CN118027744A - Oil-in-water emulsified medium oil ink and preparation method thereof - Google Patents
Oil-in-water emulsified medium oil ink and preparation method thereof Download PDFInfo
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 21
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- 239000003921 oil Substances 0.000 claims abstract description 52
- 239000002562 thickening agent Substances 0.000 claims abstract description 37
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- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 25
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 21
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- 239000004094 surface-active agent Substances 0.000 claims abstract description 18
- 239000003125 aqueous solvent Substances 0.000 claims abstract description 17
- 238000004945 emulsification Methods 0.000 claims abstract description 17
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 17
- 239000004034 viscosity adjusting agent Substances 0.000 claims abstract description 16
- 230000001804 emulsifying effect Effects 0.000 claims description 46
- 239000007788 liquid Substances 0.000 claims description 21
- 238000000227 grinding Methods 0.000 claims description 20
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 15
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- 239000007764 o/w emulsion Substances 0.000 claims description 12
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 9
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 8
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 7
- 239000004359 castor oil Substances 0.000 claims description 7
- 235000019438 castor oil Nutrition 0.000 claims description 7
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 7
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000000265 homogenisation Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical group OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- QCGOYKXFFGQDFY-UHFFFAOYSA-M 1,3,3-trimethyl-2-[3-(1,3,3-trimethylindol-1-ium-2-yl)prop-2-enylidene]indole;chloride Chemical compound [Cl-].CC1(C)C2=CC=CC=C2N(C)\C1=C\C=C\C1=[N+](C)C2=CC=CC=C2C1(C)C QCGOYKXFFGQDFY-UHFFFAOYSA-M 0.000 claims description 3
- QCDWFXQBSFUVSP-UHFFFAOYSA-N 2-phenoxyethanol Chemical compound OCCOC1=CC=CC=C1 QCDWFXQBSFUVSP-UHFFFAOYSA-N 0.000 claims description 3
- CUZKCNWZBXLAJX-UHFFFAOYSA-N 2-phenylmethoxyethanol Chemical compound OCCOCC1=CC=CC=C1 CUZKCNWZBXLAJX-UHFFFAOYSA-N 0.000 claims description 3
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims description 3
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 230000007774 longterm Effects 0.000 abstract description 10
- 239000011347 resin Substances 0.000 abstract description 7
- 229920005989 resin Polymers 0.000 abstract description 7
- 230000009467 reduction Effects 0.000 abstract description 2
- 239000000976 ink Substances 0.000 description 52
- 230000000052 comparative effect Effects 0.000 description 14
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical group OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 9
- 238000009472 formulation Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 230000000740 bleeding effect Effects 0.000 description 5
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 4
- 230000008719 thickening Effects 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 229910002016 Aerosil® 200 Inorganic materials 0.000 description 3
- IYFATESGLOUGBX-YVNJGZBMSA-N Sorbitan monopalmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O IYFATESGLOUGBX-YVNJGZBMSA-N 0.000 description 3
- 235000019445 benzyl alcohol Nutrition 0.000 description 3
- -1 dianhydride ester Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- LPMBTLLQQJBUOO-KTKRTIGZSA-N (z)-n,n-bis(2-hydroxyethyl)octadec-9-enamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)N(CCO)CCO LPMBTLLQQJBUOO-KTKRTIGZSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- 229920003081 Povidone K 30 Polymers 0.000 description 2
- 229920003082 Povidone K 90 Polymers 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
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- 239000000839 emulsion Substances 0.000 description 2
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- 238000004321 preservation Methods 0.000 description 2
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- 238000012360 testing method Methods 0.000 description 2
- WTXLVGDAKGTUEK-UHFFFAOYSA-N C(CCCCCCCC=C/CCCCCCCC)(=O)O.C=C.C=C Chemical group C(CCCCCCCC=C/CCCCCCCC)(=O)O.C=C.C=C WTXLVGDAKGTUEK-UHFFFAOYSA-N 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
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- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
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- 230000002035 prolonged effect Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention belongs to the technical field of ink, and in particular relates to oil-in-water emulsified medium-oil ink and a preparation method thereof, wherein the oil-in-water emulsified medium-oil ink comprises the following components in percentage by mass: 10-25% of dye; 25-40% of oily solvent; 30-45% of aqueous solvent; 0.5-5% of thickener; 1-3% of pH regulator; 2-3% of a surfactant; 2-5% of emulsifying agent; 0.5-2% of viscosity modifier; the thickener is a composition of fumed silica and modified oil-soluble bentonite with a mass ratio of 1-2:1; the emulsifier includes a lipophilic emulsifier and a hydrophilic emulsifier. The oil ink in the oil-in-water emulsification adopts an inorganic thickener, so that the problem of viscosity reduction after the resin molecules of the organic thickener are degraded can not occur after long-term storage; by optimizing the proportion, not only the oil-resistance property of the emulsified middle oil is improved, but also the high-low temperature resistance property of the emulsified middle oil is improved, the stability is further improved, and the long-term storage property is good.
Description
Technical Field
The invention belongs to the technical field of ink, and particularly relates to oil-in-water emulsification medium-oil ink and a preparation method thereof.
Background
The conventional ball-point pen mainly has two types, wherein the viscosity of the oil-based ball-point pen ink is high, the writing is easy to gelatinize and unclear, and the problems of poor anti-bleeding performance, ink bleeding and the like can occur by reducing the viscosity. While the neutral ball-point pen has better writing performance, but has insufficient stability or blocks the pen point, and the phenomenon of writing broken lines is prolonged. There is also provided emulsified medium oil in the market, but emulsion is easy to break, and the long-term preservation effect is poor. As in the invention patent cn201710306141.X, an acrylic thickener 940 is used to obtain a good oil-bleeding resistance and improve the stability of the ink. However, it has been found that the oil bleeding of the refill after long-term storage is poor because the acrylic resin is degraded after long-term storage, and the viscosity is lowered, resulting in poor oil bleeding resistance and poor stability. Therefore, there is a need to develop an oil-in-water emulsion type ink which is used in a ball point pen, does not bleed and can be stored for a long period of time.
Disclosure of Invention
The invention aims to solve the problems and provide an oil-in-water emulsified medium oil ink and a preparation method thereof, wherein the oil-in-water emulsified medium oil ink adopts an inorganic thickener, and the problem of viscosity reduction after long-term storage can not occur after the resin molecules of the organic thickener are degraded; by optimizing the proportion, not only the oil-resistance property of the emulsified middle oil is improved, but also the high-low temperature resistance property of the emulsified middle oil is improved, the stability is further improved, and the long-term storage property is good.
In order to achieve the aim, the invention provides oil-in-water emulsified medium oil ink which comprises the following components in percentage by mass: 10-25% of dye; 25-40% of oily solvent; 30-45% of aqueous solvent; 0.5-5% of thickener; 1-3% of pH regulator; 2-3% of a surfactant; 2-5% of emulsifying agent; 0.5-2% of viscosity modifier;
the thickener is a composition with the mass ratio of fumed silica to modified oil-soluble bentonite of 1-2:1;
the emulsifier includes a lipophilic emulsifier and a hydrophilic emulsifier.
According to the invention, the inorganic thickener composed of the fumed silica and the modified oil-soluble bentonite replaces the organic thickener resin, so that the problems that the organic thickener resin is degraded in molecular, the viscosity is reduced and the like after long-term storage are solved, and the addition of the organic bentonite not only plays a role in thickening, but also can prevent the wall hanging phenomenon of the printing ink; the combination of lipophilic and hydrophilic emulsifying agents is adopted, so that the emulsifying effect is further improved; the viscosity of the ink is further regulated by adding the viscosity regulator, and meanwhile, the high and low temperature resistance of the ink can be improved, so that the oil-in-water emulsion medium-oil ink is suitable in viscosity, free of oil bleeding and wall hanging, greatly improved in stability and capable of being stored for a long time.
Furthermore, in the technical scheme, the modified oil-soluble bentonite is obtained by modifying organic bentonite with castor oil, and the mass ratio of the organic bentonite to the castor oil is 3-4:0.5-1. The fumed silica has small particle size, large surface area, strong surface adsorption capacity, excellent dispersion performance, stability, thickening performance, thixotropic performance and other performances, and can be directly used, but because the surface of the fumed silica is hydrophilic and oleophobic, the fumed silica is easy to be compatible with water in emulsified medium oil during mixing, and therefore, the lipophilic modified oil-soluble bentonite is added for being matched with the fumed silica for use, the consistency of the water-oil can be regulated, and the stability is greatly improved. In addition, the organic bentonite can form gel in various organic solvents and oils, and has good thickening property, thixotropy, suspension stability, high-temperature stability, lubricity, film forming property, water resistance and chemical stability.
Further, in the above technical scheme, the dye is any one of solvent black 46, basic brilliant blue B, and basic red 12.
Further, in the above technical scheme, the oily solvent is one or more of benzyl alcohol, ethylene glycol phenyl ether and ethylene glycol benzyl ether; the aqueous solvent is one or more of deionized water, diethylene glycol, propylene glycol and glycerol.
Further, in the above technical scheme, the pH regulator is triethanolamine or diethanolamine, and the pH is 7-9.
Further, in the above technical scheme, the surfactant is one or two of dodecanol polyoxyethylene ether and tween 60.
Further, in the technical scheme, the mass ratio of the lipophilic emulsifier to the hydrophilic emulsifier is 1:1.5-2; the HLB of the lipophilic emulsifier is between 5 and 7, and the HLB of the hydrophilic emulsifier is between 12 and 15. According to the technical scheme, the HLB value and the proportion of the lipophilic emulsifier and the hydrophilic emulsifier are controlled, so that the emulsifying effect is good, the emulsifying is performed alternately in water-in-oil and oil-in-water during the emulsifying process, and finally the oil-in-water ink system is formed. Specifically, the lipophilic emulsifier can be selected from monooleate dianhydride ester and span40; the hydrophilic emulsifier can be selected from tween80, oleic acid diethanolamine, and polyoxyethylene alkylphenol.
Further, in the technical scheme, the viscosity modifier is a mixture of polyvinylpyrrolidone and dioctyl adipate in a mass ratio of 2-3:1. The polyvinylpyrrolidone is a synthetic water-soluble high molecular compound, has colloid protection, film forming property, cohesiveness, hygroscopicity, solubilization or condensation, and high-temperature stability, and can further improve the high-temperature stability of the ink; dioctyl adipate has cold resistance, low temperature softness, light resistance and other properties, and still has excellent viscosity stability at a lower temperature. According to the technical scheme, the polyvinylpyrrolidone and dioctyl adipate composite viscosity regulator is used, so that the high and low temperature resistance and the binding power of the ink can be improved, the volatilization of the ink can be prevented, and the stability is good. Specifically, polyvinylpyrrolidone may be PVP-K90, PVP-K30, PVP-K15.
The invention also provides a preparation method of the oil-in-water emulsified medium oil ink, which comprises the following specific steps:
S1, adding dye into a grinder, grinding for 20-30min, adding surfactant, and continuously grinding for 20-30min to obtain a grinding product;
s2, adding the ground product into an emulsifying kettle, adding an aqueous solvent and a hydrophilic emulsifier, starting a high-speed emulsifying machine for homogenizing and emulsifying for 20-40min to obtain uniform liquid A,
S3, adding an oily solvent and a lipophilic emulsifier into the uniform liquid A, and starting a high-speed emulsifying machine to carry out homogenizing emulsification for 30-50min to obtain uniform liquid B;
S4, adding the pH regulator into the uniform liquid B, uniformly stirring, adding the thickener, starting a high-speed emulsifying machine for homogenizing and emulsifying for 20-30min, finally adding the viscosity regulator, continuously homogenizing and emulsifying for 10-20mmin, enabling the viscosity of the oil-in-water ink in the emulsifying kettle to be 500-800mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil ink.
The invention firstly grinds the dye and the surfactant, refines the dye and improves the surface activity at the same time; then adding an aqueous solvent and a hydrophilic emulsifier for primary homogenization, so that the hydrophilic ink is dissolved first, and the lipophilic ink is homogenized and emulsified; adding an oily solvent and an oleophylic emulsifier for secondary homogenization to dissolve the oleophylic ink, and further homogenizing and emulsifying; finally, pH regulator, thickener, viscosity regulator auxiliary agent are added to regulate pH, viscosity, stability and the like, and the obtained oil-in-water emulsion oil ink has moderate viscosity of 500-800 mpa.s, good oil resistance, high and low temperature stability and long-term storage.
Further, in the above-mentioned embodiment S1, the dye is ground to a particle size of 0.2 μm or less; the emulsification and homogenization conditions are as follows: the pressure is-0.095 to-0.1 Mpa, and the rotating speed is 5000-8000r/min. In the technical scheme, emulsification and homogenization are carried out under the conditions of high rotation speed and negative pressure, so that generated bubbles can be removed, and the stability is further improved.
The invention has the beneficial effects that:
1. The invention uses the inorganic thickener composed of the fumed silica and the modified oil-soluble bentonite to replace the organic thickener resin, solves the problems that the organic thickener resin is degraded and the viscosity is reduced after long-term storage, can prevent the wall of the ink from being hung up after being used for a ball-point pen, and improves the thixotropy; through optimizing the proportion, the lipophilic and hydrophilic auxiliary agents are added in combination, so that the emulsification effect can be improved, and layering can be prevented; and a viscosity regulator resistant to high temperature, ageing and low temperature is added, so that the high and low temperature resistance, the adhesive force and the stability of the ink are further improved.
2. The preparation method of the invention comprises the steps of grinding the dye, homogenizing for many times, adjusting pH and viscosity, thereby effectively improving the uniformity and stability of the oil ink in the oil-in-water emulsification, and having simple operation method.
Detailed Description
The experimental methods in the following examples are conventional methods unless otherwise specified. The raw materials used in the following examples are all commercially available and commercially available unless otherwise specified.
The invention is described in further detail below with reference to examples:
Example 1
The oil-in-water emulsified medium oil ink comprises the following components in percentage by mass: 20% of dye; 27% of oily solvent; 40% of an aqueous solvent; 3% of a thickening agent; pH adjustor 2.5%; 2% of a surfactant; 5% of an emulsifying agent; 0.5% of viscosity modifier;
Wherein the dye is solvent black 46;
The oily solvent is benzyl alcohol and ethylene glycol phenyl ether with the mass ratio of 20:7;
the mass ratio of the water-based solvent to the deionized water to the propylene glycol is 1:3;
The thickener is a composition of fumed silica (AEROSIL 200) and modified oil-soluble bentonite with a mass ratio of 2:1; the modified oil-soluble bentonite is obtained by modifying the organic bentonite and the castor oil according to the mass ratio of 4:1;
The pH regulator is triethanolamine;
the surfactant is dodecanol polyoxyethylene ether;
the mass ratio of the lipophilic emulsifier to the hydrophilic emulsifier in the emulsifier is 1:1.5, and the lipophilic emulsifier is diethylene monooleate; the hydrophilic emulsifier is polyoxyethylene alkylphenol;
The viscosity modifier is a mixture of polyvinylpyrrolidone and dioctyl adipate with a mass ratio of 2:1, wherein the viscosity modifier is polyvinylpyrrolidone PVP-K90.
The preparation method comprises the following specific steps:
S1, adding dye into a grinder, grinding for 25min, adding surfactant, continuously grinding for 25min, and grinding until the particle size is below 0.2 mu m to obtain a grinding product;
S2, adding the ground product into an emulsifying kettle, adding an aqueous solvent and a hydrophilic emulsifier, starting a high-speed emulsifying machine, homogenizing and emulsifying for 30min under the pressure of-0.095 Mpa and the rotating speed of 6000r/min to obtain uniform liquid A,
S3, adding an oily solvent and an oleophylic emulsifier into the uniform liquid A, starting a high-speed emulsifying machine, and homogenizing and emulsifying for 40min under the pressure of-0.095 Mpa and the rotating speed of 6000r/min to obtain uniform liquid B;
S4, adding a pH regulator into the uniform liquid B, stirring uniformly, adding a thickening agent, starting a high-speed emulsifying machine to carry out homogenizing emulsification for 25min under the pressure of-0.095 Mpa and the rotating speed of 6000r/min, finally adding a viscosity regulator, continuing homogenizing emulsification for 15mmin, enabling the viscosity of the oil-in-water ink in the emulsifying kettle to be 500-800 mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil ink.
Example 2
The oil-in-water emulsified medium oil ink comprises the following components in percentage by mass: 17% of dye; an oily solvent 25%; 45% of an aqueous solvent; 3% of a thickening agent; pH adjustor 2.5%; 3% of a surfactant; 4% of an emulsifying agent; 0.5% of viscosity modifier;
Wherein the dye is basic brilliant blue B;
the oily solvent is benzyl alcohol and glycol phenyl ether with the mass ratio of 20:5;
The aqueous solvent is deionized water and propylene glycol with the mass ratio of 2:7;
The thickener is a composition of fumed silica (AEROSIL 200) and modified oil-soluble bentonite with a mass ratio of 1.5:1; the modified oil-soluble bentonite is obtained by modifying the organic bentonite and the castor oil according to the mass ratio of 3:1;
The pH regulator is diethanolamine;
The surfactant is tween60;
The mass ratio of the lipophilic emulsifier to the hydrophilic emulsifier in the emulsifier is 1:2, and the lipophilic emulsifier is span40; the hydrophilic emulsifier is;
The viscosity modifier is a mixture of polyvinylpyrrolidone and dioctyl adipate with a mass ratio of 2.5:1, wherein the viscosity modifier is polyvinylpyrrolidone PVP-K30.
The preparation method comprises the following specific steps:
s1, adding dye into a grinder, grinding for 20min, adding surfactant, continuously grinding for 30min, and grinding until the particle size is below 0.2 mu m to obtain a grinding product;
S2, adding the ground product into an emulsifying kettle, adding an aqueous solvent and a hydrophilic emulsifier, starting a high-speed emulsifying machine, homogenizing and emulsifying for 40min under the pressure of-0.1 Mpa and the rotation speed of 5000r/min to obtain uniform liquid A,
S3, adding an oily solvent and an oleophylic emulsifier into the uniform liquid A, starting a high-speed emulsifying machine, and homogenizing and emulsifying for 50min under the pressure of-0.1 Mpa and the rotating speed of 5000r/min to obtain uniform liquid B;
S4, adding a pH regulator into the uniform liquid B, stirring uniformly, adding a thickening agent, starting a high-speed emulsifying machine to carry out homogenizing emulsification for 30min under the pressure of-0.1 Mpa and the rotation speed of 5000r/min, finally adding a viscosity regulator, continuing homogenizing emulsification for 20mmin, enabling the viscosity of the oil-in-water ink in the emulsifying kettle to be 500-800 mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil ink.
Example 3
The oil-in-water emulsified medium oil ink comprises the following components in percentage by mass: dye 22%; 30% of an oily solvent; 38% of an aqueous solvent; 2.5% of a thickener; 1.5% of a pH regulator; 2% of a surfactant; 3% of an emulsifying agent; 1% of a viscosity modifier;
Wherein the dye is basic red 12;
The oily solvent is benzyl alcohol and glycol benzyl ether with the mass ratio of 2:1;
The aqueous solvent is deionized water, and the mass ratio of diethylene glycol is 4:15;
the thickener is a composition of fumed silica (AEROSIL 200) and modified oil-soluble bentonite with a mass ratio of 1:1; the modified oil-soluble bentonite is obtained by modifying the organic bentonite and the castor oil according to the mass ratio of 3:1;
The pH regulator is triethanolamine;
the surfactant is dodecanol polyoxyethylene ether;
the mass ratio of the lipophilic emulsifier to the hydrophilic emulsifier in the emulsifier is 1:1.5-2, and the lipophilic emulsifier is span40; the hydrophilic emulsifier is oleic acid diethanolamine;
The viscosity modifier is a mixture of polyvinylpyrrolidone and dioctyl adipate with a mass ratio of 3:1, wherein the viscosity modifier is polyvinylpyrrolidone PVP-K15.
The preparation method comprises the following specific steps:
s1, adding dye into a grinder, grinding for 30min, adding surfactant, continuously grinding for 20min, and grinding until the particle size is below 0.2 mu m to obtain a grinding product;
S2, adding the ground product into an emulsifying kettle, adding an aqueous solvent and a hydrophilic emulsifier, starting a high-speed emulsifying machine, homogenizing and emulsifying for 20min under the pressure of-0.095 Mpa and the rotating speed of 8000r/min to obtain uniform liquid A,
S3, adding an oily solvent and an oleophylic emulsifier into the uniform liquid A, starting a high-speed emulsifying machine, and homogenizing and emulsifying for 30min under the pressure of-0.09 Mpa and the rotating speed of 8000r/min to obtain uniform liquid B;
s4, adding a pH regulator into the uniform liquid B, stirring uniformly, adding a thickening agent, starting a high-speed emulsifying machine to carry out homogenizing emulsification for 20min under the pressure of-0.095 Mpa and the rotating speed of 8000r/min, finally adding a viscosity regulator, continuing homogenizing emulsification for 10mmin, enabling the viscosity of the oil-in-water ink in the emulsifying kettle to be 500-800 mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil ink.
Comparative example 1
The formulation and preparation method of the oil-in-water emulsified medium oil ink were the same as in example 1, except that the thickener was acrylic resin.
Comparative example 2
The formulation and preparation method of the oil-in-water emulsified medium oil ink were the same as in example 1, except that the thickener was fumed silica.
Comparative example 3
The formulation and preparation method were the same as in example 1 except that the thickener was a composition having a mass ratio of fumed silica to bentonite of 2:1.
Comparative example 4
The formulation and preparation method of the oil-in-water emulsified medium oil ink were the same as in example 1, except that the emulsifier was a hydrophilic emulsifier.
Comparative example 5
The formulation and preparation method of the oil-in-water emulsified medium oil ink were the same as in example 1, except that the emulsifier was a lipophilic emulsifier.
Comparative example 6
The oil-in-water emulsified medium oil ink comprises the following components in percentage by mass: 20% of dye; 27% of oily solvent; 40% of an aqueous solvent; 3.5% of a thickener; pH adjustor 2.5%; 2% of a surfactant; 5% of an emulsifying agent;
The other formulation and preparation method were the same as in example 1.
Comparative example 7
The formulation and preparation method of the oil-in-water emulsified medium oil ink were the same as in example 1, except that the viscosity modifier was polyvinylpyrrolidone.
Comparative example 8
The oil-in-water emulsified medium oil ink has the formula proportion as in example 1, and the preparation method is as follows: adding all the raw materials except the thickening agent into an emulsifying kettle, starting a high-speed emulsifying machine for homogenizing and emulsifying for 70min to obtain uniform liquid, adding the thickening agent, continuously emulsifying for 40min, keeping the viscosity of the oil-in-water printing ink in the kettle between 500 and 800 mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil printing ink.
Test examples
To further verify the performance of the oil-in-water emulsified inks prepared in examples 1 to 3 and comparative examples 1 to 7, the oil-in-water emulsified inks were tested in ball point pen cores (ball diameter 0.5 mm), with specific reference to the relevant methods in the QB/T1946-2018, GB/T26714-2019 standards:
The specific test results are shown in table 1:
TABLE 1
As can be seen from the results in Table 1, the oil-in-water emulsified medium oil ink obtained in examples 1-3 according to the formulation and the preparation method of the present invention has the advantages of no delamination during storage, good viscosity, good writing performance, high and low temperature resistance and good light irradiation resistance, and good preservation performance.
In comparative example 1, acrylic resin was used as a thickener, and was easily decomposed by high temperature and light irradiation, and was inferior in high temperature resistance, light resistance and writing property, and was liable to oil bleeding, and was unfavorable for storage.
In comparative examples 2 to 3, fumed silica alone or fumed silica in combination with ordinary bentonite had poor thickening effect due to the hydrophilic nature of fumed silica, and the overall performance was reduced as compared with that of example 1 of the present invention.
In comparative examples 4 to 5, only a single hydrophilic emulsifier or lipophilic emulsifier was used as the emulsifier, and the emulsification effect was poor, or water-in-oil condition was formed to affect the writing performance and stability.
In comparative examples 6 to 7, the viscosity was reduced as compared with example 1 without adding a viscosity modifier or with adding only polyvinylpyrrolidone, and the high temperature resistance and storage property of polyvinylpyrrolidone were deteriorated, and an oil-bleeding phenomenon occurred; however, the low temperature resistance of the mixture was poor although other properties were not very different by the addition of polyvinylpyrrolidone.
In comparative example 8, the preparation method was basically one-time mixing without grinding the dye, and the emulsification effect was inferior to that of the separate preparation in example 1, and there was a slight delamination phenomenon, thereby affecting the writing performance to some extent.
In conclusion, the oil-in-water emulsion oil ink obtained by optimizing the raw material formula and the proportion has good cohesiveness, writing performance and high and low temperature resistance, and good stability, and solves the problems that the viscosity, oil resistance and instability are affected due to the fact that the oil ink is easily degraded by adopting organic thickener resin molecules in the emulsion, and the oil-in-water emulsion oil ink can be stored for a long time under the conditions of high temperature and low temperature.
Finally, it should be emphasized that the foregoing description is merely illustrative of the preferred embodiments of the invention, and that various changes and modifications can be made by those skilled in the art without departing from the spirit and principles of the invention, and any such modifications, equivalents, improvements, etc. are intended to be included within the scope of the invention.
Claims (10)
1. The oil-in-water emulsified medium oil ink is characterized by comprising the following components in percentage by mass: 10-25% of dye; 25-40% of oily solvent; 30-45% of aqueous solvent; 0.5-5% of thickener; 1-3% of pH regulator; 2-3% of a surfactant; 2-5% of emulsifying agent; 0.5-2% of viscosity modifier;
the thickener is a composition with the mass ratio of fumed silica to modified oil-soluble bentonite of 1-2:1;
the emulsifier includes a lipophilic emulsifier and a hydrophilic emulsifier.
2. The oil-in-water emulsified medium oil ink as set forth in claim 1, wherein the modified oil-soluble bentonite is obtained by modifying organic bentonite with castor oil, and the mass ratio of the organic bentonite to the castor oil is 3-4:0.5-1.
3. The oil-in-water emulsion ink as claimed in claim 1, wherein the dye is any one of solvent black 46, basic brilliant blue B, and basic red 12.
4. The oil-in-water emulsion ink as claimed in claim 1, wherein the oily solvent is one or more of benzyl alcohol, ethylene glycol phenyl ether and ethylene glycol benzyl ether; the aqueous solvent is one or more of deionized water, diethylene glycol, propylene glycol and glycerol.
5. An oil-in-water emulsion ink as claimed in claim 1 wherein the pH adjuster is triethanolamine or diethanolamine and has a pH of 7 to 9.
6. The oil-in-water emulsion ink as claimed in claim 1, wherein the surfactant is one or two of dodecanol polyoxyethylene ether and tween 60.
7. An oil-in-water emulsified medium oil ink as claimed in claim 1, wherein the mass ratio of the lipophilic emulsifier to the hydrophilic emulsifier is 1:1.5-2; the HLB of the lipophilic emulsifier is between 5 and 7, and the HLB of the hydrophilic emulsifier is between 12 and 15.
8. The oil-in-water emulsion ink as claimed in claim 1, wherein the viscosity modifier is a mixture of polyvinylpyrrolidone and dioctyl adipate in a mass ratio of 2-3:1.
9. A method for preparing an oil-in-water emulsion ink as claimed in any one of claims 1 to 8, comprising the specific steps of:
S1, adding dye into a grinder, grinding for 20-30min, adding surfactant, and continuously grinding for 20-30min to obtain a grinding product;
s2, adding the ground product into an emulsifying kettle, adding an aqueous solvent and a hydrophilic emulsifier, starting a high-speed emulsifying machine for homogenizing and emulsifying for 20-40min to obtain uniform liquid A,
S3, adding an oily solvent and a lipophilic emulsifier into the uniform liquid A, and starting a high-speed emulsifying machine to carry out homogenizing emulsification for 30-50min to obtain uniform liquid B;
s4, adding the pH regulator into the uniform liquid B, uniformly stirring, adding the thickener, starting a high-speed emulsifying machine for homogenizing and emulsifying for 20-30min, finally adding the viscosity regulator, continuously homogenizing and emulsifying for 10-20mmin, enabling the viscosity of the oil-in-water ink in the emulsifying kettle to be 500-800mpa.s, and filtering to obtain the oil-in-water emulsified medium-oil ink.
10. The method for preparing an oil-in-water emulsion ink as claimed in claim 9, wherein in S1, the dye is ground to a particle size of 0.2 μm or less; the emulsification and homogenization conditions are as follows: the pressure is-0.095 to-0.1 Mpa, and the rotating speed is 5000-8000r/min.
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