CN116966678A - Filter material containing organic amine adsorbent and preparation method thereof - Google Patents
Filter material containing organic amine adsorbent and preparation method thereof Download PDFInfo
- Publication number
- CN116966678A CN116966678A CN202310801485.3A CN202310801485A CN116966678A CN 116966678 A CN116966678 A CN 116966678A CN 202310801485 A CN202310801485 A CN 202310801485A CN 116966678 A CN116966678 A CN 116966678A
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- Prior art keywords
- organic amine
- polycarboxylic acid
- amine adsorbent
- molecular sieve
- adsorbent
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- 150000001412 amines Chemical class 0.000 title claims abstract description 91
- 239000003463 adsorbent Substances 0.000 title claims abstract description 77
- 239000000463 material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title 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 67
- 239000002808 molecular sieve Substances 0.000 claims abstract description 59
- 239000002253 acid Substances 0.000 claims abstract description 53
- 229910052751 metal Inorganic materials 0.000 claims abstract description 52
- 239000002184 metal Substances 0.000 claims abstract description 51
- 150000003839 salts Chemical class 0.000 claims abstract description 38
- 150000001868 cobalt Chemical class 0.000 claims abstract description 4
- 159000000003 magnesium salts Chemical class 0.000 claims abstract description 4
- 150000003751 zinc Chemical class 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims description 29
- 239000011248 coating agent Substances 0.000 claims description 28
- 239000000758 substrate Substances 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 239000011230 binding agent Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- 238000011068 loading method Methods 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 34
- 239000007789 gas Substances 0.000 abstract description 25
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 48
- 230000000052 comparative effect Effects 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920002125 Sokalan® Polymers 0.000 description 6
- 239000004584 polyacrylic acid Substances 0.000 description 6
- 239000004593 Epoxy Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 230000008859 change Effects 0.000 description 4
- 150000004696 coordination complex Chemical class 0.000 description 4
- 229920003986 novolac Polymers 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000002250 absorbent Substances 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910001510 metal chloride Inorganic materials 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 239000001110 calcium chloride Substances 0.000 description 2
- 229910001628 calcium chloride Inorganic materials 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical group [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004843 novolac epoxy resin Substances 0.000 description 2
- 235000012736 patent blue V Nutrition 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920001223 polyethylene glycol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- -1 aromatic epoxides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 229910052595 hematite Inorganic materials 0.000 description 1
- 239000011019 hematite Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001444 polymaleic acid Polymers 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
-
- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
-
- 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
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0471—Surface coating material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/10—Filtering material manufacturing
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/12—Special parameters characterising the filtering material
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a filter medium containing an organic amine adsorbent, a preparation method thereof and a filter medium, wherein the filter medium containing the organic amine adsorbent comprises an organic amine adsorbent and a base material, the organic amine adsorbent is loaded on the base material, and the organic amine adsorbent comprises the following components: molecular sieve, polycarboxylic acid and metal salt, wherein, in weight percent, each part of the base material is loaded with 1-10% of polycarboxylic acid and 1-10% of metal salt; the metal salt comprises at least one of a water-soluble magnesium salt, a water-soluble cupric salt, a water-soluble cobalt salt and a water-soluble zinc salt. According to the filter medium containing an organic amine adsorbent of the present invention, a certain amount of a polycarboxylic acid and a metal salt are supported on the filter medium. The metal salt coordinates with carboxyl, has high stability and is not easy to fall off, thereby improving the adsorption capacity to alkaline gases such as organic amine and the like and having stable adsorption performance.
Description
Technical Field
The invention relates to the field of air purification, in particular to a filter material containing an organic amine adsorbent and a preparation method thereof.
Background
Most of the lower organic amines have a bad smell, for example, trimethylamine has a fishy smell. Since lower organic amines are often present in refrigerators and the like, they tend to cause gas pollution of foods.
In the related art, adsorbents commonly used for gases having bad smell include activated carbon, silica gel, and the like. However, the adsorption effect of the adsorbent on organic amines such as trimethylamine is not preferable, particularly, adsorption effect of trimethylamine at a relatively low concentration.
Molecular sieves are used as a common gas adsorbent, and reports on adsorption of trimethylamine and other organic amine gases by the molecular sieves are rarely seen at home and abroad. Molecular sieves are microporous crystalline solids having a uniform pore structure. Typically, they contain elements such as silicon, aluminum, and oxygen in their frameworks. As a catalyst, molecular sieves exhibit distinct acid activity and shape selectivity characteristics, unlike amorphous catalysts of equivalent composition. Trimethylamine concentration in industrial waste gas is usually low, and molecular sieves are effective adsorbents for treating low concentration contaminants.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, an object of the present invention is to provide a filter medium containing an organic amine adsorbent, which has high adsorption efficiency for organic amine.
Another object of the present invention is to provide a method for preparing a filter material containing an organic amine adsorbent.
According to an embodiment of the first aspect of the present invention, a filter medium containing an organic amine adsorbent includes: an organic amine adsorbent and a substrate, the organic amine adsorbent being supported on the substrate, the organic amine adsorbent comprising: molecular sieve, polycarboxylic acid and metal salt, wherein, in weight percent, each part of the base material is loaded with 1-10% of polycarboxylic acid and 1-10% of metal salt; the metal salt comprises at least one of a water-soluble magnesium salt, a water-soluble cupric salt, a water-soluble cobalt salt and a water-soluble zinc salt.
According to the filter material containing the organic amine adsorbent of the embodiment of the present invention, a certain amount of polycarboxylic acid and metal salt are supported on a substrate. The metal salt coordinates with carboxyl, has high stability and is not easy to fall off, thereby improving the adsorption capacity to alkaline gases such as organic amine and the like and having stable performance.
According to some embodiments of the invention, 4% of the polycarboxylic acid is loaded per part of the substrate; and/or 4% of the metal salt per part of the filter media.
According to some embodiments of the invention, the molecular sieve comprises at least one of a 13X molecular sieve, a 4A molecular sieve, and a 5A molecular sieve.
According to some embodiments of the invention, the molecular sieve has a specific surface area S, wherein S satisfies: 50m 2 /g≤S≤1000m 2 /g; preferably, the S satisfies: 100m 2 /g≤S≤600m 2 /g。
According to some embodiments of the invention, the polycarboxylic acid has a molecular weight of M, wherein M satisfies: m is less than or equal to 20000.
According to some embodiments of the invention, the substrate has a honeycomb structure; preferably a ceramic honeycomb or an aluminum honeycomb.
According to some embodiments of the invention, further comprising: binder, dispersant and curing agent.
According to some embodiments of the invention, the weight ratio of the organic amine adsorbent, the binder and the curing agent satisfies: 100:1 to 12:1 to 6; and/or the solid-to-liquid ratio of the organic amine adsorbent and the dispersant satisfies: 1kg/500ml to 1kg/1000ml.
According to an embodiment of the second aspect of the present invention, there is provided a method for preparing a filter according to the embodiment of the first aspect, including the steps of:
1. dissolving the metal salt and the polycarboxylic acid in water to form an aqueous solution of a metal polycarboxylic acid;
2. adding the molecular sieve into an aqueous solution of the metal polycarboxylic acid to form a mixed solution;
3. and loading the mixed solution on the substrate to obtain a coating containing the organic amine adsorbent, and drying to form the coating containing the organic amine adsorbent.
According to some embodiments of the invention, the coating has a thickness d 1 Wherein said d 1 The method meets the following conditions: d is more than or equal to 0.04nm 1 ≤0.25nm。
Additional aspects and advantages of the invention will be set forth in part in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing and/or additional aspects and advantages of the invention will become apparent and may be better understood from the following description of embodiments taken in conjunction with the accompanying drawings in which:
FIG. 1 is an XRD pattern of a 13X molecular sieve according to an embodiment of the invention, wherein a is an XRD pattern of the 13X molecular sieve (13X molecular sieve as such), b is an XRD pattern of an organic amine adsorbent (13X after CO ion exchange) in a filter material according to an embodiment 2 of the invention, and c is an XRD pattern of the organic amine adsorbent in the filter material according to an embodiment 2 of the invention after trimethylamine is adsorbed;
FIG. 2 is a comparative schematic diagram showing the color change before and after the filter material of embodiment 1 of the present invention adsorbs trimethylamine, wherein a is the filter material before adsorbing trimethylamine and b is the filter material after adsorbing trimethylamine;
fig. 3 is a schematic view of a filter structure according to an embodiment of the present invention.
Detailed Description
According to an embodiment of the first aspect of the present invention, a filter medium containing an organic amine adsorbent includes: the polybasic carboxylic acid in the organic amine adsorbent can be one or more of polymaleic acid, acrylic acid-maleic acid copolymer, polyacrylic acid and the like. In addition, the molecular sieves of the present invention may be synthesized from natural zeolites. For example, natural zeolites can be processed using hydrothermal methods to prepare syntheses.
Wherein, the organic amine adsorbent is loaded on the base material, and each part of filter material is loaded with 1 to 10 percent of polycarboxylic acid and 1 to 10 percent of metal salt in percentage by weight. In the filter of the present invention, if the amount of the polycarboxylic acid supported is less than 1% of the filter, a sufficient amount of the organic amine basic gas cannot be adsorbed; if the loading of the polycarboxylic acid is more than 10% of the filter material, the molecular sieve channels are easily blocked. Through setting, each part of filter material is loaded with 1% -10% of polycarboxylic acid, which is beneficial to improving the capability of the organic amine adsorbent for adsorbing alkaline gases such as organic amine. In the organic amine adsorbent of the present invention, if the loading of the metal salt is less than 1% of the filter medium, the metal salt cannot be sufficiently matched with the polycarboxylic acid, and a sufficient amount of the organic amine basic gas cannot be adsorbed; if the loading of the metal salt is more than 10% of the filter material, the molecular sieve channels are easily blocked. By arranging the filter materials, each part of filter materials is loaded with 1-10% of metal salt, which is beneficial to further improving the capability of the organic amine adsorbent for adsorbing alkaline gases such as organic amine.
Wherein the metal salt comprises at least one of water-soluble magnesium salt, water-soluble cupric salt, water-soluble cobalt salt and water-soluble zinc salt. Thus, in the aqueous solution, the water-soluble metal salt can be more fully mixed with the polycarboxylic acid, the metal salt can be more fully coordinated with the carboxyl, the stability is higher, the gas adsorption capacity of the adsorbent is stronger, and the adsorbent is not easy to fall off. Thereby improving the ability of the organic amine adsorbent to adsorb gases.
According to the filter material containing the organic amine adsorbent in the embodiment of the invention, a certain amount of the organic amine adsorbent is loaded on a substrate, and the organic amine adsorbent comprises a molecular sieve, a polycarboxylic acid and a metal salt. The metal salt is coordinated with the carboxyl, is fixed by the molecular sieve, has high stability and is not easy to fall off, thereby improving the adsorption capacity of the filter material to alkaline gases such as organic amine and the like, and having stable adsorption performance.
According to some embodiments of the invention, each filter is loaded with 4% polycarboxylic acid. The polycarboxylic acid is more suitable in loading, and the adsorption capacity of the filter material to alkaline gases such as organic amine is higher.
According to some embodiments of the invention, each filter is loaded with 4% metal salt. The metal loading is more suitable, the coordination of the metal and the polycarboxylic acid is better, and the adsorption capacity of the adsorbent to alkaline gases such as organic amine is higher.
According to some embodiments of the invention, the molecular sieve comprises at least one of a 13X molecular sieve, a 4A molecular sieve, and a 5A molecular sieve. The 13X molecular sieve has low silicon-aluminum content, acidity, stable molecular property, better corrosion resistance and high temperature resistance, simple and easily obtained raw materials and low cost. The 13X molecular sieve can be synthesized from natural zeolite. The 13X molecular sieve according to the invention comprises SiO 2 And Al 2 O 3 ，SiO 2 With Al 2 O 3 The molar ratio of (2) to (3). The 13X molecular sieve also comprises 15 to 20 percent of Na by weight 2 O and minor amounts of impurities, e.g. impurities including anatase (TiO 2) Hematite (Fe) 2 O 3 ) Periclase (MgO), calcium oxide (CaO) and potassium oxide (K) 2 O)。
According to other embodiments of the present invention, the molecular sieve has a specific surface area S, wherein S satisfies: 50m 2 /g≤S≤1000m 2 And/g. Thus, the molecular sieve has large specific surface area and high load, so that the filter material has stronger adsorption performance.
According to other embodiments of the invention, S satisfies: 100m 2 /g≤S≤600m 2 And/g. The molecular sieve has more proper specific surface area and can load a large amount of organic amine adsorbent, thereby ensuring the adsorption performance of the filter material.
According to some embodiments of the invention, the polycarboxylic acid has a molecular weight of M, wherein M satisfies: m is less than or equal to 20000. If the molecular weight of the polycarboxylic acid is too large, the polycarboxylic acid covers the fine pores of the molecular sieve, which results in a decrease in the adsorption capacity of the organic amine adsorbent.
According to some embodiments of the invention, M satisfies: m is more than or equal to 1000 and less than or equal to 20000. Thus, the molecular weight of the polycarboxylic acid is more suitable, which is advantageous for improving the adsorption capacity of the filter material.
According to some embodiments of the invention, the weight ratio of polycarboxylic acid, metal salt and molecular sieve in the organic amine adsorbent is 4:4:5.
according to some embodiments of the invention, the substrate has a honeycomb structure. The arrangement has large specific surface area of the base material, and is convenient for the adhesion of metal and polycarboxylic acid. Alternatively, a substrate ceramic honeycomb or an aluminum honeycomb. The setting is light in base material, and convenient filter material wide use.
According to some embodiments of the invention, the coating further comprises a dispersant, a binder, and a curing agent, wherein the weight ratio of the organic amine adsorbent, the binder, and the curing agent is such that: 100:1 to 12:1 to 6. The organic amine adsorbent in the coating can be ensured to be uniformly dispersed, the thickness of the coating is uniformly distributed, the forming and solidification are easy, and the bonding force between the coating and the filter material is strong.
According to some embodiments of the invention, the solid-to-liquid ratio of the organic amine adsorbent and the dispersant satisfies: 1kg/500ml to 1kg/1000ml. By the arrangement, the organic amine adsorbent in the coating is further ensured to be uniformly dispersed, so that the adsorption performance of the filter material on gases such as organic amine is improved.
According to some embodiments of the invention, the dispersant comprises poly (ethylene glycol) methacrylate. In this way, the organic amine adsorbent in the coating is further ensured to be uniformly dispersed.
According to some embodiments of the invention, the adhesive is a phenol novolac epoxy series resin adhesive. Therefore, the adsorption performance of the filter material can be ensured, and the adhesive force between the coating and the base material can be ensured, so that the filter material is stable in structure. Wherein the phenolic novolac epoxy series resin binder may be selected from novolac epoxy resins, preferably the phenolic novolac epoxy series resin binder comprises at least one or applicable resins selected from bisphenol a, bisphenol F, novolac epoxy resins, non-aromatic epoxides, cycloaliphatic epoxides, glycidyl esters and epoxy functional acrylic acid.
According to an embodiment of the second aspect of the present invention, there is provided a method for producing a filter material containing an organic amine adsorbent, comprising the steps of:
1. dissolving a metal salt and a polycarboxylic acid in water to form an aqueous solution of a metal polycarboxylic acid;
2. adding a molecular sieve into an aqueous solution of a metal polycarboxylic acid to form a mixed solution;
3. and loading the mixed solution on the substrate to obtain a coating containing the organic amine adsorbent, and drying to form the coating containing the organic amine adsorbent.
According to the preparation method of the specific embodiment of the invention, the metal salt and the polycarboxylic acid are dissolved in water to form an aqueous solution of the metal polycarboxylic acid, so that the complex reaction of the metal salt and the polycarboxylic acid is promoted, and the metal complex of the polycarboxylic acid is formed. The molecular sieve is added into the aqueous solution of the complex, which is favorable for the adsorption of the metal complex of the polycarboxylic acid on the molecular sieve, and the organic amine adsorbent can be formed after the drying treatment.
According to some embodiments of the invention, the concentration of metal in the aqueous solution of the metal polycarboxylic acid is 2% to 6%, preferably 4%. The concentration of the metal in the aqueous solution of the metal polycarboxylic acid is proper, so that the metal complex is formed quickly and attached on the molecular sieve.
According to some embodiments of the invention, the concentration of the polycarboxylic acid in the aqueous solution of the metal polycarboxylic acid is 2% to 6%, preferably 4%. The concentration of the polycarboxylic acid in the aqueous solution of the metal polycarboxylic acid is proper, so that the metal complex is formed and attached on the molecular sieve quickly.
According to some embodiments of the invention, the coating has a thickness d 1 Wherein d 1 The method meets the following conditions: d is more than or equal to 0.04nm 1 Less than or equal to 0.25nm. If d 1 If the thickness of the coating is less than 0.04nm, the adsorption amount of the organic amine adsorbent in the filter material is low, and the adsorption performance of the filter material on gases such as organic amine can be affected. If d 1 If the thickness of the coating is larger than 0.25nm, the filter material is difficult to process, and the mass production process can be influenced by the arrangement, so that d 1 The method meets the following conditions: d is more than or equal to 0.04nm 1 The particle size of the filter material is less than or equal to 0.25nm, so that the filter material has good adsorption performance on gases such as organic amine and the like and high filtration efficiency.
Detailed description of the preferred embodiments
Examples 1 to 5
A filter material containing organic amine adsorbent, organic amine adsorbent and base material, wherein the organic amine adsorbent comprises molecular sieve, polycarboxylic acid and metal salt, and the specific surface of the molecular sieve is 500m 2 The molecular weight of the polycarboxylic acid is 20000.
The preparation method comprises the following steps: wherein 5g of a series of 1000-mesh molecular sieves are selected and respectively put into 100mL of metal polycarboxylic acid solution of 4% metal salt and 4% polycarboxylic acid, and a stirrer is started at normal temperature to stir and soak for 12h, so as to obtain emulsion. The emulsion (i.e., the organic amine adsorbent) was then coated on a substrate having a weight of 100g, and finally dried at 110℃by an oven to obtain the organic amine adsorbent-containing filter materials of examples 1 to 5 according to the present invention, and the organic amine adsorbent-containing filter materials of comparative examples 1 to 5 (as shown in Table 1).
2. Test method
And (3) carrying out an adsorption test on the filter material containing the organic amine adsorbent, placing the adsorbent in the middle of an experimental cabin, and setting the concentration of trimethylamine to be 150ppm. The penetration time (min), the saturation time (min) and the penetration adsorption quantity (mg.g) of the organic amine adsorbent are respectively tested -1 ) And saturated adsorption amount (mg.g) -1 ). The test results are shown in Table 1.
TABLE 1 adsorption performance test results of different organic amine adsorbents
The organic amine absorbent of the embodiment of the present invention has a better ability to adsorb trimethylamine as shown by the combination of the filter materials containing the organic amine absorbent of examples 1 to 5 and the filter materials containing the organic amine absorbent of comparative examples 1 to 5, and the results of the performance test thereof. Comparative examples 1-5 and comparative example 3 demonstrate that polyacrylic acid modified molecular sieves alone do not increase the ability of an organic amine adsorbent to adsorb trimethylamine. As can be seen from comparative examples 1 and 2, the molecular sieve modified by copper chloride alone has a certain improvement of the adsorption capacity for organic amine. As is clear from comparative examples 1 and 5, the ability of calcium chloride + polyacrylic acid modified molecular sieves to adsorb trimethylamine is lower than that of unmodified molecular sieves, indicating that polyacrylic acid damages the internal structure of molecular sieve channels, resulting in partial collapse of the channels, and thus the ability of calcium chloride + polyacrylic acid modified molecular sieves to adsorb trimethylamine is significantly reduced. From the above, the organic amine adsorbent according to the embodiment of the invention has the effect of improving the adsorption performance of the molecular sieve to trimethylamine by the combined action of the transition metal and the polyacrylic acid. Further, it can be proved that the 13X molecular sieve modified by copper chloride or magnesium chloride may form a certain complex between carboxylic acid groups and transition metal ions, so that the internal structure of the molecular sieve pore canal is not damaged, but the adsorption performance of trimethylamine is improved.
As shown in fig. 1, to further verify the characterization of the modified metal chloride, the metal chloride modified 13X molecular sieve of the present invention (i.e., the organic amine adsorbent of the filter of example 2 of the present invention) was scanned using an X-ray powder diffractometer to obtain an XRD pattern as shown in fig. 1. As can be seen from fig. 1, the organic amine adsorbent of the filter material of example 2 of the present invention has no significant change in diffraction peaks before and after adsorption of trimethylamine, indicating that the structure of the organic amine adsorbent of example 2 of the present invention remains substantially stable before and after adsorption of trimethylamine gas. The diffraction peaks of the organic amine adsorbent formed by the unmodified 13X molecular sieve and the 13X molecular sieve of the invention slightly change, which shows that the modified molecular sieve has a small amount of metal elements. As can be seen from fig. 1, the molecular sieve was modified with cobalt chloride to form a cobalt chloride complex.
In addition, as can be seen by comparing the colors of the two filters of FIG. 2, an important aspect of the adsorption reaction on the surface of the modified molecular sieve is that its complex with the metal chloride is deposited on the solid surface. This chemical change can even be observed with the naked eye during the adsorption process. For example, cuCl 2 The modified molecular sieve is sky blue when trimethylamine is not adsorbed, as shown in figure 2 a, along with CuCl 2 The amount of trimethylamine adsorbed by the modified molecular sieve is increased, and the molecular sieve can be gradually changed into deep blue or blue-violet from sky blue.
Examples 6 to 11
1. A filter media was prepared, 1kg of the organic amine adsorbent of example 2 of the present invention and 1L of a poly (ethylene glycol) methacrylate solvent were placed in a vessel and dispersed at 7000rpm using a high-speed emulsifying machine for 3 hours to obtain a dispersion. 75g of a phenol novolac epoxy series binder resin was added to the dispersion solution and redispersed for 40 minutes. 40g of a curing agent based on a cycloaliphatic anhydride was added to the dispersion solution and stirred for 10 minutes to prepare a coating solution. The aluminum honeycomb surface was coated under different conditions by adjusting the viscosity of the coating liquid and the content of the binder resin to obtain the filter materials of examples 6 to 11 according to the present invention, the content of which is shown in table 2 below.
TABLE 2 composition of filter materials of EXAMPLE 6-EXAMPLE 11
2. Preparing a coating: the coating liquid prepared as above was coated on the surface of the aluminum honeycomb using an immersion method. After fixing the dried aluminum honeycomb on a dip coater, the aluminum honeycomb is vertically supported in a coating liquid and lifted for coating. After drying the solvent at room temperature, the coated aluminum honeycomb sample was heat treated in an oven at 120 ℃ for 2 hours and at 180 ℃ for 8 hours to complete the coating. The coating thickness of each coating sample is shown in table 3 below.
3. Testing the adsorption performance of the filter material: the filter media of examples 6 to 11 above were tested for trimethylamine gas removal rate in 30min in a 30L acrylic bin, wherein the honeycomb module size was (120 mm. Times.120 mm. Times.50 mm), gas concentration was measured with a gas detection tube, and gas removal rate after a specified time was calculated from the initial concentration and the final concentration. As can be seen from Table 3 below, the amine-loaded porous resin has a good effect of removing aldehyde gas components.
TABLE 3 removal of trimethylamine from various coatings and their removal rates in examples 6-11
| No. | Coating thickness (mm) | Trimethylamine removal rate (%) |
| Example 6 | 0.237 | 93 |
| Example 7 | 0.238 | 94 |
| Example 8 | 0.236 | 93 |
| Example 9 | 0.239 | 93 |
| Example 10 | 0.234 | 92 |
| Example 11 | 0.235 | 91 |
| Example 6 | 0.128 | 72 |
| Example 6 | 0.078 | 57 |
| Example 6 | 0.081 | 61 |
| Example 6 | 0.076 | 52 |
| Example 6 | 0.043 | 40 |
The filter material and the trimethylamine removal rate thereof according to the examples are combined, and it is known that the composition and thickness of the coating layer affect the filtration efficiency of the filter material.
In the description of the present specification, it should be understood that the directions or positional relationships indicated by the terms "upper", "lower", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the invention. The meaning of "plurality" is two or more. The description of "one embodiment," "some embodiments," "an exemplary embodiment," "an example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A filter medium containing an organic amine adsorbent, comprising: an organic amine adsorbent and a substrate, the organic amine adsorbent being supported on the substrate,
the organic amine adsorbent comprises: molecular sieves, polycarboxylic acids and metal salts,
wherein, each part of the base material is loaded with 1 to 10 percent of the polycarboxylic acid and 1 to 10 percent of the metal salt by weight percent;
the metal salt comprises at least one of a water-soluble magnesium salt, a water-soluble cupric salt, a water-soluble cobalt salt and a water-soluble zinc salt.
2. The filter according to claim 1, wherein 4% of the polycarboxylic acid is supported per part of the base material; and/or
Each of the substrates supported 4% of the metal salt.
3. The filter of claim 1, wherein the molecular sieve comprises at least one of a 13X molecular sieve, a 4A molecular sieve, and a 5A molecular sieve.
4. The filter according to claim 1, wherein the molecular sieve has a specific surface area S, wherein S satisfies: 50m 2 /g≤S≤1000m 2 /g; preferably, the S satisfies: 100m 2 /g≤S≤600m 2 /g。
5. The filter according to claim 1, wherein the polycarboxylic acid has a molecular weight of M, wherein M satisfies: m is less than or equal to 20000.
6. The filter according to claim 1, wherein the base material has a honeycomb structure; preferably a ceramic honeycomb or an aluminum honeycomb.
7. The filter according to any one of claims 1 to 6, further comprising: binder, dispersant and curing agent.
8. The filter according to claim 7, wherein the weight ratio of the organic amine adsorbent, the binder, and the curing agent satisfies: 100:1 to 12:1 to 6; and/or
The solid-to-liquid ratio of the organic amine adsorbent and the dispersant satisfies: 1kg/500ml to 1kg/1000ml.
9. A method for producing the filter material according to any one of claims 1 to 8, comprising the steps of:
1. dissolving the metal salt and the polycarboxylic acid in water to form an aqueous solution of a metal polycarboxylic acid;
2. adding the molecular sieve into an aqueous solution of the metal polycarboxylic acid to form a mixed solution;
3. and loading the mixed solution on the substrate to obtain a coating containing the organic amine adsorbent, and drying to form the coating containing the organic amine adsorbent.
10. The method of claim 9, wherein the coating has a thickness d 1 Wherein said d 1 The method meets the following conditions: d is more than or equal to 0.04nm 1 ≤0.25nm。
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