank or a horizontal storage tank; the volume of the raw material tank 1 is 1-20 m3；
And/or the product tank 3 is a vertical storage tank or a horizontal storage tank; the volume of the product tank 3 is 1-20 m3；
And/or the high-low boiling tank 5 is a vertical storage tank or a horizontal storage tank;
the volume of the high-low boiling tank 5 is 1-20 m3。
As a preferred embodiment of the present invention, the feed inlet of the material tank 1 is connected to a feed pipe for raw materials of silicon-based electronic products. The raw materials of the silicon-based electronic product in the raw material tank comprise liquid raw materials condensed in a cold trap, a buffer tank and a deep cooler and also comprise raw materials from the outside.
As a preferred embodiment of the invention, the raw material of the silicon-based electronic product comprises any one of silicon tetrachloride, hexachlorodisilane, tetraethoxysilane and chlorosilane or at least two of the silicon tetrachloride, the hexachlorodisilane, the tetraethoxysilane and the chlorosilane which are mixed according to any proportion.
As a preferred embodiment of the present invention, the motor of the vacuum pump 43 is a variable frequency motor; the pumping speed of the vacuum pump 43 is 0 to 100%.
As a preferred embodiment of the invention, the decompression rectification device of the silicon-based electronic product is operated at a pressure lower than the atmospheric pressure.
As a preferred embodiment of the invention, the feed inlet of the rectifying tower 21 is connected with the raw material output port of the raw material tank 1 through a delivery pump or an inert gas pressing device; wherein, the delivery pump is a centrifugal pump or a reciprocating pump.
The product generated by the rectifying tower 21 can be a low-boiling-point substance extracted from the tower top condenser 22 of the rectifying tower, a high-boiling-point substance extracted from the tower bottom of the rectifying tower 21, or a material extracted from the side of the rectifying tower.
The high-low boiling point of the rectifying column 21 may be a low-boiling point substance or a high-boiling point substance in a single column operation, or may be a mixture of low-boiling point substances or high-boiling point substances in each column in a multi-column operation.
The invention provides a decompression rectification method of a silicon-based electronic product, which utilizes the decompression rectification device of the silicon-based electronic product to carry out decompression distillation on the raw material of the silicon-based electronic product and comprises the following steps:
s1, conveying the raw material of the silicon-based electronic product in the raw material tank 1 into the rectifying tower 21, and rectifying the raw material by the rectifying tower 21 to obtain a gas phase and a liquid phase respectively;
s2, for the gas phase, the gas phase enters the tower top condenser 22 through the tower top gas outlet of the rectifying tower 21, the gas phase is condensed through the tower top condenser 22, the obtained condensed material returns to the rectifying tower 21 from one part of the condensed material outlet of the tower top condenser 22, the rectification is continued, and the other part of the condensed material enters the product tank 3; for the liquid phase, the liquid phase enters a reboiler 23 through a tower bottom liquid phase pipeline of the rectifying tower 21, is reboiled by the reboiler 23 and then returns to the rectifying tower 21 in the form of gas, the liquid phase which is not reboiled enters a high-low boiling tank 5 through a high-low boiling discharge hole of the rectifying tower 21, and is gasified by the high-low boiling tank 5 to obtain a gaseous material;
s3, mixed gas formed by uncondensed gas phase in the tower top condenser 22, gaseous materials in the high-low boiling tank 5, gas in the raw material tank 1 and gas in the product tank 3 enters a recooling device, the mixed gas is deeply cooled through the cold trap 41 and the deep cooler 44 in sequence, the cooled liquid material returns to the raw material tank 1 again to continue the cyclic rectification process, and waste gas generated by deep cooling is treated through a waste gas treatment system.
In order to better explain the decompression rectification device and method of silicon-based electronic products provided by the invention, the following specific examples are provided.
Example 1
As shown in fig. 1, the decompression rectification apparatus for silicon-based electronic products comprises two rectification towers 21, two reboilers 23, two overhead condensers 22, a cold trap 41, a buffer tank 42, a set of vacuum pumps 43, a deep cooler 44, a raw material tank 1, a product tank 3 and a high-low boiling tank 5. The raw materials from the tank area are conveyed into a raw material tank 1 through a conveying pump, the materials of the raw material tank 1 are conveyed into a rectifying tower 1# tower through a centrifugal pump, the gas at the top of the rectifying tower 1# tower enters a tower top condenser of the rectifying tower 1# tower and is cooled by a cooling medium, one part of the condensed materials returns into the rectifying tower 1# tower, one part of the condensed materials is extracted as low-boiling substances of the tower 1# tower and is conveyed into a high-low boiling tank 5, and the extracted materials at the bottom of the tower are conveyed into a rectifying tower 2# tower. The gas at the top of the rectifying tower 2# enters a condenser at the top of the rectifying tower 2# and is cooled by a cooling medium, part of the condensed material returns to the rectifying tower 2# and is extracted as a product of the rectifying tower 2# and the extracted gas at the bottom of the rectifying tower 2# is sent to a high-low boiling tank 5 as a high-boiling substance of the rectifying tower 2 #. The uncondensed gas in the condensers of the tower No. 1 and the tower No. 2 is pumped into the cold trap 41 under the action of the vacuum pump 43, the uncondensed gas is pumped into the buffer tank 42 after being cooled, the gas at the top of the buffer tank 42 is pumped into the vacuum pump 43, the pumped gas is discharged into the chiller 44, and the uncondensed gas after being further cooled is discharged into an exhaust system for treatment. In order to ensure that the liquid condensed in the cold trap 41, the buffer tank 42 and the deep cooler 44 enters the raw material tank 1, and the low-boiling substance in the 1# tower and the high-boiling substance in the 2# tower smoothly enter the high-low boiling tank 5, and the product in the 2# tower smoothly enters the product tank 3, the gas pipelines at the top of the raw material tank 1, the high-low boiling tank 5 and the product tank 3 are respectively connected to the inlet of the cold trap 41, the vacuum pump 43 is used for extracting the gas in the raw material tank 1, the high-low boiling tank 5 and the product tank 3, and the pressure in the raw material tank 1, the high-low boiling tank 5 and the product tank 3 is respectively controlled by the regulating valve. The buffer tank 42 is provided with a pressure gauge and interlocked with a motor of the vacuum pump 43.
The raw material is raw material grade ethyl orthosilicate with the purity of 99 wt%, and the balance of ethanol or trace metal impurities, and the boiling point of the raw material is 165 ℃ under normal pressure. The operating pressure in a rectifying tower 1# tower, a rectifying tower 2# tower, a raw material tank 1, a high-low boiling tank 5 and a product tank 3 is-0.075 MPaG, the interlocking pressure of a buffer tank 42 is controlled to be-0.08 MPaG, the temperature of a tower kettle of the rectifying tower is 120 ℃, the heating medium of a reboiler 23 is 0.3MPaG water vapor, the cooling medium of a tower top condenser 22 is circulating water, the temperature is 30 ℃ in, the temperature is 40 ℃ out, the reflux ratio is 15, the cooling medium of a cold trap 41 is a refrigerant at-30 ℃, and the cooling medium of a deep cooler 44 is a refrigerant at-55 ℃. The device has low operation temperature, small fluctuation range and product purity up to 99.99 wt%, and meets the requirements of silicon-based electronic products. Compared with the traditional normal pressure or rectification, the heating medium of the reboiler in the normal pressure rectification is 1.0MPaG steam, the heating medium of the reboiler in the vacuum rectification is 0.3MPaG steam, and the use amount of the heating medium of the reboiler can be saved by about 19% in the vacuum rectification under the premise of the same treatment amount. The reduced pressure rectification reduces the saturated vapor pressure of the materials in the operation process, the material quantity proportion entering the gas phase is reduced, meanwhile, measures for recovering condensable materials in the gas phase are arranged at a plurality of positions in the invention, the unnecessary consumption of raw material materials in the production process of the silicon-based electronic product is greatly reduced, and compared with a normal pressure and pressurized rectification system, the unnecessary consumption material loss can be reduced by more than 30 percent. The pressure control of the rectifying device and the pumping speed control of the vacuum pump are independently arranged, the pressure fluctuation range in the system is small, stable and controllable, and the pressure fluctuation range in the system is +/-5% of a set value. The silicon-based electronic product produced by using the vacuum rectification system has simple flow, is stable and controllable, reduces the operating temperature in the production process of the high-purity product, improves the stability in the production process of the product, is greatly beneficial to ensuring the quality of the high-purity product, reduces the consumption of a heating medium and reduces unnecessary consumption of raw materials in the production process.
Example 2
The process is the same as the process of the embodiment 1, except that the raw material is raw material-grade hexachlorodisilane, the purity is 99 wt%, the rest is silicon tetrachloride or trace heavy component impurities, and the boiling point is 145 ℃ under normal pressure. The operating pressure in a rectifying tower 1# tower, a rectifying tower 2# tower, a raw material tank 1, a high-low boiling tank 5 and a product tank 3 is-0.075 kPa, the control linkage pressure of a buffer tank is-0.08 kPaG, the temperature of a tower kettle of the rectifying tower is 100 ℃, the heating medium of a reboiler 23 is 0.2MPaG vapor, the cooling medium of a tower top condenser 22 is circulating water, the temperature is 30 ℃ in, the temperature is 40 ℃ out, the reflux ratio is 15, the cooling medium of a cold trap 41 is a refrigerant at-30 ℃, and the cooling medium of a deep cooler 44 is a refrigerant at-55 ℃. The operating temperature in full time is low, the fluctuation range is small, the product purity can reach 99.99 wt%, and the requirements of silicon-based electronic products are met. Compared with the traditional normal pressure or rectification, the heating medium of the reboiler in the normal pressure rectification is 0.2MPaG vapor, the heating medium of the reboiler in the vacuum rectification is 0.6MPaG vapor, and on the premise of the same treatment capacity, the vacuum rectification can save the using amount of the heating medium of the reboiler by about 17 percent, reduce the unnecessary consumption of materials by about 30 percent, ensure that the pressure fluctuation range in the device is small, stable and controllable, and ensure that the pressure fluctuation range in the device is +/-5 percent of the set value. The silicon-based electronic product produced by the vacuum distillation system has simple flow, is stable and controllable, reduces the operating temperature in the production process of the high-purity product, improves the stability in the production process of the product, is greatly beneficial to ensuring the quality of the high-purity product, reduces the consumption of a heating medium and reduces the unnecessary consumption of raw materials in the production process.
According to the silicon-based electronic product vacuum rectification device and the silicon-based electronic product vacuum rectification method, the vacuum rectification of the silicon-based electronic product can be realized through the structural design and the mutual connection relationship of the raw material tank, the rectification device, the product tank and the re-cooling device, and compared with a conventional vacuum rectification system in the chemical industry, the silicon-based electronic product vacuum rectification device has the advantages that the process flow is simple, the operation pressure is stable and controllable in the silicon-based electronic product production process, the fluctuation is small, and the quality of a high-purity product is guaranteed; the reduced pressure rectification reduces the saturated vapor pressure of the materials in the operation process, the material quantity proportion entering the gas phase is reduced, meanwhile, the unnecessary consumption of the raw materials in the production process of the silicon-based electronic product can be greatly reduced through the design of the secondary cooling device, and compared with a normal pressure and pressurized rectification system, the unnecessary consumption of the raw materials in the production process is reduced.
The vacuum distillation apparatus and method for silicon-based electronic products according to the present invention are described above by way of example with reference to the accompanying drawings. However, it should be understood by those skilled in the art that various modifications can be made to the vacuum distillation apparatus and method for silicon-based electronic products of the present invention without departing from the scope of the present invention. Accordingly, the scope of the invention should be determined from the content of the appended claims.
Claims (10)
1. A decompression rectification device of a silicon-based electronic product is characterized by comprising a raw material tank, a rectification device, a product tank and a recooling device; wherein,
a raw material output port, a liquid material return port and a gas circulation port are arranged on the raw material tank;
the rectifying device comprises a rectifying tower connected with the raw material output port, an overhead condenser connected with an overhead gas outlet of the rectifying tower and a reboiler connected with a tower bottom liquid phase pipeline of the rectifying tower; the outlet of the reboiler is connected with a tower bottom gas phase pipe of the rectifying tower; a high-low boiling discharge port of the rectifying tower is connected with a high-low boiling tank; a condensed material outlet of the tower top condenser is respectively connected with a material return port of the rectifying tower and a product inlet of the product tank;
the sub-cooling device comprises a cold trap, a buffer tank, a vacuum pump and a deep cooler, wherein the cold trap is respectively connected with a gas flow port of the raw material tank, an uncondensed gas outlet of the tower top condenser, a tank top gas pipeline of the product tank and a tank top gas pipeline of the high-low boiling tank, the buffer tank is connected with the uncondensed gas outlet of the cold trap, the vacuum pump is connected with the buffer tank, and the deep cooler is connected with the vacuum pump;
the condensed material outlet of the cold trap, the liquid material outlet of the buffer tank and the condensed material outlet of the deep cooler are connected with the liquid material backflow port of the raw material tank, and the non-condensed gas outlet of the deep cooler is connected with a waste gas treatment system.
2. The decompression rectification device of silicon-based electronic products according to claim 1,
a pressure gauge is arranged on the buffer tank;
the pressure gauge is interlocked with a pumping speed control valve of the vacuum pump.
3. The decompression rectification device of silicon-based electronic products according to claim 1,
a first regulating valve, a second regulating valve, a third regulating valve and a fourth regulating valve are respectively arranged at an uncondensed gas outlet of the tower top condenser, a gas flow opening of the raw material tank, a tank top gas pipeline of the product tank and a tank top gas pipeline of the high-low boiling tank;
a first pressure monitoring device, a second pressure monitoring device, a third pressure monitoring device and a fourth pressure monitoring device are respectively arranged on the top of the rectifying tower, the top of the raw material tank, the top of the product tank and the top of the high-low boiling tank;
the first regulating valve and the first pressure monitoring device, the second regulating valve and the second pressure monitoring device, the third regulating valve and the third pressure monitoring device, and the fourth regulating valve and the fourth pressure monitoring device are interlocked respectively.
4. The decompression rectification device of silicon-based electronic products according to claim 1,
the number of the rectifying devices is at least two; the rectification devices are connected in parallel or in series; wherein,
when the rectifying devices are connected in series, a rectifying tower in the first rectifying device in the series is connected with the raw material tank, and a tower bottom liquid phase pipeline of the rectifying tower in the previous rectifying device is connected with a feed inlet of the rectifying tower in the next rectifying device between the adjacent rectifying devices; and a condensed material outlet of the tower top condenser in the last rectifying device in the series is connected with the product tank, the last rectifying device is removed, and condensed material outlets of tower top condensers in other rectifying devices are connected with the high-low boiling tank.
5. The decompression rectification apparatus of silicon-based electronic products according to claim 1,
the rectifying tower is a tower or a packed tower; a tower plate is arranged in the rectifying tower, and a filling material is arranged on the tower plate; the number of the tower plates is 10-100;
and/or the reboiler is a vertical or horizontal heat exchanger; the heating medium of the reboiler is any one of water vapor, hot water and heat conducting oil;
and/or the tower top condenser is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the tower top condenser is circulating water or a refrigerant; the use temperature of a cooling medium of the overhead condenser is-60-50 ℃;
and/or the cold trap is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the cold trap is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃;
and/or the buffer tank is a vertical storage tank or a horizontal storage tank; the volume of the buffer tank is 0.2-2 m3；
And/or the vacuum pump is any one of a screw vacuum pump, a roots vacuum pump and a reciprocating pump;
and/or the deep cooler is a vertical heat exchanger or a horizontal heat exchanger; the cooling medium of the deep cooler is water or a refrigerant; the using temperature of the refrigerant is-60 to-20 ℃;
the raw material tank is a vertical storage tank or a horizontal storage tank; the body of the stock tankThe product is 1 to 20m3；
And/or the product tank is a vertical storage tank or a horizontal storage tank; the volume of the product tank is 1-20 m3；
And/or the high-low boiling tank is a vertical storage tank or a horizontal storage tank; the volume of the high-low boiling tank is 1-20 m3。
6. The decompression rectification device of silicon-based electronic products according to claim 1,
and the feed inlet of the raw material tank is connected with a conveying pipe for raw materials of the silicon-based electronic product.
7. The decompression rectification device of silicon-based electronic products according to claim 6,
the raw materials of the silicon-based electronic product comprise any one or at least two of silicon tetrachloride, hexachlorodisilane, tetraethoxysilane and chlorosilane which are mixed according to any proportion.
8. The decompression rectification apparatus of silicon-based electronic products according to claim 1,
the motor of the vacuum pump is a variable frequency motor;
the pumping speed of the vacuum pump is 0-100%.
9. The decompression rectification device of silicon-based electronic products according to claim 1,
the operating pressure of the decompression rectification device of the silicon-based electronic product is lower than the atmospheric pressure.
10. A reduced pressure distillation method of silicon-based electronic products, which is characterized in that the reduced pressure distillation method of the reduced pressure distillation device of the silicon-based electronic products as claimed in any one of claims 1 to 9 is used for carrying out reduced pressure distillation on raw materials of the silicon-based electronic products, and comprises the following steps:
conveying the raw material of the silicon-based electronic product in the raw material tank into the rectifying tower, and rectifying the raw material by the rectifying tower to respectively obtain a gas phase and a liquid phase;
for the gas phase, the gas phase enters a tower top condenser through a tower top gas outlet of the rectifying tower, the gas phase is condensed through the tower top condenser, the obtained condensed material returns to the rectifying tower from one part of a condensed material outlet of the tower top condenser, the rectification is continued, and the other part of the condensed material enters the product tank; the liquid phase enters the reboiler through a tower bottom liquid phase pipeline of the rectifying tower, is reboiled by the reboiler and then returns to the rectifying tower in a gas form, and the liquid phase which is not reboiled enters a high-low boiling tank through a high-low boiling material outlet of the rectifying tower and is gasified by the high-low boiling tank to obtain a gaseous material;
the gaseous phase that is not condensed in the top of the tower condenser, gaseous material in the high low boiling jar, the gas in the head tank and the mist that the gas in the product jar formed all get into in the recooling device, pass through in proper order the cold trap with the deep freezer is right mist cooling carries out deep cooling, and the liquid material that obtains after the cooling returns the process of continuing circulation rectification in the head tank again, and the waste gas that deep cooling produced carries out exhaust-gas treatment through exhaust treatment system.
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