CN102806069B - Composition for removing metal ions in ultra-pure ammonia and use method of same - Google Patents
Composition for removing metal ions in ultra-pure ammonia and use method of same Download PDFInfo
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- CN102806069B CN102806069B CN201210289838.8A CN201210289838A CN102806069B CN 102806069 B CN102806069 B CN 102806069B CN 201210289838 A CN201210289838 A CN 201210289838A CN 102806069 B CN102806069 B CN 102806069B
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 26
- 229910021645 metal ion Inorganic materials 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000000203 mixture Substances 0.000 title claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 12
- 238000000576 coating method Methods 0.000 claims abstract description 12
- 230000003647 oxidation Effects 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 13
- 239000007767 bonding agent Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 4
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 239000005011 phenolic resin Substances 0.000 claims description 3
- 229920001568 phenolic resin Polymers 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 claims description 2
- 229910021641 deionized water Inorganic materials 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 claims description 2
- 230000007774 longterm Effects 0.000 claims description 2
- 231100000719 pollutant Toxicity 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- 125000003158 alcohol group Chemical group 0.000 claims 1
- 239000011230 binding agent Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 claims 1
- 239000011347 resin Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 2
- 230000001070 adhesive effect Effects 0.000 abstract 2
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 description 25
- 238000002156 mixing Methods 0.000 description 6
- 238000007581 slurry coating method Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002048 multi walled nanotube Substances 0.000 description 2
- 230000005693 optoelectronics Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000002109 single walled nanotube Substances 0.000 description 2
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001555 benzenes Chemical class 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- HWGNBUXHKFFFIH-UHFFFAOYSA-I pentasodium;[oxido(phosphonatooxy)phosphoryl] phosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O HWGNBUXHKFFFIH-UHFFFAOYSA-I 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000012260 resinous material Substances 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001226 triphosphate Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a composition for removing metal ions in ultra-pure ammonia and a use method of same. The composition comprises 70-90% of carbon nano tube part A and 10-30% of adhesive part B in percentage by mass, wherein the adhesive is required to be low temperature resistant and corrosion resistant. The composition disclosed by the invention can be coated in a liquid ammonia pipeline system to form an adsorbing coating. The composition disclosed by the invention and the liquid ammonia pipeline system formed by the same have the advantages of lower cost, simple process and short production period; and an obtained metal ion removed layer obtains higher metal ion removing rate and better bonding force.
Description
Technical field
The present invention relates to go in a kind of gas generation the using method of deimpurity composition and said composition, particularly a kind ofly produce and remove the composition of metal ion and the using method of said composition for ultrapure liquefied ammonia.
Background technology
Ultra-pure ammonia is the critical material that opto-electronic device is produced.Be widely used in light emitting semiconductor device LED, solar-energy photo-voltaic cell PV, the industries such as semiconductor integrated circuit IC and liquid crystal display LCD.These years, the LED of China and solar battery technology and related industry have obtained fast development.Manufacturing in LED crystal grain and solar battery sheet process, all need to use a large amount of ultra-pure ammonias as nitrogenous source.Especially LED epitaxial wafer is in the time of growth, the purity of required ammonia is very high, also higher to the requirement of metal ion wherein, if the concentration of metal ion is higher in ammonia, can form harmful doping to LED, so the concentration of a lot of metal ions all needs to be limited in ppb rank.And current domestic LED manufactures mostly dependence on import of required ammonia, and under one's control.Visible, research and development and large-scale production electron level ultra-pure ammonia are significant for development China opto-electronics.
Iijima has found CNT (CNTs) in 1991, be now widely studied its excellent performance and application.As relatively new adsorbent, CNT has been proved to be has the great potential of removing metal ion from waste water as lead, cadmium, chromium, copper and mickel etc.The result of these researchs shows, CNT is hopeful for adsorbing metal ions.
CNT is divided into two types: (1) SWCN (SWCNTs) and (2) multi-walled carbon nano-tubes (MWCNTs).Adsorption of metal ions is very complicated to the mechanism of CNT, because there will be electrostatic attraction, and the chemical action of the surface functional group of adsorption precipitation and metal ion and CNT.
Original CNT is low-down to the adsorption capacity of metal ion, if but by nitric acid, can show and improve after clorox and potassium permanganate oxidation.But the use of the CNT after oxidation, can be discharged in the liquefied ammonia of raw materials for production, and liquefied ammonia is polluted, thereby affect the purity that ultra-pure ammonia is produced.
Summary of the invention
Goal of the invention of the present invention is in order to overcome the shortcoming in background technology, and a kind of composition is provided, and can in ultra-pure ammonia is produced, effectively remove metal ion and can not have pollution to ultra-pure ammonia, and the using method of said composition is provided.
Goal of the invention of the present invention is achieved by the following technical solution: a kind of ultra-pure ammonia is removed the composition of metal ion in producing, said composition comprises being 70～90% the CNT part A through oxidation processes and 10～30% bonding agent part B in mass, wherein, part B is made up of the dispersant of mass percent 1～5%, 40～70% diluent and 25～55% binding materials, described diluent is the solvent that alcohols or benzene class etc. can be dissolved binding material, and binding material is acrylate copolymer or resinous material preferably.
Described binding material is preferably the one in can poly-phenolic resins, the epoxy resin of withstand long term exposure-33.5 ℃ low temperature.
The caliber of the described CNT part A through oxidation processes is in 1～300 nanometer, and length is in 100 nanometer～50 micron.
The oxidation treatment solution of the described CNT part A through oxidation processes is that solution is that concentration is 30～50% nitric acid, or the concentration sulfuric acid that is 20～40%, or the concentration clorox that is 40～60%.
Ultra-pure ammonia is removed a using method for the composition of metal ion in producing, this using method comprises the following steps:
1) by the CNT through oxidation processes and bonding agent respectively by mass percentage 70～90% and 10～30% ratio be made into slurry, stir with mixer;
2) described slurry is coated in the conveying pipe of raw materials ammonia, forms the coating of 20～500 microns, then dry;
3) described dried coating sand papering, makes the CNT in coating expose coating surface, in order to adsorb the metal ion in pipeline transportation, coating is with after sand papering, utilize deionized water to clean described pipe-line system by spray gun, then dry, to remove various pollutants.
The invention has the beneficial effects as follows: utilize the slurry coating of CNT and bonding agent composition to prepare adsorption of metal ions coating, and be applied to can be in effectively removing metal ion in the conveying pipe of raw materials ammonia, have and can not cause the loss of CNT to enter in liquefied ammonia to pollute.Make the pipe-line system of removing metal ion have higher metal ion clearance, adhesion, and raw material is preferably easy to get, and technique is simple, and the production cycle is shorter.
The specific embodiment
Embodiment 1:
1, use pyrolyzed-polymer legal system for CNT.
2, with the nitric acid of 30% concentration, CNT is carried out to oxidation processes.
3, taking mass percent is 2% pentasodium triphosphate of dispersing agent, 40% diluent cyclohexanone, and 58% binding material epoxy resin, stirs after mixing, forms bonding agent.
4, taking mass percent is the CNT that 30% bonding agent and mass percent are 70%, after mixing, stirs, and forms slurry.
5, the mode that adopts brush to dip slurry coating is coated in slurry in liquefied ammonia transport system.
6, then dry at 160 ℃, and use sand papering.
7, pipe-line system is cleaned, to remove various impurity.
Embodiment 2:
1, use chemical vapor deposition for carbon nanotubes.
2, with the sulfuric acid of 20% concentration, CNT is carried out to oxidation processes.
3, taking mass percent is 1% sodium hexametaphosphate dispersant, 50% diluent dimethylbenzene, and 49% binding material phenolic resins, stirs after mixing, forms bonding agent.
4, taking mass percent is the CNT that 20% bonding agent and mass percent are 80%, after mixing, stirs, and forms slurry.
5, the mode that adopts brush to dip slurry coating is coated in slurry in liquefied ammonia transport system.
6, then dry at 150 ℃, and use sand papering.
7, pipe-line system is cleaned, to remove various impurity.
Embodiment 3:
1, use arc discharge legal system for CNT.
2, with the clorox of 50% concentration, CNT is carried out to oxidation processes.
3, taking mass percent is 3% dispersant sodium pyrophosphate, 60% diluent n-butanol, and 37% binding material polyurethane, stirs after mixing, forms bonding agent.
4, taking mass percent is the CNT that 10% bonding agent and mass percent are 90%, after mixing, stirs, and forms slurry.
5, the mode that adopts brush to dip slurry coating is coated in slurry in liquefied ammonia transport system.
6, then dry at 120 ℃, and use sand papering.
7, pipe-line system is cleaned, to remove various impurity.
Claims (3)
1. ultra-pure ammonia is removed a using method for the composition of metal ion in producing, and it is characterized in that this using method comprises the following steps:
1) by the CNT through oxidation processes and bonding agent respectively by mass percentage 70～90% and 10～30% ratio be made into slurry, stir with mixer; The caliber of the described CNT through oxidation processes is in 1～300 nanometer, length is in 100 nanometer～50 micron, described binding agent is made up of the dispersant of mass percent 1～5%, 40～70% diluent and 25～55% binding materials, diluent is alcohol or the benzene solvent that can dissolve binding material, and binding material is acrylate copolymer or resin material;
2) above-mentioned slurry is coated in the conveying pipe of raw materials ammonia, forms the coating of 20～500 microns, then dry;
3) dried coating sand papering, makes the CNT in coating expose coating surface, in order to adsorb the metal ion in pipeline transportation, coating is with after sand papering, utilize deionized water to clean pipe-line system by spray gun, then dry, to remove various pollutants.
2. ultra-pure ammonia as claimed in claim 1 is removed the using method of the composition of metal ion in producing, and it is characterized in that the binding material described in step 1) is the one in poly-phenolic resins, the epoxy resin of withstand long term exposure-33.5 ℃ low temperature.
3. ultra-pure ammonia as claimed in claim 1 is removed the using method of the composition of metal ion in producing, the oxidation treatment solution that it is characterized in that the CNT through oxidation processes described in step 1) is that concentration is 30～50% nitric acid, or the sulfuric acid that concentration is 20～40%, or the concentration clorox that is 40～60%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210289838.8A CN102806069B (en) | 2012-08-15 | 2012-08-15 | Composition for removing metal ions in ultra-pure ammonia and use method of same |
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| CN201210289838.8A CN102806069B (en) | 2012-08-15 | 2012-08-15 | Composition for removing metal ions in ultra-pure ammonia and use method of same |
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| CN102806069A CN102806069A (en) | 2012-12-05 |
| CN102806069B true CN102806069B (en) | 2014-07-02 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757596A (en) * | 2005-11-07 | 2006-04-12 | 浙江大学 | Method for preparing prefab of porous carbon nanometer tube |
| CN101462713A (en) * | 2007-12-20 | 2009-06-24 | 索尼株式会社 | Method for processing carbon nano-tube, carbon nano-tube and carbon nano-tube device |
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- 2012-08-15 CN CN201210289838.8A patent/CN102806069B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757596A (en) * | 2005-11-07 | 2006-04-12 | 浙江大学 | Method for preparing prefab of porous carbon nanometer tube |
| CN101462713A (en) * | 2007-12-20 | 2009-06-24 | 索尼株式会社 | Method for processing carbon nano-tube, carbon nano-tube and carbon nano-tube device |
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| CN102806069A (en) | 2012-12-05 |
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Address after: 215152 Anmin Road, Panyang Industrial Park, Huangdai Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Jinhong Gas Co.,Ltd. Address before: 215143 No. 6 Anmin Road, Panyang Industrial Park, Huangduo Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee before: SUZHOU JINHONG GAS Co.,Ltd. |