CN103170160A - Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane - Google Patents
Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane Download PDFInfo
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- CN103170160A CN103170160A CN201310121415XA CN201310121415A CN103170160A CN 103170160 A CN103170160 A CN 103170160A CN 201310121415X A CN201310121415X A CN 201310121415XA CN 201310121415 A CN201310121415 A CN 201310121415A CN 103170160 A CN103170160 A CN 103170160A
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- molecular sieve
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- dimethoxy
- ethane
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- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 title claims abstract description 134
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000012046 mixed solvent Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title abstract description 35
- 239000002808 molecular sieve Substances 0.000 claims abstract description 69
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 69
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001179 sorption measurement Methods 0.000 claims description 25
- 229910000077 silane Inorganic materials 0.000 claims description 24
- 230000008569 process Effects 0.000 claims description 15
- 238000001994 activation Methods 0.000 claims description 12
- 238000010926 purge Methods 0.000 claims description 9
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000000746 purification Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000008929 regeneration Effects 0.000 abstract description 3
- 238000011069 regeneration method Methods 0.000 abstract description 3
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 abstract description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000005977 Ethylene Substances 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- -1 sodium aluminum hydride Chemical compound 0.000 description 14
- SPEUIVXLLWOEMJ-UHFFFAOYSA-N 1,1-dimethoxyethane Chemical compound COC(C)OC SPEUIVXLLWOEMJ-UHFFFAOYSA-N 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 238000001514 detection method Methods 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 6
- 229920005591 polysilicon Polymers 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000002950 deficient Effects 0.000 description 4
- 238000006073 displacement reaction Methods 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- DNEHKUCSURWDGO-UHFFFAOYSA-N aluminum sodium Chemical compound [Na].[Al] DNEHKUCSURWDGO-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
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Abstract
The invention provides a water removal method by utilizing a mixed solvent of methylbenzene and 1,2-dimethoxyethane. The water removal method is characterized by causing the recycled methylbenzene and 1,2-dimethoxyethane to flow through a molecular sieve, wherein the molecular sieve is a molecular sieve abandoned in a silicane purification process. In the silicane purification process, the molecular sieve is utilized for removing ethylene in silicane, has no regeneration value after being used for multiple times and is abandoned, and the molecular sieve adopted in the water removal method provided by the invention is the molecular sieve abandoned in the silicane purification process and can remove water in the mixed solvent of methylbenzene and 1,2-dimethoxyethane, so that a water removal effect is good while the cost is saved. As the molecular sieve is crystalline state silicate or aluminosilicate with pore size, no new impurities can be introduced into the mixed solvent. Experimental results show that water content of the mixed solvent treated by the molecular sieve is reduced to be less than 1000ppm.
Description
Technical field
The present invention relates to field of polysilicon production, particularly the water-eliminating method of the mixed solvent of toluene and 1,2-dimethoxy-ethane.
Background technology
Silane thermal decomposition process is take the intermediate product of silane as purifying, and produces the method for polysilicon through thermal decomposition.Wherein, the sodium aluminum hydride method is a kind of new technology for preparing polysilicon with the main raw and auxiliary material such as sulfuric acid, silica, sodium, aluminium and hydrogen.This kind new technology mainly comprises five steps:
(1) hydrogen, sodium and reactive aluminum, prepare sodium aluminum hydride;
(2) aluminium sodium fluoride, sulfuric acid and silicon dioxde reaction obtain ocratation, sodium sulphate, aluminum sulfate and water;
(3) sodium aluminum hydride and ocratation react in the mixed solvent of toluene and 1,2-dimethoxy-ethane, obtain silane and aluminium sodium fluoride;
(4) silane is carried out purifying;
(5) thermal decomposition of silane after purifying finally obtains polysilicon and hydrogen.
In step (3), sodium aluminum hydride is the reducing agent in a kind of mixed solvent that is dissolved in toluene and 1,2-dimethoxy-ethane, and ocratation is a kind of grade oxidant of impurity of minor amount of water that contains.When sodium aluminum hydride and ocratation reaction generate silane, the mixed solvent mixed-shaped form slurry of the byproduct aluminium sodium fluoride of generation and toluene and 1,2-dimethoxy-ethane.
In downstream process, the aluminium sodium fluoride slurry separates through super-dry, and aluminium sodium fluoride forms powder, and toluene and 1,2-dimethoxy-ethane mixed solvent can reclaim the production that again is used for step (3) silane with liquid form.But in the process cycles running, the moisture in ocratation can build up in the mixed solvent of toluene and 1,2-dimethoxy-ethane.Sodium aluminum hydride contacts and may blast with large water gaging, if in solvent, water content is too high, brings potential safety hazard will for the reaction that generates silane.Because 1,2-dimethoxy-ethane and glassware for drinking water have good intersolubility, the method that adopts rectifying dewaters to the mixed solvent of toluene and 1,2-dimethoxy-ethane, and effect is relatively poor.
Summary of the invention
The technical problem that the present invention solves is to provide the water-eliminating method of the mixed solvent of a kind of toluene and 1,2-dimethoxy-ethane, and water removal effect is good, and cost is low, does not introduce new impurity.
The invention provides the water-eliminating method of the mixed solvent of a kind of toluene and 1,2-dimethoxy-ethane, it is characterized in that, with the mixed solvent of the toluene that recycles and 1,2-dimethoxy-ethane through molecular sieve;
Described molecular sieve is the molecular sieve of abandoning in the silane purge process.
Preferably, described molecular sieve is through activation process, and the method for described activation process is:
Under inert gas shielding, molecular sieve was processed in the environment of 300～400 ℃ 20～30 hours.
Preferably, described molecular sieve is the 4A molecular sieve.
Preferably, the mass ratio of the mixed solvent of described toluene and 1,2-dimethoxy-ethane and molecular sieve is (10～50): 1.
Preferably, described mixed solvent with from bottom to top flow direction through molecular sieve.
Preferably, described molecular sieve is arranged in adsorption tower.
Compared with prior art, the present invention with the mixed solvent of the toluene that recycles and 1,2-dimethoxy-ethane through molecular sieve; Described molecular sieve is the molecular sieve of abandoning in the silane purge process.In the silane purification process, utilize the ethene in molecular sieve removal silane, when after repeatedly using, regeneration is not worth, namely go out of use, the molecular sieve that the present invention adopts is that the molecular sieve of abandoning in described silane purification process is removed toluene and 1, water in 2-dimethoxy-ethane mixed solvent, not only water removal effect is good, and saves cost.Be silicate or the alumino-silicate with the crystalline state in aperture due to molecular sieve, new impurity can be incorporated in mixed solvent.Experimental result shows, the water content of the mixed solvent after processing through molecular sieve drops to below 1000ppm.
Description of drawings
Fig. 1 is the de-watering apparatus figure that is applicable to water-eliminating method of the present invention.
The specific embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these describe just as further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses the water-eliminating method of the mixed solvent of a kind of toluene and 1,2-dimethoxy-ethane, it is characterized in that, with the toluene of recovery and the mixed solvent process molecular sieve of 1,2-dimethoxy-ethane;
Described molecular sieve is the molecular sieve of abandoning in the silane purge process.
in the present invention, described toluene and 1, the water-eliminating method of the mixed solvent of 2-dimethoxy-ethane is to be applicable to a kind of water-eliminating method that the sodium aluminum hydride method is produced polysilicon process, produce in the polysilicon process in the sodium aluminum hydride method, aluminium sodium fluoride, contain a small amount of water in the ocratation that sulfuric acid and silicon dioxde reaction obtain, water can be brought into toluene and 1 when containing the reaction of the ocratation of a small amount of water and sodium aluminum hydride, in 2-dimethoxy-ethane mixed solvent, when the toluene that recycles and 1, when the water content in 2-dimethoxy-ethane mixed solvent is larger, be about to it through molecular sieve.
Described molecular sieve is the molecular sieve of abandoning in the silane purge process.In the silane purification process, utilize the ethene in molecular sieve removal silane, when after repeatedly using, regeneration is worth, namely go out of use.The inventor is used for toluene and 1 with the molecular sieve of abandoning, dewatering of 2-dimethoxy-ethane mixed solvent, because molecular sieve in the silane purifying is used for removing ethene, and processing toluene and 1, be used for during 2-dimethoxy-ethane mixed solvent dewatering, treatment media is different, so the molecular sieve of abandoning in the silane purifying has effect preferably in removal process of the present invention.
In the present invention; the molecular sieve of abandoning in the silane purge process is preferably the 4A molecular sieve; at the toluene and 1 that uses described molecular sieve cycle for the treatment of to use; before 2-dimethoxy-ethane mixed solvent; preferably first pass through activation process; the method of described activation process is preferably: under inert gas shielding, molecular sieve was processed in the environment of 300～400 ℃ 20～30 hours.Described inert gas is preferably nitrogen.The temperature of described activation process is preferably 330～380 ℃, and the time of described activation process is preferably 23～27 hours.Molecular sieve through activation process has higher moisture removal property.
In the present invention, the mass ratio of described toluene and 1,2-dimethoxy-ethane mixed solvent and molecular sieve is preferably (10～50): 1, and namely the double centner molecular sieve can be processed 1～5 ton of mixed solvent, is preferably (20～40): 1.
In order to make mixed solvent easily fast by molecular sieve, the mixed solvent of described toluene and 1,2-dimethoxy-ethane preferably with from bottom to top flow direction through molecular sieve.Described molecular sieve is preferably disposed in adsorption tower, and namely described water-eliminating method preferably carries out in adsorption tower, and the present invention does not have particular restriction to the structure of adsorption tower, selects to get final product according to those skilled in the art's general knowledge.In order to guarantee to dewater fully, the mixed solvent of described toluene and 1,2-dimethoxy-ethane can pass through a plurality of adsorption towers continuously.A plurality of adsorption towers also can be set up in parallel, and after having an adsorption tower to lose efficacy, the mixed solvent of pending toluene and 1,2-dimethoxy-ethane can be switched to other adsorption towers and remove water treatment.
Remove the device of water treatment specifically referring to Fig. 1, Fig. 1 is the de-watering apparatus figure that is applicable to water-eliminating method of the present invention, and Fig. 1 comprises the solvent tank and the adsorption tower 1 and the adsorption tower 2 that are set up in parallel of the mixed solvent of storage toluene and 1,2-dimethoxy-ethane.The mixed solvent of toluene and 1,2-dimethoxy-ethane can dewater through adsorption tower 1 or adsorption tower 2 after being flowed out by solvent tank.
Before dewatering, preferably the gas in adsorption tower is replaced the air in emptying adsorption tower in adsorption tower.Gas enters discarded combustion system, and the detection of taking a sample of the exhaust outlet of opposed firing system is measured wherein oxygen content lower than 5ppm, and organic solvent content is below 1%, and dew point stops nitrogen replacement lower than after-60 ℃.If defective, need to proceed displacement, until after qualified, can remove water treatment.
In the present invention, except after water treatment, to toluene and 1, the water content of the mixed solvent of 2-dimethoxy-ethane detects, and result shows, the front mixed solvent water content that dewaters is at 10000～20000ppm, after processing through molecular sieve, the water content in mixed solvent can reach below 1000ppm; Except before water treatment, the water content in mixed solvent is when 2000ppm is following, and the water content in the rear mixed solvent that dewaters can reach below 200ppm.
In order further to understand the present invention, below in conjunction with embodiment, the water-eliminating method of the mixed solvent of toluene provided by the invention and 1,2-dimethoxy-ethane is described, protection scope of the present invention is not limited by the following examples.
Embodiment 1
With pack into 0.4 meter of diameter of the 4A molecular sieve of abandoning in 180kg silane purge process, free height is in the adsorption tower of 2.5 meters, with molecular sieve activation process 24 hours at 320 ℃ of temperature.
After the molecular sieve of packing into, with nitrogen, adsorption tower is replaced the air in emptying tower.Gas enters waste-gas burning system, and the detection of taking a sample of the exhaust outlet of opposed firing system is measured wherein oxygen content lower than 5ppm, and organic solvent content is below 1%, and dew point stops nitrogen replacement lower than after-60 ℃.If defective, need to proceed displacement, until qualified.
The mixed solvent of the toluene that recycles and 1,2-dimethoxy-ethane is entered from the adsorption tower bottom, with the molecular sieve of flowing through of flow direction from bottom to top.
Toluene after processing and the mixed solvent of 1,2-dimethoxy-ethane are detected, the data that dewater of detection, before the mixed solvent of toluene and 1,2-dimethoxy-ethane is processed, water content is 4963ppm, the water content after processing is 325ppm.
Embodiment 2
With pack into 0.4 meter of diameter of the 4A molecular sieve of abandoning in 180kg silane purge process, free height is in the adsorption tower of 2.5 meters, with molecular sieve activation process 24 hours at 330 ℃ of temperature.
After the molecular sieve of packing into, with nitrogen, adsorption tower is replaced the air in emptying tower.Gas enters waste-gas burning system, and the detection of taking a sample of the exhaust outlet of opposed firing system is measured wherein oxygen content lower than 5ppm, and organic solvent content is below 1%, and dew point stops nitrogen replacement lower than after-60 ℃.If defective, need to proceed displacement, until qualified.
The mixed solvent of toluene and 1,2-dimethoxy-ethane is entered from the adsorption tower bottom, with the molecular sieve of flowing through of flow direction from bottom to top.
Toluene after processing and the mixed solvent of 1,2-dimethoxy-ethane are detected, the data that dewater of detection, before the mixed solvent of toluene and 1,2-dimethoxy-ethane is processed, water content is 6570ppm, the water content after processing is 437ppm.
Embodiment 3
With pack into 0.4 meter of diameter of the 4A molecular sieve of abandoning in 180kg silane purge process, free height is in the adsorption tower of 2.5 meters, with molecular sieve activation process 24 hours at 375 ℃ of temperature.
After the molecular sieve of packing into, with nitrogen, adsorption tower is replaced the air in emptying tower.Gas enters waste-gas burning system, and the detection of taking a sample of the exhaust outlet of opposed firing system is measured wherein oxygen content lower than 5ppm, and organic solvent content is below 1%, and dew point stops nitrogen replacement lower than after-60 ℃.If defective, need to proceed displacement, until qualified.
The mixed solvent of toluene and 1,2-dimethoxy-ethane is entered from the adsorption tower bottom, with the molecular sieve of flowing through of flow direction from bottom to top.
Toluene after processing and the mixed solvent of 1,2-dimethoxy-ethane are detected, the data that dewater of detection, before the mixed solvent of toluene and 1,2-dimethoxy-ethane is processed, water content is 14109ppm, the water content after processing is 989ppm.
The explanation of above embodiment just is used for helping to understand method of the present invention and core concept thereof.Should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of claim of the present invention.
To the above-mentioned explanation of the disclosed embodiments, make this area professional and technical personnel can realize or use the present invention.Multiple modification to these embodiment will be apparent concerning those skilled in the art, and General Principle as defined herein can be in the situation that do not break away from the spirit or scope of the present invention, realization in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (6)
1. the water-eliminating method of the mixed solvent of a toluene and 1,2-dimethoxy-ethane, is characterized in that, with the mixed solvent of the toluene that recycles and 1,2-dimethoxy-ethane through molecular sieve;
Described molecular sieve is the molecular sieve of abandoning in the silane purge process.
2. water-eliminating method according to claim 1, is characterized in that, described molecular sieve is through activation process, and the method for described activation process is:
Under inert gas shielding, molecular sieve was processed in the environment of 300～400 ℃ 20～30 hours.
3. water-eliminating method according to claim 2, is characterized in that, described molecular sieve is the 4A molecular sieve.
4. water-eliminating method according to claim 3, is characterized in that, the mixed solvent of described toluene and 1,2-dimethoxy-ethane and the mass ratio of molecular sieve are (10～50): 1.
5. water-eliminating method according to claim 1, is characterized in that, described mixed solvent passes through molecular sieve with flow direction from bottom to top.
6. water-eliminating method according to claim 1, is characterized in that, described molecular sieve is arranged in adsorption tower.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310121415.XA CN103170160B (en) | 2013-04-09 | 2013-04-09 | Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane |
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| CN201310121415.XA CN103170160B (en) | 2013-04-09 | 2013-04-09 | Water removal method by utilizing mixed solvent of methylbenzene and 1,2-dimethoxyethane |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151146A (en) * | 2014-08-11 | 2014-11-19 | 浙江中宁硅业有限公司 | Dehydrating method for organic solvent |
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| CN1221775A (en) * | 1997-12-31 | 1999-07-07 | 中国科学院大连化学物理研究所 | Dewatering tech. for microwater in organic solvent |
| US20120160702A1 (en) * | 2010-12-23 | 2012-06-28 | Memc Electronic Materials, Inc. | Methods for producing silane |
| CN102716731A (en) * | 2012-07-17 | 2012-10-10 | 六九硅业有限公司 | Molecular sieve regeneration method and equipment |
| CN202555005U (en) * | 2012-05-11 | 2012-11-28 | 山东鸿正电池材料科技有限公司 | Parallel-type organic solvent water removal system |
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2013
- 2013-04-09 CN CN201310121415.XA patent/CN103170160B/en not_active Expired - Fee Related
Patent Citations (4)
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|---|---|---|---|---|
| CN1221775A (en) * | 1997-12-31 | 1999-07-07 | 中国科学院大连化学物理研究所 | Dewatering tech. for microwater in organic solvent |
| US20120160702A1 (en) * | 2010-12-23 | 2012-06-28 | Memc Electronic Materials, Inc. | Methods for producing silane |
| CN202555005U (en) * | 2012-05-11 | 2012-11-28 | 山东鸿正电池材料科技有限公司 | Parallel-type organic solvent water removal system |
| CN102716731A (en) * | 2012-07-17 | 2012-10-10 | 六九硅业有限公司 | Molecular sieve regeneration method and equipment |
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| Title |
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| 翟芝明等: "废分子筛综合利用的研究", 《矿冶工程》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104151146A (en) * | 2014-08-11 | 2014-11-19 | 浙江中宁硅业有限公司 | Dehydrating method for organic solvent |
| CN104151146B (en) * | 2014-08-11 | 2016-04-13 | 浙江中宁硅业有限公司 | A kind of dewatering of organic solvent |
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| CN103170160B (en) | 2015-01-07 |
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