CN105111361A - Preparation method of nanometer latex color paste for drawing materials - Google Patents
Preparation method of nanometer latex color paste for drawing materials Download PDFInfo
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Abstract
The invention discloses a preparation method of nanometer latex color paste for drawing materials, and belongs to the technical field of fine chemical engineering and material science. The nanometer latex color paste which is high in stability and suitable for drawing is prepared by adopting a polymerizable dispersing agent, a monomer, oil-soluble dye and the like through miniemulsion polymerization. According to the prepared drawing pigment, an adhesive does not need to be additionally added, and the defect that a conventional dispersing agent in miniemulsion polymerization and products is desorbed from the particle surface is overcome. The preparation method is controllable in reaction, simple in technology, low in cost and suitable for mass production; the prepared nanometer latex color paste is bright and pure in color and good in stability, and a coloring agent which can be well combined with a substrate can be obtained without needing to additionally adding resin.
Description
Technical field
The invention discloses a kind of preparation method drawing material Nano-grade latex mill base, belong to fine chemistry industry and materials science field.
Background technology
Painting coloring agent mainly contains dyestuff and pigment two kinds, wherein dyestuff is based on substantive dyestuff and matching stain, and the subject matter of existence is that light fastness is not high, and the shelf time is not long, there is the phenomenon that colour migration moves, therefore the calligraphy and painting higher to ask for something seldom adopts this tinting material.Dispersible pigment color paste especially nano dye mill base overcomes the above-mentioned defect of dye coloring agent existence, is to paint in recent years to apply more tinting material.Tinting material, dispersion agent and other additive are scattered in water by processes such as stirring, sand milling or ultrasonication by the preparation method of aqueous color paste, and preparation process is more loaded down with trivial details, during energy charge.And due to dispersible pigment color paste and be colored between material and there is no bonding force, in painting coloring agent processing, generally will add a large amount of resin could meet the requirement of painting.
The consumption how reducing resin is the focus that scientific worker studies always.Carry out coated as patent CN104194494A discloses a kind of fine emulsion polymerization to superfine pigment, improve the method for ink-jet printed fastness; Patent CN103834234A discloses the method adopting acrylic ester monomer and dispersed dye to prepare the nano combined pigment mill base of cotton fabric transfer printing emulsion particle.Stability evaluates another important indicator of mill base quality, under normal circumstances, improve stability of pigment paste to improve by screening dispersion agent and optimization dispersing technology, as the people such as Liu Jia, Chen Hong adopt hyper-dispersant not only to improve the stability of dispersible pigment color paste dispersion significantly, but also the tinctorial strength of dispersible pigment color paste can be improved.Nano-grade latex mill base is emerging a kind of novel tinting material in recent years, and at present, this technology mainly rests in external multinational hand, and its preparation method is emulsion polymerization.Although Chinese patent CN200710179879 discloses a kind of preparation method of latex ink, its tinting material adopted is photonic crystal.
Based on this, the present invention's a kind of Nano-grade latex mill base that adopted the method for mini-emulsion polymerization to prepare, namely polymerizable surfactants, monomer and oil-soluble colourant etc. are adopted to be prepared the Nano-grade latex mill base with higher stability energy by fine emulsion polymerization, without the need to separately adding tackiness agent during drawing, to also overcome in mini-emulsion polymerization and product thereof conventional dispersant easily from the defect of particle surface De contamination, the standby emulsion colours of this legal system is bright in colour, stability is high and fastness excellent simultaneously.
Summary of the invention
The object of the invention: a kind of preparation method drawing material Nano-grade latex mill base is provided, namely with polymerizable dispersion agent for emulsifying agent, by fine emulsion polymerization, oil-soluble colourant are coated in emulsion particle, during use, emulsion particle is attached on drawing base material, oil-soluble colourant penetrate in painting canvas or drawing paper, thus obtain lovely luster, high, the resistance to resistance to migration of colour fastness can good drawing special-purpose nanometer emulsion colours.
Technical scheme of the present invention: be dissolved in the water the polymerisable emulsifier to monomer mass mark being 0.5-25% obtained aqueous phase; 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 20-60% to the massfraction of monomer here, prepares oil phase; Under stirring, joined by oil phase in aqueous phase, wherein oil phase accounts for the 5-60% of whole system, and stir speed (S.S.) is 300-1500r/min, and the time, 10-60min prepared pre-emulsion; Pre-emulsion is placed in ultrasonic cell disruptor, person's 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; Underpressure distillation, removes solubility promoter, then uses the removal of impurities of 500nm micropore filter paper filtering, and adjust ph is to neutral, obtains Nano-grade latex mill base.
Described polymerisable emulsifier is polyoxyethylene-type, allyl group (allyloxy) type, styrene type, (methyl) acrylic type, maleate type, methylene-succinic acid type, one or more of Boletic acid type, preferred vinyl carbinol polyoxypropylene ether phosphate further, vinyl carbinol ether phosphate, Hydroxyethyl acrylate-2, 4-tolylene 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.
Described monomer is the conventional soft monomer of polymerization and hard monomer composition, 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, any one or a few of toxilic acid.
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 20-60% of monomer.
Described oil-soluble colourant are 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, the black OBP of oiling, fluorescent yellow 8G, fluorescent yellow 8GF, fluorescent yellow 8GF-2, fluorescent yellow 3G, fluorescent yellow BN, the orange RF of fluorescence, scattered fluorescent yellow 10GN, scattered fluorescent yellow II, scattered fluorescent yellow 8GFF, fluorescent orange GG, dispersion fluorescent orange 2GFL, dispersion fluorescent orange 2RF, fluorescein GG, fluorescein BK, fluorescein GK, fluorescein 5B, fluorescein HFG, fluorescein 5B, fluorescein E2G, fluorescence Exocarpium Citri Rubrum RF, dispersion fluorescein G, the orange GG of dispersion fluorescence, dispersion phloxine FBS, dispersion phloxine BG, fluorescence green 3G, the green G in fluorescence lake, dispersion fluorescence green 5G, the purplish red H5B of fluorescence, C.I. disperse red 60, C.I. Disperse Red 65, C.I. DISPERSE YELLOW 7, C.I. DISPERSE YELLOW 54, C.I. dispersion yellow 64, C.I. DISPERSE YELLOW 70, C.I. DISPERSE YELLOW 71, C.I. DISPERSE YELLOW 100, C.I. EX-SF DISPERSE BLUE EX-SF 300 14, C.I. EX-SF DISPERSE BLUE EX-SF 300 26, C.I. EX-SF DISPERSE BLUE EX-SF 300 35, C.I. EX-SF DISPERSE BLUE EX-SF 300 55, C.I. Disperse Blue-56, C.I. EX-SF DISPERSE BLUE EX-SF 300 91, C.I. EX-SF DISPERSE BLUE EX-SF 300 366, C.I. any one or a few is disperseed in blue-black 1.
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.
The reagent of described adjust ph is any one in hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, sodium carbonate, ammoniacal liquor, triethylamine.
Beneficial effect of the present invention: utilize polymerizable dispersion agent, oil-soluble colourant and polymerization single polymerization monomer, Nano-grade latex mill base is prepared by fine emulsion polymerization, this method has the advantages such as the low and applicable scale operation of reaction controllability, simple, old of technique, the Nano-grade latex mill base of preparation is bright-colored pure, good stability, and do not need additionally to add resin and just can obtain the tinting material excellent with base material binding strength.
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.
Embodiment 1
0.5g propyl alcohol polyoxypropylene ether phosphate, 0.5g allyl alcohol ether/octylphenol ether phosphoric acid ester and 0.5g monomaleate sulfate are dissolved in 100g water, obtained aqueous phase; 8g solvent red 111,2.5g sherwood oil, 4.5g 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 O/W type miniemulsion is placed in reactor, stir with 215r/min speed, the aqueous solution containing 0.25g ammonium persulphate is added when temperature rises to 70 DEG C, reaction 3h, cooling discharging, be placed in Rotary Evaporators 65 DEG C and boil off organic solvent, Nano-grade latex mill base is obtained with 500nm millipore filtration filter paper filtering, Nano-grade latex mill base, in table 1, is mixed with printing gum by property indices, is imprinted on cotton, 80 DEG C of oven dry, 130 DEG C bake, and then test the washing of PRINTED FABRIC, friction and light fastness, the results are shown in Table 2.
Embodiment 2
0.5g Hydroxyethyl acrylate-2,4 toluene diisocyanate-monomethyl polyoxyethylene glycol (HEA-TDI-PEO) and 0.5g sulfonation lauryl alcohol allyl oxyglycerol butyric ester sodium salt and 0.5g mono maleate sulfonate are dissolved in 100g water, obtained aqueous phase; 5g Oil Yellow R, 1g methylene dichloride, 9g ethyl acetate are added and is dissolved in 14g ethyl propenoate, 2g dicyclopentadiene and 4g 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 O/W type miniemulsion is placed in reactor, 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, Nano-grade latex mill base is obtained with 500nm millipore filtration filter paper filtering, Nano-grade latex mill base, in table 1, is mixed with printing gum by property indices, is imprinted on cotton, 80 DEG C of oven dry, 130 DEG C bake, and then test the washing of PRINTED FABRIC, friction and light fastness, the results are shown in Table 2.
Embodiment 3
By 0.9g sulfonation lauryl alcohol methacrylic acid glycerol butyrate sodium salt and 0.6g vinylbenzene dodecyl dimethyl chloride leach in 100g water, obtained aqueous phase; 6g solvent blue 36,2g sherwood oil, 7g ethyl acetate are added and is dissolved in 10g butyl acrylate, 4g vinyl acetate and 6g 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 O/W type miniemulsion is placed in reactor, 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, Nano-grade latex mill base is obtained with 500nm millipore filtration filter paper filtering, Nano-grade latex mill base, in table 1, is mixed with printing gum by property indices, is imprinted on cotton, 80 DEG C of oven dry, 130 DEG C bake, and then test the washing of PRINTED FABRIC, friction and light fastness, the results are shown in Table 2.
Embodiment 4
0.3g sodium dodecyl allyl base succinate sodium sulfonate and 1.2g2-acrylamido-2-methyI-oropvD sodium sulfonate are dissolved in 100g water, obtained aqueous phase; 7gC.I. DISPERSE YELLOW 70,3g ethyl acetate, 6g methylene dichloride are added and is dissolved in 15g Isooctyl acrylate monomer, 3g methacrylonitril and 2g divinylic 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 O/W type miniemulsion is placed in reactor, 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, Nano-grade latex mill base is obtained with 500nm millipore filtration filter paper filtering, Nano-grade latex mill base, in table 1, is mixed with printing gum by property indices, is imprinted on cotton, 80 DEG C of oven dry, 130 DEG C bake, and then test the washing of PRINTED FABRIC, friction and light fastness, the results are shown in Table 2.
Table 1: the performance index of prepared Nano-grade latex mill base
Nano-grade latex mill base particle diameter, size-grade distribution, Zeta potential adopt Nano-ZS90 type granularity and Zeta potential analysis-e/or determining; The method of calculation of heat-resistant stability: sample places 24h at 80 DEG C, the particle diameter γ of sample before and after test processes
0, γ
1, press
calculate, S
tcharacterize Nano-grade latex mill base heat-resistant stability; Dewatering ability: sample processes 30min under the centrifugation rate of 5000r/min, gets 0.5mL central liquid, uses distilled water diluting certain multiple, by the absorbance A of the centrifugal front and back of spectrophotometric determination
0and A
1, by the ratio R of centrifugal front and back system absorbancy,
characterize the dewatering ability of Nano-grade latex mill base.
Claims (7)
1. draw a preparation method for material Nano-grade latex mill base, be dissolved in the water the polymerisable emulsifier to monomer mass mark being 0.5-25% obtained aqueous phase; 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 20-60% to the massfraction of monomer here, prepares oil phase; Under stirring, joined by oil phase in aqueous phase, wherein oil phase accounts for the 5-60% of whole system, and stir speed (S.S.) is 300-1500r/min, and time 10-60min, prepares pre-emulsion; 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; Underpressure distillation, removes solubility promoter, then uses the removal of impurities of 500nm micropore filter paper filtering, and adjust ph is to neutral, obtains Nano-grade latex mill base.
2. as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, described polymerisable emulsifier is polyoxyethylene-type, allyl group (allyloxy) type, styrene type, (methyl) acrylic type, maleate type, methylene-succinic acid type, one or more of Boletic acid type, preferred vinyl carbinol polyoxypropylene ether phosphate further, vinyl carbinol ether phosphate, Hydroxyethyl acrylate-2, 4-tolylene 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.
3. as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, described monomer is by being polymerized conventional soft monomer and hard monomer forms, 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, any one or a few of toxilic acid.
4. as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, 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, any one or a few in 1,1-trichloroethane, Virahol, acetone, butanone, tetrahydrofuran (THF), pentane, hexanaphthene, sherwood oil.
5., as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, described oil-soluble colourant are 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, the black OBP of oiling, fluorescent yellow 8G, fluorescent yellow 8GF, fluorescent yellow 8GF-2, fluorescent yellow 3G, fluorescent yellow BN, the orange RF of fluorescence, scattered fluorescent yellow 10GN, scattered fluorescent yellow II, scattered fluorescent yellow 8GFF, fluorescent orange GG, dispersion fluorescent orange 2GFL, dispersion fluorescent orange 2RF, fluorescein GG, fluorescein BK, fluorescein GK, fluorescein 5B, fluorescein HFG, fluorescein 5B, fluorescein E2G, fluorescence Exocarpium Citri Rubrum RF, dispersion fluorescein G, the orange GG of dispersion fluorescence, dispersion phloxine FBS, dispersion phloxine BG, fluorescence green 3G, the green G in fluorescence lake, dispersion fluorescence green 5G, the purplish red H5B of fluorescence, C.I. disperse red 60, C.I. Disperse Red 65, C.I. DISPERSE YELLOW 7, C.I. DISPERSE YELLOW 54, C.I. dispersion yellow 64, C.I. DISPERSE YELLOW 70, C.I. DISPERSE YELLOW 71, C.I. DISPERSE YELLOW 100, C.I. EX-SF DISPERSE BLUE EX-SF 300 14, C.I. EX-SF DISPERSE BLUE EX-SF 300 26, C.I. EX-SF DISPERSE BLUE EX-SF 300 35, C.I. EX-SF DISPERSE BLUE EX-SF 300 55, C.I. Disperse Blue-56, C.I. EX-SF DISPERSE BLUE EX-SF 300 91, C.I. EX-SF DISPERSE BLUE EX-SF 300 366, C.I. any one or a few is disperseed in blue-black 1.
6. as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, 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.
7., as claim 1 one kind draws the preparation method of material Nano-grade latex mill base, the reagent of described adjust ph is any one in hydrochloric acid, acetic acid, sodium hydroxide, sodium bicarbonate, sodium carbonate, ammoniacal liquor, triethylamine.
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| CN105111361B (en) | 2018-05-25 |
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