CN117534938A - Melamine powder for manufacturing anti-fouling tableware and preparation method thereof - Google Patents
Melamine powder for manufacturing anti-fouling tableware and preparation method thereof Download PDFInfo
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- CN117534938A CN117534938A CN202410036053.2A CN202410036053A CN117534938A CN 117534938 A CN117534938 A CN 117534938A CN 202410036053 A CN202410036053 A CN 202410036053A CN 117534938 A CN117534938 A CN 117534938A
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- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine powder Natural products NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 230000003373 anti-fouling effect Effects 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 65
- 239000007864 aqueous solution Substances 0.000 claims abstract description 61
- 238000000227 grinding Methods 0.000 claims abstract description 55
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 54
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims abstract description 52
- 239000000843 powder Substances 0.000 claims abstract description 50
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 45
- 238000004132 cross linking Methods 0.000 claims abstract description 43
- 239000000945 filler Substances 0.000 claims abstract description 41
- 238000003756 stirring Methods 0.000 claims abstract description 37
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 35
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 34
- 239000010703 silicon Substances 0.000 claims abstract description 34
- 238000001035 drying Methods 0.000 claims abstract description 29
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 27
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 27
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 27
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 27
- 239000004575 stone Substances 0.000 claims abstract description 27
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 26
- 239000004417 polycarbonate Substances 0.000 claims abstract description 26
- 229920000515 polycarbonate Polymers 0.000 claims abstract description 26
- 238000004898 kneading Methods 0.000 claims abstract description 25
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 17
- 230000032683 aging Effects 0.000 claims abstract description 13
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 18
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 12
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 claims description 12
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 claims description 12
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 12
- -1 dodecyl ethoxy sulfobetaine Chemical compound 0.000 claims description 11
- 229940117986 sulfobetaine Drugs 0.000 claims description 11
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- 239000002689 soil Substances 0.000 claims description 6
- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 30
- 238000007873 sieving Methods 0.000 description 20
- 238000009210 therapy by ultrasound Methods 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 8
- 239000004640 Melamine resin Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000908 ammonium hydroxide Substances 0.000 description 2
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920001131 Pulp (paper) Polymers 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/20—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08L61/26—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds
- C08L61/28—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with heterocyclic compounds with melamine
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The application relates to the technical field of high polymer material processing, and particularly discloses melamine powder for manufacturing anti-fouling tableware and a preparation method thereof, wherein the preparation method of the melamine powder comprises the steps of adding tetraethoxysilane, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and sodium silicate aqueous solution into ethanol aqueous solution, stirring and mixing, aging, drying and grinding to obtain silicon micropowder; mixing graphene oxide, medical stone powder and silicon micropowder, adding a grinding aid for grinding, adding a silver nitrate aqueous solution for ultrasonic dispersion, standing, centrifuging and drying to obtain modified filler; under alkaline condition, mixing melamine and formaldehyde solution for reaction to obtain prepolymer; kneading the prepolymer, modified filler, polycarbonate and crosslinking accelerator together, and then drying and ball-milling to obtain melamine powder; the melamine powder prepared by the method has the advantages of enhanced connectivity among molecular chains, high crosslinking density of melamine molecules and excellent comprehensive mechanical property, antibacterial property, heat resistance and chemical resistance.
Description
Technical Field
The application relates to the technical field of polymer material processing, in particular to melamine powder for manufacturing anti-fouling tableware and a preparation method thereof.
Background
The melamine resin is a novel thermosetting plastic prepared by taking urea formaldehyde resin or melamine formaldehyde resin as a base material and adding wood pulp cellulose, a hardening agent and other additives. Melamine tableware is a plastic product widely used in recent years, and has rich color and looks like porcelain or ivory, so that the melamine tableware is also called as a porcelain-like product. Most of common melamine tableware is characterized by safety, drop resistance, durability and easy cleaning.
The melamine tableware is easy to be stained with greasy dirt and bacteria to grow on the surface in the use process, and has the problems of poor high-temperature stability, easy separation of formaldehyde and melamine monomers when contacting high-temperature environment or high-temperature food, and the like. In the prior art, the high temperature resistance and the antibacterial performance of melamine tableware are improved by adding high temperature resistant inorganic filler and silver-loaded antibacterial agent. However, the inorganic filler, silver-loaded antibacterial agent and the like have poor compatibility and dispersibility with melamine resin, and although the high temperature resistance and antibacterial property of the melamine resin can be improved to a certain extent, other properties such as wear resistance, toughness and the like of the melamine resin are adversely affected. Based on the above statements, the present application proposes a melamine powder for making anti-soil tableware and a method for preparing the same.
Disclosure of Invention
In order to solve the problems that the surface of the existing melamine tableware is easy to be stained with greasy dirt and bacteria are bred in the using process, the high-temperature stability is poor, formaldehyde and melamine monomers are easy to separate out when the melamine tableware is contacted with a high-temperature environment or high-temperature food, and the like, the application provides melamine powder for manufacturing the anti-fouling tableware and a preparation method thereof.
In a first aspect, the present application provides melamine powder for making anti-soil tableware, which adopts the following technical scheme:
a preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, adding tetraethoxysilane and vinyl trimethoxysilane into an ethanol water solution, stirring and mixing uniformly, adding tetramethyl ammonium hydroxide for mixing, then adding a sodium silicate water solution for stirring and mixing, aging, drying and grinding to obtain silicon micro powder;
s2, mixing graphene oxide, medical stone powder and silicon micropowder, adding a grinding aid, mixing and grinding, adding a silver nitrate aqueous solution, performing ultrasonic dispersion, standing, centrifuging and drying to obtain a modified filler;
s3, mixing melamine with 37 mass percent formaldehyde solution under an alkaline condition to react to obtain a prepolymer;
s4, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together for kneading, and then placing the kneaded mixture into a baking oven at 100-120 ℃ for drying and ball milling to obtain melamine powder.
Preferably, in the step S1, the mass ratio of the ethanol aqueous solution to the ethyl orthosilicate to the vinyl trimethoxysilane to the tetramethylammonium hydroxide to the sodium silicate aqueous solution is 22-24:3-5:1:0.02-0.04:7-9.
Preferably, the mass fraction of the ethanol water solution is 55-65%, and the mass fraction of the sodium silicate water solution is 20-24%.
Preferably, in the step S2, the mass ratio of the graphene oxide to the medical stone powder to the silicon micropowder to the grinding aid to the silver nitrate solution is 1-1.5:3-4:1-2:0.1-0.2:14-16.
Preferably, the grinding aid is dodecyl ethoxy sulfobetaine and/or stearyl trimethyl ammonium chloride.
Preferably, the mass fraction of the silver nitrate aqueous solution in the step S2 is 0.8-1.2%.
Preferably, in the step S2, the ultrasonic frequency is 18-23kHz, the ultrasonic power is 280-300W, and the ultrasonic time is 0.8-1h.
Preferably, the alkaline condition in the step S3 means that the pH value is 8.5-9.5; the alkaline regulator is sodium hydroxide or ammonium hydroxide.
Preferably, the reaction temperature in the step S3 is 70-90 ℃ and the reaction time is 2-3h.
Preferably, in the step S3, the mass ratio of the melamine to the formaldehyde solution is 1:6-8.
Preferably, the mass ratio of the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator in the step S4 is 56-60:13-15:20-22:1-2.
Preferably, the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3-5:1.
Preferably, the kneading temperature in the step S4 is 60 to 100℃and the kneading time is 60 to 80 minutes.
In a second aspect, the present application provides a method for preparing melamine powder for making anti-fouling tableware, which adopts the following technical scheme:
melamine powder for preparing anti-fouling tableware is prepared by the preparation method.
In summary, the present application has the following beneficial effects:
according to the preparation method, tetraethoxysilane and vinyltrimethoxysilane are used as silicon sources, tetramethylammonium hydroxide is used as a catalyst, and sodium silicate aqueous solution is added after reaction, so that a reaction product is stabilized, the surface activity of the obtained silicon micropowder is high by controlling the form and performance of the finally prepared silicon micropowder, and the mixing performance of the silicon micropowder, graphene oxide and medical stone powder is improved. According to the method, the graphene oxide, the medical stone powder and the silicon micro powder are mixed, added with the grinding aid for grinding, so that the grinding efficiency and the filler dispersibility can be improved, the obtained modified filler is favorable for improving the crosslinking performance of melamine molecules, and the mechanical property, the heat resistance and the antibacterial performance of the prepared melamine powder are enhanced.
According to the method, the prepolymer prepared by reacting melamine with 37% by mass of formaldehyde solution is kneaded together with the modified filler, the polycarbonate and the crosslinking accelerator, and the crosslinking accelerator compounded by itaconic acid and sodium persulfate is added, so that the crosslinking reaction rate of the prepolymer and other raw materials can be accelerated, the connection between melamine powder molecular chains is enhanced, the crosslinking density of melamine molecules is improved, and the mechanical property, heat resistance and chemical resistance of the finally prepared melamine powder are enhanced.
Detailed Description
The present application is described in further detail below with reference to examples.
Examples 1-5 provide melamine powder for making anti-soil tableware and a method of making the same.
Example 1
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
Example 2
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 23:4:1:0.03:8, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 60% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 22% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1.2:3.5:1.5:0.15:15, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding grinding aid to mix and grind for 2 hours, adding 1% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 20kHz, controlling the ultrasonic power to be 290W, carrying out ultrasonic treatment for 0.9 hour, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is stearyl trimethyl ammonium chloride;
s3, controlling the mass ratio of melamine to formaldehyde solution to be 1:7, adding melamine and formaldehyde solution with mass fraction of 37% into a reaction kettle together, adding ammonium hydroxide to adjust pH to 8.5, and mixing and reacting at 80 ℃ for 2.5 hours to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 58:14:21:1.5, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 80 ℃, kneading for 70min, then placing the kneader in a 110 ℃ oven to dry to constant weight, ball-milling and sieving with a 90-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 4:1.
Example 3
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 24:5:1:0.04:9, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 65% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding the sodium silicate aqueous solution with the mass fraction of 24% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1.5:4:2:0.2:16, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 1.2% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 23kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 1 hour, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:8, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9, and mixing and reacting for 2 hours at the temperature of 90 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 60:15:22:2, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 100 ℃, kneading for 60min, then placing the kneader in a 120 ℃ oven to dry to constant weight, ball-milling and sieving with a 100-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 5:1.
Example 4
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid comprises dodecyl ethoxy sulfobetaine and stearyl trimethyl ammonium chloride in a mass ratio of 1:1;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
Example 5
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid comprises dodecyl ethoxy sulfobetaine and stearyl trimethyl ammonium chloride in a mass ratio of 3.5:1;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
In order to verify the overall properties of melamine powder for making anti-soil tableware prepared in examples 1 to 5 of the present application, comparative examples 1 to 5 were set as follows:
comparative example 1
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, tetramethyl ammonium hydroxide to a sodium silicate aqueous solution to be 22:4:0.02:7, adding the ethyl orthosilicate to the ethanol aqueous solution with the mass fraction of 55% while stirring at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding the sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, grinding and sieving with a 200-mesh sieve to obtain silicon micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
Comparative example 2
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to ethyl orthosilicate to vinyl trimethoxy silane to sodium silicate aqueous solution to tetramethyl ammonium hydroxide to be 22:3:1:7:0.02, adding the ethyl orthosilicate to vinyl trimethoxy silane to the ethanol aqueous solution with the mass fraction of 55% while stirring at the stirring rate of 300r/min, stirring and mixing for 40min to be uniform, adding tetramethyl ammonium hydroxide to continue stirring and mixing for 90min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silicon micro powder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
Comparative example 3
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micropowder to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micropowder, grinding for 2 hours, adding silver nitrate aqueous solution with the mass fraction of 0.8%, performing ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, performing ultrasonic power to be 300W, performing ultrasonic treatment for 0.8 hour, standing for 1 hour, centrifuging at a rotating speed of 8000r/min for 5 minutes, and drying at the temperature of 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3:1.
Comparative example 4
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator comprises itaconic acid.
Comparative example 5
A preparation method of melamine powder for making anti-fouling tableware comprises the following preparation steps:
s1, controlling the mass ratio of an ethanol aqueous solution to an ethyl orthosilicate, vinyl trimethoxysilane, tetramethyl ammonium hydroxide and a sodium silicate aqueous solution to be 22:3:1:0.02:7, adding the ethyl orthosilicate and the vinyl trimethoxysilane into the ethanol aqueous solution with the mass fraction of 55% at room temperature at the stirring rate of 300r/min, stirring and mixing for 40min until the mixture is uniform, adding tetramethyl ammonium hydroxide and mixing for 60min, adding a sodium silicate aqueous solution with the mass fraction of 20% and continuously stirring and mixing for 30min, aging for 8h, drying to constant weight at the temperature of 80 ℃, and grinding and sieving with a 200-mesh sieve to obtain silica micropowder;
s2, controlling the mass ratio of graphene oxide to medical stone powder to silicon micro powder to grinding aid to silver nitrate solution to be 1:3:1:0.1:14, mixing 325-mesh graphene oxide to 180-mesh medical stone powder to 200-mesh silicon micro powder, adding the grinding aid to mix and grind for 2 hours, adding 0.8% silver nitrate aqueous solution by mass fraction to carry out ultrasonic dispersion, controlling the ultrasonic frequency to be 18kHz, controlling the ultrasonic power to be 300W, carrying out ultrasonic treatment for 0.8 hours, standing for 1 hour, centrifuging for 5 minutes at a rotating speed of 8000r/min, and drying at 80 ℃ to constant weight to obtain modified filler; wherein the grinding aid is dodecyl ethoxy sulfobetaine;
s3, controlling the mass ratio of the melamine to the formaldehyde solution to be 1:6, adding the melamine and the formaldehyde solution with the mass fraction of 37% into a reaction kettle together, adding sodium hydroxide to adjust the pH value to 9.5, and mixing and reacting for 3 hours at the temperature of 70 ℃ to obtain a prepolymer;
s4, controlling the mass ratio of the prepolymer to the modified filler to the polycarbonate to the crosslinking accelerator to be 56:13:20:1, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together, controlling the kneading temperature to be 60 ℃, kneading for 80 minutes, then placing the kneader in a 100 ℃ oven to dry to constant weight, ball-milling and sieving the mixture with a 80-mesh sieve to obtain melamine powder; wherein the crosslinking accelerator is sodium persulfate.
Performance detection
Melamine powders prepared in examples 1 to 5 and comparative examples 1 to 5 of the present application were hot-pressed (hot-pressing temperature 165 ℃ C., molding pressure 180 kgf/cm) 2 Molding time 20 s), and cooling to room temperature to obtain a test sample with a size of 60mmx20mmx5 mm.
The impact strength is tested by referring to the national standard GB/T3403.2-2013;
performing antibacterial performance test on the material by referring to international standard ISO 22196-2011;
measuring the formaldehyde migration quantity and the melamine migration quantity by referring to the national standard GB 4806.6-2016;
the specific test results are shown in table 1 below.
Table 1:
as can be seen from the data shown in table 1: the melamine powder for making the anti-fouling tableware prepared in the embodiment 1-5 has the comprehensive performance obviously superior to that of the comparative embodiment 1-5, has obvious advantages in the aspects of impact strength, antibacterial property, safety and the like, and has wide market prospect.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (10)
1. A method for preparing melamine powder for making anti-fouling tableware, which is characterized by comprising the following preparation steps:
s1, adding tetraethoxysilane and vinyl trimethoxysilane into an ethanol water solution, stirring and mixing uniformly, adding tetramethyl ammonium hydroxide for mixing, then adding a sodium silicate water solution for stirring and mixing, aging, drying and grinding to obtain silicon micro powder;
s2, mixing graphene oxide, medical stone powder and silicon micropowder, adding a grinding aid, mixing and grinding, adding a silver nitrate aqueous solution, performing ultrasonic dispersion, standing, centrifuging and drying to obtain a modified filler;
s3, mixing melamine with 37 mass percent formaldehyde solution under an alkaline condition to react to obtain a prepolymer;
s4, adding the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator into a kneader together for kneading, and then placing the kneaded mixture into a baking oven at 100-120 ℃ for drying and ball milling to obtain melamine powder.
2. The method for preparing melamine powder for making anti-fouling tableware according to claim 1, wherein the mass ratio of the ethanol aqueous solution, the ethyl orthosilicate, the vinyl trimethoxy silane, the tetramethyl ammonium hydroxide and the sodium silicate aqueous solution in the step S1 is 22-24:3-5:1:0.02-0.04:7-9.
3. The method for preparing melamine powder for use in the production of anti-fouling tableware according to claim 2, wherein the mass fraction of the aqueous ethanol solution is 55-65% and the mass fraction of the aqueous sodium silicate solution is 20-24%.
4. The method for preparing melamine powder for making anti-fouling tableware according to claim 1, wherein in the step S2, the mass ratio of graphene oxide, medical stone powder, silica micropowder, grinding aid and silver nitrate solution is 1-1.5:3-4:1-2:0.1-0.2:14-16.
5. The method for preparing melamine powder for use in making anti-soil tableware according to claim 4, wherein the grinding aid is dodecyl ethoxy sulfobetaine and/or stearyl trimethyl ammonium chloride.
6. The method for preparing melamine powder for use in the production of anti-fouling tableware according to claim 1, wherein the mass fraction of the silver nitrate aqueous solution in step S2 is 0.8-1.2%.
7. The method for preparing melamine powder for use in the production of anti-fouling tableware according to claim 1, wherein the mass ratio of melamine to formaldehyde solution in step S3 is 1:6-8.
8. The method for preparing melamine powder for making anti-fouling tableware according to claim 1, wherein the mass ratio of the prepolymer, the modified filler, the polycarbonate and the crosslinking accelerator in the step S4 is 56-60:13-15:20-22:1-2.
9. The method for preparing melamine powder for use in making anti-soil tableware according to claim 8, wherein the crosslinking accelerator comprises itaconic acid and sodium persulfate in a mass ratio of 3-5:1.
10. Melamine powder for use in the manufacture of anti-fouling cutlery, characterized in that it is obtainable by a process according to any one of claims 1-9.
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