CN103349846B - Device for rectifying and purifying decamethyl cyclopenta siloxane through organosilicon high boiling point compound and purifying process - Google Patents
Device for rectifying and purifying decamethyl cyclopenta siloxane through organosilicon high boiling point compound and purifying process Download PDFInfo
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- CN103349846B CN103349846B CN201310285459.6A CN201310285459A CN103349846B CN 103349846 B CN103349846 B CN 103349846B CN 201310285459 A CN201310285459 A CN 201310285459A CN 103349846 B CN103349846 B CN 103349846B
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- storage tank
- epipodium
- rectifying column
- tank
- high boiling
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- 238000009835 boiling Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 18
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 title abstract description 4
- 150000001875 compounds Chemical class 0.000 title abstract 2
- 238000003860 storage Methods 0.000 claims abstract description 67
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000010992 reflux Methods 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 17
- 238000000926 separation method Methods 0.000 claims abstract description 9
- -1 polycyclic compound Chemical class 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims description 42
- 239000007788 liquid Substances 0.000 claims description 33
- 238000007599 discharging Methods 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- HTDJPCNNEPUOOQ-UHFFFAOYSA-N hexamethylcyclotrisiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O1 HTDJPCNNEPUOOQ-UHFFFAOYSA-N 0.000 claims description 4
- GSANOGQCVHBHIF-UHFFFAOYSA-N tetradecamethylcycloheptasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 GSANOGQCVHBHIF-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000012856 packing Methods 0.000 claims description 3
- 230000000717 retained effect Effects 0.000 claims 1
- 125000003367 polycyclic group Chemical group 0.000 abstract 1
- 238000009833 condensation Methods 0.000 description 6
- 230000005494 condensation Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 238000004587 chromatography analysis Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000002199 base oil Substances 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000008407 cosmetic solvent Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
Abstract
The invention discloses a device for rectifying and purifying decamethyl cyclopenta siloxane through organosilicon high boiling point compound and a purifying process. The device comprises a polycyclic compound storage tank, a rectifying tower, a return tank, a reflux pump and a vacuum buffer tank. The purifying process is that a polycyclic raw material in the polycyclic compound storage tank enters into the rectifying tower from the middle parts of the rectifying tower and is heated by a reboiler; decompressed rectifying and separation are performed under the condition of vacuum, and gas phase of D5 is obtained at the tower top of the rectifying tower; after condensed by a condenser, part of the D5 flows back to the top of the rectifying tower through flow regulation, and the other part of qualified D5 is sent to a D5 storage tank through extraction regulation. The device provided by the invention is simple in structure and convenient to construct and install. The purifying process provided by the invention has the advantages of high raw material utilization ratio and high product purity.
Description
Technical field
The present invention relates to a kind of chemical production equipment and production technology, particularly relate to a kind of process units and the purifying technique that utilize high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane.
Background technology
Decamethylcyclopentaandoxane has another name called decamethylcyclopentasiloxane, is called for short D
5, refer to a kind of volatile poly dimethyl alkylene oxide, form primarily of D5.No. CAS is 541-02-6, and molecular formula is C
10h
30o
5si
5.Decamethylcyclopentaandoxane outward appearance is colourless transparent oil liquid, is volatile, silicone oil with low viscosity.It and most alcohol have good compatibility with other cosmetic solvents, and tasteless, nontoxic, non-stimulated, clean non-greasy, can be used as basic substance or carrier, the ductility had and smear.Therefore D
5can be used as the base oil of various personal care product, can be used alone, also can mutually blending use and and other solvent used in combination.
Dimethyldichlorosilane, by after hydrolysis, cracking, mainly generates dimethyl siloxane mixed methylcyclosiloxane (DMC), octamethylcy-clotetrasiloxane (D wherein
4) usually separated separately, for the production of high-temperature silicon disulfide rubber, the high boiling organosilicon point ring body mixture more than remaining five rings and five rings formed, common name epipodium.Main containing decamethylcyclopentaandoxane (D in epipodium
5), ten diformazan basic ring six siloxanes (D
6) and tetradecamethylcycloheptasiloxane (D
7) etc., and have the hexamethyl cyclotrisiloxane (D of trace
3) and octamethylcy-clotetrasiloxane (D
4).
Octamethylcy-clotetrasiloxane (D is separated for dimethyl siloxane mixed methylcyclosiloxane (DMC)
4) afterwards in remaining high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane process units not yet have relevant report at present.
Summary of the invention
The present invention is directed to the problems referred to above, provide one and utilize high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane process units and purifying technique.This described process units structure is simple, and raw material utilization efficiency is high, the decamethylcyclopentaandoxane (D of rectifying gained
5) high purity more than 99.5%.
Technical scheme of the present invention is:
High boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane device of the present invention, comprise epipodium storage tank, rectifying column, return tank, reflux pump, vacuum buffer tank, it is characterized in that rectifying column charging aperture is communicated with the discharging opening of epipodium storage tank, rectifying tower top discharging opening is communicated with the charging aperture of condenser, and rectifier bottoms discharging opening is communicated with the charging aperture of high boiling mixture storage tank; The charging aperture of return tank is communicated with the discharging opening of condenser; The charging aperture of reflux pump is communicated with the discharging opening of return tank, the discharging opening of reflux pump respectively with rectifying column tower top, low boiling mixture storage tank and D
5the charging aperture of storage tank is communicated with; Return tank is communicated with vacuum buffer tank;
Described epipodium storage tank, for storage of raw materials high boiling organosilicon point ring body mixture;
Described rectifying column, is separated epipodium mixture for rectification under vacuum;
Described return tank, for collecting refluxer;
Described vacuum buffer tank, for compensator or trimmer pressure, prevents from pouring in down a chimney, and also reaches stable vacuum simultaneously;
Described low boiling mixture storage tank, hexamethyl cyclotrisiloxane (D a small amount of in primary recipient epipodium
3) and octamethylcy-clotetrasiloxane (D
4);
Described D
5storage tank, for receiving highly purified decamethylcyclopentaandoxane (D
5) finished product;
Described high boiling mixture storage tank, primary recipient ten diformazan basic ring six siloxanes (D
6) and tetradecamethylcycloheptasiloxane (D
7) etc. material.
Preferably, between epipodium storage tank and the pipeline of rectifying column, be provided with measuring pump, be convenient to reaction and carry out continuously.
Preferably, control valve is provided with between described raw material epipodium storage tank and the pipeline of rectifying column; Described control valve selects check valve or two-way valve, comprises hand-operated valve or motor-driven valve.
Preferably, described rectifier adopts screen waviness packings structure, and bottom adopts bubble cap plate, to reduce production cost, reduces leakage, improves rectification efficiency.
Preferably, described rectifier bottoms is provided with reboiler, makes being respectively separated mutually after rectification under vacuum.
Preferably, described vacuum buffer tank is connected with two stage pump, the first order is water ring pump, and the second level is Roots vaccum pump.
Purifying technique of the present invention is:
Epipodium raw material in epipodium storage tank enters in rectifying column in the middle part of rectifying column, is heated by reboiler, under 0.005-0.03MPa vacuum condition, carries out rectification under vacuum separation.Rectifying column column bottom temperature controls at 140 ~ 160 DEG C, and tower top temperature controls at 120 ~ 125 DEG C, and rectifying column tower top obtains D
5gas phase, through condenser condenses, the condensate liquid obtained flows into return tank by potential difference, and when return tank inner condensat liquid remains on suitable liquid level, by reflux pump, a part is back to rectifying column tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank.Rectifying column materials at bottom of tower is extraction D when keeping certain liquid level
6, D
7epipodium, deliver to high boiling mixture storage tank.
Advantage of the present invention is: the present invention is used for high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane, and purification raw material comes from DMC rectifying and extracts D
4after residue higher boiling ring body mixture.Process units structure of the present invention is simple, and construction install convenience, raw material availability is high, and product purity is high, is conducive to applying.
Accompanying drawing explanation
Fig. 1 is the structural representation of process units of the present invention.
1-epipodium storage tank 2-measuring pump 3-rectifying column 4-reboiler
5-high-boiling components (D
6, D
7) storage tank 6-condenser 7-return tank
8-reflux pump 9-low-boiling-point substance (D
3, D
4) storage tank 10-D
5storage tank
11-vacuum buffer tank 12-Roots vaccum pump 13-water ring pump
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is further illustrated;
As shown in Figure 1, one utilizes high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane process units,
Comprise epipodium storage tank 1, rectifying column 3, return tank 7, reflux pump 8, vacuum buffer tank 11, the material inlet of rectifying column 3 is communicated with the discharging opening of raw material high boiling organosilicon point ring body mixture epipodium storage tank 1, rectifying column 3 tower top discharging opening is communicated with the charging aperture of condenser 6, and rectifying column 3 bottom discharge mouth is communicated with the charging aperture of high boiling mixture storage tank 5; The charging aperture of return tank 7 is communicated with the discharging opening of condenser 6; The charging aperture of reflux pump 8 is communicated with the discharging opening of return tank 7, the discharging opening of reflux pump 8 respectively with rectifying column 3 tower top, low boiling mixture storage tank 9 and D
5the charging aperture of storage tank 10 is communicated with; Return tank 7 is communicated with vacuum buffer tank 11.
Described epipodium storage tank 1, for storage of raw materials high boiling organosilicon point ring body mixture;
Described rectifying column 3, is separated epipodium mixture for rectification under vacuum;
Described return tank 7, for collecting refluxer;
Described vacuum buffer tank 11, for compensator or trimmer pressure, prevents from pouring in down a chimney, and also reaches stable vacuum simultaneously;
Described low boiling mixture storage tank 9, mainly accepts hexamethyl cyclotrisiloxane (D a small amount of in epipodium
3) and octamethylcy-clotetrasiloxane (D
4);
Described D
5storage tank 10, for receiving highly purified decamethylcyclopentaandoxane (D
5) finished product;
Described high boiling mixture storage tank 5, primary recipient ten diformazan basic ring six siloxanes (D
6) and tetradecamethylcycloheptasiloxane (D
7) etc. material.
Preferably, between the pipeline of epipodium storage tank 1 and rectifying column 3, be provided with measuring pump, be convenient to reaction and carry out continuously.
Preferably, control valve is provided with between described raw material epipodium storage tank 1 and the pipeline of rectifying column 3; Described control valve selects check valve or two-way valve, comprises hand-operated valve or motor-driven valve.
Preferably, described rectifying column 3 top adopts screen waviness packings structure, and bottom adopts bubble cap plate, to reduce production cost, reduces leakage, improves rectification efficiency.
Preferably, bottom described rectifying column 3, be provided with reboiler, make being respectively separated mutually after rectification under vacuum.
Preferably, described vacuum buffer tank 11 is connected with two stage pump, the first order is water ring pump 13, and the second level is Roots vaccum pump 12.
Purifying technique of the present invention is: the raw material high boiling organosilicon point ring body mixture in epipodium storage tank 1 enters in tower in the middle part of rectifying column 3, is heated, carry out rectification under vacuum separation by reboiler 4.Vacuum utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Rectifying column 3 tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on certain liquid level, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10.Rectifying column 3 materials at bottom of tower after cooler cooling, the extraction D when keeping certain liquid level at the bottom of tower
6, D
7epipodium, deliver to high boiling mixture storage tank 5.
now enumerate the embodiment of several concrete purifying technique
embodiment one
(D is extracted in DMC rectifying to raw material high boiling organosilicon point ring body mixture in epipodium storage tank 1
4after residue higher boiling ring body mixture) enter in tower in the middle part of rectifying column 3, heated by reboiler 4, under vacuum 0.01MPa condition, carry out rectification under vacuum separation.Vacuum system utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Column bottom temperature controls at 145 DEG C, and tower top temperature controls at 125 DEG C, and tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on liquid level 40%, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10, finished product D
5purity is 99.66% through gas chromatographic analysis.Kettle material after cooler cooling, the extraction D when keeping tower reactor certain liquid level
6, D
7epipodium, deliver to storage tank 5.
embodiment two
(D is extracted in DMC rectifying to raw material high boiling organosilicon point ring body mixture in epipodium storage tank 1
4after residue higher boiling ring body mixture) enter in tower in the middle part of rectifying column 3, heated by reboiler 4, under vacuum 0.01MPa condition, carry out rectification under vacuum separation.Vacuum system utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Column bottom temperature controls at 150 DEG C, and tower top temperature controls at 120 DEG C, and tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on liquid level 60%, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10, finished product D
5purity is 99.92% through gas chromatographic analysis.Kettle material after cooler cooling, the extraction D when keeping tower reactor certain liquid level
6, D
7epipodium, deliver to storage tank 5.
embodiment three
(D is extracted in DMC rectifying to raw material high boiling organosilicon point ring body mixture in epipodium storage tank 1
4after residue higher boiling ring body mixture) enter in tower in the middle part of rectifying column 3, heated by reboiler 4, under vacuum 0.02MPa condition, carry out rectification under vacuum separation.Vacuum system utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Column bottom temperature controls at 156 DEG C, and tower top temperature controls at 122 DEG C, and tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on liquid level 40%, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10, finished product D
5purity is 99.64% through gas chromatographic analysis.Kettle material after cooler cooling, the extraction D when keeping tower reactor certain liquid level
6, D
7epipodium, deliver to storage tank 5.
embodiment four
Epipodium in epipodium storage tank 1 enters in tower in the middle part of rectifying column 3, is heated by reboiler 4, under vacuum 0.02MPa condition, carries out rectification under vacuum separation.Vacuum system utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Column bottom temperature controls at 150 DEG C, and tower top temperature controls at 121 DEG C, and tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on liquid level 60%, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10, finished product D
5purity is 99.83% through gas chromatographic analysis.Kettle material after cooler cooling, the extraction D when keeping tower reactor certain liquid level
6, D
7epipodium, deliver to storage tank 5.
embodiment five
(D is extracted in DMC rectifying to raw material high boiling organosilicon point ring body mixture in epipodium storage tank 1
4after residue higher boiling ring body mixture) enter in tower in the middle part of rectifying column 3, heated by reboiler 4, under vacuum 0.03MPa condition, carry out rectification under vacuum separation.Vacuum system utilizes two stage pump, and the first order is water ring pump 13, and the second level is Roots vaccum pump 12.Column bottom temperature controls at 160 DEG C, and tower top temperature controls at 124 DEG C, and tower top obtains D
5gas phase, through condenser 6 condensation, condensate liquid flows into return tank 7 by potential difference, and when return tank 7 inner condensat liquid remains on liquid level 40%, by reflux pump 8, a part is back to tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank 10, finished product D
5purity is 99.59% through gas chromatographic analysis.Kettle material after cooler cooling, the extraction D when keeping tower reactor certain liquid level
6, D
7epipodium, deliver to storage tank 5.
Claims (2)
1. the device of a high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane, comprise: epipodium storage tank, rectifying column, return tank, reflux pump, vacuum buffer tank, it is characterized in that rectifying column charging aperture is communicated with the discharging opening of epipodium storage tank, rectifying tower top discharging opening is communicated with the charging aperture of condenser, and rectifier bottoms discharging opening is communicated with the charging aperture of high boiling mixture storage tank; The charging aperture of return tank is communicated with the discharging opening of condenser; The charging aperture of reflux pump is communicated with the discharging opening of return tank, the discharging opening of reflux pump respectively with rectifying column tower top, low boiling mixture storage tank and D
5the charging aperture of storage tank is communicated with; Return tank is communicated with vacuum buffer tank;
Described epipodium storage tank, for storage of raw materials high boiling organosilicon point ring body mixture;
Described rectifying column, is separated epipodium mixture for rectification under vacuum;
Described return tank, for collecting refluxer;
Described vacuum buffer tank, for compensator or trimmer pressure, prevents from pouring in down a chimney, and also reaches stable vacuum simultaneously;
Described low boiling mixture storage tank, hexamethyl cyclotrisiloxane D a small amount of in primary recipient epipodium
3with octamethylcy-clotetrasiloxane D
4;
Described D
5storage tank, for receiving highly purified decamethylcyclopentaandoxane D
5finished product;
Described high boiling mixture storage tank, primary recipient ten diformazan basic ring six siloxanes D
6and tetradecamethylcycloheptasiloxane D
7deng material; Be provided with measuring pump between epipodium storage tank and the pipeline of rectifying column, be convenient to reaction and carry out continuously; Control valve is provided with between described raw material epipodium storage tank and the pipeline of rectifying column; Described control valve selects check valve or two-way valve, comprises hand-operated valve or motor-driven valve; Described rectifier adopts screen waviness packings structure, and bottom adopts bubble cap plate, to reduce production cost, reduces leakage, improves rectification efficiency; Described rectifier bottoms is provided with reboiler, makes being respectively separated mutually after rectification under vacuum; Described vacuum buffer tank is connected with two stage pump, and the first order is water ring pump, and the second level is Roots vaccum pump.
2. the technique of high boiling organosilicon point ring body mixture rectification and purification decamethylcyclopentaandoxane according to claim 1, it is characterized by this processing step at least to comprise: the epipodium raw material in epipodium storage tank enters in rectifying column in the middle part of rectifying column, heated by reboiler, under 0.005-0.03MPa vacuum condition, carry out rectification under vacuum separation; Rectifying column column bottom temperature controls at 140 ~ 160 DEG C, and tower top temperature controls at 120 ~ 125 DEG C, and rectifying column tower top obtains D
5gas phase, through condenser condenses, the condensate liquid obtained flows into return tank by potential difference, and when return tank inner condensat liquid remains on suitable liquid level, by reflux pump, a part is back to rectifying column tower top through Flow-rate adjustment, the D that a part is qualified
5regulate through extraction and deliver to D
5storage tank, rectifying column materials at bottom of tower is extraction D when being retained to certain liquid level
6, D
7epipodium, deliver to high boiling mixture storage tank.
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CN106582052B (en) * | 2016-12-20 | 2018-11-16 | 湖北兴瑞化工有限公司 | A kind of method and device of organosilicon ring body mixture rectifying |
CN111234227B (en) * | 2020-03-07 | 2022-08-19 | 江西赣江新区有机硅创新研究院有限公司 | Low-molecular-weight methyl silicone oil and preparation method thereof |
CN113603718B (en) * | 2021-07-28 | 2023-11-24 | 湖北兴瑞硅材料有限公司 | Vacuum process for cracking dimethyl dichlorosilane hydrolysate |
CN114669071B (en) * | 2022-04-06 | 2024-09-10 | 中国恩菲工程技术有限公司 | Vacuum rectification device and method for silicon-based electronic product |
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