CN105000568A - Method for preparing high-dispersive white carbon black from fluorine-containing gas - Google Patents
Method for preparing high-dispersive white carbon black from fluorine-containing gas Download PDFInfo
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- CN105000568A CN105000568A CN201510401398.4A CN201510401398A CN105000568A CN 105000568 A CN105000568 A CN 105000568A CN 201510401398 A CN201510401398 A CN 201510401398A CN 105000568 A CN105000568 A CN 105000568A
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Abstract
The invention relates to a method for preparing high-dispersive white carbon black from fluorine-containing gas, and belongs to the technical field of chemical production. According to the method, a dispersant with the concentration being 10-48% is mixed with gas absorption liquid with the concentration being 5-30%, and a mixture is ultrasonically atomized for 0.5-3 hours to obtain atomized gas; and the atomized gas and the fluorine-containing gas are subjected to a mixed reaction at -20 DEG C to 130 DEG C for 0.5-2 hours, the obtained solid is subjected to multistage water-washing and solid-liquid separation and is dried until the surface humidity is lower than 0.8%, and the dried solid is ground and screened by a 20-60-mesh sieve to obtain the high-dispersive white carbon black. The technological method is simple, technical parameters are easy to control, the reaction cost is low, and a product produced with the process is high in purity, good in quality and excellent in dispersity.
Description
Technical field
The present invention relates to a kind of method that fluoro-gas prepares high-dispersion white carbon black, belong to chemical production technical field.
Background technology
White carbon black is because having good gumminess, reinforcing, also there is dispersion, suspension, thixotropy characteristic, make its using value high, ripe application is had in fields such as daily chemicals, chemurgy product, rubber item and papermaking, along with degree of depth industrialization development, white carbon black opens the fields such as medicine, information, optics, improves the development potentiality of white carbon black further, so white carbon black is in industrial or agricultural and in lifely have significant application value.
The traditional preparation methods of industrial white carbon black is divided into two kinds: the precipitator method and vapor phase process; The precipitator method utilize water glass acidifying to obtain white carbon black, and its technique is relatively simple, but product quality is lower; Vapor phase process utilizes silane pyrohydrolysis to produce white carbon black, its product quality is high, but raw materials cost is high, processing condition are harsh, nowadays, dissociating method rises gradually, utilize nonmetalliferous ore and extension thereof for preparing white carbon black in silicon source, the silicon-dioxide of crystallization and silicate are transformed into amorphous silicon di-oxide, the standby white carbon black of this legal system is active, purity is high, but operation is numerous and diverse, preparation condition is harsh.
Present invention process is for above method Problems existing, propose a kind of method adopting fluoro-gas to prepare high-dispersion white carbon black, greatly reduce reaction conditions, energy consumption, equipment material requirement and material cost, and white carbon black product can be made to reach the standard of vapor phase process, and industrial prospect is wide.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, present invention process, for realizing low cost, less energy-consumption, low requirement, high performance production, provides a kind of method that fluoro-gas prepares high-dispersion white carbon black.
Its technical scheme, specifically comprises the following steps:
(1) absorption liquid atomization: to be 10 ~ 48% dispersion agents by concentration with concentration be, and 5 ~ 30% ammoniacal liquor carry out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 0.5 ~ 3h, through being separated, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 0.5 ~ 2h under temperature is-20 ~ 130 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 1 ~ 6 washing, solid-liquid separation, is after < 0.8% by white carbon black, proceed to pulverizer through pulverizing, crossing 20 ~ 60 mesh sieves, obtain high-dispersion white carbon black.
In described step (1), dispersion agent is one or more mixtures in Macrogol 200, poly(oxyethylene glycol) 400, ethanol, silane coupling agent, fatty acid ester, zinc soap.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 1 ~ 10:100.
In described step (1), ultrasonic frequency is 0.02 ~ 300MHz, and ultrasonic power is 1 ~ 30kw, and preferred ultrasonic frequency is 0.5 ~ 50MHz, and ultrasonic power is 8 ~ 23kw.
Described ultrasonic atomizatio process is≤15 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 1 ~ 8:1.
Fluoro-gas is one in silicon tetrafluoride, hydrogen fluoride or two kinds of mixtures in described step (2).
For silicon tetrafluoride and hydrofluoric mass ratio are 0 ~ 5:1 or 1:0 ~ 7 in described fluoro-gas.
Dry employing vacuum-drying or cold air drying in described step (3).
Described vacuum-drying temperature is 30 ~ 70 DEG C, and vacuum tightness is 0 ~ 1000Pa; Further preferable temperature is 35 ~ 60 DEG C, and vacuum tightness is 50 ~ 800Pa; Preferable temperature is 46 DEG C further again, and vacuum tightness is 580Pa.
Described cold air drying temperature is-15 ~ 15 DEG C, and atmospheric moisture is≤0.5%.
The liquid produced after solid-liquid separation in described step (3), through concentrated, recrystallization, drying, obtains fluoride salt product.
Described fluoride salt product is Sodium Fluoride, sodium aluminum fluoride.
Beneficial effect of the present invention
1. by the application of ultrasonic atomization technology, dispersion agent is fully absorbed, and improve wetting ability and the lipophilicity of atomizing gas, in addition, atomization technique can reduce the volatility of gas; By multi-stage water wash method, effectively regulate wetting ability and the hydrophobicity of product surface, and then be easy to the surface property controlling product, improve product surface stability; Utilize the means of washing, solid-liquid separation, greatly reduce the Oil repellent of product surface, and then enhance the purity of white carbon black.
2. by appropriately adjusting technical parameter in processing step and related process, first, control the mass volume ratio of dispersion agent and ammoniacal liquor, the specific absorption of dispersion agent is maximized, by controlling ultrasonic atomization technology parameter and atomizing gas particle diameter, improve the consistency of atomizing gas both sexes, secondly, strict control mixing temperature and time, atomizing gas and fluoro-gas are fully reacted, and then Improving The Quality of Products, carry out traditional detection and analysis in conjunction with to the quality of product, known: SiO in this product
2content reaches more than 95wt%, can illustrate that this product purity is high; The specific surface area of this product reaches 200m
2/ more than g, much larger than the specific surface area that Traditional preparation obtains, and then becomes positive correlation by specific surface area with dispersiveness, ensure that the high dispersive performance of white carbon black.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that fluoro-gas of the present invention prepares high-dispersion white carbon black.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done description.
Embodiment 1
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 38% dispersion agent by concentration with concentration be, and 10% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 1.5h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1h in temperature under-17 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 3 washings, solid-liquid separation, is after 0.5% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 25 mesh sieves.
In described step (1), dispersion agent is Macrogol 200.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 1:100.
In described step (1), ultrasonic frequency is 0.3MHz, and ultrasonic power is 15kw.
Described ultrasonic atomizatio process is 10 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 4:1.
In described step (2), fluoro-gas is hydrogen fluoride.
Dry employing vacuum-drying in described step (3).
Described vacuum-drying temperature is 65 DEG C, and vacuum tightness is 900Pa.
The liquid produced after solid-liquid separation in described step (3), through concentrated, recrystallization, drying, obtains fluoride salt product.
Described fluoride salt product is Sodium Fluoride, sodium aluminum fluoride.
Embodiment 2
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 16% dispersion agent by concentration with concentration be, and 7% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 2h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 0.8h under temperature is 3 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 5 washings, solid-liquid separation, is after 0.09% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 40 mesh sieves.
In described step (1), dispersion agent is ethanol.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 3:100.
In described step (1), ultrasonic frequency is 176MHz, and ultrasonic power is 27kw.
Described ultrasonic atomizatio process is 4.5 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 7:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 3:1 in described fluoro-gas
Dry employing vacuum-drying in described step (3).
Described vacuum-drying temperature is 32 DEG C, and vacuum tightness is 450Pa.
Embodiment 3
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 25% dispersion agent by concentration with concentration be, and 17% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 0.5h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1.3h under temperature is 117 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 1 washing, solid-liquid separation, is after 0.3% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 30 mesh sieves.
In described step (1), dispersion agent is the mixture of Macrogol 200, ethanol, silane coupling agent.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 9:100.
In described step (1), ultrasonic frequency is 46MHz, and ultrasonic power is 14kw.
Described ultrasonic atomizatio process is 8 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 7.5:1.
In described step (2), fluoro-gas is silicon tetrafluoride.
Dry employing cold air drying in described step (3).
Described cold air drying temperature is-13 DEG C, and atmospheric moisture is 0.4%.
Embodiment 4
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 13% dispersion agent by concentration with concentration be, and 21% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 3h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 2h under temperature is 98 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 4 washings, solid-liquid separation, is after 0.6% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 60 mesh sieves.
In described step (1), dispersion agent is the mixture of ethanol and silane coupling agent.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 6.5:100.
In described step (1), ultrasonic frequency is 295MHz, and ultrasonic power is 2kw.
Described ultrasonic atomizatio process is 1.2 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 1:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 1:1 in described fluoro-gas.
Dry employing cold air drying in described step (3).
Described cold air drying temperature is 10 DEG C, and atmospheric moisture is 0.09%.
Embodiment 5
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 30% dispersion agent by concentration with concentration be, and 28% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 3h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1.5h under temperature is 46 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 6 washings, solid-liquid separation, is after 0.05% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 33 mesh sieves.
In described step (1), dispersion agent is the mixture of Macrogol 200, poly(oxyethylene glycol) 400, fatty acid ester.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 10:100.
In described step (1), ultrasonic frequency is 53MHz, and ultrasonic power is 1 ~ 30kw.
Described ultrasonic atomizatio process is 5 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 7:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 1:6 in described fluoro-gas.
Dry employing vacuum-drying in described step (3).
Described vacuum-drying temperature is 56 DEG C, and vacuum tightness is 135Pa.
Embodiment 6
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 40% dispersion agent by concentration with concentration be, and 21% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 2.5h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1.7h under temperature is 25 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 6 washings, solid-liquid separation, is after 0.1% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 47 mesh sieves.
In described step (1), dispersion agent is the mixture of Macrogol 200, poly(oxyethylene glycol) 400, fatty acid ester, zinc soap.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 3:100.
In described step (1), ultrasonic frequency is 0.08MHz, and ultrasonic power is 12kw.
Described ultrasonic atomizatio process is 0.7 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 2:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 5:1 in described fluoro-gas.
Dry employing cold air drying in described step (3).
Described cold air drying temperature is 3 DEG C, and atmospheric moisture is 0.25%.
Embodiment 7
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 18% dispersion agent by concentration with concentration be, and 6% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 2h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1h in temperature under-5 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 3 washings, solid-liquid separation, is after 0.1% by white carbon black, proceed to pulverizer and obtain high-dispersion white carbon black through pulverizing, crossing 53 mesh sieves.
In described step (1), dispersion agent is the mixture of Macrogol 200, poly(oxyethylene glycol) 400, ethanol, silane coupling agent, fatty acid ester, zinc soap.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 6:100.
In described step (1), ultrasonic frequency is 25MHz, and ultrasonic power is 3kw.
Described ultrasonic atomizatio process is 0.25 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 2.5:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 1:2 in described fluoro-gas.
Dry employing cold air drying in described step (3).
Described cold air drying temperature is 8 DEG C, and atmospheric moisture is 0.3%.
Embodiment 8
Fluoro-gas prepares a method for high-dispersion white carbon black, the steps include:
(1) absorption liquid atomization: to be 29% dispersion agent by concentration with concentration be, and 25% ammoniacal liquor carries out mixing being placed on is atomized in still, after carrying out ultrasonic atomizatio process 1.5h, through separation, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 1.8h under temperature is 76 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 6 washings, solid-liquid separation, is after 0.15% by white carbon black, proceed to pulverizer through pulverizing, crossing 55 mesh sieves, obtain high-dispersion white carbon black.
In described step (1), dispersion agent is the mixture of poly(oxyethylene glycol) 400, silane coupling agent.
In described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 3:100.
In described step (1), ultrasonic frequency is 0.6MHz, and ultrasonic power is 16kw.
Described ultrasonic atomizatio process is 0.3 μm to the particle diameter of atomizing gas.
In described step (2), atomizing gas and fluoro-gas throughput ratio are 1:1.
The middle fluoro-gas of described step (2) is silicon tetrafluoride, the mixture of both hydrogen fluoride.
For silicon tetrafluoride and hydrofluoric mass ratio are 1:5 in described fluoro-gas.
Dry employing cold air drying in described step (3).
Described cold air drying temperature is-6 DEG C, and atmospheric moisture is 0.07%.
Test example 1
Adopt traditional detection mode, carry out detection contrast to white carbon black prepared by vapor phase process, the precipitator method, dissociating method, embodiment 1-8 scheme, its result is as shown in table 1 below:
Table 1
| SiO 2Content (wt%) | Specific surface area (m 2/g) |
| Vapor phase process | 98.1 | 120 |
| The precipitator method | 91.3 | 136 |
| Dissociating method | 97.2 | 174 |
| Embodiment 1 | 98.1 | 289 |
| Embodiment 2 | 98.5 | 283 |
| Embodiment 3 | 99.7 | 292 |
| Embodiment 4 | 97.7 | 294 |
| Embodiment 5 | 99.5 | 212 |
| Embodiment 6 | 96.8 | 287 |
| Embodiment 7 | 98.1 | 191 |
| Embodiment 8 | 96.7 | 287 |
As seen from the above table, compared with the white carbon black prepared with vapor phase process, the precipitator method, dissociating method, adopt the whiteness, the SiO that implement white carbon black prepared by 1-8 scheme
2content is higher, and this illustrates, and white carbon black purity of the present invention is high, Functionality, quality and appealing design; By contrast, the specific surface area of the white carbon black that the specific surface area of white carbon black prepared by embodiment 1-8 scheme is prepared much larger than vapor phase process, the precipitator method, dissociating method, can release: white carbon black of the present invention has high dispersive performance.
Claims (10)
1. fluoro-gas prepares a method for high-dispersion white carbon black, it is characterized in that, comprises the following steps:
(1) absorption liquid atomization: to be 10 ~ 48% dispersion agents by concentration with concentration be, and 5 ~ 30% ammoniacal liquor mix to be placed on is atomized in still, after ultrasonic atomizatio process 0.5 ~ 3h, be separated, atomized gas and remaining liq, wherein, remaining liq indwelling is stand-by;
(2) hybrid reaction: atomizing gas and fluoro-gas are carried out hybrid reaction 0.5 ~ 2h under temperature is-20 ~ 130 DEG C of conditions, obtains white carbon black;
(3) wash: the solid drying of acquisition to surface moisture, through 1 ~ 6 washing, solid-liquid separation, is after < 0.8% by white carbon black, proceed to pulverizer through pulverizing, crossing 20 ~ 60 mesh sieves, obtain high-dispersion white carbon black.
2. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, in described step (1), dispersion agent is one or more mixtures in Macrogol 200, poly(oxyethylene glycol) 400, ethanol, silane coupling agent, fatty acid ester, zinc soap.
3. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, in described step (1), the mass volume ratio of dispersion agent and ammoniacal liquor is 1 ~ 10:100.
4. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, in described step (1), ultrasonic frequency is 0.02 ~ 300MHz, and ultrasonic power is 1 ~ 30kw.
5. fluoro-gas according to claim 4 prepares the method for high-dispersion white carbon black, it is characterized in that, described ultrasonic frequency is 0.5 ~ 50MHz, and ultrasonic power is 8 ~ 23kw.
6. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, the particle diameter of described atomizing gas is≤15 μm.
7. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, in described step (2), atomizing gas and fluoro-gas throughput ratio are 1 ~ 8:1.
8. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, fluoro-gas is one in silicon tetrafluoride, hydrogen fluoride or two kinds of mixtures in described step (2).
9. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, dry employing vacuum-drying or cold air drying in described step (3).
10. fluoro-gas according to claim 1 prepares the method for high-dispersion white carbon black, it is characterized in that, the liquid produced after solid-liquid separation in described step (3), through concentrated, recrystallization, drying, obtains fluoride salt product.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293655A (en) * | 2007-04-26 | 2008-10-29 | 侯振海 | Novel method for preparing high purity silicon dioxide |
| CN103588209A (en) * | 2013-11-01 | 2014-02-19 | 青岛星火化工技术有限公司 | Method for recovery and comprehensive utilization of SiF4 gas |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101293655A (en) * | 2007-04-26 | 2008-10-29 | 侯振海 | Novel method for preparing high purity silicon dioxide |
| CN103588209A (en) * | 2013-11-01 | 2014-02-19 | 青岛星火化工技术有限公司 | Method for recovery and comprehensive utilization of SiF4 gas |
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Application publication date: 20151028 |