CN117229753B - Beautifying glue with night fluorescent beautifying effect - Google Patents
Beautifying glue with night fluorescent beautifying effect Download PDFInfo
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- CN117229753B CN117229753B CN202311494588.6A CN202311494588A CN117229753B CN 117229753 B CN117229753 B CN 117229753B CN 202311494588 A CN202311494588 A CN 202311494588A CN 117229753 B CN117229753 B CN 117229753B
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- strontium aluminate
- fluorescent powder
- beautifying
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- 239000003292 glue Substances 0.000 title claims abstract description 50
- 230000000694 effects Effects 0.000 title claims abstract description 41
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 82
- 239000005084 Strontium aluminate Substances 0.000 claims abstract description 72
- 239000000843 powder Substances 0.000 claims abstract description 72
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 63
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 59
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 37
- 239000011737 fluorine Substances 0.000 claims abstract description 37
- 230000003796 beauty Effects 0.000 claims abstract description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 27
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 26
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 25
- 230000003449 preventive effect Effects 0.000 claims abstract description 24
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000853 adhesive Substances 0.000 claims abstract description 12
- 230000001070 adhesive effect Effects 0.000 claims abstract description 12
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 102
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 35
- 229910052710 silicon Inorganic materials 0.000 claims description 35
- 239000010703 silicon Substances 0.000 claims description 35
- 238000002360 preparation method Methods 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 239000000243 solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 7
- KQQCTWHSWXCZHB-UHFFFAOYSA-N azane;propan-2-ol Chemical compound N.CC(C)O KQQCTWHSWXCZHB-UHFFFAOYSA-N 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- 229940089951 perfluorooctyl triethoxysilane Drugs 0.000 claims description 6
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 6
- AVYKQOAMZCAHRG-UHFFFAOYSA-N triethoxy(3,3,4,4,5,5,6,6,7,7,8,8,8-tridecafluorooctyl)silane Chemical compound CCO[Si](OCC)(OCC)CCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F AVYKQOAMZCAHRG-UHFFFAOYSA-N 0.000 claims description 6
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- GRWPYGBKJYICOO-UHFFFAOYSA-N 2-methylpropan-2-olate;titanium(4+) Chemical compound [Ti+4].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] GRWPYGBKJYICOO-UHFFFAOYSA-N 0.000 claims description 4
- JEVCLNJEBFWVPD-UHFFFAOYSA-N n-methyl-2-[[2-(methylcarbamoyl)phenyl]disulfanyl]benzamide Chemical compound CNC(=O)C1=CC=CC=C1SSC1=CC=CC=C1C(=O)NC JEVCLNJEBFWVPD-UHFFFAOYSA-N 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 2
- 238000002791 soaking Methods 0.000 abstract description 5
- 239000002537 cosmetic Substances 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 14
- 238000005034 decoration Methods 0.000 description 9
- FNWBQFMGIFLWII-UHFFFAOYSA-N strontium aluminate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Al+3].[Sr+2].[Sr+2] FNWBQFMGIFLWII-UHFFFAOYSA-N 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 6
- 239000001913 cellulose Substances 0.000 description 6
- 239000004590 silicone sealant Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000003373 anti-fouling effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 239000000314 lubricant Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical class [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 239000005083 Zinc sulfide Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000002519 antifouling agent Substances 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004313 glare Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Abstract
A beauty glue with night fluorescent beautifying effect belongs to the technical field of adhesives, and consists of alpha, omega-dihydroxy polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose, hydrophobic fumed silica, a catalyst, a cross-linking agent and a mildew preventive; the obtained beauty glue has the tensile bonding strength of 3.96-4.25 MPa at 23 ℃, the bonding breaking area of 0%, the surface drying time of 19-23 min, the curing speed of 6.28-6.54 mm/24h, the tensile strength of 2.86-3.20 MPa at 23 ℃, the tensile strength of 2.62-2.73 MPa at-40 ℃, the Shore hardness of 50-54 at 23 ℃, the Shore hardness of 55-58 at-40 ℃ and the brightness of 3.59-3.75 cd/m before water resistance and soaking 2 The brightness after 148h of soaking is 3.38-3.51 cd/m 2 。
Description
Technical Field
The invention relates to a beauty glue with night fluorescent beautifying effect, belonging to the technical field of high polymer materials.
Background
The beautifying glue is mainly used for home decoration and beauty, is an upgrade and optimization of traditional glass glue or silicone glue in terms of material property, and has the characteristics of stain resistance, easy cleaning, antibiosis, mildew resistance, high tensile strength and the like. The commercial beauty glue can be divided into dealcoholized beauty glue and ketoxime-removed beauty glue according to the difference of release small molecules during solidification. The dealcoholized cosmetic glue releases small molecular substances generally alcohols such as methanol, ethanol (commonly called alcohol) and the like during solidification; the ketoxime-removing type cosmetic glue generally releases small molecular substances such as ketoxime and the like during solidification. Compared with alcohols small molecules, the serious hazard of ketoxime substances to human bodies is already recognized in the industry, so dealcoholized cosmetic adhesives are more and more favored in the market. The dealcoholized cosmetic glue products on the market at present have quite excellent performance, are rich and colorful in color, and can well improve the texture and the aesthetic degree of interior decoration, but with the vigorous development of fluorescent materials and the increasingly high standards of people on the aesthetic aspect of home decoration, the cosmetic glue products with night fluorescent beautifying effect are attracting attention.
The night fluorescent material needs to have the function of continuously emitting light in the dark, the long-afterglow fluorescent powder can meet the requirement, the traditional long-afterglow fluorescent powder mainly comprises zinc sulfide series, but the zinc sulfide fluorescent powder is easy to decompose, has short afterglow time and certain radioactivity, and is not suitable for household use. The rare earth strontium aluminate fluorescent powder has high fluorescence intensity, long afterglow time, no radioactivity, no toxicity and no harm, and is very suitable for the beauty glue for home decoration. Despite the advantages of rare earth strontium aluminate fluorescent powder, the defect of easy hydrolysis still affects the lasting fluorescence performance, and particularly when the rare earth strontium aluminate fluorescent powder is used for indoor decoration cosmetic glue, the waterproof performance of the cosmetic glue and the waterproof performance of the rare earth strontium aluminate fluorescent powder doped in the kitchen and the bathroom are more strictly required.
Chinese patent CN110229647a discloses a fluorescent silicone sealant for glass decoration, which is characterized in that the transparency reaches 70-85%, and comprises the following raw materials in parts by weight: hydroxy-terminated dimethylsiloxane: 85-110 parts of plasticizer: 10-25 parts of a lubricant; silica: 10-25 parts of a lubricant; fluorescent powder: 0.1-2 parts; crosslinking agent: 6-9 parts; catalyst: 0.01 to 0.3 part of the silicone sealant is adopted for bonding, and the silicone sealant has the effect of transparent fluorescent glare under the irradiation of lamplight after use. The patent does not specify which type of phosphor is used, and how water resistance is not very exact. Similar silicone adhesive with fluorescent function, for example, chinese patent CN103937443A discloses fluorescent anti-fouling silicone sealant for ceramic tile caulking and a preparation method thereof, wherein the raw material formula comprises the following components in parts by weight: 80-120 parts of base polymer, 0-30 parts of plasticizer, 0-30 parts of antifouling agent, 20-60 parts of active calcium carbonate, 5-20 parts of fumed silica, 5-20 parts of fluorescent additive, 0.1-3 parts of mildew preventive, 1-10 parts of cross-linking agent, 0.5-10 parts of catalyst and 1-5 parts of tackifier. The patent does not specify specific components and types of fluorescent additives, and the fluorescent antifouling silicone sealant disclosed in the patent has good water resistance and hydrophobicity, but does not disclose whether the fluorescent function can last for a long time in a humid environment.
The above can show that the rare earth strontium aluminate fluorescent powder has no mature technical scheme for the household decoration and beauty glue, and in view of the special poor water resistance of the fluorescent powder, the industry needs to find an effective technical method to overcome the difficult problem so as to promote the material with excellent fluorescent performance to bring more beautiful feeling to the household decoration industry.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention provides a beautifying adhesive with night fluorescent beautifying effect, which realizes the following aims: the fluorescent cosmetic glue for home decoration has the advantages of good water resistance, strong flexibility, lasting fluorescent property and excellent adhesive force.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the specific formula of the beauty glue with the night fluorescent beautifying effect comprises the following components in parts by weight:
70-100 parts of alpha, omega-dihydroxy polydimethylsiloxane,
5-9 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
3-11 parts of fluorine modified nano cellulose,
2-6 parts of hydrophobic fumed silica,
1-3 parts of catalyst,
3-6 parts of cross-linking agent,
0.5-0.8 parts of mildew inhibitor;
the particle size of the hydrophobic fumed silica is 20-100 nm;
the catalyst is one of isopropyl titanate and tert-butyl titanate;
the cross-linking agent is one of methyltrimethoxysilane and methyltriethoxysilane;
the mildew preventive is one of N, N-dimethyl-N '-phenyl (fluorodichloro methyl thio) sulfonamide and 2,2' -dithiobis (N-methylbenzamide);
the following is a further improvement of the above technical scheme:
step 1, preparation of fluorine modified nanocellulose
Mixing nano cellulose, perfluorooctyl triethoxysilane, 3-isocyanatopropyl triethoxysilane and dimethyl sulfoxide, uniformly dispersing the nano cellulose by strong stirring, controlling the stirring speed to be 200-500 r/min, heating to 170-200 ℃, carrying out reflux reaction for 5-8 hours, cooling to room temperature, filtering, washing the filtered solid with deionized water for 3-5 times, and drying at 80-95 ℃ for 6-9 hours to obtain fluorine modified nano cellulose;
the length of the nanocellulose is 50-100 nm, and the width of the nanocellulose is 5-20 nm.
Step 2, preparation of organic silicon coated rare earth strontium aluminate fluorescent powder
Adding isopropanol and rare earth strontium aluminate fluorescent powder into a flask, controlling the temperature to be 50-80 ℃, stirring at the speed of 600-1000 r/min, simultaneously dropwise adding an isopropanol solution of organic silicon and an ammonia isopropanol mixed solution into the flask, controlling the dropwise adding speeds of the two liquids to be 8-15 mL/min, continuing to react for 1-4 hours after dropwise adding, stopping reacting, cooling to room temperature, vacuum-filtering the liquid after the reaction is completed, washing the filtrate with absolute ethyl alcohol for 3-5 times, putting into an oven, and drying at the temperature of 75-95 ℃ for 1-2 hours to obtain the organic silicon coated rare earth strontium aluminate fluorescent powder;
the mass ratio of the isopropanol to the rare earth strontium aluminate fluorescent powder is 10-20:3;
the particle size of the rare earth strontium aluminate fluorescent powder is 600-1000 meshes;
the isopropyl alcohol solution of the organic silicon consists of ethyl orthosilicate, methyltriethoxysilane and isopropyl alcohol, wherein the mass ratio of the ethyl orthosilicate to the methyltriethoxysilane to the isopropyl alcohol is 1-6:2-9:30-50;
the addition amount of the isopropanol solution of the organic silicon is 1-1.5 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass ratio of the ammonia water to the isopropanol is 10-25:100;
the addition amount of the ammonia water isopropanol mixed solution is 1-1.3 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass concentration of the ammonia water is 10-20%.
Step 3, preparation of the beauty glue
According to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 20000-35000 r/min for 3-7 hours at a high speed, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1-2 hours, discharging and filling, and sealing by nitrogen filling to obtain the beautifying adhesive with the night fluorescent beautifying effect.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the invention, the surface of the nano-cellulose is modified by using perfluorooctyl triethoxysilane and 3-isocyanatopropyl triethoxysilane, so that the hydrophilic nano-cellulose is changed into surface with strong hydrophobicity, fluorine with strong hydrophobicity is introduced into the organosilicon body of the cosmetic glue by the modification, the overall hydrophobicity of the matrix is improved, the strontium aluminate fluorescent powder can be effectively protected from hydrolysis reaction caused by the influence of moisture, and in addition, the strength and toughness of the organosilicon matrix are improved by the fluorine modified nano-cellulose;
2. according to the invention, the strontium aluminate fluorescent powder is effectively coated by two substances of tetraethoxysilane and methyltriethoxysilane, and the treatment not only enhances the hydrophobicity of the surface of the strontium aluminate fluorescent powder and reduces the possibility of hydrolysis reaction, but also promotes the dispersion uniformity of the strontium aluminate fluorescent powder in the organosilicon matrix of the beauty gel, thereby improving the fluorescence effect of the beauty gel and prolonging the service life of the continuous fluorescence performance;
3. the beauty glue with night fluorescent beautifying effect has the tensile bonding strength of 3.96-4.25 MPa at 23 ℃, bonding failure area of 0%, surface drying time of 19-23 min, curing speed of 6.28-6.54 mm/24h, tensile strength of 2.86-3.20 MPa at 23 ℃, tensile strength of 2.62-2.73 MPa at-40 ℃, shore hardness of 50-54 at-40 ℃, and brightness of 3.59-3.75 cd/m before water resistance soaking 2 The brightness after 148h of soaking is 3.38-3.51 cd/m 2 。
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and explanation only and is not intended to limit the present invention.
Example 1: beautifying glue with night fluorescent beautifying effect
Step 1, preparation of fluorine modified nanocellulose
Mixing nano cellulose, perfluorooctyl triethoxysilane, 3-isocyanatopropyl triethoxysilane and dimethyl sulfoxide, stirring strongly to uniformly disperse the nano cellulose, controlling stirring speed to be 350 r/min, heating to 180 ℃, carrying out reflux reaction for 7 hours, cooling to room temperature, filtering, washing the filtered solid with deionized water for 4 times, and drying at 90 ℃ for 8 hours to obtain fluorine modified nano cellulose;
the length of the nanocellulose is 80nm, and the width of the nanocellulose is 10nm.
Step 2, preparation of organic silicon coated rare earth strontium aluminate fluorescent powder
Adding isopropanol and rare earth strontium aluminate fluorescent powder into a flask, controlling the temperature to be 60 ℃, stirring at 900 revolutions per minute, simultaneously dropwise adding an isopropanol solution of organic silicon and an ammonia isopropanol mixed solution into the flask, controlling the dropwise adding rate of the two liquids to be 12mL/min, continuing to react for 3 hours after the dropwise adding is finished, stopping reacting, cooling to room temperature, carrying out vacuum suction filtration on the liquid after the reaction is finished, washing filtrate with absolute ethyl alcohol for 4 times, putting into a baking oven, and drying at 80 ℃ for 1.6 hours to obtain the organic silicon coated rare earth strontium aluminate fluorescent powder;
the mass ratio of the isopropanol to the rare earth strontium aluminate fluorescent powder is 17:3;
the particle size of the rare earth strontium aluminate fluorescent powder is 800 meshes;
the isopropyl alcohol solution of the organic silicon consists of ethyl orthosilicate, methyltriethoxysilane and isopropyl alcohol, and the mass ratio of the ethyl orthosilicate to the methyltriethoxysilane to the isopropyl alcohol is 4:7:45;
the adding amount of the isopropyl alcohol solution of the organic silicon is 1.3 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass ratio of the ammonia water to the isopropanol is 17:100;
the addition amount of the ammonia water isopropanol mixed solution is 1.2 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass concentration of the ammonia water is 14%.
Step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
90 parts of alpha, omega-dihydroxy polydimethylsiloxane,
8 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
7 parts of fluorine modified nano-cellulose,
5 parts of hydrophobic fumed silica,
2 parts of catalyst,
5 parts of cross-linking agent,
0.6 parts of mildew preventive;
the particle size of the hydrophobic fumed silica is 60nm;
the catalyst is isopropyl titanate;
the cross-linking agent is methyltrimethoxysilane;
the mildew preventive is N, N-dimethyl-N' -phenyl (fluorodichloro methyl thio) sulfonamide;
according to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 30000 revolutions per minute for 6 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1.6 hours, discharging and filling, and sealing by nitrogen to obtain the beautifying adhesive with the night fluorescent beautifying effect.
Example 2: beautifying glue with night fluorescent beautifying effect
Step 1, preparation of fluorine modified nanocellulose
Mixing nano cellulose, perfluorooctyl triethoxysilane, 3-isocyanatopropyl triethoxysilane and dimethyl sulfoxide, stirring strongly to uniformly disperse the nano cellulose, controlling the stirring speed to be 200 r/min, heating to 170 ℃, carrying out reflux reaction for 5 hours, cooling to room temperature, filtering, washing the filtered solid with deionized water for 3 times, and drying at 80 ℃ for 6 hours to obtain fluorine modified nano cellulose;
the length of the nanocellulose is 50nm, and the width is 5nm.
Step 2, preparation of organic silicon coated rare earth strontium aluminate fluorescent powder
Adding isopropanol and rare earth strontium aluminate fluorescent powder into a flask, controlling the temperature to be 50 ℃, stirring at the speed of 600 revolutions per minute, simultaneously dropwise adding an isopropanol solution of organic silicon and an ammonia isopropanol mixed solution into the flask, controlling the dropwise adding speed of 8mL/min of both liquids, continuing to react for 1 hour after the dropwise adding is finished, stopping reacting, cooling to room temperature, carrying out vacuum suction filtration on the liquid after the reaction is finished, washing filtrate with absolute ethyl alcohol for 3 times, putting into a baking oven, and drying at the temperature of 75 ℃ for 1 hour to obtain the organic silicon coated rare earth strontium aluminate fluorescent powder;
the mass ratio of the isopropanol to the rare earth strontium aluminate fluorescent powder is 10:3;
the particle size of the rare earth strontium aluminate fluorescent powder is 600 meshes;
the isopropyl alcohol solution of the organic silicon consists of ethyl orthosilicate, methyltriethoxysilane and isopropyl alcohol, and the mass ratio of the ethyl orthosilicate to the methyltriethoxysilane to the isopropyl alcohol is 1:2:30;
the adding amount of the isopropyl alcohol solution of the organic silicon is 1 time of the mass of the rare earth strontium aluminate fluorescent powder;
the mass ratio of the ammonia water to the isopropanol is 10:100;
the addition amount of the ammonia isopropanol mixed solution is 1 time of the mass of the rare earth strontium aluminate fluorescent powder;
the mass concentration of the ammonia water is 10%.
Step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
70 parts of alpha, omega-dihydroxy polydimethylsiloxane,
5 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
3 parts of fluorine modified nano cellulose,
2 parts of hydrophobic fumed silica,
1 part of catalyst,
3 parts of cross-linking agent,
0.5 parts of mildew preventive;
the particle size of the hydrophobic fumed silica is 20nm;
the catalyst is tert-butyl titanate;
the cross-linking agent is methyltriethoxysilane;
the mildew preventive is 2,2' -dithiobis (N-methylbenzamide);
according to a specific formula with night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 20000 revolutions per minute for 3 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1 hour, discharging, filling, and sealing by nitrogen to obtain the beautifying adhesive with night fluorescent beautifying effect.
Example 3: beautifying glue with night fluorescent beautifying effect
Step 1, preparation of fluorine modified nanocellulose
Mixing nano cellulose, perfluorooctyl triethoxysilane, 3-isocyanatopropyl triethoxysilane and dimethyl sulfoxide, stirring strongly to uniformly disperse the nano cellulose, controlling the stirring speed to be 500 r/min, heating to 200 ℃, carrying out reflux reaction for 8 hours, cooling to room temperature, filtering, washing the filtered solid with deionized water for 5 times, and drying at 95 ℃ for 9 hours to obtain fluorine modified nano cellulose;
the length of the nanocellulose is 100nm, and the width of the nanocellulose is 20nm.
Step 2, preparation of organic silicon coated rare earth strontium aluminate fluorescent powder
Adding isopropanol and rare earth strontium aluminate fluorescent powder into a flask, controlling the temperature to be 80 ℃, stirring at the speed of 1000 revolutions per minute, simultaneously dropwise adding an isopropanol solution of organic silicon and an ammonia isopropanol mixed solution into the flask, controlling the dropwise adding speed of both liquids to be 15mL/min, continuing to react for 4 hours after dropwise adding is finished, stopping reacting, cooling to room temperature, carrying out vacuum suction filtration on the liquid after the reaction is finished, washing filtrate with absolute ethyl alcohol for 5 times, putting into a baking oven, and drying at the temperature of 95 ℃ for 2 hours to obtain the organic silicon coated rare earth strontium aluminate fluorescent powder;
the mass ratio of the isopropanol to the rare earth strontium aluminate fluorescent powder is 20:3;
the particle size of the rare earth strontium aluminate fluorescent powder is 1000 meshes;
the isopropyl alcohol solution of the organic silicon consists of tetraethoxysilane, methyltriethoxysilane and isopropyl alcohol, and the mass ratio of the tetraethoxysilane to the methyltriethoxysilane to the isopropyl alcohol is 6:9:50;
the addition amount of the isopropyl alcohol solution of the organic silicon is 1.5 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass ratio of the ammonia water to the isopropanol is 25:100;
the addition amount of the ammonia water isopropanol mixed solution is 1.3 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass concentration of the ammonia water is 20%.
Step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
100 parts of alpha, omega-dihydroxy polydimethylsiloxane,
9 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
11 parts of fluorine modified nano-cellulose,
6 parts of hydrophobic fumed silica,
3 parts of catalyst,
6 parts of cross-linking agent,
0.8 parts of mildew preventive;
the particle size of the hydrophobic fumed silica is 100nm;
the catalyst is tert-butyl titanate;
the cross-linking agent is methyltriethoxysilane;
the mildew preventive is N, N-dimethyl-N' -phenyl (fluorodichloro methyl thio) sulfonamide;
according to a specific formula with night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 35000 r/min for 7 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 2 hours, discharging, filling, and sealing by nitrogen to obtain the beautifying adhesive with night fluorescent beautifying effect.
Comparative example 1: based on the example 1, the preparation of the fluorine modified nanocellulose in the step 1 and the preparation of the beauty gel in the step 3 are not carried out, and the equivalent of 7 parts of fluorine modified nanocellulose is replaced by 7 parts of alpha, omega-dihydroxypolydimethylsiloxane, and the specific operation is as follows:
step 1, preparation of fluorine modified nanocellulose is not carried out;
step 2, the operation is the same as in example 1;
step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
97 parts of alpha, omega-dihydroxy polydimethylsiloxane,
8 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
5 parts of hydrophobic fumed silica,
2 parts of catalyst,
5 parts of cross-linking agent,
0.6 parts of mildew preventive;
the particle size of the hydrophobic fumed silica is 60nm;
the catalyst is isopropyl titanate;
the cross-linking agent is methyltrimethoxysilane;
the mildew preventive is N, N-dimethyl-N' -phenyl (fluorodichloro methyl thio) sulfonamide;
according to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 30000 revolutions per minute for 6 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1.6 hours, discharging and filling, and sealing by nitrogen to obtain the beautifying adhesive with the night fluorescent beautifying effect.
Comparative example 2: based on the example 1, the preparation of the fluorine modified nanocellulose in the step 1 is not carried out, and in the preparation of the fluorine modified nanocellulose in the step 3 and the beauty glue, the equivalent of 7 parts of fluorine modified nanocellulose is replaced by 7 parts of nanocellulose, and the specific operation is as follows:
step 1, preparation of fluorine modified nanocellulose is not carried out;
step 2, the operation is the same as in example 1;
step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
90 parts of alpha, omega-dihydroxy polydimethylsiloxane,
8 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
7 parts of nano cellulose,
5 parts of hydrophobic fumed silica,
2 parts of catalyst,
5 parts of cross-linking agent,
0.6 parts of mildew preventive;
the length of the nanocellulose is 80nm, and the width of the nanocellulose is 10nm;
the particle size of the hydrophobic fumed silica is 60nm;
the catalyst is isopropyl titanate;
the cross-linking agent is methyltrimethoxysilane;
the mildew preventive is N, N-dimethyl-N' -phenyl (fluorodichloro methyl thio) sulfonamide;
according to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 30000 revolutions per minute for 6 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1.6 hours, discharging and filling, and sealing by nitrogen to obtain the beautifying adhesive with the night fluorescent beautifying effect.
Comparative example 3: based on the embodiment 1, the preparation of the organic silicon coated rare earth strontium aluminate fluorescent powder in the step 2 is not carried out, and in the preparation of the organic silicon coated rare earth strontium aluminate fluorescent powder in the step 3 and the beauty glue, the 8 parts of organic silicon coated rare earth strontium aluminate fluorescent powder is replaced by 8 parts of rare earth strontium aluminate fluorescent powder in equal quantity, and the specific operation is as follows:
step 1, the operation is the same as in example 1;
step 2, preparing the organic silicon coated rare earth strontium aluminate fluorescent powder is not carried out;
step 3, preparation of the beauty glue
The specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
90 parts of alpha, omega-dihydroxy polydimethylsiloxane,
8 parts of rare earth strontium aluminate fluorescent powder,
7 parts of fluorine modified nano-cellulose,
5 parts of hydrophobic fumed silica,
2 parts of catalyst,
5 parts of cross-linking agent,
0.6 parts of mildew preventive;
the particle size of the rare earth strontium aluminate fluorescent powder is 800 meshes;
the particle size of the hydrophobic fumed silica is 60nm;
the catalyst is isopropyl titanate;
the cross-linking agent is methyltrimethoxysilane;
the mildew preventive is N, N-dimethyl-N' -phenyl (fluorodichloro methyl thio) sulfonamide;
according to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 30000 revolutions per minute for 6 hours, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1.6 hours, discharging and filling, and sealing by nitrogen to obtain the beautifying adhesive with the night fluorescent beautifying effect.
Performance test:
the following performance tests were performed on the beauty gel with night fluorescent beautification obtained in examples 1, 2 and 3 and comparative examples 1, 2 and 3:
1. stretch-bonding: tensile bond strength and bond failure area at 23 ℃ were tested with reference to GB/T16776-2005;
2. surface drying time: reference GB/T13477.3-2017 test;
3. curing speed: reference GB/T13477.3-2017 test;
4. tensile strength: tensile strength at 23 ℃ and-40 ℃ was tested with reference to GB/T528-2009;
5. shore hardness: shore hardness at 23 ℃ and-40 ℃ is tested by referring to GB/T531.1-2008;
6. water resistance: coating the beauty glue obtained in 3 examples and 3 comparative examples on an aluminum alloy substrate, drying at normal temperature for 72 hours to obtain a corresponding beauty glue sample, irradiating the sample with a common 40-watt fluorescent lamp for 20 minutes, turning off the power supply, testing the luminous brightness after the power supply is turned off for 10 minutes, then putting the beauty glue sample into clear water for soaking for 148 hours, taking out the sample for naturally airing, irradiating the sample with the common 40-watt fluorescent lamp for 20 minutes, and testing the luminous brightness of the sample after the power supply is turned off for 10 minutes;
the specific test results are shown in Table 1:
as can be seen from the data in table 1, the comparative example 1 does not contain fluorine modified nanocellulose, the tensile adhesion, the surface drying time and the curing speed are not greatly different from those of the three examples, the tensile strength is obviously reduced, the fluorine modified nanocellulose has obvious enhancement effect on the beauty treatment gel, the shore hardness comparative example 1 is not greatly different from the examples, the water resistance comparative example 1 is obviously lower than that of the three examples, and the fluorine modified nanocellulose has obvious effect on improving the overall hydrophobicity of the beauty treatment gel; the direct addition of nanocellulose in comparative example 2 greatly reduces the tensile adhesion, is far lower than that of three examples, the surface drying time is prolonged, the curing speed is reduced, the tensile strength is reduced, the Shore hardness is increased, the direct addition of nanocellulose has negative effects on all properties of the cosmetic glue, the water resistance of comparative example 2 is far worse than that of three examples, the nanocellulose has poor compatibility with organosilicon matrix in the cosmetic glue, the nanocellulose is a strong polar substance, water is easy to absorb, and the negative effects on the whole cosmetic glue matrix are too great without surface hydrophobicity modification; the strontium aluminate phosphor of comparative example 3 does not coat and the tensile adhesion becomes poor, probably because the strontium aluminate phosphor does not coat, the dispersion uniformity in the silicone matrix of the cosmetic gel becomes poor, the tensile adhesion of the cosmetic gel is negatively affected, the surface drying time and the curing speed of comparative example 3 are not significantly different from those of the examples, and the tensile strength is far worse than those of the three examples, which indicates that the strontium aluminate phosphor does not coat has a great influence on the dispersion in the silicone matrix of the cosmetic gel, the shore hardness of comparative example 3 is increased, the toughness of the silicone matrix of the cosmetic gel is affected by the strontium aluminate phosphor does not coat, the water resistance of comparative example 3 is worst, the strontium aluminate phosphor does not coat and is easily hydrolyzed, and the fluorescence performance of the cosmetic gel is severely reduced.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (3)
1. A beautifying glue with night fluorescent beautifying effect is characterized in that:
the specific formula of the beautifying glue with night fluorescent beautifying effect comprises the following components in parts by weight:
70-100 parts of alpha, omega-dihydroxy polydimethylsiloxane,
5-9 parts of organic silicon coated rare earth strontium aluminate fluorescent powder,
3-11 parts of fluorine modified nano cellulose,
2-6 parts of hydrophobic fumed silica,
1-3 parts of catalyst,
3-6 parts of cross-linking agent,
0.5-0.8 parts of mildew inhibitor;
the preparation method of the fluorine modified nanocellulose comprises the following steps: mixing nano cellulose, perfluorooctyl triethoxysilane, 3-isocyanatopropyl triethoxysilane and dimethyl sulfoxide, uniformly dispersing the nano cellulose by strong stirring, controlling the stirring speed to be 200-500 r/min, heating to 170-200 ℃, carrying out reflux reaction for 5-8 hours, cooling to room temperature, filtering, washing the filtered solid with deionized water for 3-5 times, and drying at 80-95 ℃ for 6-9 hours to obtain fluorine modified nano cellulose;
the length of the nanocellulose is 50-100 nm, and the width of the nanocellulose is 5-20 nm;
the preparation method of the organosilicon coated rare earth strontium aluminate fluorescent powder comprises the following steps: adding isopropanol and rare earth strontium aluminate fluorescent powder into a flask, controlling the temperature to be 50-80 ℃, stirring at the speed of 600-1000 r/min, simultaneously dropwise adding an isopropanol solution of organic silicon and an ammonia isopropanol mixed solution into the flask, controlling the dropwise adding speeds of the two liquids to be 8-15 mL/min, continuing to react for 1-4 hours after dropwise adding, stopping reacting, cooling to room temperature, vacuum-filtering the liquid after the reaction is completed, washing the filtrate with absolute ethyl alcohol for 3-5 times, putting into a baking oven, and drying at the temperature of 75-95 ℃ for 1-2 hours to obtain the organic silicon coated rare earth strontium aluminate fluorescent powder;
the mass ratio of the isopropanol to the rare earth strontium aluminate fluorescent powder is 10-20:3;
the particle size of the rare earth strontium aluminate fluorescent powder is 600-1000 meshes;
the isopropyl alcohol solution of the organic silicon consists of ethyl orthosilicate, methyltriethoxysilane and isopropyl alcohol, wherein the mass ratio of the ethyl orthosilicate to the methyltriethoxysilane to the isopropyl alcohol is 1-6:2-9:30-50;
the addition amount of the isopropanol solution of the organic silicon is 1-1.5 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass ratio of the ammonia water to the isopropanol is 10-25:100;
the addition amount of the ammonia water isopropanol mixed solution is 1-1.3 times of the mass of the rare earth strontium aluminate fluorescent powder;
the mass concentration of the ammonia water is 10-20%.
2. The beauty gel with night fluorescent beautification function according to claim 1, characterized in that:
the particle size of the hydrophobic fumed silica is 20-100 nm;
the catalyst is one of isopropyl titanate and tert-butyl titanate;
the cross-linking agent is one of methyltrimethoxysilane and methyltriethoxysilane;
the mildew preventive is one of N, N-dimethyl-N '-phenyl (fluorodichloro methyl thio) sulfonamide and 2,2' -dithiobis (N-methylbenzamide).
3. The beauty gel with night fluorescent beautification function according to claim 1, characterized in that:
the preparation method of the beauty glue comprises the following steps: according to a specific formula with the night fluorescent beautifying effect in parts by weight, adding alpha, omega-dihydroxyl polydimethylsiloxane, organosilicon coated rare earth strontium aluminate fluorescent powder, fluorine modified nanocellulose and hydrophobic fumed silica into a dispersing kettle, dispersing at a dispersing rate of 20000-35000 r/min for 3-7 hours at a high speed, adding a catalyst, a cross-linking agent and a mildew preventive, continuing dispersing for 1-2 hours, discharging and filling, and sealing by nitrogen filling to obtain the beautifying adhesive with the night fluorescent beautifying effect.
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| CN111278942A (en) * | 2017-10-26 | 2020-06-12 | 3M创新有限公司 | Compositions and methods and articles comprising silicone-based binders and cellulose nanocrystals |
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| GB625027A (en) * | 1945-06-22 | 1949-06-21 | Du Pont | Improvements in or relating to fluorescent screens |
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