CN115105850B - Electronic grade trichlorosilane purifying device and method - Google Patents
Electronic grade trichlorosilane purifying device and method Download PDFInfo
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- CN115105850B CN115105850B CN202210716920.8A CN202210716920A CN115105850B CN 115105850 B CN115105850 B CN 115105850B CN 202210716920 A CN202210716920 A CN 202210716920A CN 115105850 B CN115105850 B CN 115105850B
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- crude distillation
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- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 239000005052 trichlorosilane Substances 0.000 title claims abstract description 129
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004821 distillation Methods 0.000 claims abstract description 363
- 238000001179 sorption measurement Methods 0.000 claims abstract description 49
- 239000012535 impurity Substances 0.000 claims abstract description 48
- 239000003463 adsorbent Substances 0.000 claims abstract description 38
- 238000012856 packing Methods 0.000 claims abstract description 24
- 238000000746 purification Methods 0.000 claims abstract description 21
- 239000000945 filler Substances 0.000 claims abstract description 13
- 229910052796 boron Inorganic materials 0.000 claims abstract description 9
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011574 phosphorus Substances 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims description 67
- 239000000463 material Substances 0.000 claims description 57
- 238000003825 pressing Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 13
- 230000008016 vaporization Effects 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000011049 filling Methods 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 8
- 230000004927 fusion Effects 0.000 abstract description 4
- 238000000605 extraction Methods 0.000 description 20
- 239000007788 liquid Substances 0.000 description 18
- 239000012071 phase Substances 0.000 description 7
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 7
- 229920005591 polysilicon Polymers 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005984 hydrogenation reaction Methods 0.000 description 6
- 238000011084 recovery Methods 0.000 description 6
- 238000009835 boiling Methods 0.000 description 3
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 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
- 230000001419 dependent effect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/146—Multiple effect distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- 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
-
- 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
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
-
- 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
Abstract
The invention discloses an electronic grade trichlorosilane purifying device and method, wherein the device comprises the following components: the crude distillation tower group comprises at least n crude distillation towers which are connected in series, wherein n is more than or equal to 3, the crude distillation tower is a filler tower, an adsorption unit is arranged on the filler of any one of the 2 nd-n stages of the crude distillation tower, the adsorption unit is used for adsorbing and removing impurities containing boron and phosphorus in crude trichlorosilane, and the crude distillation tower group is used for removing light component and heavy component impurities in the crude trichlorosilane through crude fraction separation; and the rectifying tower is connected with the crude rectifying tower group and is used for obtaining electronic grade trichlorosilane through rectification. The invention realizes the fusion of crude distillation purification and adsorption impurity removal of trichlorosilane, can effectively remove trace impurities in the trichlorosilane in the process of crude distillation, and greatly improves the purification efficiency of the trichlorosilane; the adsorption unit is arranged on the packing of the crude distillation column, so that overtemperature and overpressure of an adsorption column caused by heat release in the adsorption process in the prior art are avoided, and long-period stable operation of the adsorbent is ensured.
Description
Technical Field
The invention belongs to the technical field of polysilicon production, and particularly relates to an electronic grade trichlorosilane purification device and method.
Background
Trichlorosilane is an important raw material for producing polysilicon, more than 80% of the total polysilicon production quantity in the world adopts an improved Siemens method, high-purity trichlorosilane and hydrogen are utilized to carry out chemical vapor deposition reaction in a CVD reduction furnace to produce polysilicon, and the quality of the polysilicon is greatly dependent on the purity of the trichlorosilane. The purity of the trichlorosilane in the photovoltaic industry is generally required to be more than 6N, the purity of the trichlorosilane in the semiconductor industry is required to be 9N or higher, and the impurities reach the PPb level. However, the content of impurities in trichlorosilane synthesized through chlorination or cold hydrogenation reaction is very high, and metal impurities, particularly boron and phosphorus impurities, have great influence on the electrical performance of polysilicon.
In the prior art, boron and phosphorus impurities in trichlorosilane are removed in a rectification mode or a rectification and adsorption combined mode, so that the purification of the trichlorosilane is realized, heat can be released in the adsorption process of the adsorbent, the adsorbent in the adsorption column is concentrated and piled up, the heat dissipation effect of the adsorption column is reduced, the local overtemperature of the adsorption column is easily caused, the adsorption effect is reduced, the adsorbent is deactivated, and even safety accidents are caused when the adsorption heat is overhigh.
Therefore, how to solve the problem of over-temperature in the adsorption process of the adsorbent and ensure the normal operation of the adsorbent becomes a difficult problem for the technicians in the technical field.
Disclosure of Invention
The invention aims to solve the technical problems of the prior art, and provides an electronic grade trichlorosilane purification device and method, which solve the problems of overtemperature and overpressure of an adsorption column caused by heat release in the adsorption process in the prior art.
The technical scheme adopted for solving the technical problem of the invention is to provide an electronic grade trichlorosilane purifying device, which comprises:
the crude distillation tower group comprises at least n crude distillation towers which are connected in series, wherein n is more than or equal to 3, the crude distillation tower is a filler tower, an adsorption unit is arranged on the filler of any one of the 2 nd-n stages of the crude distillation tower, the adsorption unit is used for adsorbing and removing impurities containing boron and phosphorus in crude trichlorosilane, and the crude distillation tower group is used for removing light component and heavy component impurities in the crude trichlorosilane through crude fraction separation;
and the rectifying tower is connected with the crude rectifying tower group and is used for obtaining electronic grade trichlorosilane through rectification.
Preferably, n=3, and the crude distillation column group includes:
the first-stage crude distillation column is used for introducing crude trichlorosilane, and removing light component impurities flowing through the first-stage crude distillation column;
the second-stage crude distillation column is connected with the tower kettle of the first-stage crude distillation column, and heavy component impurities flowing through the second-stage crude distillation column are removed through the second-stage crude distillation column;
and the third-stage crude distillation column is connected with the top of the second-stage crude distillation column, light component impurities flowing through the third-stage crude distillation column are removed through the third-stage crude distillation column, and an adsorption unit is arranged on the packing of the second-stage crude distillation column or the third-stage crude distillation column.
Preferably, the adsorption unit includes: the adsorbent and the fixing component thereof are used for fixedly filling the adsorbent into the crude distillation column where the adsorbent is positioned.
Preferably, the fixing member includes: the bottom support plate is used for supporting the bottom of the adsorbent, and the upper pressing plate is used for pressing the upper part of the adsorbent; the bottom supporting plate and the upper pressing plate are circular in shape, the size of the bottom supporting plate and the upper pressing plate are consistent with the inner diameter of the crude distillation column in which the bottom supporting plate and the upper pressing plate are positioned, the outer diameter of the bottom supporting plate and the upper pressing plate are attached to the inner wall of the crude distillation column in which the bottom supporting plate and the upper pressing plate are positioned, and sieve holes are formed in the bottom supporting plate and the upper pressing plate; the diameter of the adsorbent is larger than that of the sieve holes arranged on the bottom supporting plate and the upper pressing plate.
Preferably, the adsorption unit includes: the adsorbent is fixed on the surface of the adsorbent filler by bonding. The adsorption unit is a composite filler loaded with adsorbent.
Preferably, the first-stage crude distillation column, the second-stage crude distillation column, the third-stage crude distillation column and the rectifying column all comprise 10 sections of packing arranged in the column, wherein the feeding position of the first-stage crude distillation column is the upper part of the fifth section of packing in the first-stage crude distillation column, the feeding position of the second-stage crude distillation column is the upper part of the second section of packing in the second-stage crude distillation column, the feeding position of the third-stage crude distillation column is the upper part of the eighth section of packing in the third-stage crude distillation column, and the feeding position of the rectifying column is the upper part of the second section of packing in the rectifying column.
Preferably, the electronic grade trichlorosilane purifying device further comprises:
the first-stage crude distillation tower reboiler is used for heating and vaporizing the discharged materials of the tower bottoms of the first-stage crude distillation tower, and is respectively connected with the tower bottoms of the first-stage crude distillation tower and the tower top of the second-stage crude distillation tower, and the discharged materials of the tower bottoms of the first-stage crude distillation tower exchange heat with the discharged materials of the tower top of the second-stage crude distillation tower;
the second-stage crude distillation tower reboiler is used for heating and vaporizing the discharged materials of the tower bottoms of the second-stage crude distillation tower, and is respectively connected with the tower bottoms of the second-stage crude distillation tower and the tower top of the third-stage crude distillation tower, and the discharged materials of the tower bottoms of the second-stage crude distillation tower exchange heat with the discharged materials of the tower top of the third-stage crude distillation tower;
the third-stage crude distillation tower reboiler is used for heating and vaporizing the discharged material of the tower bottom of the third-stage crude distillation tower, and is respectively connected with the tower bottom of the third-stage crude distillation tower and the tower top of the rectifying tower, and the discharged material of the tower bottom of the third-stage crude distillation tower exchanges heat with the discharged material of the tower top of the rectifying tower;
and the rectifying tower reboiler is connected with the tower kettle of the rectifying tower and is used for heating and vaporizing the discharged materials of the tower kettle of the rectifying tower.
Preferably, the electronic grade trichlorosilane purifying device further comprises:
the first-stage crude distillation column top cooler is connected with the top of the first-stage crude distillation column and is used for cooling materials discharged from the top of the first-stage crude distillation column;
the first-stage crude distillation column reflux pump is respectively connected with the first-stage crude distillation column top cooler and the top of the first-stage crude distillation column, and is used for partially extracting the materials cooled by the first-stage crude distillation column top cooler and refluxing the rest parts into the first-stage crude distillation column;
the second-stage crude distillation column top cooler is connected with the top of the second-stage crude distillation column and is used for cooling materials discharged from the top of the second-stage crude distillation column;
the second-stage crude distillation column reflux pump is respectively connected with the second-stage crude distillation column top cooler and the top of the second-stage crude distillation column, and is used for pumping part of the material cooled by the second-stage crude distillation column top cooler into the third-stage crude distillation column, and the rest part of the material flows back into the second-stage crude distillation column;
the third-stage crude distillation column top cooler is connected with the top of the third-stage crude distillation column and is used for cooling materials discharged from the top of the third-stage crude distillation column;
the third-stage crude distillation column reflux pump is respectively connected with the third-stage crude distillation column top cooler and the top of the third-stage crude distillation column, and is used for partially extracting the materials cooled by the third-stage crude distillation column top cooler and refluxing the rest parts into the third-stage crude distillation column;
the rectifying tower top cooler is connected with the rectifying tower top and is used for cooling materials discharged from the rectifying tower top;
and the rectifying tower reflux pump is respectively connected with the rectifying tower top cooler and the rectifying tower top, and is used for extracting part of the materials cooled by the rectifying tower top cooler and refluxing the rest part into the rectifying tower.
The invention also provides a method for purifying the electronic grade trichlorosilane by using the electronic grade trichlorosilane purifying device, which comprises the following steps of:
and (3) introducing the crude trichlorosilane into the electronic grade trichlorosilane purifying device to purify, so as to obtain the electronic grade trichlorosilane.
Preferably, the temperature of the top of the first-stage crude distillation column is 50-55 ℃, and the temperature of the bottom of the first-stage crude distillation column is 55-65 ℃.
Preferably, the temperature of the top of the second-stage crude distillation column is 73-76 ℃ and the temperature of the bottom of the second-stage crude distillation column is 77-80 ℃.
Preferably, the top temperature of the third-stage crude distillation column is 90-95 ℃ and the bottom temperature is 95-100 ℃.
Preferably, the temperature of the top of the rectifying tower is 90-95 ℃ and the temperature of the bottom of the rectifying tower is 110-115 ℃.
The electronic grade trichlorosilane purifying device and method have the following remarkable effects:
the fusion of crude distillation purification and adsorption impurity removal of the trichlorosilane is realized, trace impurities in the trichlorosilane can be effectively removed in the crude distillation process, and the purification efficiency of the trichlorosilane is greatly improved; the adsorption unit is arranged on the packing of the crude distillation column, so that overtemperature and overpressure of an adsorption column caused by heat release in the adsorption process in the prior art are avoided, and long-period stable operation of the adsorbent is ensured.
Drawings
Fig. 1 is a schematic structural view of an electronic grade trichlorosilane purifying apparatus in embodiment 2 of the present invention.
In the figure: 1. a crude trichlorosilane feed line; 2. a first-stage crude distillation column; 3. a first-stage crude distillation column top cooler; 4. a first-stage crude distillation column reflux drum; 5. a first-stage crude distillation column reflux pump; 6. a first-stage crude distillation column top extraction line; 7. a second-stage crude distillation column; 8. a first stage crude distillation column reboiler; 9. a second-stage crude distillation column top cooler; 10. a second-stage crude distillation column reflux drum; 11. a second-stage crude distillation column reflux pump; 12. a third-stage crude distillation column; 13. a second stage crude distillation column reboiler; 14. a third-stage crude distillation column top cooler; 15. a third-stage crude distillation column reflux drum; 16. a third-stage crude distillation column reflux pump; 17. a third-stage crude distillation column reboiler; 18. a rectifying tower top cooler; 19. a rectifying tower reflux drum; 20. a rectifying column reflux pump; 21. a rectifying tower; 22. a rectifying column reboiler; 23. a second-stage crude distillation column bottom liquid extraction line; 24. a third-stage crude distillation column top extraction line; 25. a rectifying tower top extraction line; 26. an adsorbent; 27. an upper press plate; 28. a bottom support plate; 29. and a rectifying tower kettle is provided with a line.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and detailed description for the purpose of better understanding of the technical solution of the present invention to those skilled in the art.
Embodiments of the present patent are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present patent and are not to be construed as limiting the present patent.
Example 1
The embodiment provides an electronic grade trichlorosilane purifying device, which comprises:
the crude distillation tower group comprises at least n crude distillation towers which are connected in series, wherein n is more than or equal to 3, the crude distillation tower is a filler tower, an adsorption unit is arranged on the filler of any one of the 2 nd-n stages of the crude distillation tower, the adsorption unit is used for adsorbing and removing impurities containing boron and phosphorus in crude trichlorosilane, and the crude distillation tower group is used for removing light component and heavy component impurities in the crude trichlorosilane through crude fraction separation;
and the rectifying tower is connected with the crude rectifying tower group and is used for obtaining electronic grade trichlorosilane through rectification.
The embodiment also provides a method for purifying electronic grade trichlorosilane by using the electronic grade trichlorosilane purifying device, which comprises the following steps:
and (3) introducing the crude trichlorosilane into the electronic grade trichlorosilane purifying device to purify, so as to obtain the electronic grade trichlorosilane.
The electronic grade trichlorosilane purifying device and method in the embodiment have the following remarkable effects:
the fusion of crude distillation purification and adsorption impurity removal of the trichlorosilane is realized, trace impurities in the trichlorosilane can be effectively removed in the crude distillation process, and the purification efficiency of the trichlorosilane is greatly improved; the adsorption unit is arranged on the packing of the crude distillation column, so that overtemperature and overpressure of an adsorption column caused by heat release in the adsorption process in the prior art are avoided, and long-period stable operation of the adsorbent is ensured.
Example 2
As shown in fig. 1, this embodiment provides an electronic grade trichlorosilane purifying apparatus, including:
the crude distillation tower group comprises at least n crude distillation towers which are connected in series, wherein n is more than or equal to 3, the crude distillation tower is a filler tower, an adsorption unit is arranged on the filler of any one of the 2 nd-n stages of the crude distillation tower, the adsorption unit is used for adsorbing and removing impurities containing boron and phosphorus in crude trichlorosilane, and the crude distillation tower group is used for removing light component and heavy component impurities in the crude trichlorosilane through crude fraction separation;
the rectifying tower 21 is connected with the crude rectifying tower group, and the rectifying tower 21 is used for obtaining electronic grade trichlorosilane through rectification.
Preferably, n=3, and the crude distillation column group includes:
the first-stage crude distillation column 2 is used for introducing crude trichlorosilane, and removing light component impurities flowing through the first-stage crude distillation column 2;
the second-stage crude distillation column 7 is connected with the tower kettle of the first-stage crude distillation column 2, and heavy component impurities flowing through the second-stage crude distillation column 7 are removed through the second-stage crude distillation column 7;
the third-stage crude distillation column 12 is connected with the top of the second-stage crude distillation column 7, light component impurities flowing through the third-stage crude distillation column 12 are removed by the third-stage crude distillation column 12, and an adsorption unit is arranged on the packing of the second-stage crude distillation column 7 or the third-stage crude distillation column 12.
Specifically, in this embodiment, n=3, and the adsorption unit is disposed on the second-stage crude distillation column 7 in this embodiment. The first-stage crude distillation column 2 is connected with a crude trichlorosilane feed pipeline 1, and the crude trichlorosilane feed is prepared by cold hydrogenation reaction.
Specifically, in this embodiment, the first-stage crude distillation column 2, the second-stage crude distillation column 7, the third-stage crude distillation column 12, and the rectifying column 21 are all packed columns.
Preferably, the adsorption unit includes: the adsorbent 26 and its fixing member are used for fixing and filling the adsorbent 26 in the crude distillation column where it is located.
Preferably, the fixing member includes: a bottom support plate 28, an upper press plate 27, wherein the bottom support plate 28 is used for supporting the bottom of the adsorbent 26, and the upper press plate 27 is used for pressing on the upper part of the adsorbent 26; the bottom supporting plate 28 and the upper pressing plate 27 are circular in shape, the size of the bottom supporting plate is consistent with the inner diameter of the crude distillation column in which the bottom supporting plate 28 and the upper pressing plate 27 are positioned, the outer diameter of the bottom supporting plate is attached to the inner wall of the crude distillation column in which the bottom supporting plate 28 and the upper pressing plate 27 are positioned, and sieve holes are formed in the bottom supporting plate 28 and the upper pressing plate; the diameter of the adsorbent 26 is larger than the diameter of the mesh provided on the bottom support plate 28 and the upper press plate 27.
Preferably, the adsorption unit includes: the adsorbent 26 and the adsorbent packing, and the adsorbent 26 is fixed on the surface of the adsorbent packing by adhesion. The adsorption unit is a composite filler loaded with adsorbent.
Preferably, the first-stage crude distillation column 2, the second-stage crude distillation column 7, the third-stage crude distillation column 12 and the rectifying column 21 all comprise 10 sections of packing arranged in the columns, wherein the feeding position of the first-stage crude distillation column 2 is the upper part of the fifth section of packing in the first-stage crude distillation column, the feeding position of the second-stage crude distillation column 7 is the upper part of the second section of packing in the second-stage crude distillation column, the feeding position of the third-stage crude distillation column 12 is the upper part of the eighth section of packing in the third-stage crude distillation column, and the feeding position of the rectifying column 21 is the upper part of the second section of packing in the rectifying column.
Preferably, the electronic grade trichlorosilane purifying device further comprises:
the first-stage crude distillation column reboiler 8 is used for heating and vaporizing the discharged materials of the tower bottoms of the first-stage crude distillation column 2, and the first-stage crude distillation column reboiler 8 is respectively connected with the tower bottoms of the first-stage crude distillation column 2 and the tower top of the second-stage crude distillation column 7, and the discharged materials of the tower bottoms of the first-stage crude distillation column 2 exchange heat with the discharged materials of the tower top of the second-stage crude distillation column 7;
a second-stage crude distillation column reboiler 13 for heating and vaporizing the discharged material from the bottom of the second-stage crude distillation column 7, wherein the second-stage crude distillation column reboiler 13 is respectively connected with the bottom of the second-stage crude distillation column 7 and the top of the third-stage crude distillation column 12, and the discharged material from the bottom of the second-stage crude distillation column 7 exchanges heat with the discharged material from the top of the third-stage crude distillation column 12;
the third-stage crude distillation column reboiler 17 is used for heating and vaporizing the discharged material of the tower bottom of the third-stage crude distillation column 12, the third-stage crude distillation column reboiler 17 is respectively connected with the tower bottom of the third-stage crude distillation column 12 and the tower top of the rectifying column 21, and the discharged material of the tower bottom of the third-stage crude distillation column 12 exchanges heat with the discharged material of the tower top of the rectifying column 21;
and a rectifying tower reboiler 22 connected with the tower kettle of the rectifying tower 21, wherein the rectifying tower reboiler 22 is used for heating and vaporizing the discharged materials of the tower kettle of the rectifying tower 21.
Preferably, the electronic grade trichlorosilane purifying device further comprises:
the first-stage crude distillation column top cooler 3 is connected with the top of the first-stage crude distillation column 2, and the first-stage crude distillation column top cooler 3 is used for cooling materials discharged from the top of the first-stage crude distillation column 2;
the first-stage crude distillation column reflux pump 5 is respectively connected with the first-stage crude distillation column top cooler 3 and the top of the first-stage crude distillation column 2, and the first-stage crude distillation column reflux pump 5 is used for partially extracting the materials cooled by the first-stage crude distillation column top cooler 3 and refluxing the rest parts into the first-stage crude distillation column 2; a first-stage crude distillation column top extraction line 6 is arranged on a connecting pipe line between the first-stage crude distillation column reflux pump 5 and the top of the first-stage crude distillation column 2;
the second-stage crude distillation column top cooler 9 is connected with the top of the second-stage crude distillation column 7, and the second-stage crude distillation column top cooler 9 is used for cooling materials discharged from the top of the second-stage crude distillation column 7; specifically, in this embodiment, the second-stage crude distillation column top cooler 9 is connected to the first-stage crude distillation column reboiler 8, and the second-stage crude distillation column top cooler 9 is connected to the top of the second-stage crude distillation column 7 through the first-stage crude distillation column reboiler 8;
the second-stage crude distillation column reflux pump 11 is respectively connected with the second-stage crude distillation column top cooler 9 and the top of the second-stage crude distillation column 7, the second-stage crude distillation column reflux pump 11 is used for pumping part of the materials cooled by the second-stage crude distillation column top cooler 9 into the third-stage crude distillation column 12, and the rest part of the materials reflux into the second-stage crude distillation column 7;
the tower bottom of the second-stage crude distillation tower 7 is connected with a second-stage crude distillation tower bottom liquid extraction line 23;
a third-stage crude distillation column top cooler 14 connected to the top of the third-stage crude distillation column 12, the third-stage crude distillation column top cooler 14 being configured to cool the material discharged from the top of the third-stage crude distillation column 12; specifically, in this embodiment, the third-stage crude distillation column top cooler 14 is connected to the second-stage crude distillation column reboiler 13, and the third-stage crude distillation column top cooler 14 is connected to the top of the third-stage crude distillation column 12 through the second-stage crude distillation column reboiler 13;
the third-stage crude distillation column reflux pump 16 is respectively connected with the third-stage crude distillation column top cooler 14 and the top of the third-stage crude distillation column 12, and the third-stage crude distillation column reflux pump 16 is used for partially extracting the materials cooled by the third-stage crude distillation column top cooler 14 and refluxing the rest parts into the third-stage crude distillation column 12; a third-stage crude distillation column top extraction line 24 is arranged on a connecting pipe line between the third-stage crude distillation column reflux pump 16 and the top of the third-stage crude distillation column 12;
a rectifying tower top cooler 18 connected with the rectifying tower 21 top, the rectifying tower 21 top cooler being used for cooling the material discharged from the rectifying tower 21 top; specifically, in this embodiment, the rectifying column top cooler 18 is connected to the third-stage crude rectifying column reboiler 17, and the rectifying column top cooler 18 is connected to the rectifying column 21 top through the third-stage crude rectifying column reboiler 17;
the rectifying tower reflux pump 20 is respectively connected with the rectifying tower top cooler 18 and the rectifying tower 21, and the rectifying tower reflux pump 20 is used for extracting part of the materials cooled by the rectifying tower top cooler 18 and refluxing the rest part into the rectifying tower 21. A rectifying column top extraction line 25 is provided on a connecting line between the rectifying column reflux pump 20 and the rectifying column 21 top. The rectifying column 21 is provided with a rectifying column bottom extraction line 29 at the bottom.
Specifically, the electronic grade trichlorosilane purification device in this embodiment further includes:
the first-stage crude distillation column reflux tank 4 is arranged between the first-stage crude distillation column top cooler 3 and the first-stage crude distillation column reflux pump 5, and the first-stage crude distillation column reflux tank 4 is respectively connected with the first-stage crude distillation column top cooler 3 and the first-stage crude distillation column reflux pump 5;
the second-stage crude distillation column reflux tank 10 is arranged between the second-stage crude distillation column top cooler 9 and the second-stage crude distillation column reflux pump 11, and the second-stage crude distillation column reflux tank 10 is respectively connected with the second-stage crude distillation column top cooler 9 and the second-stage crude distillation column reflux pump 11;
the third-stage crude distillation column reflux tank 15, the third-stage crude distillation column reflux tank 15 is arranged between the third-stage crude distillation column top cooler 14 and the third-stage crude distillation column reflux pump 16, and the third-stage crude distillation column reflux tank 15 is respectively connected with the third-stage crude distillation column top cooler 14 and the third-stage crude distillation column reflux pump 16;
the rectifying tower reflux tank 19, the rectifying tower reflux tank 19 is set up between rectifying tower top cooler 18, rectifying tower reflux pump 20, rectifying tower reflux tank 19 is connected with rectifying tower top cooler 18, rectifying tower reflux pump 20 separately.
The embodiment also provides a method for purifying electronic grade trichlorosilane by using the electronic grade trichlorosilane purifying device, which comprises the following steps:
and (3) introducing the crude trichlorosilane into the electronic grade trichlorosilane purifying device to purify, so as to obtain the electronic grade trichlorosilane.
Specifically, the crude trichlorosilane in this example is crude trichlorosilane produced by a cold hydrogenation reaction
Preferably, the temperature of the top of the first-stage crude distillation column 2 is 50-55 ℃, and the temperature of the column bottom is 55-65 ℃.
Preferably, the temperature of the top of the second-stage crude distillation column 7 is 73-76 ℃ and the temperature of the column bottom is 77-80 ℃.
Preferably, the temperature of the top of the third-stage crude distillation column 12 is 90-95 ℃ and the temperature of the column bottom is 95-100 ℃.
Preferably, the temperature of the top of the rectifying tower 21 is 90-95 ℃ and the temperature of the tower bottom is 110-115 ℃.
The cold hydrogenation crude trichlorosilane enters a first-stage crude distillation column 2, hydrogen chloride, dichlorosilane and light component impurities in the crude trichlorosilane are removed through a first-stage crude distillation column top extraction line 6, the purified trichlorosilane enters a second-stage crude distillation column 7, heavy component impurities in the trichlorosilane are removed through a second-stage crude distillation column bottom liquid extraction line 23, the trichlorosilane extracted from the top of the second-stage crude distillation column 7 enters a third-stage crude distillation column 12, light component impurities in the trichlorosilane are removed through a third-stage crude distillation column top extraction line 24 in a further separation mode, the trichlorosilane purified through three-stage rectification enters a rectification column 21, heavy component impurities in the trichlorosilane are removed through a rectification column bottom extraction line 29 in a further separation mode, and an electronic-stage trichlorosilane product is extracted from the rectification column top 21 through a rectification column top extraction line 25.
The crude distillation column group and the rectifying column 21 in this embodiment use differential pressure coupling to recover heat, wherein the rectifying column 21 uses steam heating, the gas phase at the top of the rectifying column 21 is used as a heat source to heat the reboiler 17 of the third crude distillation column, the gas phase at the top of the third crude distillation column 12 is used as a heat source to heat the reboiler 13 of the second crude distillation column, and the gas phase at the top of the second crude distillation column 7 is used as a heat source to heat the reboiler 8 of the first crude distillation column.
Specifically, the method for purifying the electronic grade trichlorosilane by feeding the crude trichlorosilane liquid from the cold hydrogenation into an electronic grade trichlorosilane purifying device specifically comprises the following steps:
the method comprises the steps that crude trichlorosilane liquid from cold hydrogenation enters a first-stage crude distillation column 2 through a crude trichlorosilane feed line 1, the crude trichlorosilane liquid flows downwards from a feed port of the first-stage crude distillation column 2, contacts and exchanges heat with trichlorosilane steam from a column bottom in a countercurrent mode, hydrogen chloride, dichlorosilane and light component impurities in the crude trichlorosilane are subjected to heat change into steam to be separated from the trichlorosilane liquid, the trichlorosilane extracted from the column bottom of the first-stage crude distillation column 2 enters a second-stage crude distillation column 7, gas phase at the top of the first-stage crude distillation column 2 enters a first-stage crude distillation column top cooler 3 to be condensed into liquid, then enters a first-stage crude distillation column reflux tank 4, part of the liquid returns to the first-stage crude distillation column 2 as reflux after being pressurized by a rectification first-stage crude distillation column reflux pump 5, and the other part of the liquid is extracted to be separated into dichlorosilane DCS and trichlorosilane TCS through a first-stage crude distillation column top extraction line 6 to a recovery system;
the trichlorosilane from the first-stage crude distillation column 2 is subjected to rectification and purification in the second-stage crude distillation column 7, meanwhile, the steam rising from the column bottom of the second-stage crude distillation column 7 and the liquid flowing downwards from the column top of the second-stage crude distillation column 7 pass through the adsorbent 26, the impurities in the trichlorosilane are adsorbed, the light and heavy component impurities in the trichlorosilane are separated and removed through the double functions of rectification and purification and adsorption and impurity removal,
the gas phase trichlorosilane at the top of the second-stage crude distillation column 7 enters a reboiler 8 of the first-stage crude distillation column for heat exchange, then enters a cooler 9 at the top of the second-stage crude distillation column for condensation into liquid, then enters a reflux tank 10 of the second-stage crude distillation column, part of the liquid is pressurized by a reflux pump 11 of the second-stage crude distillation column to be used as reflux of the second-stage crude distillation column 7, the other part of the liquid is taken as the top of the column to enter a third-stage crude distillation column 12, and the trichlorosilane containing heavy component impurities, which is taken from a liquid extraction line 23 of the bottom of the second-stage crude distillation column, enters a high-boiling recovery column for separation and recovery;
the trichlorosilane from the second-stage crude distillation column 7 is subjected to rectification and purification in a third-stage crude distillation column 12, light component impurities in the trichlorosilane are separated and removed, the trichlorosilane extracted from the column bottom of the third-stage crude distillation column 12 enters a rectification column 21, gas phase from the column top of the third-stage crude distillation column 12 enters a second-stage crude distillation column reboiler 13 for heat exchange, enters a third-stage crude distillation column top cooler 14 for condensation into a liquid phase, enters a third-stage crude distillation column reflux tank 15, part of the trichlorosilane is pressurized by a third-stage crude distillation column reflux pump 16 and returns to the third-stage crude distillation column 12 as reflux, and the other part of the trichlorosilane containing light component impurities extracted from the column top of the third-stage crude distillation column 12 is separated and recovered from the low-boiling recovery column through a third-stage crude distillation column top extraction line 24;
the trichlorosilane from the third-stage crude distillation column 12 is rectified and purified in the rectifying column 21, heavy component impurities in the trichlorosilane are separated and removed again, gas-phase trichlorosilane from the top of the rectifying column 21 enters a third-stage crude distillation column reboiler 17 for heat exchange, enters a rectifying column reflux tank 19 after being condensed into liquid by a rectifying column top cooler 18, and then part of the liquid is pressurized by a rectifying column reflux pump 20 to be used as reflux and returned to the rectifying column 21, and the other part of the liquid is used as high-purity trichlorosilane from the top of the rectifying column 21 to be fed into a tank area through a rectifying column top extraction line 25, and the trichlorosilane containing heavy component impurities extracted from a rectifying column bottom extraction line 29 enters a high-boiling recovery column for separation and recovery.
Specifically, in this example, the impurity content of B, P of the crude trichlorosilane which enters the first-stage crude distillation column 2 through the crude trichlorosilane feed line 1 is 100 to 500ppb, and the impurity content of B, P in the high-purity trichlorosilane obtained through the rectifying column top extraction line 25 is 1 to 10ppb.
Specifically, the unit consumption of product steam of the electronic grade trichlorosilane purification device in the embodiment is 36.8t/tSi, namely, the unit consumption of the product steam is 36.8t for each ton of produced polysilicon.
The electronic grade trichlorosilane purifying device and method in the embodiment have the following remarkable effects:
1. the fusion of crude distillation purification and adsorption impurity removal of the trichlorosilane is realized, trace impurities in the trichlorosilane can be effectively removed in the crude distillation process, and the purification efficiency of the trichlorosilane is greatly improved;
2. the trichlorosilane in the crude distillation tower is gasified and condensed for a plurality of times, so that the trichlorosilane is adsorbed for a plurality of times in the tower, and the adsorption impurity removal effect is greatly improved;
3. the adsorption unit is arranged on the packing of the crude distillation column, so that overtemperature and overpressure of an adsorption column caused by heat release in the adsorption process in the prior art are avoided, and long-period stable operation of the adsorbent is ensured.
It is to be understood that the above embodiments are merely illustrative of the application of the principles of the present invention, but not in limitation thereof. Various modifications and improvements may be made by those skilled in the art without departing from the spirit and substance of the invention, and are also considered to be within the scope of the invention.
Claims (9)
1. An electronic grade trichlorosilane purification device, comprising:
the crude distillation column group comprises 3 crude distillation columns which are connected in series, the crude distillation columns are filler columns, the adsorption unit is used for adsorbing and removing impurities containing boron and phosphorus in crude trichlorosilane, the crude distillation column group is used for removing light component and heavy component impurities in the crude trichlorosilane through crude fraction separation, and the crude distillation column group comprises:
a first-stage crude distillation column for introducing crude trichlorosilane, removing light component impurities flowing through the first-stage crude distillation column,
the second-stage crude distillation column is connected with the tower bottom of the first-stage crude distillation column, heavy component impurities flowing through the second-stage crude distillation column are removed through the second-stage crude distillation column,
the third level crude distillation column is connected with the top of the second level crude distillation column, removes the light component impurity that flows through the third level crude distillation column, is provided with adsorption unit on the packing of second level crude distillation column or third level crude distillation column, adsorption unit includes: the adsorbent is fixed on the surface of the adsorbent filler by bonding,
the adsorption unit includes: adsorbent and fixed part thereof, fixed part includes: the bottom support plate is used for supporting the bottom of the adsorbent, and the upper pressing plate is used for pressing the upper part of the adsorbent; the bottom supporting plate and the upper pressing plate are circular in shape, the size of the bottom supporting plate and the upper pressing plate are consistent with the inner diameter of the crude distillation column in which the bottom supporting plate and the upper pressing plate are positioned, the outer diameter of the bottom supporting plate and the upper pressing plate are attached to the inner wall of the crude distillation column in which the bottom supporting plate and the upper pressing plate are positioned, and sieve holes are formed in the bottom supporting plate and the upper pressing plate; the diameter of the adsorbent is larger than the diameter of the sieve holes arranged on the bottom supporting plate and the upper pressing plate, and the fixing part is used for fixedly filling the adsorbent into the crude distillation column where the adsorbent is positioned;
and the rectifying tower is connected with the crude rectifying tower group and is used for obtaining electronic grade trichlorosilane through rectification.
2. The electronic grade trichlorosilane purification device according to claim 1, wherein the first-stage crude distillation column, the second-stage crude distillation column, the third-stage crude distillation column and the rectifying column all comprise 10 sections of packing arranged in the column, wherein the feeding position of the first-stage crude distillation column is the upper part of the fifth section of packing in the first-stage crude distillation column, the feeding position of the second-stage crude distillation column is the upper part of the second section of packing in the second-stage crude distillation column, the feeding position of the third-stage crude distillation column is the upper part of the eighth section of packing in the third-stage crude distillation column, and the feeding position of the rectifying column is the upper part of the second section of packing in the rectifying column.
3. The electronic grade trichlorosilane purification apparatus of claim 1, further comprising:
the first-stage crude distillation tower reboiler is used for heating and vaporizing the discharged materials of the tower bottoms of the first-stage crude distillation tower, and is respectively connected with the tower bottoms of the first-stage crude distillation tower and the tower top of the second-stage crude distillation tower, and the discharged materials of the tower bottoms of the first-stage crude distillation tower exchange heat with the discharged materials of the tower top of the second-stage crude distillation tower;
the second-stage crude distillation tower reboiler is used for heating and vaporizing the discharged materials of the tower bottoms of the second-stage crude distillation tower, and is respectively connected with the tower bottoms of the second-stage crude distillation tower and the tower top of the third-stage crude distillation tower, and the discharged materials of the tower bottoms of the second-stage crude distillation tower exchange heat with the discharged materials of the tower top of the third-stage crude distillation tower;
the third-stage crude distillation tower reboiler is used for heating and vaporizing the discharged material of the tower bottom of the third-stage crude distillation tower, and is respectively connected with the tower bottom of the third-stage crude distillation tower and the tower top of the rectifying tower, and the discharged material of the tower bottom of the third-stage crude distillation tower exchanges heat with the discharged material of the tower top of the rectifying tower;
and the rectifying tower reboiler is connected with the tower kettle of the rectifying tower and is used for heating and vaporizing the discharged materials of the tower kettle of the rectifying tower.
4. The electronic grade trichlorosilane purification apparatus of claim 1, further comprising:
the first-stage crude distillation column top cooler is connected with the top of the first-stage crude distillation column and is used for cooling materials discharged from the top of the first-stage crude distillation column;
the first-stage crude distillation column reflux pump is respectively connected with the first-stage crude distillation column top cooler and the top of the first-stage crude distillation column, and is used for partially extracting the materials cooled by the first-stage crude distillation column top cooler and refluxing the rest parts into the first-stage crude distillation column;
the second-stage crude distillation column top cooler is connected with the top of the second-stage crude distillation column and is used for cooling materials discharged from the top of the second-stage crude distillation column;
the second-stage crude distillation column reflux pump is respectively connected with the second-stage crude distillation column top cooler and the top of the second-stage crude distillation column, and is used for pumping part of the material cooled by the second-stage crude distillation column top cooler into the third-stage crude distillation column, and the rest part of the material flows back into the second-stage crude distillation column;
the third-stage crude distillation column top cooler is connected with the top of the third-stage crude distillation column and is used for cooling materials discharged from the top of the third-stage crude distillation column;
the third-stage crude distillation column reflux pump is respectively connected with the third-stage crude distillation column top cooler and the top of the third-stage crude distillation column, and is used for partially extracting the materials cooled by the third-stage crude distillation column top cooler and refluxing the rest parts into the third-stage crude distillation column;
the rectifying tower top cooler is connected with the rectifying tower top and is used for cooling materials discharged from the rectifying tower top;
and the rectifying tower reflux pump is respectively connected with the rectifying tower top cooler and the rectifying tower top, and is used for extracting part of the materials cooled by the rectifying tower top cooler and refluxing the rest part into the rectifying tower.
5. A method for purifying electronic grade trichlorosilane using the electronic grade trichlorosilane purifying apparatus according to any one of claims 1 to 4, comprising the steps of:
introducing the crude trichlorosilane into the electronic grade trichlorosilane purifying device of any one of claims 1 to 4 for purification to obtain the electronic grade trichlorosilane.
6. The method for purifying electronic grade trichlorosilane of claim 5, wherein the top temperature of the first-stage crude distillation column is 50-55 ℃ and the bottom temperature is 55-65 ℃.
7. The method for purifying electronic grade trichlorosilane of claim 5, wherein the temperature of the top of the second-stage crude distillation column is 73-76 ℃ and the temperature of the bottom of the column is 77-80 ℃.
8. The method for purifying electronic grade trichlorosilane of claim 5, wherein the top temperature of the third stage crude distillation column is 90-95 ℃ and the bottom temperature is 95-100 ℃.
9. The method for purifying electronic grade trichlorosilane of claim 5, wherein the temperature at the top of the rectifying tower is 90-95 ℃ and the temperature at the bottom of the rectifying tower is 110-115 ℃.
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