CN116622333B - Preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive - Google Patents
Preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive Download PDFInfo
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- CN116622333B CN116622333B CN202310911995.6A CN202310911995A CN116622333B CN 116622333 B CN116622333 B CN 116622333B CN 202310911995 A CN202310911995 A CN 202310911995A CN 116622333 B CN116622333 B CN 116622333B
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- mildew
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- beautifying
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- 238000009966 trimming Methods 0.000 title claims abstract description 77
- 239000000853 adhesive Substances 0.000 title claims abstract description 74
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 44
- 238000004132 cross linking Methods 0.000 claims abstract description 47
- 239000000843 powder Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 26
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 18
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 18
- 239000003112 inhibitor Substances 0.000 claims abstract description 16
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 14
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 14
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 239000012975 dibutyltin dilaurate Substances 0.000 claims abstract description 8
- JJQZDUKDJDQPMQ-UHFFFAOYSA-N dimethoxy(dimethyl)silane Chemical compound CO[Si](C)(C)OC JJQZDUKDJDQPMQ-UHFFFAOYSA-N 0.000 claims abstract description 8
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims abstract description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229940083037 simethicone Drugs 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 82
- 238000003756 stirring Methods 0.000 claims description 67
- 238000006243 chemical reaction Methods 0.000 claims description 46
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 41
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 34
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 31
- 239000008367 deionised water Substances 0.000 claims description 29
- 229910021641 deionized water Inorganic materials 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000007864 aqueous solution Substances 0.000 claims description 20
- PFKFTWBEEFSNDU-UHFFFAOYSA-N carbonyldiimidazole Chemical compound C1=CN=CN1C(=O)N1C=CN=C1 PFKFTWBEEFSNDU-UHFFFAOYSA-N 0.000 claims description 20
- 229920001661 Chitosan Polymers 0.000 claims description 19
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 claims description 19
- 239000000725 suspension Substances 0.000 claims description 19
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 15
- 238000000498 ball milling Methods 0.000 claims description 14
- 230000003449 preventive effect Effects 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 229920002643 polyglutamic acid Polymers 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 10
- FYGDTMLNYKFZSV-URKRLVJHSA-N (2s,3r,4s,5s,6r)-2-[(2r,4r,5r,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5r,6s)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1[C@@H](CO)O[C@@H](OC2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-URKRLVJHSA-N 0.000 claims description 9
- 229920002498 Beta-glucan Polymers 0.000 claims description 9
- 239000002244 precipitate Substances 0.000 claims description 9
- 239000011787 zinc oxide Substances 0.000 claims description 9
- GGAUUQHSCNMCAU-ZXZARUISSA-N (2s,3r)-butane-1,2,3,4-tetracarboxylic acid Chemical compound OC(=O)C[C@H](C(O)=O)[C@H](C(O)=O)CC(O)=O GGAUUQHSCNMCAU-ZXZARUISSA-N 0.000 claims description 7
- QBLDFAIABQKINO-UHFFFAOYSA-N barium borate Chemical compound [Ba+2].[O-]B=O.[O-]B=O QBLDFAIABQKINO-UHFFFAOYSA-N 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 230000018044 dehydration Effects 0.000 claims 1
- 238000006297 dehydration reaction Methods 0.000 claims 1
- 238000009775 high-speed stirring Methods 0.000 abstract description 17
- 230000009974 thixotropic effect Effects 0.000 abstract description 14
- 238000007688 edging Methods 0.000 abstract description 12
- 239000002537 cosmetic Substances 0.000 description 32
- 239000003292 glue Substances 0.000 description 14
- 230000000694 effects Effects 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 239000004408 titanium dioxide Substances 0.000 description 12
- 239000004590 silicone sealant Substances 0.000 description 9
- 239000003921 oil Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 7
- 229920001971 elastomer Polymers 0.000 description 7
- 238000001125 extrusion Methods 0.000 description 7
- 239000011324 bead Substances 0.000 description 6
- 230000003796 beauty Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 229920002379 silicone rubber Polymers 0.000 description 6
- 239000004945 silicone rubber Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 239000013464 silicone adhesive Substances 0.000 description 4
- 229920002873 Polyethylenimine Polymers 0.000 description 3
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 2
- 244000082946 Tarchonanthus camphoratus Species 0.000 description 2
- 235000005701 Tarchonanthus camphoratus Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000003431 cross linking reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000010705 motor oil Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- RJQXTJLFIWVMTO-TYNCELHUSA-N Methicillin Chemical compound COC1=CC=CC(OC)=C1C(=O)N[C@@H]1C(=O)N2[C@@H](C(O)=O)C(C)(C)S[C@@H]21 RJQXTJLFIWVMTO-TYNCELHUSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 125000004183 alkoxy alkyl group Chemical group 0.000 description 1
- 150000001495 arsenic compounds Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000000385 dialysis solution Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 229960003085 meticillin Drugs 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001470 polyketone Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive, which belongs to the technical field of beautifying trimming adhesives and comprises the steps of preparing ultrafine powder, preparing a multi-branching crosslinking-promoting agent, preparing an inorganic mixed mildew inhibitor and mixing; adding hydroxyl-terminated polydimethylsiloxane, simethicone and ultrafine powder into a kneader for mixing and dehydrating, and cooling to obtain a base material; adding the obtained base material, the multi-branching crosslinking promoter, the methyltrimethoxysilane, the dimethyldimethoxysilane, the 3-aminopropyl triethoxysilane, the inorganic mixed mildew inhibitor and the dibutyl tin dilaurate into a high-speed stirrer for high-speed stirring; the high-power mildew-proof dealcoholization type beautifying edging adhesive prepared by the invention has good mildew resistance, high tearing strength, good oil resistance and puncture resistance, is not easy to generate oily dialyzate, can improve the cohesiveness, deep curing speed and elasticity of the high-power mildew-proof dealcoholization type beautifying edging adhesive, and reduces the dependence of extrudability and thixotropic property on temperature.
Description
Technical Field
The invention relates to the technical field of beautifying trimming glue, in particular to a preparation method of high-power mildew-proof dealcoholization beautifying trimming glue.
Background
The room temperature vulcanized silicone rubber has excellent electrical property and chemical inertness, heat resistance, aging resistance, flame resistance, moisture resistance, air permeability and the like, and is classified into a plurality of types such as deacidification type, fat removal type, dealcoholization type, deamination type, polyketone removal type and the like according to different chain agents; the dealcoholized room temperature vulcanized silicone rubber is characterized in that dealcoholization reaction is generated in the curing process, alcohol substances are volatilized, and the dealcoholization reaction can be used for curing the silicone rubber, so that a good sealing effect is achieved.
The dealcoholized room temperature vulcanized silicone rubber is the type which is most studied, has the most variety and the fastest quantity developed by all companies in the eighties world, has greatly improved in vulcanization speed, storage stability, cohesiveness and flame retardance, becomes a main variety and development direction of room temperature vulcanized silicone rubber, has wider and wider application range, and is particularly used as dealcoholized cosmetic edge-trimming rubber, and the dealcoholized room temperature vulcanized silicone rubber is rapidly expanding in the field of construction.
Compared with other cosmetic edging products, the dealcoholized cosmetic edging glue has the advantages of strong cohesiveness, high curing speed and good elasticity, has small dependence on temperature of extrusion and thixotropy, has good extrusion and thixotropy in a temperature range of-4 ℃ to 40 ℃, and also has excellent ageing resistance, ultraviolet resistance linearity and ozone resistance, but the dealcoholized cosmetic edging glue has poor mildew resistance, so black spots and yellowing are easy to appear, and the dealcoholized cosmetic edging glue has the defects of low tearing strength, poor oil resistance and puncture intolerance.
In order to overcome the above-mentioned disadvantages, the most commonly used method at present is to add a mildew inhibitor to the dealcoholized cosmetic edging glue, thereby improving the mildew resistance of the dealcoholized cosmetic edging glue, in addition, modified filler and crosslinking aid are added, so as to improve the crosslinking density, change dispersion crosslinking into concentrated crosslinking, thereby improving the tearing strength, oil resistance and puncture resistance of the dealcoholized cosmetic edging glue, and avoid the generation of oily dialyzate, but on one hand, the addition of the mildew inhibitor can affect the cohesiveness of the cosmetic edging glue, and on the other hand, the time required for crosslinking is correspondingly prolonged while the crosslinking density is improved, so that the deep curing speed is reduced, in addition, the elasticity of the dealcoholized cosmetic edging glue is affected, so that the dependence of extrudability and thixotropic property on temperature is increased.
Chinese patent CN113881393B discloses a kind of silicone adhesive with mildew-proof effect, which is prepared by using polydimethylsiloxane as raw material, and adding compound mildew inhibitor during the preparation of silicone adhesive with mildew-proof effect; the compound mildew inhibitor comprises nano zinc oxide and camphor wood powder extract; wherein the weight ratio of the nano zinc oxide to the camphorwood powder extract is 5-10:1; the prepared silicone adhesive with the mildew-proof effect has the inhibition effect on conventional mould and bacteria and also has the inhibition effect on methicillin-resistant staphylococcus aureus, but the prepared silicone adhesive with the mildew-proof effect has low tearing strength, poor oil resistance and puncture resistance.
Chinese patent CN108676544B discloses a high temperature resistant and mildew proof silicone sealant and a preparation method thereof, the high temperature resistant and mildew proof silicone sealant comprises the following components in parts by weight: 50-100 parts of alpha, omega-dihydroxypolysiloxane, 5-20 parts of reinforcing filler, 5-20 parts of methyl phenyl silicone oil, 40-100 parts of high-temperature-resistant filler, 0.05-0.2 part of mildew inhibitor, 3-15 parts of cross-linking agent, 0.001-1 part of catalyst and 0.2-1 part of coupling agent, and the prepared high-temperature-resistant mildew-resistant silicone sealant has the advantages of good elasticity, high tensile strength and elongation at break, excellent high-temperature resistance and moisture resistance, but slow deep curing speed, and large dependence of extrudability and thixotropic property on temperature.
Chinese patent CN103756630B discloses a single-component mildew-proof transparent dealcoholized silicone sealant and preparation method, which is prepared by adding mildew-proof agent based on transparent dealcoholized silicone sealant, wherein the mildew-proof agent is an organic arsenic compound taking polyether polyol as carrier, and based on 100 parts of alkoxyl alkyl terminated polysiloxane, the added weight portion is 0.1-2 parts; the prepared single-component mildew-proof transparent dealcoholized silicone sealant has the advantages of excellent mildew-proof effect, low odor, yellowing resistance and fast deep curing, but has poor oil resistance and no puncture resistance.
Chinese patent CN111793463B discloses a preparation method of antibacterial and mildew-proof silicone sealant and a product thereof, the preparation method comprises: preparing quaternized polyethyleneimine; blending silicone sealant and quaternized polyethyleneimine, wherein the addition amount of the quaternized polyethyleneimine is 1-20wt%; the prepared antibacterial mildew-proof silicone sealant has good antibacterial mildew-proof effect and higher mechanical property, but has weak cohesiveness and low deep curing speed.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, which has the advantages of good mildew resistance, high tearing strength, good oil resistance and puncture resistance, difficult generation of oily dialyzate, and capability of improving the cohesiveness, deep curing speed and elasticity of the high-power mildew-proof dealcoholization type beautifying trimming adhesive and reducing the dependence of extrudability and thixotropic property on temperature.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive comprises the following steps: preparing ultrafine powder, preparing a multi-branching crosslinking promoter, preparing an inorganic mixed mildew inhibitor, and mixing;
adding superfine calcium carbonate and deionized water into a high-speed reaction kettle, carrying out ultrasonic vibration while stirring at a high speed, controlling the stirring speed of the high-speed stirring to be 800-1000rpm, stopping high-speed stirring and ultrasonic vibration after the ultrasonic vibration frequency is 20-30kHz and 25-35min, and obtaining superfine calcium carbonate suspension; adding silver nitrate, deionized water and polyvinyl amine into a reaction kettle, controlling the temperature of the reaction kettle to 35-40 ℃, controlling the stirring speed to 200-300rpm, slowly adding superfine calcium carbonate suspension after stirring for 30-40min, controlling the adding speed of the superfine calcium carbonate suspension to 18-22g/min, continuing stirring for 40-50min after adding, then adding carboxymethyl chitosan and beta-glucan, continuing stirring and simultaneously carrying out ultraviolet irradiation, controlling the wavelength during ultraviolet irradiation to 320-380nm, stopping ultraviolet irradiation after 4-5h, adding gamma-polyglutamic acid aqueous solution, stirring for 45-55min, adding carboxymethyl chitosan aqueous solution, stirring for 1.5-2h, centrifuging, controlling the rotating speed during centrifuging to 7000-8000rpm for 8-10min, and drying precipitate at 110-120 ℃ after centrifuging to obtain superfine powder;
in the preparation of the ultrafine powder, the mass ratio of the ultrafine calcium carbonate to the deionized water in the ultrafine calcium carbonate suspension is 3-4:130-140;
the mass ratio of the silver nitrate to the deionized water to the polyvinyl amine to the superfine calcium carbonate suspension to the carboxymethyl chitosan to the beta-glucan to the gamma-polyglutamic acid aqueous solution to the carboxymethyl chitosan aqueous solution is 5-5.5:200-220:3-3.5:60-65:0.1-0.12:0.08-0.1:2-3:3-4;
the mass fraction of the gamma-polyglutamic acid aqueous solution is 4-5%;
the mass fraction of the carboxymethyl chitosan aqueous solution is 3-4%;
the grain diameter of the superfine calcium carbonate is 0.05-0.08 mu m;
the preparation of the multi-branching crosslinking promoter comprises the steps of adding rutile type nano titanium dioxide and deionized water into a closed reaction kettle, controlling the temperature of the closed reaction kettle to be 30-35 ℃, controlling the stirring speed to be 180-220rpm, stirring for 30-40min, adding 3-aminopropyl triethoxysilane and ammonia water, replacing air in the closed reaction kettle with nitrogen for 2-3 times, heating to 40-45 ℃, preserving heat for 4-5h at 40-45 ℃, filtering, respectively cleaning with 30-40mL of absolute ethyl alcohol and 30-40mL of deionized water, and then drying at 115-120 ℃ to obtain the aminated titanium dioxide; adding tetrahydrofuran and butane tetracarboxylic acid into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 30-35 ℃, controlling the stirring speed to 180-220rpm, using nitrogen to replace air in the closed reaction kettle for 2-3 times, then dropwise adding a tetrahydrofuran solution of N, N' -carbonyl diimidazole, controlling the dropwise adding speed to be 3-4g/min, continuing stirring for 4-4.5h after the dropwise adding is finished, adding aminated titanium dioxide, continuing stirring for 5-6h, centrifuging, controlling the rotating speed during centrifuging to be 7000-8000rpm, controlling the time to be 12-15min, washing a precipitate for 2-3 times by using deionized water after centrifuging is finished, and drying at 110-120 ℃ to obtain the multi-branching crosslinking agent;
in the preparation of the multi-branching crosslinking promoter, the mass ratio of the rutile type nano titanium dioxide to the deionized water to the 3-aminopropyl triethoxysilane to the ammonia water is 5-5.3:400-410:10-10.5:2-2.5;
tetrahydrofuran, butane tetracarboxylic acid and N, N' -carbonyl diimidazole, wherein the mass ratio of the aminated titanium dioxide to the tetrahydrofuran solution is 32-35:24-26:80-85:11-13;
the mass fraction of the tetrahydrofuran solution of the N, N' -carbonyl diimidazole is 20-25%;
the particle size of the rutile type nano titanium dioxide is 50-90nm;
the mass concentration of the ammonia water is 25-28%;
the preparation of the inorganic mixed mildew preventive comprises the following steps: mixing barium metaborate, sodium metaborate and zinc oxide, performing ball milling, controlling the rotation speed during ball milling to be 300-400rpm, the ball-material ratio to be 15-20:1, and the time to be 40-50min, adding 3-aminopropyl triethoxysilane, and continuing ball milling for 1-1.5h to obtain the inorganic mixed mildew preventive;
in the preparation of the inorganic mixed mildew preventive, the mass ratio of barium metaborate, sodium metaborate, zinc oxide and 3-aminopropyl triethoxysilane is 30-35:20-25:12-15:3-3.5;
adding hydroxyl-terminated polydimethylsiloxane, simethicone and ultrafine powder into a kneader, mixing and dehydrating for 80-90min at 120-130 ℃, and cooling to room temperature to obtain a base material; adding the obtained base material, the multi-branching crosslinking promoter, the methyltrimethoxysilane, the dimethyldimethoxysilane, the 3-aminopropyl triethoxysilane, the inorganic mixed mildew inhibitor and the dibutyltin dilaurate into a high-speed stirrer to carry out high-speed stirring, controlling the vacuum degree of the high-speed stirring to be 0.08-0.09MPa and the rotating speed to be 300-350rpm, and stirring for 90-100min to obtain the high-power mildew-proof alcohol type beautifying trimming adhesive;
in the mixed material, the mass ratio of hydroxyl-terminated polydimethylsiloxane, simethicone, ultrafine powder, multi-branching crosslinking promoter, methyltrimethoxysilane, dimethyldimethoxysilane, 3-aminopropyl triethoxysilane, inorganic mixed mildew inhibitor and dibutyltin dilaurate is 140-145:14-16:20-22:13-15:6-7:2-3:6-7:1-1.2:0.4-0.5;
the viscosity of the hydroxyl-terminated polydimethylsiloxane is 50000-100000 mPa.s at 25 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the mildew resistance of the prepared beautifying trimming adhesive can be improved by adding ultrafine powder into a mixed material, and the mildew resistance grade of the prepared beautifying trimming adhesive is 0 grade;
(2) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the tearing strength of the prepared beautifying trimming adhesive can be improved by adding ultrafine powder into a mixed material, and the tearing strength of the prepared beautifying trimming adhesive is 46-48N/mm;
(3) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, the penetration resistance of the prepared beautifying trimming adhesive can be improved by adding ultrafine powder into a mixed material, and the Shore hardness A of the prepared beautifying trimming adhesive is 46-49HA;
(4) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the multi-branching crosslinking promoter is added into the mixed materials, so that the cohesiveness of the prepared beautifying trimming adhesive can be improved, the 100% stretching cohesiveness of the prepared beautifying trimming adhesive is nondestructive, and the bonding property of cold-drawn hot-pressing +/-50% is nondestructive;
(5) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the deep curing speed of the prepared beautifying trimming adhesive can be improved by adding the multi-branching crosslinking promoter into the mixed material, the curing depth of the prepared beautifying trimming adhesive is 3.2-3.4mm when the curing time is 12h, and the curing depth is 4.5-4.8mm when the curing time is 24 h;
(6) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the elasticity of the prepared beautifying trimming adhesive can be improved by adding the multi-branching crosslinking-promoting agent into the mixed material, and the elastic recovery rate of the prepared beautifying trimming adhesive is 87-91%;
(7) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, disclosed by the invention, the multi-branching crosslinking promoter is added into a mixed material, so that the oil resistance of the prepared beautifying trimming adhesive can be improved, the tensile strength of the prepared beautifying trimming adhesive is 3.1-3.4MPa, the elongation at break is 527-535%, and after the prepared beautifying trimming adhesive is completely soaked in 10w-30 engine oil for 7d at 120 ℃, the tensile strength is 3.1-3.3MPa, and the elongation at break is 522-531%;
(8) According to the preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive, the multi-branching crosslinking promoter is added into the mixed materials, so that the prepared beautifying trimming adhesive is not easy to generate oily dialyzate, and the surface of the prepared beautifying trimming adhesive is free of oily dialyzate after being placed for 100 days in an environment with the temperature of 40 ℃ and the humidity of 60%;
(9) According to the preparation method of the high-power mildew-proof dealcoholization type cosmetic edge-trimming adhesive, the dependence of extrudability and thixotropic property on temperature can be reduced by adding the ultrafine powder and the multi-branching crosslinking promoter into a mixed material, the prepared cosmetic edge-trimming adhesive has the extrudability of 250-280mL/min at the temperature of-4 ℃, the extrudability of 260-280mL/min at the temperature of 23 ℃, the extrudability of 260-280mL/min at the temperature of 40 ℃, the thixotropic index at the temperature of-4 ℃ of 5.0-5.2, the thixotropic index at the temperature of 23 ℃ of 5.1-5.4 and the thixotropic index at the temperature of 40 ℃ of 5.1-5.5.
Detailed Description
Specific embodiments of the present invention will now be described in order to provide a clearer understanding of the technical features, objects and effects of the present invention.
Example 1
A preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive specifically comprises the following steps:
1. preparing ultra-fine powder: adding 3g of superfine calcium carbonate and 130g of deionized water into a high-speed reaction kettle, carrying out ultrasonic vibration while carrying out high-speed stirring, controlling the stirring speed of the high-speed stirring to be 800rpm, stopping high-speed stirring and ultrasonic vibration after the ultrasonic vibration frequency is 20kHz and 25min, and obtaining superfine calcium carbonate suspension; adding 5g of silver nitrate, 200g of deionized water and 3g of polyvinylamine into a reaction kettle, controlling the temperature of the reaction kettle to 35 ℃, controlling the stirring speed to 200rpm, slowly adding 60g of superfine calcium carbonate suspension after stirring for 30min, controlling the adding speed of the superfine calcium carbonate suspension to 18g/min, continuing stirring for 40min after adding, then adding 0.1g of carboxymethyl chitosan and 0.08g of beta-glucan, continuing stirring and simultaneously carrying out ultraviolet irradiation, controlling the wavelength at the time of ultraviolet irradiation to 320nm, stopping ultraviolet irradiation after 4h, adding 2g of gamma-polyglutamic acid aqueous solution with the mass fraction of 4%, stirring for 45min, adding 3g of carboxymethyl chitosan aqueous solution with the mass fraction of 3%, stirring for 1.5h, centrifuging, controlling the rotating speed at the time of centrifuging to 7000rpm, controlling the time to 8min, and drying the precipitate at the temperature of 110 ℃ after centrifuging to obtain superfine powder;
the particle size of the superfine calcium carbonate is 0.05 mu m;
2. preparation of a multi-branched crosslinking promoter: adding 5g of rutile type nano titanium dioxide and 400g of deionized water into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 30 ℃, controlling the stirring speed to 180rpm, stirring for 30min, adding 10g of 3-aminopropyl triethoxysilane and 2g of ammonia water, replacing air in the closed reaction kettle with nitrogen for 2 times, heating to 40 ℃, preserving heat at 40 ℃ for 4 hours, filtering, respectively cleaning with 30mL of absolute ethyl alcohol and 30mL of deionized water, and drying at 115 ℃ to obtain aminated titanium dioxide; adding 32g of tetrahydrofuran and 24g of butane tetracarboxylic acid into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 30 ℃, controlling the stirring speed to 180rpm, using nitrogen to replace air in the closed reaction kettle for 2 times, then dropwise adding 80g of a tetrahydrofuran solution of N, N' -carbonyl diimidazole with the mass fraction of 20%, controlling the dropwise adding speed to be 3g/min, continuing stirring for 4 hours after the dropwise adding, adding 11g of aminated titanium dioxide, continuing stirring for 5 hours, centrifuging, controlling the rotating speed during centrifuging to 7000rpm for 12 minutes, washing precipitate for 2 times by using deionized water after centrifuging, and drying at 110 ℃ to obtain the multi-branching crosslinking accelerator;
the particle size of the rutile type nano titanium dioxide is 50nm;
the mass concentration of the ammonia water is 25%;
3. preparing an inorganic mixed mildew preventive: mixing 30g of barium metaborate, 20g of sodium metaborate and 12g of zinc oxide, performing ball milling, controlling the rotation speed during ball milling to 300rpm, controlling the ball-material ratio to be 15:1 and the time to be 40min, then adding 3g of 3-aminopropyl triethoxysilane, and continuing ball milling for 1h to obtain the inorganic mixed mildew preventive;
4. mixing: adding 140g of hydroxyl-terminated polydimethylsiloxane, 14g of simethicone and 20g of ultrafine powder into a kneader, mixing and dehydrating for 80min at 120 ℃, and cooling to room temperature to obtain a base material; adding the obtained base material, 13g of multi-branching crosslinking promoter, 6g of methyltrimethoxysilane, 2g of dimethyl dimethoxy silane, 6g of 3-aminopropyl triethoxy silane, 1g of inorganic mixed mildew inhibitor and 0.4g of dibutyltin dilaurate into a high-speed stirrer, stirring at a high speed, controlling the vacuum degree of the high-speed stirring to be 0.08MPa and the rotating speed to be 300rpm, and stirring for 90min to obtain the high-power mildew-proof alcohol type beautifying trimming adhesive;
the viscosity of the hydroxyl-terminated polydimethylsiloxane was 50000 mPas at 25 ℃.
Example 2
A preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive specifically comprises the following steps:
1. preparing ultra-fine powder: adding 3.5g of superfine calcium carbonate and 135g of deionized water into a high-speed reaction kettle, carrying out ultrasonic vibration while carrying out high-speed stirring, controlling the stirring speed of the high-speed stirring to 900rpm, stopping high-speed stirring and ultrasonic vibration after the ultrasonic vibration frequency is 25kHz and 30min to obtain superfine calcium carbonate suspension; adding 5.2g of silver nitrate, 210g of deionized water and 3.2g of polyvinyl amine into a reaction kettle, controlling the temperature of the reaction kettle to 38 ℃, controlling the stirring speed to 250rpm, slowly adding 62g of superfine calcium carbonate suspension after stirring for 35min, controlling the adding speed of the superfine calcium carbonate suspension to 20g/min, continuing stirring for 45min after the adding is finished, then adding 0.11g of carboxymethyl chitosan and 0.09g of beta-glucan, continuing stirring and simultaneously carrying out ultraviolet irradiation, controlling the wavelength at 350nm during ultraviolet irradiation to 4.5h, stopping ultraviolet irradiation, adding 2.5g of gamma-polyglutamic acid aqueous solution with the mass fraction of 4.5%, stirring for 50min, adding 3.5g of carboxymethyl chitosan aqueous solution with the mass fraction of 3.5%, stirring for 1.8h, centrifuging, controlling the rotating speed at 7500rpm for 9min, and drying the precipitate at 115 ℃ after the centrifuging is finished to obtain superfine powder;
the grain diameter of the superfine calcium carbonate is 0.06 mu m;
2. preparation of a multi-branched crosslinking promoter: adding 5.2g of rutile type nano titanium dioxide and 405g of deionized water into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 32 ℃, controlling the stirring speed to 200rpm, stirring for 35min, adding 10.2g of 3-aminopropyl triethoxysilane and 2.2g of ammonia water, replacing air in the closed reaction kettle with nitrogen for 2 times, heating to 42 ℃, preserving heat at 42 ℃ for 4.5h, filtering, respectively cleaning with 35mL of absolute ethanol and 35mL of deionized water, and drying at 118 ℃ to obtain aminated titanium dioxide; adding 34g of tetrahydrofuran and 25g of butane tetracarboxylic acid into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 32 ℃, controlling the stirring speed to 200rpm, using nitrogen to replace air in the closed reaction kettle for 3 times, then dropwise adding 82g of a tetrahydrofuran solution of N, N' -carbonyl diimidazole with the mass fraction of 22%, controlling the dropwise adding speed to be 3.5g/min, continuing stirring for 4.2h after the dropwise adding is finished, then adding 12g of aminated titanium dioxide, continuing stirring for 5.5h, centrifuging, controlling the rotating speed during centrifuging to 7500rpm, controlling the time to be 14min, washing a precipitate for 2 times by using deionized water after centrifuging is finished, and drying at 115 ℃ to obtain the multi-branching crosslinking promoter;
the particle size of the rutile type nano titanium dioxide is 80nm;
the mass concentration of the ammonia water is 26%;
3. preparing an inorganic mixed mildew preventive: mixing 32g of barium metaborate, 22g of sodium metaborate and 14g of zinc oxide, performing ball milling, controlling the rotation speed during ball milling to be 350rpm, controlling the ball-to-material ratio to be 18:1, and controlling the time to be 45min, then adding 3.2g of 3-aminopropyl triethoxysilane, and continuing ball milling for 1.2h to obtain the inorganic mixed mildew preventive;
4. mixing: adding 142g of hydroxy-terminated polydimethylsiloxane, 15g of simethicone and 21g of ultrafine powder into a kneader, mixing and dehydrating for 85min at 125 ℃, and cooling to room temperature to obtain a base material; adding the obtained base material, 14g of multi-branching crosslinking promoter, 6.5g of methyltrimethoxysilane, 2.5g of dimethyl dimethoxy silane, 6.5g of 3-aminopropyl triethoxy silane, 1.1g of inorganic mixed mildew inhibitor and 0.4g of dibutyltin dilaurate into a high-speed stirrer, stirring at a high speed, controlling the vacuum degree of the high-speed stirring to be 0.085MPa and the rotating speed to be 320rpm, and stirring for 95min to obtain high-power mildew-proof alcohol type beautifying trimming adhesive;
the viscosity of the hydroxyl-terminated polydimethylsiloxane was 80000 mPas at 25 ℃.
Example 3
A preparation method of high-power mildew-proof dealcoholization type beautifying trimming adhesive specifically comprises the following steps:
1. preparing ultra-fine powder: adding 4g of superfine calcium carbonate and 140g of deionized water into a high-speed reaction kettle, carrying out ultrasonic vibration while carrying out high-speed stirring, controlling the stirring speed of the high-speed stirring to be 1000rpm, stopping high-speed stirring and ultrasonic vibration after the ultrasonic vibration frequency is 30kHz and 35min, and obtaining superfine calcium carbonate suspension; adding 5.5g of silver nitrate, 220g of deionized water and 3.5g of polyvinyl amine into a reaction kettle, controlling the temperature of the reaction kettle to 40 ℃, controlling the stirring speed to 300rpm, slowly adding 65g of superfine calcium carbonate suspension after stirring for 40min, controlling the adding speed of the superfine calcium carbonate suspension to 22g/min, continuing stirring for 50min after adding, then adding 0.12g of carboxymethyl chitosan and 0.1g of beta-glucan, continuing stirring and simultaneously carrying out ultraviolet irradiation, controlling the wavelength at the ultraviolet irradiation to be 380nm, stopping ultraviolet irradiation after 5h, adding 3g of gamma-polyglutamic acid aqueous solution with the mass fraction of 5%, stirring for 55min, adding 4g of carboxymethyl chitosan aqueous solution with the mass fraction of 4%, stirring for 2h, centrifuging, controlling the rotating speed at 8000rpm for 10min, and drying the precipitate at 120 ℃ after centrifuging to obtain superfine powder;
the particle size of the superfine calcium carbonate is 0.08 mu m;
2. preparation of a multi-branched crosslinking promoter: adding 5.3g of rutile type nano titanium dioxide and 410g of deionized water into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 35 ℃, controlling the stirring speed to 220rpm, stirring for 40min, adding 10.5g of 3-aminopropyl triethoxysilane and 2.5g of ammonia water, replacing air in the closed reaction kettle with nitrogen for 3 times, heating to 45 ℃, preserving heat at 45 ℃ for 5h, filtering, respectively cleaning with 40mL of absolute ethyl alcohol and 40mL of deionized water, and drying at 120 ℃ to obtain aminated titanium dioxide; adding 35g of tetrahydrofuran and 26g of butane tetracarboxylic acid into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 35 ℃, controlling the stirring speed to 220rpm, using nitrogen to replace air in the closed reaction kettle for 3 times, then dropwise adding 85g of a 25% N, N' -carbonyl diimidazole tetrahydrofuran solution, controlling the dropwise adding speed to be 4g/min, continuing stirring for 4.5h after the dropwise adding is finished, then adding 13g of aminated titanium dioxide, continuing stirring for 6h, centrifuging, controlling the rotating speed during centrifuging to be 8000rpm, controlling the time to be 15min, washing the precipitate for 3 times by using deionized water after centrifuging is finished, and drying at 120 ℃ to obtain the multi-branching crosslinking promoter;
the particle size of the rutile type nano titanium dioxide is 90nm;
the mass concentration of the ammonia water is 28%;
3. preparing an inorganic mixed mildew preventive: mixing 35g of barium metaborate, 25g of sodium metaborate and 15g of zinc oxide, performing ball milling, controlling the rotation speed at 400rpm during ball milling, controlling the ball-material ratio at 20:1 and the time at 50min, then adding 3.5g of 3-aminopropyl triethoxysilane, and continuing ball milling for 1.5h to obtain the inorganic mixed mildew preventive;
4. mixing: 145g of hydroxy-terminated polydimethylsiloxane, 16g of simethicone and 22g of ultra-fine powder are added into a kneader, mixed and dehydrated for 90min at 130 ℃, and cooled to room temperature, thus obtaining a base material; adding the obtained base material, 15g of multi-branching crosslinking promoter, 7g of methyltrimethoxysilane, 3g of dimethyl dimethoxy silane, 7g of 3-aminopropyl triethoxy silane, 1.2g of inorganic mixed mildew inhibitor and 0.5g of dibutyltin dilaurate into a high-speed stirrer, stirring at a high speed, controlling the vacuum degree of the high-speed stirring to be 0.09MPa and the rotating speed to be 350rpm, and stirring for 100min to obtain high-power mildew-proof alcohol type beautifying trimming adhesive;
the viscosity of the hydroxyl-terminated polydimethylsiloxane at 25 ℃ is 100000 mPa.s.
Comparative example 1
The preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive in the embodiment 2 is characterized in that: the step of preparing ultrafine powder in step 1 was omitted, and 21g of ultrafine calcium carbonate having a particle size of 0.06 μm was used in the mixture in step 3 instead of the addition of 21g of ultrafine powder.
Comparative example 2
The preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive in the embodiment 2 is characterized in that: omitting the step of preparing the multi-branching crosslinking promoter in the step 2, and omitting the addition of the multi-branching crosslinking promoter in the step 3.
Test example 1
The high-power mildew-proof dealcoholization type beautifying trimming adhesive prepared in examples 1-3 and comparative examples 1-2 was tested for mildew-proof grade, tear strength, tensile strength, elongation at break, shore hardness, 100% stretching adhesion, cold-drawing hot-pressing + -50% adhesion, curing depth, elastic recovery rate, and the test results were as follows:
from the above results, it can be seen that the addition of the ultra-fine powder can improve the mildew resistance, tear strength, tensile strength, elongation at break and Shore hardness, and the multi-branching crosslinking-promoting agent can improve the cohesiveness, deep curing speed and elasticity;
the preparation of the ultrafine powder mainly comprises the steps of coating and modifying the surface of ultrafine calcium carbonate by using gamma-polyglutamic acid and carboxymethyl chitosan aqueous solution, wherein when the carboxymethyl chitosan and beta-glucan are added together, the reduction effect on silver ions is mainly achieved, the beta-glucan can play a role in synergistically reducing the silver ions, the silver ions become nano silver after reduction, an auxiliary mildew preventive is achieved, the mildew resistance of the beauty treatment edge bead rubber is improved, if the nano silver is independently added, the auxiliary mildew preventive is achieved, the nano silver is easy to agglomerate, the nano silver after agglomeration can influence the crosslinking of the beauty treatment edge bead rubber, so that the tearing strength, tensile strength, elongation at break and Shore hardness of the beauty treatment edge bead rubber are reduced, the nano silver is loaded on the ultrafine calcium carbonate, and then the coating and modifying are achieved by using gamma-polyglutamic acid and carboxymethyl chitosan aqueous solution, the dispersion of the loaded ultrafine calcium carbonate in the beauty treatment edge bead rubber is facilitated, the nano calcium carbonate can also be dispersed in the beauty treatment edge bead rubber, and the mechanical elongation of the nano calcium carbonate can be better avoided, and the beauty treatment edge bead rubber can be better prevented from being subjected to the mechanical elongation;
the added multi-branched crosslinking promoter is multi-carboxyl titanium dioxide, the compatibility between the titanium dioxide and other components of the cosmetic edge trimming adhesive can be improved through a multi-carboxyl structure, the titanium dioxide is beneficial to the dispersion of the titanium dioxide in the cosmetic edge trimming adhesive, and in addition, as the multi-carboxyl titanium dioxide has very high reactivity, the multi-carboxyl titanium dioxide can also play a role in promoting the crosslinking in the curing process of the cosmetic edge trimming adhesive, so that the crosslinking speed and the crosslinking density of the cosmetic edge trimming adhesive are improved, and the cohesiveness, the deep curing speed and the elasticity of the cosmetic edge trimming adhesive are improved.
Test example 2
The high-power mildew-proof dealcoholization type beautifying trimming adhesive test samples prepared in the examples 1-3 and the comparative examples 1-2 are completely soaked in 10w-30 engine oil, and after being soaked for 7d at 120 ℃, the tensile strength and the elongation at break of the test samples are tested, and the test results are as follows:
from the above results, it can be seen that the multi-branched crosslinking promoter can improve the oil resistance of the cosmetic edge finishing adhesive;
the added multi-branching crosslinking promoter is the multi-carboxyl titanium dioxide, so that the crosslinking density in the cosmetic edge-trimming adhesive can be improved, and the crosslinking density on the surface of the cosmetic edge-trimming adhesive can be improved, thereby avoiding the oil agent from penetrating into the cosmetic edge-trimming adhesive and damaging the interior of the cosmetic edge-trimming adhesive.
Test example 3
The high-power mildew-proof dealcoholization type beautifying trimming adhesive test samples prepared in examples 1-3 and comparative examples 1-2 were allowed to stand for 100d in an environment with a temperature of 40 ℃ and a humidity of 60%, and then were observed for oily dialyzates on the surfaces of the test samples, and the observation results were as follows:
from the above results, it can be seen that the multi-branched crosslinking promoter can prevent the cosmetic edge-trimming adhesive from producing oily dialyzate;
the added multi-branching crosslinking promoter is the multi-carboxyl titanium dioxide, so that on one hand, the crosslinking density of the surface of the cosmetic trimming adhesive can be improved, and on the other hand, a certain lubrication effect can be achieved in the preparation of the cosmetic trimming adhesive, so that the adding amount of the dimethyl silicone oil is reduced, and the precipitation of the dimethyl silicone oil is avoided.
Test example 4
The high-power mildew-proof dealcoholization type beautifying edging adhesive prepared in examples 1-3 and comparative examples 1-2 was tested according to GB/T16776-2005 standard for extrudability at-4 ℃, 23 ℃, 40 ℃ and thixotropic index at-4 ℃, 23 ℃, 40 ℃ as follows:
the thixotropic index test method comprises the following steps: testing by using a Boli flywheel viscometer, wherein a rotor is T-E95, respectively testing a viscosity value V2 at a rotating speed of 2rpm and a viscosity value V20 at 20rpm, and then calculating V2/V20 as a thixotropic index;
from the above results, it can be seen that the addition of both the ultrafine powder and the multi-branched crosslinking promoter can reduce the temperature dependence of the extrudability and thixotropic properties of the cosmetic trim;
the particle sizes of the added calcium carbonate and titanium dioxide are smaller, and the extrusion property and thixotropic property of the cosmetic edge-trimming adhesive can be improved by adding the small-particle-size additive, but the smaller the particle size is, the easier the agglomeration and the difficult the dispersion are, and the lower the temperature is, the less the dispersion of the calcium carbonate and the titanium dioxide in the cosmetic edge-trimming adhesive is, so that the dependence of the extrusion property and the thixotropic property on the temperature is increased; the superfine calcium carbonate is modified to prepare superfine powder, and the titanium dioxide is modified to prepare the multi-branching crosslinking promoter, so that the compatibility of the superfine calcium carbonate and the titanium dioxide with the cosmetic trimming glue is improved, the purpose of improving the dispersion uniformity of the interior of the cosmetic trimming glue is achieved, the addition of the small-particle-size additive with uniform dispersion can improve the fluidity and the consistency of the cosmetic trimming glue during extrusion and stirring during standing, and the extrusion property and the thixotropy of the cosmetic trimming glue are improved, and meanwhile, the dependence of the extrusion property and the thixotropy on temperature is reduced.
The percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited thereto, but it is to be understood that modifications and equivalents of some of the technical features described in the foregoing embodiments may be made by those skilled in the art, although the present invention has been described in detail with reference to the foregoing embodiments. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. The preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive is characterized by comprising the following steps of: preparing ultrafine powder, preparing a multi-branching crosslinking promoter, preparing an inorganic mixed mildew inhibitor, and mixing;
adding superfine calcium carbonate into deionized water to uniformly disperse, so as to obtain superfine calcium carbonate suspension; adding silver nitrate, deionized water and polyvinyl amine into a reaction kettle, controlling the temperature of the reaction kettle to 35-40 ℃, stirring, slowly adding superfine calcium carbonate suspension, continuing stirring after the addition is finished, then adding carboxymethyl chitosan and beta-glucan, continuing stirring, simultaneously carrying out ultraviolet irradiation, adding gamma-polyglutamic acid aqueous solution, stirring, adding carboxymethyl chitosan aqueous solution, stirring, centrifuging, and drying to obtain superfine powder;
adding rutile type nano titanium dioxide and deionized water into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 30-35 ℃, stirring, adding 3-aminopropyl triethoxysilane and ammonia water, using nitrogen to replace air in the closed reaction kettle, heating to 40-45 ℃, preserving heat for 4-5 hours at 40-45 ℃, filtering, cleaning filter residues, and drying to obtain aminated titanium dioxide; adding tetrahydrofuran and butane tetracarboxylic acid into a closed reaction kettle, controlling the temperature of the closed reaction kettle to 30-35 ℃, stirring, using nitrogen to replace air in the closed reaction kettle, then dropwise adding a tetrahydrofuran solution of N, N' -carbonyl diimidazole, continuing stirring after the dropwise adding is finished, then adding aminated titanium dioxide, continuing stirring, centrifuging, washing precipitate, and drying to obtain a multi-branching crosslinking-promoting agent;
the preparation of the inorganic mixed mildew preventive comprises the following steps: mixing barium metaborate, sodium metaborate and zinc oxide, performing ball milling, adding 3-aminopropyl triethoxysilane, and performing ball milling to obtain an inorganic mixed mildew preventive;
adding hydroxyl-terminated polydimethylsiloxane, simethicone and ultrafine powder into a kneader for mixing and dehydrating, and then cooling to room temperature to obtain a base material; adding the obtained base material, the multi-branching crosslinking promoter, the methyltrimethoxysilane, the dimethyldimethoxysilane, the 3-aminopropyl triethoxysilane, the inorganic mixed mildew inhibitor and the dibutyltin dilaurate into a high-speed stirrer, and uniformly stirring to obtain the high-power mildew-proof alcohol type beautifying trimming adhesive.
2. The method for preparing the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of ultrafine powder, the mass ratio of ultrafine calcium carbonate to deionized water in the ultrafine calcium carbonate suspension is 3-4:130-140;
the mass ratio of the silver nitrate to the deionized water to the polyvinyl amine to the superfine calcium carbonate suspension to the carboxymethyl chitosan to the beta-glucan to the gamma-polyglutamic acid aqueous solution to the carboxymethyl chitosan aqueous solution is 5-5.5:200-220:3-3.5:60-65:0.1-0.12:0.08-0.1:2-3:3-4.
3. The method for preparing the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of the ultrafine powder, the mass fraction of the gamma-polyglutamic acid aqueous solution is 4-5%;
the mass fraction of the carboxymethyl chitosan aqueous solution is 3-4%;
the adding speed of the superfine calcium carbonate suspension is 18-22g/min.
4. The method for preparing high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of ultrafine powder, the particle size of the ultrafine calcium carbonate is 0.05-0.08 μm;
the wavelength of the ultraviolet light is 320-380nm, and the time is 4-5h.
5. The method for preparing the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of the multi-branching crosslinking accelerator, the mass ratio of rutile type nano titanium dioxide to deionized water to 3-aminopropyl triethoxysilane to ammonia water is 5-5.3:400-410:10-10.5:2-2.5;
the mass ratio of tetrahydrofuran to butane tetracarboxylic acid to tetrahydrofuran solution of N, N' -carbonyl diimidazole to aminated titanium dioxide is 32-35:24-26:80-85:11-13.
6. The method for preparing the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of the multi-branching crosslinking promoter, the mass fraction of the tetrahydrofuran solution of the N, N' -carbonyl diimidazole is 20-25%;
the dropping speed of the tetrahydrofuran solution of the N, N' -carbonyl diimidazole is 3-4g/min;
the particle size of the rutile type nano titanium dioxide is 50-90nm;
the mass concentration of the ammonia water is 25-28%.
7. The method for preparing the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein in the preparation of the inorganic mixed mildew preventive, the mass ratio of barium metaborate, sodium metaborate, zinc oxide and 3-aminopropyl triethoxysilane is 30-35:20-25:12-15:3-3.5.
8. The preparation method of the high-power mildew-proof dealcoholization type beautifying trimming adhesive according to claim 1, wherein the mass ratio of hydroxyl-terminated polydimethylsiloxane, simethicone, ultrafine powder, multi-branched crosslinking accelerator, methyltrimethoxysilane, dimethyldimethoxysilane, 3-aminopropyl triethoxysilane, inorganic mixed mildew inhibitor and dibutyltin dilaurate in the mixture is 140-145:14-16:20-22:13-15:6-7:2-3:6-7:1-1.2:0.4-0.5;
the viscosity of the hydroxyl-terminated polydimethylsiloxane is 50000-100000 mPa.s at 25 ℃.
9. The method for preparing the high-power mildew-proof dealcoholized beautifying trimming adhesive according to claim 1, wherein the temperature of mixing and dehydration is 120-130 ℃ and the time is 80-90min.
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Denomination of invention: A preparation method for a high magnification anti mold and alcohol removing cosmetic edge adhesive Granted publication date: 20230915 Pledgee: Shandong Linqu Rural Commercial Bank Co.,Ltd. Pledgor: Shandong Wosai New Material Technology Co.,Ltd. Registration number: Y2024980011934 |
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