CN115521499B - Organic porous material and preparation method and application thereof - Google Patents
Organic porous material and preparation method and application thereof Download PDFInfo
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- CN115521499B CN115521499B CN202110705513.2A CN202110705513A CN115521499B CN 115521499 B CN115521499 B CN 115521499B CN 202110705513 A CN202110705513 A CN 202110705513A CN 115521499 B CN115521499 B CN 115521499B
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- 239000011148 porous material Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 90
- 238000000034 method Methods 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 25
- 239000003571 electronic cigarette Substances 0.000 claims abstract description 23
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 67
- 238000010438 heat treatment Methods 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 36
- 229920000742 Cotton Polymers 0.000 claims description 30
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 27
- 239000006260 foam Substances 0.000 claims description 23
- 238000006243 chemical reaction Methods 0.000 claims description 21
- 238000002156 mixing Methods 0.000 claims description 16
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical class O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical group Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 239000003607 modifier Substances 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 13
- 238000005187 foaming Methods 0.000 claims description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 230000006835 compression Effects 0.000 claims description 12
- 238000007906 compression Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 230000002378 acidificating effect Effects 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical group CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 8
- 239000003377 acid catalyst Substances 0.000 claims description 8
- 239000004088 foaming agent Substances 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 239000004094 surface-active agent Substances 0.000 claims description 8
- 238000000748 compression moulding Methods 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 5
- 150000005846 sugar alcohols Polymers 0.000 claims description 5
- 239000011162 core material Substances 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 3
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- 238000004880 explosion Methods 0.000 abstract description 2
- 238000005086 pumping Methods 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 67
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 12
- 241000208125 Nicotiana Species 0.000 description 11
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 8
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 8
- 238000003860 storage Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 238000010521 absorption reaction Methods 0.000 description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 229920001223 polyethylene glycol Polymers 0.000 description 5
- 238000000889 atomisation Methods 0.000 description 4
- FJKROLUGYXJWQN-UHFFFAOYSA-N papa-hydroxy-benzoic acid Natural products OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 4
- 229960004889 salicylic acid Drugs 0.000 description 4
- 239000004640 Melamine resin Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- -1 maleic acid glycoside Chemical class 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 235000019504 cigarettes Nutrition 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 239000011976 maleic acid Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000006408 oxalic acid Nutrition 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical group 0.000 description 2
- 229920000909 polytetrahydrofuran Polymers 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000008098 formaldehyde solution Substances 0.000 description 1
- 150000002433 hydrophilic molecules Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24F—SMOKERS' REQUISITES; MATCH BOXES; SIMULATED SMOKING DEVICES
- A24F40/00—Electrically operated smoking devices; Component parts thereof; Manufacture thereof; Maintenance or testing thereof; Charging means specially adapted therefor
- A24F40/70—Manufacture
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/40—Chemically modified polycondensates
- C08G12/42—Chemically modified polycondensates by etherifying
- C08G12/424—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds
- C08G12/425—Chemically modified polycondensates by etherifying of polycondensates based on heterocyclic compounds based on triazines
- C08G12/427—Melamine
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08J2361/32—Modified amine-aldehyde condensateS
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention relates to the technical field of electronic cigarette oil guide materials, in particular to an organic porous material and a preparation method and application thereof. The apparent density rho of the organic porous material provided by the invention is 10kg/m 3 ‑500kg/m 3 The porosity P is 50% -99%; the organic porous material is formed by melamine formaldehyde resin modified by hydrophilic groups. The organic porous material provided by the invention effectively realizes quick oil guide, and under the premise of ensuring enough capillary action, the electronic cigarette oil can not freely leak out, and can effectively lock and control the oil, thereby preventing the occurrence of free electronic cigarette oil and avoiding the phenomena of oil leakage and oil explosion in the pumping process.
Description
Technical Field
The invention relates to the technical field of electronic cigarette oil guide materials, in particular to an organic porous material and a preparation method and application thereof.
Background
In most electronic cigarette atomizers, a porous medium is needed to connect the tobacco tar with the electronic heating element, and the porous medium is often a material rich in pore structure and high in porosity, such as porous ceramics, synthetic fibers, and the like. However, the above materials find that the fiber oil guiding material has the problems of difficult molding and poor assembly consistency in application, and the porous ceramic has difficulty in achieving high porosity (such as more than 90%). Therefore, it is urgently needed to find an electronic cigarette oil-guiding cotton material which has the advantages of regular structure, easy molding and high porosity.
Melamine foam (melamine formaldehyde resin foam) is produced by a foaming process of melamine resin, and melamine resin is produced by polycondensation of melamine and formaldehyde. Melamine foam has a rich three-dimensional network structure, extremely high porosity and stable chemical structure, and is widely applied to the fields of heat preservation, heat insulation, sound absorption, shock absorption, cleaning protection and the like. In the application research, the melamine foam has the above excellent properties which can be applied to the oil guiding structural unit in the electronic cigarette atomizer.
However, if the existing melamine foam is directly used as the oil-guiding cotton material of the electronic cigarette, the following defects exist:
1) The capillary action formed by the existing melamine foam can not effectively balance the influence of the gravity of tobacco tar, so that the material has poor oil control capability when being used as an oil guide cotton lock, and serious liquid leakage phenomenon occurs;
2) The prior melamine foam is used as an oil guiding cotton material, so that the oil guiding device cannot keep good consistency in the assembly process, the oil guiding cotton cannot be effectively attached to a heating element, and the atomizer is easy to dry burn or generate serious oil frying phenomenon in the suction process.
Disclosure of Invention
The invention aims to overcome the defects that the existing melamine foam is used as an oil guiding cotton material, the formed capillary action of the melamine foam cannot effectively balance the influence of smoke oil gravity, so that the oil guiding cotton material has poor oil locking and controlling capability and even can generate liquid leakage, the oil guiding cotton cannot maintain good consistency in the assembly process, and the oil guiding cotton cannot be effectively attached to a heating element, so that an atomizer is easy to dry burn or seriously explode oil in the suction process, and further provides an organic porous material and a preparation method and application thereof.
In order to achieve the above purpose, the invention adopts the following technical scheme:
an organic porous material with apparent density rho of 10kg/m 3 -500kg/m 3 The porosity P is 50% -99%; the organic porous material is formed by melamine formaldehyde resin modified by hydrophilic groups. Alternatively, the organic porous material may have an apparent density ρ of 10kg/m 3 、16kg/m 3 、20kg/m 3 、39kg/m 3 、40kg/m 3 、50kg/m 3 、100kg/m 3 、150kg/m 3 、155kg/m 3 、200kg/m 3 、250kg/m 3 、300kg/m 3 、350kg/m 3 、380kg/m 3 、400kg/m 3 、450kg/m 3 、500kg/m 3 The porosity P may be 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 96%, 98%, 99%.
Preferably, the hydrophilic group is at least one of a hydroxyl group and a carbonyl group. Preferably, the hydroxyl groups are modified with polyols including, but not limited to, glycerol, polyethylene glycol, polyvinyl alcohol, and polytetrahydrofuran, preferably, the polyols are selected from one or more of glycerol, polyethylene glycol; the carbonyl group is obtained by modification with a polycarboxylic acid including, but not limited to, one or more of salicylic acid, maleic acid glycoside, oxalic acid or citric acid, preferably the polycarboxylic acid is selected from salicylic acid and citric acid.
The hydroxyl modified melamine formaldehyde resin has the structure shown below:
wherein m, p and k are the same or different and are each independently selected from integers of 1-100. Alternatively, m, p, k are each independently selected from 1, 3, 7, 10, 20, 30, 50, 70, 80, 100.
Preferably, the preparation method of the melamine formaldehyde resin modified by hydrophilic groups comprises the following steps:
1) Mixing formaldehyde aqueous solution with melamine, and heating and reacting under alkaline condition to obtain prepolymer solution;
2) Adding a hydrophilic modifier into the prepolymer solution obtained in the step 1), and heating and reacting under an acidic condition to obtain the melamine formaldehyde resin modified by hydrophilic groups.
Preferably, in the step 1), the mass fraction of the formaldehyde aqueous solution is 30-40%; the mole ratio of formaldehyde to melamine is (3-5) 1; preferably, the molar ratio of formaldehyde to melamine is 3:1, said formaldehyde being formaldehyde in aqueous formaldehyde solution.
In the step 2), the hydrophilic modifier is at least one selected from polyalcohol and polycarboxylic acid, and the molar ratio of the hydrophilic modifier to melamine is (1-5): 1. Alternatively, the molar ratio of hydrophilic modifier to melamine is 1:1, 2:1, 3:1, 4:1, 5:1. The polyhydric alcohol includes, but is not limited to, glycerol, polyethylene glycol, polyvinyl alcohol and polytetrahydrofuran, the polycarboxylic acid includes, but is not limited to, one or more of salicylic acid, maleic acid glycoside, oxalic acid or citric acid, preferably the polycarboxylic acid is selected from salicylic acid and citric acid. The melamine resin prepared by controlling the raw material adding proportion has stable molecular structure, high water absorption, high safety and proper strength, and ensures the assembly consistency.
Preferably, the method comprises the steps of,
in the step 1), the pH value under the alkaline condition is 8.0-9.0, the heating reaction temperature is 75-85 ℃, and the heating reaction time is 0.5-3h; the alkaline conditions are adjusted by adding a base to the mixed solution of aqueous formaldehyde and melamine, including but not limited to sodium hydroxide, sodium carbonate.
In the step 2), the pH value of the acidic condition is 3.0-5.0, the heating reaction temperature is 70-85 ℃, and the heating reaction time is 1-5h. The acidic conditions are established by adding acids to the solution, including but not limited to hydrochloric acid, sulfuric acid, phosphoric acid.
Preferably, the organic porous material is 130kg/m 3 ≤ρ≤500kg/m 3 ，50％≤P≤98％。
The organic porous material can be used as an oil guide material of an oil guide device in an atomization device, such as an oil guide cotton for electronic cigarettes.
The invention also provides a preparation method of the organic porous material, which comprises the following steps:
1) Hydrophilic modification of melamine formaldehyde resin;
2) Foaming, compression molding to obtain the organic porous material.
Preferably, the hydrophilic modification comprises the steps of:
1) Mixing formaldehyde aqueous solution with melamine, and heating and reacting under alkaline condition to obtain prepolymer solution;
2) Adding a hydrophilic modifier into the prepolymer solution obtained in the step 1), and heating and reacting under an acidic condition to obtain the melamine formaldehyde resin modified by hydrophilic groups.
Preferably, the method comprises the steps of,
in the step 1), the mass fraction of the formaldehyde aqueous solution is 30-40%; the mole ratio of formaldehyde to melamine is (3-5) 1;
in the step 2), the hydrophilic modifier is at least one selected from polyalcohol and polycarboxylic acid, and the molar ratio of the hydrophilic modifier to melamine is (1-5): 1.
Preferably, the method comprises the steps of,
in the step 1), the pH value under the alkaline condition is 8.0-9.0, the heating reaction temperature is 75-85 ℃, and the heating reaction time is 0.5-3h;
in the step 2), the pH value of the acidic condition is 3.0-5.0, the heating reaction temperature is 70-85 ℃, and the heating reaction time is 1-5h.
The present invention is not particularly limited to a foaming method, and may be a conventional foaming process, preferably, the foaming method includes the steps of:
mixing the melamine formaldehyde resin solution modified by hydrophilic groups, an acid catalyst, a foaming agent and a surfactant, and heating to react after mixing to obtain the melamine formaldehyde resin foam.
Preferably, the hydrophilic group modified melamine formaldehyde resin solution is prepared by mixing hydrophilic group modified melamine formaldehyde resin and a solvent, and the solid content of the hydrophilic group modified melamine formaldehyde resin solution is 30-50%.
Preferably, the mass ratio of the hydrophilic group modified melamine formaldehyde resin solution to the acid catalyst to the foaming agent to the surfactant is 100 (1-5): 1-10): 1-5;
the foaming heating temperature is 150-250 ℃ and the heating time is 10-200min.
The solvent, acid catalyst, foaming agent and surfactant may be conventional solvents, acid catalyst, foaming agent and surfactant used in the foaming process in the art, for example, the solvent is methanol, the acid catalyst is hydrochloric acid or phosphoric acid, the foaming agent is n-pentane, and the surfactant is silicone oil or tween 80.
In the foaming method, the reaction mixture is dried after the reaction is finished, the drying temperature is 110-140 ℃, and the drying time is 8-15h. Alternatively, the drying step may be performed in an oven.
The compression molding method may be a compression molding method commonly used in the art, including but not limited to a normal temperature compression molding method and a hot press molding method. Preferably, the compression molding method is a hot press molding method.
Preferably, the melamine formaldehyde resin foam obtained through foaming treatment is subjected to hot press molding to obtain the organic porous material, wherein the hot press temperature is 150-300 ℃, the hot press pressure is 100kPa-2.5MPa, the pressure maintaining time is 0.5-120min, and the compression ratio is (2-50): 1. In particular embodiments the hot pressing temperature may be 160 ℃, 180 ℃, 200 ℃, 220 ℃, 250 ℃, 280 ℃; the hot pressing pressure can be 100kPa, 200kPa, 500kPa, 800kPa, 1MPa, 2MPa, and the dwell time can be 0.5min, 1min, 5min, 10min, 30min, 50min, 80min, 100min, 120min; the compression ratio may be 1:1, 2:1, 5:1, 10:1, 15:1, 20:1, 25:1, 30:1, 40:1, 50:1. The compression ratio refers to the volume ratio of melamine formaldehyde resin foam before hot pressing to after hot pressing.
The invention also provides a liquid guide element, wherein the liquid guide element material is the organic porous material or the organic porous material prepared by the preparation method. The application forms of the organic porous material used as the oil-guiding cotton comprise an oil-guiding cotton sheet, a stamping ring oil-guiding sheet, a cylindrical oil-guiding device, a foam oil-guiding cotton core for a cotton core heating body and the like. The liquid guide element can process the oil guide cotton base material into oil guide devices in different application occasions by adopting methods such as mechanical cutting, hot pressing treatment, cold die stamping, numerical control machine tool machining and the like. According to the invention, the porous material is used for preparing the oil guide device, the oil guide rate of the oil guide device exceeds that of most fiber cotton, and the crosslinked three-dimensional net structure can lock more tobacco tar, so that the tobacco tar is more efficient and convenient to transport, and a material guarantee is provided for preventing dry burning and supporting larger smoke quantity.
The invention also provides a heating body, wherein the main body material of the heating body or the cotton core material in the heating body is the organic porous material or the organic porous material prepared by the preparation method. The porous material used in the invention is used as the oil-guiding cotton, has uniform and compact foam holes, stable structure, certain mechanical strength and good processing consistency, and is an ideal material for oil absorption and supply of the heating element.
The invention also provides an atomization device, which is provided with the liquid guide element and/or the heating element.
The invention also provides an application of the organic porous material or the organic porous material prepared by the preparation method in an atomization device.
Optionally, the atomization device is an electronic cigarette.
The invention has the beneficial effects that:
1) The apparent density rho of the organic porous material provided by the invention is 10kg/m 3 -500kg/m 3 The porosity P is 50% -99%; the organic porous material is formed by melamine formaldehyde resin modified by hydrophilic groups.
The porous material formed by the melamine formaldehyde resin modified by hydrophilic groups is used as the oil-guiding cotton material for the electronic cigarettes for the first time, the porous material formed by the melamine formaldehyde resin modified by hydrophilic groups has better hydrophilicity, basically does not fall off powder, has no suction pathogenic hidden danger, has better processability and safety, has uniform and compact foam holes in a three-dimensional reticular porous structure, has stable structure, has proper compressive strength and regular appearance structure, effectively ensures the processing consistency of the material, and avoids the phenomenon that the atomizer is easy to dry burn or seriously explode oil in the suction process because the oil-guiding cotton and a heating element cannot be effectively attached. Meanwhile, the apparent density and the porosity of the organic porous material are controlled, the hydrophilicity, the apparent density and the porosity of the porous material are matched with each other, so that quick oil guiding is effectively realized, the electronic cigarette oil can not freely leak out on the premise of ensuring enough capillary action, and the oil can be effectively locked and controlled, so that the free electronic cigarette oil is prevented, the phenomena of oil leakage and oil explosion in the sucking process are avoided, and meanwhile, the porous material has larger oil absorption, supplies more oil to a heating body, can effectively reduce the dry burning risk and reduce the sucking scorching smell.
The porous material formed by melamine formaldehyde resin modified by hydrophilic groups is used as the oil-guiding cotton for the electronic cigarettes, and the apparent density and the porosity of the porous material are controlled, so that the porous material can be quickly infiltrated and adsorbed to various electronic cigarette oils (especially cigarette oils with main components of propylene glycol and glycerol), can resist long-term soaking of the cigarette oils, is safe and reliable, and is an ideal electronic cigarette oil transmission medium.
2) The organic porous material provided by the invention further comprises at least one of hydroxyl and carbonyl. The melamine formaldehyde resin modified by hydrophilic groups has more active groups such as-O-, -CO-and the like in the molecular structure, the structure ensures that the polymer molecules have better flexibility and more hydrophilic molecules, further the hydrophilicity of the porous material can be further improved, the porous material is not easy to fall off powder and is not fragile, the processability and the safety are better, the melamine formaldehyde resin is subjected to hydrophilic modification by adopting hydroxyl and carbonyl groups, and the porous material is matched with specific apparent density and porosity at the same time, so that the obtained porous material is used as the oil guiding cotton for electronic cigarettes, the oil storage capacity and the oil guiding rate of the oil guiding cotton material can be effectively improved, and the effect of effectively locking oil and controlling oil while rapidly guiding oil is realized.
3) The organic porous material provided by the invention further has the structure shown in the formula I, and the porous material is used as the oil-guiding cotton for the electronic cigarette by matching the specific structure with the specific apparent density and the specific porosity, so that the oil storage capacity and the oil-guiding rate of the oil-guiding cotton material can be further improved, and the oil locking and oil controlling can be ensured while the oil is rapidly guided.
4) The preparation method of the melamine formaldehyde resin modified by hydrophilic groups comprises the following steps: mixing formaldehyde aqueous solution with melamine, and heating and reacting under alkaline condition to obtain prepolymer solution; adding a hydrophilic modifier into the prepolymer solution obtained in the step 1), and heating and reacting under an acidic condition to obtain the melamine formaldehyde resin modified by hydrophilic groups. According to the melamine formaldehyde resin modified by the hydrophilic groups, which is prepared by the preparation method, the porous material formed by the melamine formaldehyde resin is matched with specific apparent density and porosity, and the obtained porous material is used as the oil-guiding cotton for electronic cigarettes, so that the oil storage capacity and the oil-guiding rate of the oil-guiding cotton material can be effectively improved, and the oil locking and oil controlling can be ensured while the oil is quickly guided.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of the organic porous material prepared in step 3) of example 6;
FIG. 2 is a scanning electron microscope image of the melamine formaldehyde resin foam prepared in step 2) of example 6.
FIG. 3 is an infrared spectrum of a melamine formaldehyde resin modified with hydrophilic groups prepared in example 1.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides an organic porous material which can be used as an oil guide cotton for electronic cigarettes, and the preparation method of the organic porous material comprises the following steps:
1) 150g of formaldehyde aqueous solution (the mass fraction of the formaldehyde aqueous solution is 38%) and 75g of melamine are added into a closed reaction kettle to be mixed, then sodium hydroxide is added to adjust the pH of the solution to 8.0, and the mixture is heated and heated to react for 2 hours at 80 ℃ to obtain a prepolymer solution; 1786g of polyethylene glycol (the weight average molecular weight of the polyethylene glycol is Mw=1000) is added into the prepolymer solution, then 8% hydrochloric acid solution with mass fraction is added to adjust the pH of the solution to 4.0, and the mixture is heated and heated to 70 ℃ for reaction for 1h, so that hydrophilic group modified melamine formaldehyde resin is obtained, and the hydrophilic group modified melamine formaldehyde resin has a structure shown in a formula I.
2) Mixing the hydrophilic group modified melamine formaldehyde resin prepared in the step 1) with methanol to prepare hydrophilic group modified melamine formaldehyde resin solution; placing 100g of hydrophilic group modified melamine formaldehyde resin solution (the solid content of the hydrophilic group modified melamine formaldehyde resin solution is 35%), 5g of hydrochloric acid solution with mass fraction of 8%, 5g of n-pentane and 4g of tween 80 into a reaction kettle, mixing, placing into a microwave oven for heating reaction, wherein the heating reaction temperature is 150 ℃, the heating reaction time is 120min, and placing the reaction mixture into an oven for drying at 120 ℃ for 10h after the reaction is finished to obtain melamine formaldehyde resin foam;
3) And (3) carrying out hot press molding on the melamine formaldehyde resin foam on a flat plate hot press, wherein the hot press temperature is 250 ℃, the hot press pressure is 100kPa, the pressure maintaining time is 30min, and the compression ratio is 1:1, so as to obtain the organic porous material.
Example 2
This example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 2:1.
Example 3
This example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 5:1.
Example 4
This example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 20:1.
Example 5
This example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 50:1.
Example 6
This example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 10:1.
Comparative example 1
This comparative example provides an organic porous material which differs from example 1 only in that the compression ratio in step 3) is 80:1.
Comparative example 2
The comparative example provides an organic porous material, which is prepared by the following steps:
1) Adding 150g of formaldehyde aqueous solution (the mass fraction of the formaldehyde aqueous solution is 38%) and 75g of melamine into a closed reaction kettle, mixing, adding sodium hydroxide to adjust the pH of the solution to 8.0, heating to 80 ℃ for reaction for 2 hours, adding 8% hydrochloric acid solution to adjust the pH of the solution to 4.0, and reacting at 70 ℃ for 1 hour to obtain melamine formaldehyde resin;
2) Mixing the melamine formaldehyde resin prepared in the step 1) with methanol to prepare a melamine formaldehyde resin solution; placing 100g of melamine formaldehyde resin solution (the solid content of the melamine formaldehyde resin solution is 35%), 5g of hydrochloric acid solution with mass fraction of 8%, 5g of n-pentane and 4g of tween 80 into a reaction kettle, mixing, placing into a microwave oven for heating reaction, wherein the heating reaction temperature is 150 ℃, the heating reaction time is 120min, and placing the reaction mixture into an oven for drying at 120 ℃ for 10h after the reaction is finished to obtain melamine formaldehyde resin foam;
3) And (3) carrying out hot press molding on the melamine formaldehyde resin foam on a flat plate hot press, wherein the hot press temperature is 250 ℃, the hot press pressure is 100kPa, the pressure maintaining time is 30min, and the compression ratio is 20:1, so as to obtain the organic porous material.
Test example 1
The melamine formaldehyde resin foam prepared in the step 2) of the above example 6 and the organic porous material prepared in the step 3) were respectively tested for their electron microscopic scanning images, and the results are shown in fig. 2 and 1.
As can be seen from FIG. 2, the melamine formaldehyde resin foam structure before hot pressing treatment is in a regular cross-linked network structure, the average pore diameter is between 200 and 300 mu m, and the average pore diameter of the organic porous material obtained after hot pressing is below 100 mu m (as shown in FIG. 1), so that the cell structure is more compact.
Test example 2
The hydrophilically modified melamine formaldehyde resin prepared in example 1 was tested for infrared spectrum, and the results are shown in fig. 3.
As can be seen from FIG. 3, compared with the standard infrared spectrogram of the melamine formaldehyde resin which is not hydrophilically modified, the infrared absorption peak positions of the melamine formaldehyde resin which is modified by polyhydroxy are completely consistent, but the infrared absorption peak intensity of hydroxyl is obviously increased, which indicates that the hydroxyl number and density of the melamine formaldehyde resin which is hydrophilically modified are obviously increased, and the modification is beneficial to improving the hydrophilia of the resin and the porous material obtained after foaming and hot pressing.
Test example 3
The organic porous materials prepared in examples 1 to 6 and comparative examples 1 to 2 were respectively tested for apparent density, porosity, compressive strength, oil storage amount and oil transfer rate, and the test results are shown in Table 1.
Wherein the apparent density is tested according to GB/T6343-2009 test standard;
the porosity is tested according to GB/T21650.2-2008 test standard;
compressive strength is tested according to GB/T8813-2008 test standard;
the oil storage is tested according to the following test method: cutting the organic porous materials prepared in examples 1-6 and comparative examples 1-2 into regular 2 cm-by-2 cm-sample blocks, weighing the mass of the blocks (marked as the initial mass of the blocks), soaking the blocks into 50 mg of standard tobacco tar, removing bubbles in vacuum to ensure that the tobacco tar fully wets the blocks, fishing out the blocks from the tobacco tar, placing the blocks on a self-made steel wire mesh bracket for 15min, and weighing the mass of the blocks (marked as the mass after the blocks are soaked) after the tobacco tar does not drip; oil storage= (mass after sample immersion-initial mass of sample)/initial mass of sample.
The oil transfer rate was tested according to the following test method: the organic porous materials prepared in examples 1 to 6 and comparative examples 1 to 2 were cut into regular 1cm pieces, 20 μl of standard tobacco tar (50 mg standard tobacco tar) liquid was dropped onto the surface of the horizontally placed pieces using a 10ml precision injection syringe, the time required for the droplets to completely sink into the pieces was observed under an electron microscope, and the ratio of the standard tobacco tar liquid volume to the time required for the droplets to completely sink into the pieces was calculated to obtain the oil guiding rate.
TABLE 1 results of physical Properties test of organic porous materials
| Numbering device | Apparent density of | Porosity of the porous material | Compressive Strength | Oil storage capacity | Oil transfer rate |
| Example 1 | 10kg/m 3 | 99％ | 12kPa | 160g/g | 20μl/s |
| Example 2 | 16kg/m 3 | 98％ | 18kPa | 75g/g | 15μl/s |
| Example 3 | 39kg/m 3 | 96％ | 50kPa | 30g/g | 10μl/s |
| Example 4 | 155kg/m 3 | 85％ | 130kPa | 12g/g | 5μl/s |
| Example 5 | 380kg/m 3 | 60％ | 360kPa | 5g/g | 2μl/s |
| Example 6 | 80kg/m 3 | 91％ | 75kPa | 27g/g | 8μl/s |
| Comparative example 1 | 500kg/m 3 | 38％ | 500kPa | 2g/g | 1μl/s |
| Comparative example 2 | 154kg/m 3 | 86％ | 131kPa | 6g/g | 1μl/s |
As can be seen from the results in Table 1, by controlling the porosity and apparent density of the porous material, the porous material has the compressive strength suitable for the oil guide cotton for electronic cigarettes, has excellent oil storage capacity and oil guide rate, and can effectively lock and control oil while rapidly guiding oil. Meanwhile, due to the proper compressive strength, the material is easier to mold and process, and the assembly consistency of the product is greatly improved.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (17)
1. An organic porous material applied to electronic cigarettes is characterized in that the apparent density rho is 10kg/m 3
-500kg/m 3 The porosity P is 50% -99%;
the organic porous material is formed by melamine formaldehyde resin modified by hydrophilic groups;
the hydrophilic group is at least one of hydroxyl and carbonyl;
the preparation method of the melamine formaldehyde resin modified by the hydrophilic group comprises the following steps:
1) Mixing formaldehyde aqueous solution with melamine, and heating and reacting under alkaline condition to obtain prepolymer solution;
2) Adding a hydrophilic modifier into the prepolymer solution obtained in the step 1), and heating and reacting under an acidic condition to obtain melamine formaldehyde resin modified by hydrophilic groups;
the mole ratio of formaldehyde to melamine is (3-5) 1;
in the step 2), the hydrophilic modifier is at least one selected from polyalcohol and polycarboxylic acid, and the molar ratio of the hydrophilic modifier to melamine is (1-5): 1.
2. The organic porous material according to claim 1, wherein,
in the step 1), the mass fraction of the formaldehyde aqueous solution is 30-40%.
3. The organic porous material according to claim 1 or 2, wherein,
in the step 1), the pH value under the alkaline condition is 8.0-9.0, the heating reaction temperature is 75-85 ℃, and the heating reaction time is 0.5-3h;
in the step 2), the pH value of the acidic condition is 3.0-5.0, the heating reaction temperature is 70-85 ℃, and the heating reaction time is 1-5h.
4. The organic porous material of claim 1, wherein 130kg/m 3 ≤ρ≤500kg/m 3 ，50％≤P≤98％。
5. The preparation method of the organic porous material is characterized by comprising the following steps of:
1) Hydrophilic modification of melamine formaldehyde resin;
2) Foaming, compression molding to obtain the organic porous material;
the hydrophilic modification comprises the following steps:
1) Mixing formaldehyde aqueous solution with melamine, and heating and reacting under alkaline condition to obtain prepolymer solution;
2) Adding a hydrophilic modifier into the prepolymer solution obtained in the step 1), and heating and reacting under an acidic condition to obtain melamine formaldehyde resin modified by hydrophilic groups;
the mole ratio of formaldehyde to melamine is (3-5) 1;
in the step 2), the hydrophilic modifier is at least one selected from polyalcohol and polycarboxylic acid, and the molar ratio of the hydrophilic modifier to melamine is (1-5): 1.
6. The method for producing an organic porous material according to claim 5, wherein,
in the step 1), the mass fraction of the formaldehyde aqueous solution is 30-40%.
7. The method for producing an organic porous material according to claim 5 or 6, wherein,
in the step 1), the pH value under the alkaline condition is 8.0-9.0, the heating reaction temperature is 75-85 ℃, and the heating reaction time is 0.5-3h;
in the step 2), the pH value of the acidic condition is 3.0-5.0, the heating reaction temperature is 70-85 ℃, and the heating reaction time is 1-5h.
8. The method for producing an organic porous material according to claim 5, wherein said foaming method comprises the steps of:
mixing the melamine formaldehyde resin solution modified by hydrophilic groups, an acid catalyst, a foaming agent and a surfactant, and heating to react after mixing to obtain the melamine formaldehyde resin foam.
9. The method for preparing an organic porous material according to claim 8, wherein the hydrophilic group modified melamine formaldehyde resin solution is prepared by mixing hydrophilic group modified melamine formaldehyde resin and a solvent, and the solid content of the hydrophilic group modified melamine formaldehyde resin solution is 30-50%.
10. The method for producing an organic porous material according to claim 8 or 9, wherein,
the mass ratio of the hydrophilic group modified melamine formaldehyde resin solution to the acid catalyst to the foaming agent to the surfactant is 100 (1-5): 1-10): 1-5;
the foaming heating temperature is 150-250 ℃ and the heating time is 10-200min.
11. The method for producing an organic porous material according to claim 9, wherein,
the solvent is methanol, the acid catalyst is hydrochloric acid or phosphoric acid, the foaming agent is n-pentane, and the surfactant is silicone oil and Tween 80.
12. The method according to claim 5, wherein the compression molding method is a hot press molding method in which a hot press temperature is 150 ℃ to 300 ℃, a hot press pressure is 100kPa to 2.5MPa, a dwell time is 0.5min to 120min, and a compression ratio is (1 to 50): 1.
13. A liquid guiding element, characterized in that the liquid guiding element material is the organic porous material according to any one of claims 1-4 or the organic porous material prepared by the preparation method according to any one of claims 5-12.
14. A heating element, characterized in that the main body material of the heating element or the cotton core material in the heating element is the organic porous material according to any one of claims 1 to 4 or the organic porous material prepared by the preparation method according to any one of claims 5 to 12.
15. An atomizing device, characterized in that the atomizing device has the liquid guiding member according to claim 13, and/or the heat generating body according to claim 14.
16. Use of an organic porous material prepared by the preparation method of any one of claims 5 to 12 in an atomizing device.
17. The use of claim 16, wherein the atomizing device is an electronic cigarette.
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