EP2804694A1 - Chemischer filter mit trockenmittelwaben sowie herstellungsverfahren dafür - Google Patents
Chemischer filter mit trockenmittelwaben sowie herstellungsverfahren dafürInfo
- Publication number
- EP2804694A1 EP2804694A1 EP13706714.6A EP13706714A EP2804694A1 EP 2804694 A1 EP2804694 A1 EP 2804694A1 EP 13706714 A EP13706714 A EP 13706714A EP 2804694 A1 EP2804694 A1 EP 2804694A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- desiccant
- chemical filter
- matrix
- silicate
- range
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
- 239000002274 desiccant Substances 0.000 title claims abstract description 120
- 239000000126 substance Substances 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims description 40
- 238000004519 manufacturing process Methods 0.000 title claims description 11
- 239000011159 matrix material Substances 0.000 claims abstract description 75
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 26
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000010457 zeolite Substances 0.000 claims abstract description 23
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 19
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 claims abstract description 19
- 229910052914 metal silicate Inorganic materials 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 14
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 12
- 239000000741 silica gel Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- 239000002808 molecular sieve Substances 0.000 claims abstract description 6
- 239000007800 oxidant agent Substances 0.000 claims abstract description 6
- 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 6
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 45
- 239000000356 contaminant Substances 0.000 claims description 35
- 238000011068 loading method Methods 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 24
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 23
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 21
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 20
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 19
- 239000004115 Sodium Silicate Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 235000019353 potassium silicate Nutrition 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 13
- 239000000499 gel Substances 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 13
- 239000012855 volatile organic compound Substances 0.000 claims description 13
- 239000000376 reactant Substances 0.000 claims description 12
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000003365 glass fiber Substances 0.000 claims description 11
- 239000004133 Sodium thiosulphate Substances 0.000 claims description 10
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 10
- 239000012286 potassium permanganate Substances 0.000 claims description 10
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 10
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 10
- 239000004964 aerogel Substances 0.000 claims description 9
- 239000000835 fiber Substances 0.000 claims description 9
- 239000000017 hydrogel Substances 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 9
- 239000000123 paper Substances 0.000 claims description 9
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 7
- 239000012784 inorganic fiber Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000004111 Potassium silicate Substances 0.000 claims description 4
- 150000007513 acids Chemical class 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000002655 kraft paper Substances 0.000 claims description 4
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical group [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims description 4
- 229910052913 potassium silicate Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- 239000003463 adsorbent Substances 0.000 description 28
- 238000001179 sorption measurement Methods 0.000 description 28
- 229910052799 carbon Inorganic materials 0.000 description 20
- 238000005470 impregnation Methods 0.000 description 13
- 239000000243 solution Substances 0.000 description 13
- 239000002904 solvent Substances 0.000 description 11
- 239000011148 porous material Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 230000008929 regeneration Effects 0.000 description 7
- 238000011069 regeneration method Methods 0.000 description 7
- 239000011149 active material Substances 0.000 description 6
- 230000002378 acidificating effect Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000011084 recovery Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 238000007791 dehumidification Methods 0.000 description 4
- 239000011152 fibreglass Substances 0.000 description 4
- 239000011261 inert gas Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 230000001172 regenerating effect Effects 0.000 description 3
- 150000004760 silicates Chemical class 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-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
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 229910052634 enstatite Inorganic materials 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 2
- 235000019645 odor Nutrition 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 239000011591 potassium Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- -1 water glass silicates Chemical class 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical class S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000000274 adsorptive effect Effects 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 150000003842 bromide salts Chemical class 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001143 conditioned effect Effects 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 231100001240 inorganic pollutant Toxicity 0.000 description 1
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000012229 microporous material Substances 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/26—Drying gases or vapours
- B01D53/28—Selection of materials for use as drying agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/2805—Sorbents inside a permeable or porous casing, e.g. inside a container, bag or membrane
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
- B01J20/3234—Inorganic material layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/106—Silica or silicates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/30—Physical properties of adsorbents
- B01D2253/34—Specific shapes
- B01D2253/342—Monoliths
- B01D2253/3425—Honeycomb shape
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/708—Volatile organic compounds V.O.C.'s
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/90—Odorous compounds not provided for in groups B01D2257/00 - B01D2257/708
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F2203/00—Devices or apparatus used for air treatment
- F24F2203/10—Rotary wheel
- F24F2203/1032—Desiccant wheel
- F24F2203/1036—Details
Definitions
- the present invention relates to a chemical filter for removal of contaminants from air present in industrial or domestic environments. More particularly, the present invention relates to a desiccant based honeycomb chemical filter. The present invention also relates to a method for the manufacture of a desiccant based honeycomb chemical filter.
- this invention relates to a desiccant based chemical filter, such as a honeycomb chemical filter, for the removal of contaminants from air present in industrial or domestic environments.
- the present invention also provides to a method for the manufacture of a desiccant based honeycomb chemical filter.
- the contaminants to be removed are typically gaseous contaminants but can also comprise contaminants in the form of fine liquid droplets which are not easily removable by conventional means.
- the term 'desiccant' as used herein is intended to cover both macroporous and microporous desiccant or desiccants.
- the desiccant or desiccants based honeycomb matrix used in the invention is impregnated with different impregnating materials.
- the invention also provides methods for removal of gaseous contaminants, pollutants and odors from industrial processes using the said chemical filter.
- This invention also relates to a process for manufacturing macroporous /microporous desiccant or desiccants based honeycomb matrix impregnated with different impregnants for removing gaseous contaminants contained in air or odour in the air.
- Odours in industrial environments, and also in non-industrial environments such as passenger compartments of transportation vehicles are due to volatile organic compounds present in the circulating air. These organic compounds are formed in high levels but at relatively low concentrations from engine exhaust, solvents, gas turbines, cogeneration plants, petrochemical plants, and in many industrial processes where waste gases contain materials such as solvent vapors, inks, paints, etc.
- Volatile organic compounds comprise not only hydrocarbons, whether saturated, unsaturated, or aromatic, but also contain oxygenated materials such as alcohols, esters, ethers, and acids, nitrogen containing compounds (principally amines), sulfur containing materials (mercaptans and thioethers) and halogen-containing materials, especially chlorine-substituted hydrocarbons but also organic fluorides and bromides.
- oxygenated materials such as alcohols, esters, ethers, and acids
- nitrogen containing compounds principally amines
- sulfur containing materials mercaptans and thioethers
- halogen-containing materials especially chlorine-substituted hydrocarbons but also organic fluorides and bromides.
- a traditional method for solvent recovery from humid air comprised an adsorption system which typically was operated till the solvent concentration in the outlet gas stream reached a detectable preset breakthrough level. When this level was reached, the flow of gas to the adsorber was stopped. The adsorbent bed then contained solvent, other condensable organic contaminants, and some amount of water dependent on the inlet relative humidity of the solvent laden gas stream.
- This method was subsequently modified by the introduction of a hot inert gas or steam, either saturated or superheated, which displaces the solvent from the adsorbent to produce a solvent/water mixture upon condensation.
- a hot inert gas or steam either saturated or superheated
- two adsorber beds were used, where one was adsorbing while the other bed underwent regeneration.
- Further developments in regenerating and recovering solvents from adsorbent beds involve the use of inert gases or air and low temperature condensation of the solvent from the regenerating gas/air. However, these techniques are not directly applicable in all given situations where required.
- U.S. Pat. No. 4,421 ,532 discloses a process for the recovery of VOCs from industrial waste gases by thermal swing adsorption including the use of hot inert gases circulating in a closed cycle to desorb the VOCs.
- U.S. Pat. No. 4, 134,743 discloses a process and apparatus where the adsorbent body is a wheel of thin sheets or layers of fibrous material containing about 10 to 90% by weight of a freely divided molecular sieve material.
- the apparatus includes a means for passing air to be processed in one direction through the wheel and a means for passing a regenerative air stream countercurrent to the air to be processed.
- a cooling stream is provided in a direction co-current with the air stream.
- U.S. Pat. No. 4,887,438 discloses a desiccant assisted air conditioning system for delivering dehumidified refrigerated air to a conditioned space based on an adsorbent wheel.
- Meckler teaches the use of a desiccant wheel coated with silica gel, or a preferred hygroscopic salt, lithium chloride, to remove moisture from air.
- This citation teaches the use of waste heat from the refrigeration condenser to heat the reactivation air and employs a liquid refrigerant injection into the compressor to increase the pressure ratio in a positive displacement compressor to counter the problem of "thermal dumpback".
- Thermal dumpback is the associated heat conducted from the desiccant wheel to the treated air which occurs following the exposure of the wheel to heated regeneration air. This associated heat adds to the overall cooling load on the refrigeration system.
- U.S. Pat. No. 5,242,473 discloses a gas dehumidifying apparatus which exhibits improved dehumidification efficiency to provide a treated gas with a high dryness level employing two dehumidifier rotors, wherein the second rotor uses a synthetic zeolite.
- Gas to be dehumidified is passed first to a silica gel coated rotor and then to the zeolite coated rotor.
- the rotors are regenerated by supplying a stream of heated gas through the second rotor and then the first rotor so that the adsorbent in the first rotor is regenerated at a lower temperature than the zeolite in the second rotor.
- a portion of the treated gas is used to countercurrently cool the rotors following regeneration.
- adsorbent that is used.
- Hydrophilic adsorbents such as silica gel are typically chosen for dehumidification applications, but are poor adsorbents for volatile organic contaminant removal.
- hydrophobic adsorbents such as high silica zeolites are typically recommended for VOC removal applications, but are poor adsorbents for dehumidification application.
- applications for both dehumidification and VOC removal may typically require both types of adsorbents.
- adsorbent-coated paper and some adsorbent salts have a limited range of humidity and temperature within which they can maintain structural integrity. This failure also limits the regeneration medium to dry, moderate temperature gases and air. Contact between the adsorbent and gas stream and hence adsorbent capacity for VOCs is limited to very thin layers of adsorbent on the surface of the fiber. This feature also limits the ultimate life of adsorbent wheel, resulting in frequent wheel replacement.
- Filters are generally devices such as a membrane or a layer that is designed to block or contain objects or substances while letting others through. Filtration media are generally of three types - mechanical, biological and chemical. Chemical filters are preferred for removal of gaseous contaminants in a given environment since they provide air purification by both adsorbing and absorbing odours by adsorbents/impregnated adsorbents such as potassium permanganate by controlled oxidizing action.
- Gaseous contaminants either could be inorganic or organic.
- selection of adsorbents to adsorb gas or reactants for adsorbing gas/impregnates is very important for the chemical filter media. As discussed above, a single chemical filter media may not adequately control multiple contaminants or classes of AMC.
- One object of the present invention is to provide a desiccant based honeycomb chemical filter where the desiccant is generated in situ, and impregnated with oxidizing chemicals, acidic or alkaline chemicals, or reducing chemicals to remove/contain gaseous contaminants, where the loading percentage of the impregnants is significantly higher than thought possible in the art.
- the primary object of the present invention is to increase the capability of removing gaseous contaminants whether, acidic, alkaline, or organic and increase chemical filter life by the use of higher amounts of impregnants.
- a further object of this invention is to produce a desiccant based honeycomb matrix with or without active carbon or hydrophobic zeolite for impregnation with different impregnants/reactants to remove gaseous contaminants.
- Another object of the invention is to provide a desiccant based honeycomb matrix where pressure loss is minimized.
- the desiccant may or may not contain active carbon or hydrophobic zeolite and may or may not be impregnated with impregnants for enhanced removal of different contaminants.
- a further object of the invention is to provide a desiccant based honeycomb matrix chemical filter that provides an energy saving, and may be with or without active carbon or hydrophobic zeolite, and may be impregnated with different impregnants or un-impregnated, while also enabling enhanced odour control.
- the present invention provides a honeycomb matrix comprising a desiccant prepared in-situ, for use as a chemical filter, as described herein below.
- the present invention provides a desiccant based honeycomb chemical filter comprising a matrix formed of a substrate having a desiccant generated in situ or deposited thereon, said desiccant being selected from the group consisting of metal silicates, silica gel, molecular sieves, activated alumina, activated carbon or hydrophobic zeolite, and any mixture thereof, said substrate being further impregnated with one or more of an oxidizing agent, or an alkali metal hydroxide, or strong or weak acid(s), or reducing agents.
- the substrate comprises an inorganic substance or an organic substance or a mixture thereof.
- the substance is in the form of a fiber or a pulp.
- the inorganic fiber is selected from the group consisting of glass fiber, Kraft paper, ceramic paper and any combination thereof, and is preferably a glass fiber.
- the desiccant is selected from a metal silicate and silica gel or combination of metal silicate and activated carbon and/or a hydrophobic desiccant such as zeolites selected from HISIV and ZSM-5
- the metal silicate is selected from potassium silicate and sodium silicate, preferably where the silicate is a neutral grade sodium silicate.
- the ratio of Si0 2 to Na 2 0 is in the range of 1 :2.0 to 1 :4.0, preferably in the range of 1 :3.
- the impregnated material is selected from the group consisting of potassium permanganate, sodium permanganate, potassium hydroxide, sodium hydroxide, phosphoric acid and sodium thiosulphate.
- the loading of the impregnated material in the matrix is in the range of 4% to 40 %, preferably about 20%.
- the binder is preferably absent.
- the basic weight of the substrate is in the range of 50 to 150 gsm, preferably in the range of 80 to 120 gsm.
- the present invention also provides a method for manufacture of a desiccant based honeycomb chemical filter, comprising the steps of
- the method when used in a situation comprising in situ generation fo desiccant comprises the following steps
- a substrate material with a desiccant forming material or a desiccant selected from the group consisting of metal silicates, silica gel, molecular sieves (hydrophillic or hydrophobic), activated alumina, activated carbon, and any mixture thereof, wherein the desiccant forming material is in the form of a solution with a concentration in the range of 15 - 40 %; (ii) drying the treated material to reduce moisture content thereof to a range of 15-40%;
- step iii washing the gel matrix obtained in step iii to remove excess reactants and unwanted by-products;
- step (vii) drying the treated aerogel matrix of step (vi) above at a temperature in the range of 50 - 140°C to obtain said chemical filter.
- the present invention provides a solution for the problems in the art of ensuring maximum efficiency in adsorption of chemical contaminants using a honeycomb based chemical filter using a desiccant.
- Honeycomb matrixes can be formed from a variety of substrates such as plastic sheet, metal/aluminum foil, organic and/or inorganic fiber substrates which are "paper" like, and which may be quite porous.
- the deposition or loading of a desiccant material on the substrate is a function, generally, of the substrate of choice, the amount of desiccant that is to be deposited or loaded, and the temperature at which the air/matrix is intended for use.
- known techniques for deposition or loading the desiccant on the substrate to prepare the matrix are coating, impregnation and in situ synthesis.
- Coating and impregnation are chosen where the desiccant powder is produced in bulk and are intended for industrial applications other than HVAC air treatment.
- In situ synthesis is generally chosen in case of desiccant material such as silica gels and metal silicates.
- the desiccant is generated in situ, and impregnated with oxidizing chemicals, acidic or alkaline chemicals to remove/contain gaseous contaminants, and the loading percentage of impregnants is significantly higher than thought possible in the art.
- the desiccant based honeycomb matrix can be made with or without active carbon or hydrophobic zeolite, for impregnation with different impregnants/ reactants to remove gaseous contaminants. Another significant feature of the invention is that pressure loss is minimized in the desiccant based honeycomb matrix.
- the desiccant may or may not contain active carbon or hydrophobic zeolite and may or may not be impregnated with impregnants for enhanced removal of different contaminants.
- the desiccant based honeycomb matrix chemical filter of the invention also provides an energy saving, and may be with or without active carbon, and may be impregnated with different impregnants or un-impregnated, while also enabling enhanced odour control.
- air to be treated generally contains several gaseous contaminants, e.g. VOCs, odour, and the like. It is desirable to remove these through the desiccant matrix.
- gaseous contaminants e.g. VOCs, odour, and the like.
- gaseous contaminants are sometime water soluble and together are condensed in the macro porous desiccant mainly through capillary adsorption.
- the prior art contains some references to the use of microporous desiccants. However, these desiccants generally have limited capillary adsorption and therefore limited adsorption of gaseous contaminants.
- the prior art also shows a limited loading capability for both the desiccant and any impregnants due to the fact that generally the desiccant is coated or impregnated on the substrate.
- adsorption in these cases is a surface phenomena. This necessarily results in the use of less dense paper, typically in the range of 20 to 80 gsm thickness.
- the requirement of coating of the substrate is generally a limiting factor in the substrate choice, and it was considered unfeasible to increase the density of the substrate without compromising on the surface area required for adsorption.
- honeycomb matrix comprising a desiccant prepared in- situ, for use as a chemical filter, as described herein below.
- the invention is achieved by a macroporous or microporous desiccant based honeycomb matrix.
- the substrate is made from various inorganic or organic substances or combinations thereof.
- the substance can be a fiber or pulp.
- the inorganic fiber is selected from glass fibre, Kraft paper, ceramic paper, etc. and is preferably glass fiber.
- the desiccants that can be synthesized in situ preferably comprise metal silicate/ silica gel which provide a high adsorption capacity.
- the process comprises laminating water glass treated/ impregnated glass fiber in the shape of either a honeycomb or as a block.
- the matrix is treated with either water soluble salts (whether divalent or trivalent) or any acid (whether organic or inorganic) to convert the water glass silicate into the active desiccant material with a pore diameter in the range of 10 - 70 A 0 , a pore volume of 0.10-0.80gm/cc and surface area of 300-700 m 2 .
- the desiccant based honeycomb matrix is generally a flat and/or corrugated sheet of the fiber glass substrate where the active desiccant has been synthesized into the pores.
- the fiber glass substrate used in the present invention is a highly porous material having the fiber diameter of 4-15 micron, fiber length 6-10mm, thickness in the range of 0.10-0.75 mm.
- the binder content of the fiber glass substrate used in the process is not greater than 8% and the preferred binder used in making substrate is polyvinyl alcohol or combination with acrylic. It is advisable to use a low content of organic binder in the substrate so that the percentage of organic content in the desiccant based honeycomb matrix is also reduced.
- the need for adding an external binder is avoided where the water soluble silicate desiccant is generated in situ.
- the silicate material itself carries out the function of a desiccant once treated with suitable reactant/s.
- Water soluble silicates can be used for this purpose, .
- binders may also be used where the desiccant is coated on the matrix.
- the basic weight of the substrate used in the process is 50-150 gsm, preferably between 80 to 120 gsm.
- the fiber used in the making of such substrates can be of electrical grade fiber.
- the flat sheet that is to be corrugated is first passed through the desired concentration of water glass solution (from 15-40%, preferably 30%), with or without active carbon material or hydrophobic zeolite.
- the sheets are dried in a drying chamber, preferably using infra-red heating to ensure that the moisture content is in the desired range of 15-40%, preferably 20%.
- water soluble silicates such as potassium silicate can also be used, sodium silicate is preferable due to its cost efficiency, high solubility of its byproducts, higher bonding strength and easy availability.
- neutral grade water soluble silicate preferably sodium silicate to impregnate the fiber glass substrate. It is observed that the presence of high alkali content in alkaline grade as compared to neutral grade silicate necessitates use of a large quantity of reactants. Use of alkaline grade sodium silicate also results in a higher rate of gelation than neutral grade sodium silicate. The gelling rate adversely affects the characteristics of the desiccants.
- the process of in situ synthesis of the desiccant material on the substrate can be accomplished simultaneously with the deposition of active carbon and/or hydrophobic zeolite material such as HISIV or ZS 05.
- active carbon and/or hydrophobic zeolitic material enhances the level of odour removal and also provides a significant enhancement in structural strength of the substrate itself.
- Active carbon (and/or hydrophobic zeolitic material) in the form of powder is mixed with water soluble silicate or any suitable binder-inorganic or organic_prior to the formation of the desiccant in situ.
- the corrugated sheet is produced by passing the silicate (or silicate and active carbon or hydrophobic zeolite) impregnated flat sheet through a toothed roller. Moisture content of the silicate or silicate and active carbon or hydrophobic zeolite impregnated sheets, grade of water glass, corrugated rolls, the control of clearances on the adhesive rolls and the curing heat of the adhesive are important in making a single facer unit.
- the corrugated sheet and the flat sheet are pressed together using additional rolls of the same material that is used for corrugation. It is preferable to avoid the use of adhesive while making single facer, even with the same water glass used for impregnation, in order to avoid powdering or higher pressure drops after synthesis. This is achieved by keeping higher moisture content in the flat sheet.
- the single facer that is a combination of flat and corrugated sheets can be converted into either a block or a cylindrical shape.
- Neutral grade sodium silicate is preferably applied to ensure adhesion of the single facers sequentially prior to stacking or winding.
- Application of Si0 2 : Na 2 0 in the range of 1:2.0 To 1:4.0 preferably 1:3.0 before winding or stacking of the single facer gives additional strength to the honeycomb matrix.
- the honeycomb matrix that is produced is then dried to enhance the adhesion of the sheets. If the ratio of Si0 2 :Na 2 0 is ⁇ 2, the bonding strength is weaker and if ratio of Si0 2 : Na 2 0 is above 4.0 the adhesive strength is less.
- honeycomb matrix produced above either in block or cylindrical form is then soaked in water soluble metal salt/salts or strong or weak acid/acids- inorganic or organic in different proportions and other forms of solution to produce silicate hydrogel.
- the reaction between water glass silicates with metal salts to form insoluble metal silicate hydro gel is given in table below:
- the element is further dried under specified conditions to convert the hydrogel into the aerogel. It is observed that the type of silicate, types of salts its pH, concentration, temperature and time during which the gel is aged or otherwise treated, greatly affects the gel characteristics such as pore diameter, pore volume, surface area, adsorption capacity etc., The other important factors which affects gel characteristics are salt contents and surface tension of the liquid medium as it is being evaporated from the pores of the gel.
- the manufacture of the desiccant based honeycomb matrix chemical filter of the invention comprises laminating water glass treated/impregnated glass fiber substrate (with or without carbon or hydrophobic zeolite ) in the form/shape of cylinder or block, treating this element with one or more water soluble divalent trivalent salt(s) or organic or inorganic acid(s) - strong or weak, to convert the water glass into active material, and then impregnating the active material with different impregnants.
- the produced aerogel is immersed / impregnated with a solution of oxidizing agent(s), alkaline solution and weak acid solution or any reactants suitable for removing gaseous contaminants of different concentration at different temperature for different soak time.
- oxidizing agent(s) e.g., sodium bicarbonate
- alkaline solution e.g., sodium bicarbonate
- weak acid solution e.g., sodium bicarbonate
- Time required for full impregnation varies as a function of the structure of the adsorbent, temperature and other factors.
- the honeycomb material is then placed in an oven and heated till free moisture and water evaporate or are driven out of the mixture leaving impregnating material within the pores of honeycomb silicate aerogel material and/or silicate hydrogel and activated carbon or hydrophobic zeolite.
- the drying temperature of the impregnated honeycomb material is in the range of 50-140°C.
- the exposure time in the heating is varied with quality and quantity of materials, heating efficiency and other factors.
- impregnants used are potassium and sodium permanganate, sodium or potassium hydroxide, weak acids such as phosphoric acid, and a reducing agent such as sodium thiosulphate.
- the loading of impregnants depends on various factors such as types of desiccants, concentration of impregnants, soak time, temperature, number of dips, etc.
- Macroporous or microporous desiccant (with or without active carbon) material supported honeycomb matrix is impregnated with potassium/sodium permanganate solution in a range of 5 to 40%, preferably 15% concentration in case of potassium permanganate and 30% in case of sodium permanganate, at 10°C to 90°C, most preferably at 70°C for 5 to 60 minutes, most preferably for 15 minutes, to get the maximum impregnant loading without affecting the mechanical strength of the matrix and water/CTC adsorption capacity.
- Table 1 gives details of factors that affect percentage of loading of impregnant (KMn0 4 vs. NaMn0 4 ) and adsorption capacity of impregnated honeycomb desiccant based matrix.
- Macroporous or microporous desiccant (with or without active carbon and/or hydrophobic zeolitic material) material supported honeycomb matrix is impregnated with potassium hydroxide solution in the range of 2 to 15%, most preferably 6%, at 10°C to 50°C, most preferably at 30°C for 5 to 60 minutes, most preferably for 15 minutes to get the maximum impregnant loading without affecting the mechanical strength of the matrix and water/CTC adsorption capacity.
- Table 2 gives details of factors affecting the % of loading of impregnant (KOH) and adsorption capacity of impregnated honeycomb desiccant based matrix.
- Macroporous or microporous (with or without active carbon) material supported honeycomb matrix is impregnated with phosphoric acid solution in the range of 2 to 15%, most preferably 8%, at 10°C to 50°C, most preferably ai 30°C for 5 to 60 minutes, most preferably for 15 minutes to get the maximum impregnant loading without affecting mechanical strength of the matrix and water/CTC adsorption capacity.
- Table 3 gives details of factors affecting percentage loading of impregnant (Phosphoric acid) and adsorption capacity of impregnated honeycomb desiccant based matrix.
- Macroporous or microporous (with or without active carbon or hydrophobic zeolite) material supported honeycomb matrix is impregnated with sodium thiosulphate solution in the range of 5 to 45%, preferably 15 %, at 10°C to 50°C, most preferably at 30°C for 5 to 60 minutes, preferably for 15 minutes to get maximum impregnant loading without affecting the mechanical strength of the matrix and water/CTC adsorption capacity.
- Table 4 gives details of factors affecting % of loading of impregnant (Sodium thiosulphate) and adsorption capacity of impregnated honeycomb desiccant based matrix:
- the present invention provides several significant advantages over prior art methods. Some of these are summarized below.
- potassium permanganate can also be impregnated to a large loading percentage on microporous material. 2. There is an enhancement in the extent of loading due to several factors, some of which are given below:
- the GSM of the substrate is significantly higher than that used in the prior art.
- the GSM generally ranges from 50 to 150 gsm, preferably between 80 to 120 gsm. This enables higher desiccant loading on the substrate leading to a larger impregnate loading of the impregnate;
- Desiccant can be combined with active carbon or hydrophobic zeolite , preferably by mixing the carbon powder or a hydrophobic desiccant such as zeolitic material selected from HISIV or ZSM-05 with a suitable binder, preferably inorganic prior to formation of the desiccant in situ. This enables capture/encapsulation of the carbon particles within the desiccant. This enabies an enhancement in odour control, VOC adsorption, and in the structural strength of the matrix itself.
- zeolitic material selected from HISIV or ZSM-05
- the invention enables if required, a sacrifice of the surface area of the matrix to enable multiple fluid geometries, and allows lower pressure drops without any significant material sacrifice of the performance.
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IN178DE2012 | 2012-01-20 | ||
PCT/IB2013/000062 WO2013108117A1 (en) | 2012-01-20 | 2013-01-19 | Desiccant based honeycomb chemical filter and method of manufacture thereof |
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EP13706714.6A Withdrawn EP2804694A1 (de) | 2012-01-20 | 2013-01-19 | Chemischer filter mit trockenmittelwaben sowie herstellungsverfahren dafür |
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EP (1) | EP2804694A1 (de) |
KR (1) | KR20150003716A (de) |
CN (1) | CN104470632A (de) |
AU (2) | AU2013210811A1 (de) |
BR (1) | BR112014017899A8 (de) |
CA (1) | CA2865123A1 (de) |
MX (1) | MX2014008803A (de) |
WO (1) | WO2013108117A1 (de) |
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CN106999833A (zh) | 2014-10-06 | 2017-08-01 | 康宁股份有限公司 | 蜂窝体过滤器制品及其制造方法 |
CN104841369A (zh) * | 2015-05-15 | 2015-08-19 | 陈君武 | 一种蜂窝网活性炭过滤器空气滤芯及其制备方法 |
WO2017040283A1 (en) * | 2015-08-28 | 2017-03-09 | Serionix, Inc. | Gas filters for basic contaminants |
KR101938369B1 (ko) | 2015-12-09 | 2019-01-14 | 주식회사 엘지화학 | 산화금속-실리카 복합 에어로겔의 제조방법 및 이로부터 제조된 산화금속-실리카 복합 에어로겔 |
WO2017099488A1 (ko) * | 2015-12-09 | 2017-06-15 | 주식회사 엘지화학 | 산화금속-실리카 복합 에어로겔의 제조방법 및 이로부터 제조된 산화금속-실리카 복합 에어로겔 |
KR102002050B1 (ko) | 2015-12-15 | 2019-10-21 | 주식회사 엘지화학 | 산화금속-실리카 복합 에어로겔의 제조방법 및 이로부터 제조된 산화금속-실리카 복합 에어로겔 |
CN105597532B (zh) * | 2016-03-11 | 2018-01-23 | 浙江大学 | 一种用于隧道、停车场空间多污染气体的净化装置及其净化方法 |
CN105944663B (zh) * | 2016-07-11 | 2018-04-13 | 中国工程物理研究院材料研究所 | 用于气体深度脱水的分子筛整体式吸附剂的制备方法 |
CN106975272A (zh) * | 2017-04-20 | 2017-07-25 | 北海蓝晖环保科技有限公司 | 一种污水过滤材料 |
CN109704356B (zh) * | 2017-10-26 | 2021-05-11 | 中国石油化工股份有限公司 | Eu-1沸石分子筛的合成方法 |
JP7205866B2 (ja) * | 2018-08-28 | 2023-01-17 | 株式会社西部技研 | ハニカム吸着体及びそれを用いた除湿空調装置 |
CN112107992A (zh) * | 2019-06-21 | 2020-12-22 | 南京云香纳米技术有限公司 | 一种有害气体去除介质及其制备方法 |
CN111617749A (zh) * | 2020-07-02 | 2020-09-04 | 江苏博霖环保科技有限公司 | 一种蜂窝状分子筛吸附型材的制备方法 |
CN112619597B (zh) * | 2020-12-17 | 2023-05-05 | 北京泷涛环境科技有限公司 | 一种分子筛基玻璃纤维骨架吸附材料及其制备方法与应用 |
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JP2003103165A (ja) * | 2001-09-28 | 2003-04-08 | Nichias Corp | ケミカルフィルター及びその再生方法 |
SE529160C2 (sv) * | 2004-12-27 | 2007-05-15 | Svenska Aerogel Ab | En metod för framställning av agglomerat av utfällt silikamaterial, ett mikroporöst material innefattande sådana agglomerat och användning därav |
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2013
- 2013-01-19 AU AU2013210811A patent/AU2013210811A1/en not_active Abandoned
- 2013-01-19 KR KR20147023304A patent/KR20150003716A/ko not_active Application Discontinuation
- 2013-01-19 CN CN201380010260.0A patent/CN104470632A/zh active Pending
- 2013-01-19 EP EP13706714.6A patent/EP2804694A1/de not_active Withdrawn
- 2013-01-19 MX MX2014008803A patent/MX2014008803A/es unknown
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- 2013-01-19 BR BR112014017899A patent/BR112014017899A8/pt not_active Application Discontinuation
- 2013-01-19 WO PCT/IB2013/000062 patent/WO2013108117A1/en active Application Filing
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2017
- 2017-07-31 AU AU2017208389A patent/AU2017208389A1/en not_active Abandoned
Non-Patent Citations (1)
Title |
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ANONYMOUS: "Sodium silicate - Wikipedia", 12 November 2018 (2018-11-12), XP055530034, Retrieved from the Internet <URL:https://en.wikipedia.org/wiki/Sodium_silicate> [retrieved on 20181204] * |
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AU2017208389A1 (en) | 2017-08-17 |
KR20150003716A (ko) | 2015-01-09 |
AU2013210811A1 (en) | 2014-09-11 |
CN104470632A (zh) | 2015-03-25 |
BR112014017899A2 (de) | 2017-06-20 |
MX2014008803A (es) | 2015-08-05 |
WO2013108117A1 (en) | 2013-07-25 |
BR112014017899A8 (pt) | 2017-07-11 |
CA2865123A1 (en) | 2013-07-25 |
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