CN108557785A - A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material - Google Patents
A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material Download PDFInfo
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- C01B21/00—Nitrogen; Compounds thereof
- C01B21/082—Compounds containing nitrogen and non-metals and optionally metals
- C01B21/083—Compounds containing nitrogen and non-metals and optionally metals containing one or more halogen atoms
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- C08J2455/00—Characterised by the use of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08J2423/00 - C08J2453/00
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Abstract
Present invention relates particularly to a kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece includes：Gas storage tank, nickel metallic reactors, potassium hydroxide wash tower, heat-exchange system and distillation system；The invention has the advantages that compared with the prior art,：This covering device is provided with gas reservoir as buffering equipment, is conducive to the stability of flow operations；Potassium hydroxide wash is used without using adsorbent zeolite, effectively extends the continuity except acid tower operation；A kind of antimony molybdenum doping material of liner effectively extends the service life of complete equipment on flow passage components.
Description
Technical field
The invention belongs to equipment technical fields；Dress is purified more particularly to a kind of Nitrogen trifluoride using antimony molybdenum doping material
It sets.
Background technology
Nitrogen trifluoride is a kind of oxidant, but is stable gas at normal temperatures, when temperature rises to 350 DEG C or so Shi Qi
Reactivity is suitable with oxygen.Since Nitrogen trifluoride is dissociable at NF at high temperature2And F, therefore its reactivity is similar to fluorine.Nitrogen trifluoride
Mainly as fluorization agent when with other element reactions.Since it is used in electronics industry the etching of circuit, so it is related
Preparation and purification technology receives the concern of people.
CN203112506U discloses a kind of rectifying and adsorbs the device of preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride.Needle
To the existing device for preparing Nitrogen trifluoride due to some defects in structure, can not well remove in thick Nitrogen trifluoride
Impurity obtains the Nitrogen trifluoride of high-purity, the demand being unable to meet production, a kind of rectifying of the utility model offer and absorption purification
Nitrogen trifluoride prepares the device of high-purity Nitrogen trifluoride, by vial（1）, water trap（2）, sodium peroxide packed column（3）, it is thio
Metabisulfite solution bottle（4）, oxygen trap in air（5）And Nitrogen trifluoride trap（6）Connecting pipeline company is passed sequentially through in order
It connects one and constitutes.The device is not only reasonable for structure, easy to operate, and can prepare the Nitrogen trifluoride of high-purity, is a kind of
Preferably prepare the device of high-purity Nitrogen trifluoride.
CN101973535A discloses a kind of Nitrogen trifluoride rectifying preparing molten-salt growth method and prepared by adsorption method purification
The technology of high-purity Nitrogen trifluoride is mainly dried by fused-salt bath, demister, KOH absorption device, left condenser, molecular sieve
Device, right condenser, filling pump, connecting valve are constituted by being assembled into one by connecting pipeline by its system function.Reasonable design makes
It is ideal Nitrogen trifluoride fabricating technology with convenience.
CN102101657A discloses a kind of rectifying and adsorbs the technology 1 of preparing high-purity nitrogen trifluoride by purifying nitrogen trifluoride,
Mainly by oxygen trap, Nitrogen trifluoride in vial, water trap, sodium peroxide packed column, hypo solution bottle, air
Trap is constituted by being assembled into one by connecting pipeline by its system function.Reasonable design, it is easy to use, it is ideal borontrifluoride
Nitrogen fabricating technology.
Either with chemical method, still the thick gas of nitrogen trifluoride made from electrolysis all contains N2、O2、F2、HF、N2O、
NHF2、N2F2Equal impurity.That there are product purities is low for existing Nitrogen trifluoride purification process, and the perishable disadvantage of equipment limits pure
Change the industrialization of Nitrogen trifluoride.
Invention content
Insufficient present in background technology in order to overcome, the present invention provides a kind of Nitrogen trifluoride using antimony molybdenum doping material
Purification devices.
Technical solution used in the present invention is：
A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece include：Gas storage tank, nickel metal are anti-
Device, potassium hydroxide is answered to wash tower, heat-exchange system and distillation system；The gas storage tank is equipped with gas voltage stabilizer, can be steady
The stability of the fixed entire subtractive process of holding；The nickel metallic reactors are arranged behind gas reservoir, anti-in nickel metal
Difluoride can be decomposed by answering in device；The potassium hydroxide is washed tower and is arranged behind nickel metallic reactors, is divided into level-one and washes tower
Tower is washed with two level, washing storage in tower has potassium hydroxide wash, and the sour gas in nickel metallic reactors is removed；The heat is handed over
Parallel operation setting is washed in potassium hydroxide behind tower, and the moisture in gas is removed and is cooled down to gas；The distillation system setting
Behind heat exchanger, it is divided into level-one rectifying column and two-stage rectification tower, gas of nitrogen trifluoride is arranged in the bottom of level-one rectifying column
It removes, into two-stage rectification tower, is then excluded by the top of two-stage rectification tower, obtain high-purity gas of nitrogen trifluoride；It is characterized in that
A kind of antimony molybdenum doping material of liner on the Nitrogen trifluoride purification devices flow passage components.
Ranging from 170-350 DEG C of the nickel metallic reactors interior reaction temperature.
Gas temperature is dropped to -120 ~ -40 DEG C by the heat exchanger.
A kind of antimony molybdenum doping material is prepared as follows：
According to mass fraction, by 0.5-2 parts of trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, 45-60 parts
Polyether ketone resin, 0.01-0.08 parts of poly- dihydroxy indole, 10-20 parts of acrylonitrile-butadiene-styrene copolymer, 4-
8 parts of dodecyl phenol polyethenoxy ether, 5-20 parts of polyamide, 10-50 parts of antimony molybdenum dopings be modified reinforcing fillers, 0.1-1.5 parts
Bis- fluoro- 5- formyl phenylboronic acids pinacol esters of 2,6-, 0.1-3 parts of 2- butyl maleates and methyl vinyl ether it is poly-
Conjunction object, 0.2-1.2 parts of graphenes and 5-20 parts of silicone oil, which are added in premixing machine, to be premixed uniformly, and premix temperature is 60-70 DEG C, when
Between 30-50min；Then it adding the premix in hot pressing die, hot pressing is carried out after exhaust, hot pressing temperature is 180-250 DEG C, when
Between be 3-7h；Then material is added in screw extruder progress melting mixing film extrusion, you can obtain a kind of antimony molybdenum and mix
Miscellaneous material.
The antimony molybdenum doping is modified reinforcing filler and is prepared as follows：
According to mass fraction, by 50-70 parts of glass fiber powder, 3-8 parts of calcium carbonate crystal whisker, 5-10 parts of aluminium borate whisker,
2-7 parts of silicon carbide whisker, 3-8 parts of molybdenum carbide and 8-16 parts of white graphite, which is added in grinder, grinds 50-70min, so
Afterwards by mixed powder and 0.8-1.6 parts of isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters, 0.5-1.5 parts of the 1- last of the ten Heavenly stems
Base -3- methylimidazoles hexafluoro antimonate and the mixing of 100-150 parts of ethyl alcohol, are added to 60-70 DEG C, are stirred to react 50-80min,
Then it filters, obtained powder is handled into 180-240min at 100-120 DEG C, you can obtain a kind of antimony molybdenum doping and be modified enhancing filling out
Material.
The invention has the advantages that compared with the prior art,：This covering device is provided with gas reservoir and is set as buffering
It is standby, be conducive to the stability of flow operations；Potassium hydroxide wash is used without using adsorbent zeolite, is effectively extended except acid tower operates
Continuity；A kind of antimony molybdenum doping material of liner effectively extends the service life of complete equipment on flow passage components.
Specific implementation mode
Below by specific embodiment, the invention will be further described：
Embodiment 1
A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece include：Gas storage tank, nickel metal are anti-
Device, potassium hydroxide is answered to wash tower, heat-exchange system and distillation system；The gas storage tank is equipped with gas voltage stabilizer, can be steady
The stability of the fixed entire subtractive process of holding；The nickel metallic reactors are arranged behind gas reservoir, anti-in nickel metal
Difluoride can be decomposed by answering in device；The potassium hydroxide is washed tower and is arranged behind nickel metallic reactors, is divided into level-one and washes tower
Tower is washed with two level, washing storage in tower has potassium hydroxide wash, and the sour gas in nickel metallic reactors is removed；The heat is handed over
Parallel operation setting is washed in potassium hydroxide behind tower, and the moisture in gas is removed and is cooled down to gas；The distillation system setting
Behind heat exchanger, it is divided into level-one rectifying column and two-stage rectification tower, gas of nitrogen trifluoride is arranged in the bottom of level-one rectifying column
It removes, into two-stage rectification tower, is then excluded by the top of two-stage rectification tower, obtain high-purity gas of nitrogen trifluoride；It is characterized in that
A kind of antimony molybdenum doping material of liner on the Nitrogen trifluoride purification devices flow passage components.
Ranging from 170-350 DEG C of the nickel metallic reactors interior reaction temperature.
Gas temperature is dropped to -120 ~ -40 DEG C by the heat exchanger.
A kind of antimony molybdenum doping material is prepared as follows：
According to mass fraction, by 1 part of trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, 50 parts of polyether-ketone
Resin, 0.03 part of poly- dihydroxy indole, 15 parts of acrylonitrile-butadiene-styrene copolymer, 4-8 parts of dodecylphenol
Polyoxyethylene ether, 12 parts of polyamide, 30 parts of antimony molybdenum dopings are modified reinforcing filler, 0.9 part of bis- fluoro- 5- Fonnylphenyls boron of 2,6-
Sour pinacol ester, the polymer of 1.4 parts of 2- butyl maleates and methyl vinyl ether, 0.7 part of graphene and 12 parts of silicon
Oil, which is added in premixing machine, to be premixed uniformly, and premix temperature is 65 DEG C, time 40min；Then hot pressing die is added the premix to
In, hot pressing is carried out after exhaust, hot pressing temperature is 210 DEG C, time 5h；Then material is added in screw extruder and is melted
Melt mixing extrusion film forming, you can obtain a kind of antimony molybdenum doping material.
The antimony molybdenum doping is modified reinforcing filler and is prepared as follows：
According to mass fraction, by 60 parts of glass fiber powder, 5 parts of calcium carbonate crystal whisker, 8 parts of aluminium borate whisker, 5 parts of carbonization
Silicon wafer palpus, 5 parts of molybdenum carbide and 12 parts of white graphite are added in grinder and grind 60min, then by mixed powder and 1.2 parts
Isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters, 1 part of 1- decyls -3- methylimidazoles hexafluoro antimonate and 130 parts
Ethyl alcohol mixing, be added to 65 DEG C, be stirred to react 60min, then filter, obtained powder is handled into 220min at 110 DEG C, i.e.,
A kind of antimony molybdenum doping modification reinforcing filler can be obtained.
Embodiment 2
A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece include：Gas storage tank, nickel metal are anti-
Device, potassium hydroxide is answered to wash tower, heat-exchange system and distillation system；The gas storage tank is equipped with gas voltage stabilizer, can be steady
The stability of the fixed entire subtractive process of holding；The nickel metallic reactors are arranged behind gas reservoir, anti-in nickel metal
Difluoride can be decomposed by answering in device；The potassium hydroxide is washed tower and is arranged behind nickel metallic reactors, is divided into level-one and washes tower
Tower is washed with two level, washing storage in tower has potassium hydroxide wash, and the sour gas in nickel metallic reactors is removed；The heat is handed over
Parallel operation setting is washed in potassium hydroxide behind tower, and the moisture in gas is removed and is cooled down to gas；The distillation system setting
Behind heat exchanger, it is divided into level-one rectifying column and two-stage rectification tower, gas of nitrogen trifluoride is arranged in the bottom of level-one rectifying column
It removes, into two-stage rectification tower, is then excluded by the top of two-stage rectification tower, obtain high-purity gas of nitrogen trifluoride；It is characterized in that
A kind of antimony molybdenum doping material of liner on the Nitrogen trifluoride purification devices flow passage components.
Ranging from 170-350 DEG C of the nickel metallic reactors interior reaction temperature.
Gas temperature is dropped to -120 ~ -40 DEG C by the heat exchanger.
A kind of antimony molybdenum doping material is prepared as follows：
According to mass fraction, by 0.5 part of trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, 45 parts of polyethers
Ketone resin, 0.01 part of poly- dihydroxy indole, 10 parts of acrylonitrile-butadiene-styrene copolymer, 4 parts of dodecylphenol
Polyoxyethylene ether, 5 parts of polyamide, 10 parts of antimony molybdenum dopings are modified reinforcing filler, 0.1 part of bis- fluoro- 5- Fonnylphenyls boron of 2,6-
Sour pinacol ester, the polymer of 0.1 part of 2- butyl maleates and methyl vinyl ether, 0.2 part of graphene and 5 parts of silicone oil
It is added in premixing machine and premixes uniformly, premix temperature is 60 DEG C, time 30min；Then it adds the premix in hot pressing die,
Hot pressing is carried out after exhaust, hot pressing temperature is 180 DEG C, time 3h；Then material is added in screw extruder and is melted
Mixing extrusion forms a film, you can obtains a kind of antimony molybdenum doping material.
The antimony molybdenum doping is modified reinforcing filler and is prepared as follows：
According to mass fraction, by 50 parts of glass fiber powder, 3 parts of calcium carbonate crystal whisker, 5 parts of aluminium borate whisker, 2 parts of carbonization
Silicon wafer palpus, 3 parts of molybdenum carbide and 8 parts of white graphite are added in grinder and grind 50min, then by mixed powder and 0.8 part
Isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters, 0.5 part of 1- decyls -3- methylimidazoles hexafluoro antimonate and 100
The ethyl alcohol mixing of part, is added to 60 DEG C, is stirred to react 50min, then filters, obtained powder is handled 180min at 100 DEG C,
It can be obtained a kind of antimony molybdenum doping modification reinforcing filler.
Embodiment 3
A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece include：Gas storage tank, nickel metal are anti-
Device, potassium hydroxide is answered to wash tower, heat-exchange system and distillation system；The gas storage tank is equipped with gas voltage stabilizer, can be steady
The stability of the fixed entire subtractive process of holding；The nickel metallic reactors are arranged behind gas reservoir, anti-in nickel metal
Difluoride can be decomposed by answering in device；The potassium hydroxide is washed tower and is arranged behind nickel metallic reactors, is divided into level-one and washes tower
Tower is washed with two level, washing storage in tower has potassium hydroxide wash, and the sour gas in nickel metallic reactors is removed；The heat is handed over
Parallel operation setting is washed in potassium hydroxide behind tower, and the moisture in gas is removed and is cooled down to gas；The distillation system setting
Behind heat exchanger, it is divided into level-one rectifying column and two-stage rectification tower, gas of nitrogen trifluoride is arranged in the bottom of level-one rectifying column
It removes, into two-stage rectification tower, is then excluded by the top of two-stage rectification tower, obtain high-purity gas of nitrogen trifluoride；It is characterized in that
A kind of antimony molybdenum doping material of liner on the Nitrogen trifluoride purification devices flow passage components.
Ranging from 170-350 DEG C of the nickel metallic reactors interior reaction temperature.
Gas temperature is dropped to -120 ~ -40 DEG C by the heat exchanger.
A kind of antimony molybdenum doping material is prepared as follows：
According to mass fraction, by 2 parts of trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, 60 parts of polyether-ketone
Resin, 0.08 part of poly- dihydroxy indole, 20 parts of acrylonitrile-butadiene-styrene copolymer, 8 parts of dodecylphenol are poly-
Ethylene oxide ether, 20 parts of polyamide, 50 parts of antimony molybdenum dopings are modified reinforcing filler, 1.5 parts of bis- fluoro- 5- formyl phenylboronic acids of 2,6-
Pinacol ester, the polymer of 3 parts of 2- butyl maleates and methyl vinyl ether, 1.2 parts of graphenes and 20 parts of silicone oil add
It is uniform to enter into premixing machine premix, premix temperature is 70 DEG C, time 50min；Then it adds the premix in hot pressing die, arranges
Hot pressing is carried out after gas, hot pressing temperature is 250 DEG C, time 7h；Then material is added in screw extruder melt and is mixed
Refine film extrusion, you can obtain a kind of antimony molybdenum doping material.
The antimony molybdenum doping is modified reinforcing filler and is prepared as follows：
According to mass fraction, by 70 parts of glass fiber powder, 8 parts of calcium carbonate crystal whisker, 10 parts of aluminium borate whisker, 7 parts of carbon
SiClx whisker, 8 parts of molybdenum carbide and 16 parts of white graphite are added in grinder and grind 70min, then by mixed powder and 1.6
The isopropyl three of part（Dioctylphyrophosphoric acid acyloxy）Titanate esters, 1.5 parts of 1- decyls -3- methylimidazoles hexafluoro antimonate and
150 parts of ethyl alcohol mixing, is added to 70 DEG C, is stirred to react 80min, then filters, obtained powder is handled at 120 DEG C
240min, you can obtain a kind of antimony molybdenum doping modification reinforcing filler.
Comparative example 1
It is not added with trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, the other the same as in Example 1.
Comparative example 2
It is not added with polyether ketone resin, the other the same as in Example 1.
Comparative example 3
It is not added with antimony molybdenum doping and is modified reinforcing filler, the other the same as in Example 1.
Comparative example 4
Not addition polymerization dihydroxy indole, the other the same as in Example 1.
Comparative example 5
It is not added with molybdenum carbide, the other the same as in Example 1.
Comparative example 6
It is not added with 2,6-, bis- fluoro- 5- formyl phenylboronic acids pinacol esters, the other the same as in Example 1.
Comparative example 7
It is not added with the polymer of 2- butyl maleates and methyl vinyl ether, the other the same as in Example 1.
Comparative example 8
It is not added with 1- decyl -3- methylimidazole hexafluoro antimonates, the other the same as in Example 1.
Table：Properties of sample made from different process compares.
Claims (4)
1. a kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material, critical piece include：Gas storage tank, nickel metal
Reactor, potassium hydroxide wash tower, heat-exchange system and distillation system；The gas storage tank is equipped with gas voltage stabilizer, energy
The stability of the stable entire subtractive process of holding；The nickel metallic reactors are arranged behind gas reservoir, in nickel metal
Difluoride can be decomposed in reactor；The potassium hydroxide is washed tower and is arranged behind nickel metallic reactors, is divided into level-one and washes
Tower and two level wash tower, and washing storage in tower has potassium hydroxide wash, and the sour gas in nickel metallic reactors is removed；The heat
Exchanger setting is washed in potassium hydroxide behind tower, and the moisture in gas is removed and is cooled down to gas；The distillation system is set
It sets behind heat exchanger, is divided into level-one rectifying column and two-stage rectification tower, gas of nitrogen trifluoride is in the bottom of level-one rectifying column
It excludes, into two-stage rectification tower, is then excluded by the top of two-stage rectification tower, obtain high-purity gas of nitrogen trifluoride；Its feature exists
In liner antimony molybdenum doping material on the Nitrogen trifluoride purification devices flow passage components；
The antimony molybdenum doping material is prepared as follows：
According to mass fraction, by 0.5-2 parts of trifluoro propyl dimethyl silicone polymer/PEG-10 cross-linked polymers, 45-60 parts
Polyether ketone resin, 0.01-0.08 parts of poly- dihydroxy indole, 10-20 parts of acrylonitrile-butadiene-styrene copolymer, 4-
8 parts of dodecyl phenol polyethenoxy ether, 5-20 parts of polyamide, 10-50 parts of antimony molybdenum dopings be modified reinforcing fillers, 0.1-1.5 parts
Bis- fluoro- 5- formyl phenylboronic acids pinacol esters of 2,6-, 0.1-3 parts of 2- butyl maleates and methyl vinyl ether it is poly-
Conjunction object, 0.2-1.2 parts of graphenes and 5-20 parts of silicone oil, which are added in premixing machine, to be premixed uniformly, and premix temperature is 60-70 DEG C, when
Between 30-50min；Then it adding the premix in hot pressing die, hot pressing is carried out after exhaust, hot pressing temperature is 180-250 DEG C, when
Between be 3-7h；Then material is added in screw extruder progress melting mixing film extrusion, you can obtain a kind of antimony molybdenum and mix
Miscellaneous material.
2. a kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material according to claim 1, it is characterised in that：Institute
Ranging from 170-350 DEG C of the nickel metallic reactors interior reaction temperature stated.
3. a kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material according to claim 1, it is characterised in that：Institute
Gas temperature is dropped to -120 ~ -40 DEG C by the heat exchanger stated.
4. a kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material according to claim 1, it is characterised in that：Institute
Antimony molybdenum doping modification reinforcing filler is stated to be prepared as follows：
According to mass fraction, by 50-70 parts of glass fiber powder, 3-8 parts of calcium carbonate crystal whisker, 5-10 parts of aluminium borate whisker,
2-7 parts of silicon carbide whisker, 3-8 parts of molybdenum carbide and 8-16 parts of white graphite, which is added in grinder, grinds 50-70min, so
Afterwards by mixed powder and 0.8-1.6 parts of isopropyl three（Dioctylphyrophosphoric acid acyloxy）Titanate esters, 0.5-1.5 parts of the 1- last of the ten Heavenly stems
Base -3- methylimidazoles hexafluoro antimonate and the mixing of 100-150 parts of ethyl alcohol, are added to 60-70 DEG C, are stirred to react 50-80min,
Then it filters, obtained powder is handled into 180-240min at 100-120 DEG C, you can obtain a kind of antimony molybdenum doping and be modified enhancing filling out
Material.
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| CN201810436698.XA CN108557785A (en) | 2018-05-09 | 2018-05-09 | A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material |
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| CN201810436698.XA CN108557785A (en) | 2018-05-09 | 2018-05-09 | A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material |
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| CN201810436698.XA Pending CN108557785A (en) | 2018-05-09 | 2018-05-09 | A kind of Nitrogen trifluoride purification devices using antimony molybdenum doping material |
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Application publication date: 20180921 |