CN105111805A - Preparation method of nanometer latex ink for drawing materials - Google Patents
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Abstract
The invention discloses a preparation method of nanometer latex ink for drawing materials, and belongs to the technical field of fine chemical engineering and material science. Nanometer latex color paste is prepared by adopting a polymerizable dispersing agent through miniemulsion polymerization and a pressure-reduction solvent removing method, and then the nanometer latex ink is prepared by adding related auxiliaries such as a moisturizing agent, a surface active agent and a light stabilizer. According to the prepared jet drawing latex ink, an adhesive does not need to be additionally added, jetting is fluent, colors are pure, and a jet drawing pattern has the higher color fastness. The preparation method has the advantages of being simple in production technology, low in cost, feasible in operation and the like and has a good market development prospect.
Description
Technical field
The invention discloses a kind of preparation method drawing material Nano-grade latex ink, belong to fine chemistry industry and materials science field.
Background technology
Jet ink mainly contains dye ink and paint ink according to toner classification.Dye ink color is pure, bright-colored, easy to prepare, with low cost, and its deficiency is the destruction of chemical stability and poor water resistance, easy light and oxygen.For the deficiency of dye ink, domestic and international investigator additive in dye selection and ink is selected and has done a large amount of work in exploitation, as patent CN102719113A and CN102304306A openly adopts the method for the fast light ink of special construction preparation of dyestuff respectively; Patent CN102618116A and US6641257B1 disclose in ink set, add special construction chemical assistant to improve the photostabilization of ink.
Except dye ink, paint ink is also the tinting material that air brushing is commonly used.Paint ink water-fast, photostabilization good, stable chemical performance, the pattern of air brushing can be preserved for a long time.But because paint ink is a suspension system, the stability in storage of ink is bad, and does not have bonding force between pigment and air brushing base material, how to address these problems is the focus that numerous scientific workers study always.Current, the Main promoting the fastness of paint ink has two kinds, one is add tackiness agent, linking agent or employing at ink set to have dispersion and the multi-functional dispersion agent of fixation, as patent CN200910034352, CN200910184371, CN200710024154 and patent CN201410450059; Another kind method is by proper method at surface of pigments coated polymer, and has the paint ink of nucleocapsid structure as tinting material preparation, as patent CN201410442547, CN201310494969 and CN201210486821 etc.Above-mentioned two kinds of methods cut both ways, in the market commercial paint ink mainly above-mentioned two kinds.
Nano-grade latex ink for ink-jet print is a kind of Novel spray-drawing coloured material of development in recent years, has that stability is high, jet performance good and the advantage such as bright-colored, causes the common concern of people.The preparation method of this ink mainly concentrates on emulsion polymerization, fine emulsion polymerization etc., and as patent CN103834234A adopts fine emulsion polymerization to prepare dispersed dye/emulsion particle compound pigment formulate ink, this ink may be used for the ink-jet printed of cotton fabric.Adopt the report of mini-emulsion polymerization and solvent distillation technique synergy preparation Nano-grade latex ink for ink-jet print less.Based on this, the invention discloses a kind of method preparing Nano-grade latex ink for ink-jet print of picture material, utilize mini-emulsion polymerization and solvent distillation technique synergy preparation Nano-grade latex mill base, then add the preparation of nano latex ink for ink-jet prints such as wetting Agent for Printing Inks, photostabilizer, sterilant, tensio-active agent and pH adjusting agent, the standby latex ink of this legal system has that color is pure, particle diameter is little, be evenly distributed, print the advantage that stability is high, colour fastness is high.
Summary of the invention
The object of the invention: a kind of preparation method drawing material Nano-grade latex ink is provided, with polymerizable dispersion agent for emulsifying agent, take oil-soluble colourant as coloured material, by mini-emulsion polymerization and solvent under reduced pressure distillation technique coordinate system for Nano-grade latex mill base, then with Nano-grade latex mill base for major colorants, by adding wetting Agent for Printing Inks in formula, tensio-active agent, photostabilizer, antiseptic-germicide, pH adjusting agent prepares air brushing Nano-grade latex ink for ink-jet print, when air brushing uses, emulsion particle is attached on picture material base material, oil-soluble colourant penetrate in painting canvas or drawing paper, thus obtain lovely luster, colour fastness is high, the picture material ink that resistance to migration energy is good.
Technical scheme of the present invention: by the Nano-grade latex mill base to system quality mark 10%-60%, the water-soluble cosolvent of 5-50%, 0.5%-5% tensio-active agent, 0.01-2% photostabilizer, 0.1-0.5% antiseptic-germicide, finally adds water and fills 100%, stirs 30-120min with agitator with the speed of 300-1500r/min, adjust ph, to 7-9, then obtains Nano-grade latex ink for ink-jet print with 0.5 μm of filter paper filtering.
Nano-grade latex mill base used is prepared by the method for mini-emulsion polymerization, and its concrete preparation method is the obtained aqueous phase that is dissolved in the water by the polymerisable emulsifier being 0.5-25% to monomer mass mark; To be that 10-50% oil-soluble colourant are added in the mixed solvent of monomer and solubility promoter composition to monomer mass mark, solubility promoter be 1-30% to the massfraction of monomer here, prepares oil phase; Under stirring, joined by oil phase in aqueous phase, wherein oil phase is 10-60% to the massfraction of system, stirs 10-60min, prepare pre-emulsion under 300-1500r/min stir speed (S.S.); Pre-emulsion is placed in ultrasonic cell disruptor, sand mill or high pressure microjet to process 3-120min and prepare miniemulsion; Be under the condition of 150-300r/min in stir speed (S.S.) by miniemulsion, be warmed up to 60-90 DEG C, drip initiator initiated polymerization, reaction 2-12 hour; Solubility promoter is removed in underpressure distillation, then obtains Nano-grade latex mill base with 500nm micropore filter paper filtering.
Preparation Nano-grade latex mill base polymerisable emulsifier used is one in vinyl carbinol polyoxypropylene ether phosphate, vinyl carbinol ether phosphate, Hydroxyethyl acrylate-2,4 toluene diisocyanate-monomethyl polyoxyethylene glycol, sulfonation lauryl alcohol allyl oxyglycerol butyric ester sodium salt, sulfonation lauryl alcohol methacrylic acid glycerol butyrate sodium salt, vinylbenzene dodecyl dimethyl ammonium chloride, sodium dodecyl allyl base succinate sodium sulfonate, 2-acrylamido-2-methyI-oropvD sodium sulfonate, monomaleate sulfate, mono maleate sulfonate or two kinds.
Preparation Nano-grade latex mill base monomer used is by being polymerized conventional soft monomer and hard monomer forms, and soft monomer is any one or a few in ethyl propenoate, butyl acrylate and Isooctyl acrylate monomer, and consumption accounts for the 50-80% of monomer total amount, hard monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, methylvinylether, methacrylic acid, butyl methacrylate, Rocryl 410, methacrylic acid glycol ester, glycidyl methacrylate, methacrylonitril, vinyl acetate, vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, hy-droxybutyl, propylene cyanogen, vinylbenzene, vinyl toluene, ethyl styrene, isopropyl styrene, butylstyrene, dicyclopentadiene, any one or a few of toxilic acid.
The dyestuff preparing Nano-grade latex mill base used is solvent red 27, solvent red 111, solvent of red 135, transparent red HRR, transparent red BR, transparent red B, transparent red GS, transparent red EG, transparent red FB, solvent yellow 176, solvent yellow 114, solvent yellow 98, solvent yellow 56, solvent yellow 93, solvent yellow 16, Oil Yellow R, transparent yellow 3G, transparent yellow 2G, transparent yellow HLR, transparent yellow 3GL, lemon yellow TS, lemon yellow 136, solvent orange 63, solvent orange 60, transparent orange 3G, orange 3G, transparent violet B, transparent purple R, transparent violet RR, transparent violet FBL, solvent blue 19 22, solvent blue 19 04, solvent blue 36, solvent blue 35, transparent violet 3R, transparent blue 2N, transparent blue AP, transparent blue GP, transparent blue 2B, transparent blue RR, transparent blue 3R, transparent green 5B, transparent green G, one in the black OBP of oiling.
The solubility promoter preparing Nano-grade latex mill base used is methyl alcohol, ethanol, ether, glycol dimethyl ether, ethyl acetate, methylene dichloride, chloroform, 1,1-ethylene dichloride, 1,2-ethylene dichloride, 1,1,1-trichloroethane, dithiocarbonic anhydride, Virahol, acetone, butanone, tetrahydrofuran (THF), pentane, hexanaphthene, sherwood oil, any one or a few mixture of solvent naphtha, consumption accounts for the 1-30% of monomer.
The initiator that preparation Nano-grade latex mill base adopts is any one in ammonium persulphate, Potassium Persulphate, BP, tertbutyl peroxide, peroxidized t-butyl perbenzoate or azo-bis-isobutyl cyanide, more preferably ammonium persulphate, consumption is the preferred 0.5-3% to monomer mass mark further.
The water-soluble cosolvent that preparation Nano-grade latex ink for ink-jet print adopts is ethanol, ethylene glycol, n-propyl alcohol, 1,2-propylene glycol, propyl carbinol, 1, one or more in 4-butyleneglycol, 1,6-hexylene glycol, glycol ether, Triethylene glycol, Macrogol 200, poly(oxyethylene glycol) 400, Polyethylene Glycol-600, glycerine.
The tensio-active agent that preparation Nano-grade latex ink for ink-jet print adopts is polysorbate40, polysorbate60, polysorbate65, tween 80, Triton X-10, triton x-100, class of department 20, class 40 of department, class 60 of department, class 80 of department, paregal O-10, peregal O-25.
The photostabilizer that preparation Nano-grade latex ink for ink-jet print adopts is the one in salicylate class, benzophenone, Oxamides, organo-nickel compounds class, replacement propylene cyanogen class, hindered amines, benzotriazole category, triazines.
The sterilant that preparation Nano-grade latex ink for ink-jet print adopts is the one in ethyl vanillin aldehydes, vanilla acids, imidazoles, thiazoles, anilid class, quaternary ammonium salts, two croak class, isothiazolone derivative, phenols.
The reagent of the adjust ph that preparation Nano-grade latex ink for ink-jet print adopts is the one in hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, ammoniacal liquor, triethylamine.
Beneficial effect of the present invention: adopt fine emulsion polymerization and underpressure distillation to remove solvent method and prepare Nano-grade latex mill base, solubility promoter is utilized to promote the content of Nano-grade latex mill base oil-soluble dyestuff, there is mill base production technique simple, the advantages such as operation is simple and feasible, the nano color paste of preparation has the advantages such as bright-colored, stability is high and jeting effect is good, solve the defect in air brushing dyestuff and paint ink preparation, there is market development prospect well.
Embodiment
Below by examples of implementation, set forth outstanding advantages of the present invention and distinguishing feature further, but the present invention is in no way limited to examples of implementation.
Example 1
1g vinyl carbinol polyoxypropylene ether phosphate, 0.5g vinyl carbinol ether phosphate are added dissolving 100g in water, obtained aqueous phase; 8g solvent red 111,2.5g sherwood oil, 2.5g acetone are added and is dissolved in 13g butyl acrylate, 3g isopropyl styrene and 4g Vinyl Acetate Monomer, stir, obtained oil phase; Oil phase is joined in aqueous phase under whipped state, with the speed emulsification 30min of 900r/min, processes 12min under being then placed in ultrasonic cell disrupte machine ice-water bath state and obtain O/W type miniemulsion.Then reactor is placed at O/W type miniemulsion, stir with 215r/min speed, the aqueous solution containing 0.2g ammonium persulphate is added when temperature rises to 65 DEG C, reaction 3h, cooling discharging, be placed in Rotary Evaporators 65 DEG C and boil off organic solvent, obtain Nano-grade latex mill base with 500nm millipore filtration filter paper filtering.
Get 50g Nano-grade latex mill base, add 3g n-propyl alcohol, 2g ethylene glycol, 1.5g1 successively, 2-propylene glycol, 2g propyl carbinol, 1.5g1,4-butyleneglycol, 4g Triton X-10 and 1g paregal O-10, stir 50min, by sodium bicarbonate adjust ph to 8.1 with 700r/min under agitator, filtration obtains latex ink, and the indices of ink is as table 1.Then for the stamp of painting canvas, test washing, friction and light fastness, the results are shown in Table 2.
Example 2
0.7g Hydroxyethyl acrylate-2,4 toluene diisocyanate-monomethyl polyoxyethylene glycol and 0.8g vinylbenzene dodecyl dimethyl ammonium chloride being added is dissolved in 100g water, obtained aqueous phase; 10g Oil Yellow R, 3g methylene dichloride, 2g ethyl acetate are added and is dissolved in 10g ethyl propenoate, 7g dicyclopentadiene and 3g butylstyrene monomer, stir, obtained oil phase; Oil phase is joined in aqueous phase under whipped state, with the speed emulsification 30min of 650r/min, processes 8min under being then placed in ultrasonic cell disrupte machine ice-water bath state and obtain O/W type miniemulsion.Then reactor is placed at O/W type miniemulsion, stir with 200r/min speed, the aqueous solution containing 0.2g ammonium persulphate is added when temperature rises to 70 DEG C, reaction 3h, cooling discharging, be placed in Rotary Evaporators 60 DEG C and boil off organic solvent, obtain Nano-grade latex mill base with 500nm millipore filtration filter paper filtering.
Get 50g Nano-grade latex mill base, add 3.5g ethylene glycol, 1g Macrogol 200,1.5g propyl carbinol, 2g1 successively, 4-butyleneglycol and 2g glycerine, 1.5g Triton X-10, class of 1.5g department 20 and 2g peregal O-25, stir 40min, by sodium bicarbonate adjust ph to 7.8 with 800r/min under agitator, filtration obtains latex ink, and the indices of ink is as table 1.Then for the stamp of painting canvas, test washing, friction and light fastness, the results are shown in Table 2.
Example 3
To be that 0.9g sodium dodecyl allyl base succinate sodium sulfonate and 0.6g sulfonation lauryl alcohol allyl oxyglycerol butyric ester sodium salt add and be dissolved in 100g water to monomer mass mark, obtained aqueous phase; 8g solvent blue 35,0.4g lauryl mercaptan, 2g sherwood oil, 3g ethyl acetate are added and is dissolved in 13g Isooctyl acrylate monomer, 4g vinyl acetate and 3g hy-droxybutyl monomer, stir, obtained oil phase; Oil phase is joined in aqueous phase under whipped state, with the speed emulsification 60min of 700r/min, processes 9min under being then placed in ultrasonic cell disrupte machine ice-water bath state and obtain O/W type miniemulsion.Then reactor is placed at O/W type miniemulsion, stir with 200r/min speed, the aqueous solution containing 0.25g ammonium persulphate is added when temperature rises to 70 DEG C, reaction 4h, cooling discharging, be placed in Rotary Evaporators 60 DEG C and boil off organic solvent, obtain Nano-grade latex mill base with 500nm millipore filtration filter paper filtering.
Get 50g Nano-grade latex mill base, add 3g propyl carbinol, 1g1 successively, 4-propylene glycol, 2.5g Triethylene glycol, 1.5g Polyethylene Glycol-600 and 3g glycerine, 4g Triton X-10 and 1g paregal O-10,50min is stirred with 700r/min under agitator, by sodium bicarbonate adjust ph to 7.5, filter and obtain latex ink, the indices of ink is as table 1.Then for the stamp of painting canvas, test washing, friction and light fastness, the results are shown in Table 2.
Example 4
To be that 0.3g vinylbenzene dodecyl dimethyl ammonium chloride and 1.2g2-acrylamido-2-methyI-oropvD sodium sulfonate add and be dissolved in 100g water to monomer mass mark, obtained aqueous phase; Black for 9g oiling OBP, 0.4g hexadecanol, 3g ethyl acetate, 2g sherwood oil are added and is dissolved in 12g Isooctyl acrylate monomer, 4g methacrylonitril and 4g isopropyl styrene monomer, stir, obtained oil phase; Oil phase is joined in aqueous phase under whipped state, with the speed emulsification 30min of 900r/min, processes 12min under being then placed in ultrasonic cell disrupte machine ice-water bath state and obtain O/W type miniemulsion.Then reactor is placed at O/W type miniemulsion, stir with 215r/min speed, the aqueous solution containing 0.2g ammonium persulphate is added when temperature rises to 65 DEG C, reaction 3h, cooling discharging, be placed in Rotary Evaporators 65 DEG C and boil off organic solvent, obtain Nano-grade latex mill base with 500nm millipore filtration filter paper filtering.
Get 50g Nano-grade latex mill base, add 2g ethanol, 2.5g1 successively, 2-propylene glycol, 2g propyl carbinol, 1.5g1,4-butyleneglycol and 2g glycerine, 4g Triton X-10 and 1g paregal O-10, stir 50min, by sodium bicarbonate adjust ph to 8.1 with 700r/min under agitator, filtration obtains latex ink, and the indices of ink is as table 1.Then for the stamp of painting canvas, test washing, friction and light fastness, the results are shown in Table 2.
Table 1: the indices of latex ink
Table 2: the colour fastness of stamp painting canvas
Although the present invention with preferred embodiment openly as above; but it is also not used to limit the present invention, any person skilled in the art, without departing from the spirit and scope of the present invention; all can do various changes and modification, what therefore protection scope of the present invention should define with claims is as the criterion.
Claims (7)
1. draw the preparation method of material Nano-grade latex ink for one kind, by the Nano-grade latex mill base to system quality mark 10%-60%, the water-soluble cosolvent of 5-50%, 0.5%-5% tensio-active agent, 0.01-2% photostabilizer, 0.1-0.5% antiseptic-germicide, finally add water and fill 100%, stir 30-120min with agitator with the speed of 300-1500r/min, adjust ph, to 7-9, then obtains Nano-grade latex ink for ink-jet print with 0.5 μm of filter paper filtering.
2. as claim 1, a kind of preparation method drawing material Nano-grade latex ink, described Nano-grade latex mill base is prepared by the method for mini-emulsion polymerization, and its concrete preparation method is the obtained aqueous phase that is dissolved in the water by the polymerisable emulsifier being 0.5-25% to monomer mass mark; To be that 10-50% oil-soluble colourant are added in the mixed solvent of monomer and solubility promoter composition to monomer mass mark, solubility promoter be 1-30% to the massfraction of monomer here, prepares oil phase; Under stirring, joined by oil phase in aqueous phase, wherein oil phase is 10-60% to the massfraction of system, stirs 10-60min, prepare pre-emulsion under 300-1500r/min stir speed (S.S.); Pre-emulsion is placed in ultrasonic cell disruptor, sand mill or high pressure microjet to process 3-120min and prepare miniemulsion; Be under the condition of 150-300r/min in stir speed (S.S.) by miniemulsion, be warmed up to 60-90 DEG C, drip initiator initiated polymerization, reaction 2-12 hour; Solubility promoter is removed in underpressure distillation, then obtains Nano-grade latex mill base with 500nm micropore filter paper filtering;
Described polymerisable emulsifier is one in vinyl carbinol polyoxypropylene ether phosphate, vinyl carbinol ether phosphate, Hydroxyethyl acrylate-2,4 toluene diisocyanate-monomethyl polyoxyethylene glycol, sulfonation lauryl alcohol allyl oxyglycerol butyric ester sodium salt, sulfonation lauryl alcohol methacrylic acid glycerol butyrate sodium salt, vinylbenzene dodecyl dimethyl ammonium chloride, sodium dodecyl allyl base succinate sodium sulfonate, 2-acrylamido-2-methyI-oropvD sodium sulfonate, monomaleate sulfate, mono maleate sulfonate or two kinds;
Described monomer is by being polymerized conventional soft monomer and hard monomer forms, and soft monomer is any one or a few in ethyl propenoate, butyl acrylate and Isooctyl acrylate monomer, and consumption accounts for the 50-80% of monomer total amount, hard monomer is methyl methacrylate, β-dimethyl-aminoethylmethacrylate, methylvinylether, methacrylic acid, butyl methacrylate, Rocryl 410, methacrylic acid glycol ester, glycidyl methacrylate, methacrylonitril, vinyl acetate, vinylformic acid, Hydroxyethyl acrylate, Propylene glycol monoacrylate, hy-droxybutyl, propylene cyanogen, vinylbenzene, vinyl toluene, ethyl styrene, isopropyl styrene, butylstyrene, dicyclopentadiene, any one or a few of toxilic acid,
Described dyestuff is solvent red 27, solvent red 111, solvent of red 135, transparent red HRR, transparent red BR, transparent red B, transparent red GS, transparent red EG, transparent red FB, solvent yellow 176, solvent yellow 114, solvent yellow 98, solvent yellow 56, solvent yellow 93, solvent yellow 16, Oil Yellow R, transparent yellow 3G, transparent yellow 2G, transparent yellow HLR, transparent yellow 3GL, lemon yellow TS, lemon yellow 136, solvent orange 63, solvent orange 60, transparent orange 3G, orange 3G, transparent violet B, transparent purple R, transparent violet RR, transparent violet FBL, solvent blue 19 22, solvent blue 19 04, solvent blue 36, solvent blue 35, transparent violet 3R, transparent blue 2N, transparent blue AP, transparent blue GP, transparent blue 2B, transparent blue RR, transparent blue 3R, transparent green 5B, transparent green G, one in the black OBP of oiling,
Described solubility promoter is methyl alcohol, ethanol, ether, glycol dimethyl ether, ethyl acetate, methylene dichloride, chloroform, 1,1-ethylene dichloride, 1,2-ethylene dichloride, 1,1,1-trichloroethane, dithiocarbonic anhydride, Virahol, acetone, butanone, tetrahydrofuran (THF), pentane, hexanaphthene, sherwood oil, any one or a few mixture of solvent naphtha, consumption accounts for the 1-30% of monomer;
Described initiator is any one in ammonium persulphate, Potassium Persulphate, BP, tertbutyl peroxide, peroxidized t-butyl perbenzoate or azo-bis-isobutyl cyanide, more preferably ammonium persulphate, consumption is the preferred 0.5-3% to monomer mass mark further.
3. as claim 1, a kind of preparation method drawing material Nano-grade latex ink, described water-soluble cosolvent is ethanol, ethylene glycol, n-propyl alcohol, 1,2-propylene glycol, propyl carbinol, 1, one or more in 4-butyleneglycol, 1,6-hexylene glycol, glycol ether, Triethylene glycol, Macrogol 200, poly(oxyethylene glycol) 400, Polyethylene Glycol-600, glycerine.
4. as claim 1, a kind of preparation method drawing material Nano-grade latex ink, described tensio-active agent is polysorbate40, polysorbate60, polysorbate65, tween 80, Triton X-10, triton x-100, class of department 20, class 40 of department, class 60 of department, class 80 of department, paregal O-10, peregal O-25.
5. as claim 1, draw a preparation method for material Nano-grade latex ink, described photostabilizer is the one in salicylate class, benzophenone, Oxamides, organo-nickel compounds class, replacement propylene cyanogen class, hindered amines, benzotriazole category, triazines.
6., as claim 1, a kind of preparation method drawing material Nano-grade latex ink, described sterilant is a kind of in ethyl vanillin aldehydes, vanilla acids, imidazoles, thiazoles, anilid class, quaternary ammonium salts, two croak class, isothiazolone derivative, phenols.
7., as claim 1, a kind of preparation method drawing material Nano-grade latex ink, the reagent of described adjust ph is the one in hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, ammoniacal liquor, triethylamine.
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| CN107418644A (en) * | 2017-06-02 | 2017-12-01 | 太原理工大学 | A kind of briquette binder preparation method and application |
| CN107418644B (en) * | 2017-06-02 | 2019-11-01 | 太原理工大学 | A kind of application of briquette binder |
| CN111572111A (en) * | 2020-05-29 | 2020-08-25 | 江苏雷鸟伪装纺织新材料有限公司 | Quilting seam and line sewn composite heat-proof infrared detection stealth fabric |
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