CN103073959B - Washable coating material and preparation method thereof - Google Patents
Washable coating material and preparation method thereof Download PDFInfo
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- CN103073959B CN103073959B CN201310029421.2A CN201310029421A CN103073959B CN 103073959 B CN103073959 B CN 103073959B CN 201310029421 A CN201310029421 A CN 201310029421A CN 103073959 B CN103073959 B CN 103073959B
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Abstract
The invention provides a washable coating material and a preparation method thereof. The coating material comprises the following components by weight percentage: 20-25% of titaniferous microcrystalline cellulose composite powder, 12-16% of slag powder, 0.15-0.2% of polyurethane, 2-5% of titanium dioxide, 0.1-0.5% of silica sol, 3-5% of silica powder and the balance of 3-methyl-2-butylene-1-alcohol acetate composite solution, wherein the slag powder comprises the following components by weight percentage: 36-40% of CaO, 13-15% of Al2O3, 6-9% of MgO, 0.3-0.5% of FeO and the balance of SiO2; the particle size of the slag powder is 80-100 micrometers; the fineness of titanium dioxide is 80-100 micrometers; the particle size of the titaniferous microcrystalline cellulose composite powder is 80-100 nanometers; and the particle size of the silica powder is 0.5-0.8 millimeters.
Description
Technical field
The invention belongs to paint field, relate to a kind of washing fastness coated material and preparation method thereof.
Background technology
201210007801.1 number to application discloses that a kind of production method of environment-friendly type coating, the method quartz sand mine tailing produces resistance to acids and bases and abrasion resistance environment-friendly type coating, comprises the steps: 1., the preparation of aqueous polyvinyl acetate emulsion: preparation 4 ~ 5ml massfraction is the ammonium persulfate solution of 5%; The ammonium persulfate solution of 15 ~ 19g vinyl acetate and 1 ~ 3ml is added in reaction vessel, stirs, heating in water bath, reflux at keeping temperature 65 ~ 75 DEG C; When the disappearance that refluxes, temperature are in time rising to 80 ~ 83 DEG C, in 2h, at the uniform velocity drip 22 ~ 25g vinyl acetate and remaining ammonium persulfate solution with dropping funnel; After reinforced, be warming up to 90 ~ 95 DEG C, insulation 30min, until without backflow; Cooling down to 50 DEG C, adjustment pH to 5 ~ 6, to obtain final product; 2., quartz sand mine tailing polyvinyl acetate emulsion coating be prepared in reaction vessel, add 18 ~ 22g deionized water, under agitation, add 8 ~ 12g titanium dioxide, 7 ~ 9g talcum powder and 5 ~ 12g quartz sand mine tailing gradually, dispersed with stirring is even; Under agitation add aqueous polyvinyl acetate emulsion and 1 ~ 5g polyvinyl alcohol that 1. 30 ~ 50g step prepared, stir, obtain coating.The step 1. middle conditioning agent adjusting pH is the sodium hydrogen carbonate solution of massfraction 5%.Coating is cream-coloured to white stiff flow-like.Abrasion resistance is greater than 6000 times.Water tolerance is greater than 160 hours.
Above-mentioned coating Problems existing is that wash-resistant property is poor.
Summary of the invention
Object of the present invention is exactly for above-mentioned technological deficiency, and provide a kind of washing fastness coated material, this coated material has good thermal insulation, and has high wash-resistant property.
Another object of the present invention is to provide above-mentioned washing fastness coated material preparation method, and this preparation method's technique is simple, and production cost is low, is suitable for suitability for industrialized production.
Coated material of the present invention not only for building, and can be used for outdoor goods, clothes, military affairs etc. in needs insulation, the extensive application of heat insulation occasion.
The object of the invention is to be achieved through the following technical solutions:
A kind of washing fastness coated material, in this coated material, the weight percent of each composition is:
Titaniferous Microcrystalline Cellulose composite powder 20-25%, slag powder 12-16%, urethane 0.15-0.2%, titanium dioxide 2-5%, silicon sol 0.1-0.5%, silica powder 3-5%, all the other are 3-M2BOL acetic ester composite solution;
Wherein in slag powder, the weight percent of each composition is: CaO36-40%, Al
2o
313-15%, MgO6-9%, FeO0.3-0.5%, all the other are SiO
2; The particle diameter of slag powder is 80-100 μm; The fineness 80-100 μm of titanium dioxide.
The particle diameter of titaniferous Microcrystalline Cellulose composite powder is 80-100nm, and the particle diameter of silica powder is 0.5-0.8mm.
The preparation method of above-mentioned washing fastness coated material, the method comprises the following steps:
1) preparation of titaniferous Microcrystalline Cellulose composite powder:
Under ice-water bath, be slowly added dropwise in Virahol by titanium tetrachloride, add concentrated hydrochloric acid, stir, then drip ammoniacal liquor in solution, form solution A, wherein the volume ratio of titanium tetrachloride, Virahol, concentrated hydrochloric acid and ammoniacal liquor is 90:420:4.8:135;
By Microcrystalline Cellulose and the vitriol oil with 1: 20 weight ratio mix, in 50-55 DEG C of supersound process 1h under ultrasonic frequency 50kHz power, 400W, obtain milk-white coloured suspension B, stand-by; Wherein the particle diameter of Microcrystalline Cellulose is 70-75nm;
By aforesaid liquid A with solution B in mass ratio for 1:1.3-1.5 mixes, at ultrasonic frequency 50kHz after mixing, power is in 50-55 DEG C of ultrasonic agitation 1-2h under 400W; Then by gained mixed solution at 95 DEG C of rotary evaporation in vacuo, obtain solid gel, then 115-125 DEG C of drying, is milled into powder, obtains titaniferous Microcrystalline Cellulose composite powder;
2) preparation of 3-M2BOL acetic ester composite solution:
The weight percent of each raw material used is: dioctyl phthalate (DOP) 4-6%, propyl carbinol 1-2%, polyvinyl alcohol 5-6%, Potassium Persulphate 0.15-0.19%, 3-M2BOL acetic ester 45-50%, and surplus is water;
First dioctyl phthalate (DOP) is mixed with propyl carbinol, stir and make it dissolve, form solution first stand-by;
Added by water in a container, be heated to 80 DEG C, under agitation add polyvinyl alcohol, be warming up to 95 DEG C, insulation is to all dissolving; After to be dissolved, stop heating making temperature be down to 68 ~ 70 DEG C, under agitation add 3-M2BOL acetic ester, form solution second stand-by;
By solution first and the mixing of solution second, add Potassium Persulphate, be uniformly mixed, be warmed up between 65 ~ 70 DEG C, stop 1-2 hour, obtain 3-M2BOL acetic ester composite solution, stand-by;
3) washing fastness coated material preparation: wherein the weight percent of each composition is: nano level titaniferous Microcrystalline Cellulose composite powder 20-25%, slag powder 12-16%, urethane 0.15-0.2%, titanium dioxide 2-5%, silicon sol 0.1-0.5%, silica powder 3-5%, all the other are 3-M2BOL acetic ester composite solution, each composition is put into container and stirs.
The particle diameter of slag powder is 80-100 μm; Titanium dioxide has fineness 80-100 μm; The particle diameter of titaniferous Microcrystalline Cellulose composite powder is 80-100nm, and the particle diameter of silica powder is 0.5-0.8mm.
Step 1) described in the mass percentage concentration of concentrated hydrochloric acid be 37%; Described ammoniacal liquor mass percentage concentration is 28%/; The described vitriol oil to be mass percentage concentration be 50% concentrated sulfuric acid solution.
The present invention has following beneficial effect compared to existing technology:
Nano level titaniferous Microcrystalline Cellulose composite powder in coated material composition of the present invention, has a large amount of micro interfaces, has good thermal insulation; And there is higher body cohesive strength, significantly improve the abrasion resistance of coated material.
Urethane in coated material, silicon sol and 3-M2BOL acetic ester composite solution combine, by strengthening the cross-link intensity of adhesive material (3-M2BOL acetic ester composite solution) in nano coating, substantially increase the cohesive strength of coated substrate.In addition, silicon sol and 3-M2BOL acetic ester composite solution and nano level titaniferous Microcrystalline Cellulose composite powder have good avidity, also can significantly improve the intensity of coating.
Slag powder in coated material composition of the present invention has microcosmic vesicular structure, both can improve the heat-insulating capability of material, and cost of material is cheap, reduces production cost.
Coated material of the present invention its there is good abrasion resistance, and there is satisfactory stability and practicality, the field such as outdoor building, fabric can be widely used in.
Accompanying drawing illustrates:
Fig. 1 is the tissue of the coated material that the embodiment of the present invention 1 obtains.
As seen from Figure 1, this coated material is uniformly distributed.
Embodiment:
In following embodiment, raw material model: silicon sol (881), polyvinyl alcohol (1788).
Embodiment one:
The preparation method of washing fastness coated material of the present invention, the method comprises the following steps:
1) preparation of titaniferous Microcrystalline Cellulose composite powder:
Under ice-water bath (0 DEG C), 90mL titanium tetrachloride is slowly added dropwise in 420mL Virahol, solution, 4.8mL concentrated hydrochloric acid (mass percentage concentration is 37%) is added in solution, stir, drip 135mL ammoniacal liquor (mass percentage concentration 28%) again, form solution A.
By Microcrystalline Cellulose and mass percentage concentration be 50% concentrated sulfuric acid solution with 1: 20 weight ratio mix, in 50-55 DEG C of supersound process 1h under ultrasonic frequency 50kHz power, 400W, obtain milk-white coloured suspension B, stand-by; Wherein the particle diameter of Microcrystalline Cellulose is 70-75nm;
By aforesaid liquid A with solution B in mass ratio for 1:1.3 mixes, at ultrasonic frequency 50kHz after mixing, power is in 50-55 DEG C of ultrasonic agitation 1.5h under 400W; Then evaporated at 95 DEG C of vacuum rotatings (rotating speed 1000r/min) by gained mixed solution, obtain solid gel, then 120 DEG C of dryings, are milled into powder, obtain titaniferous Microcrystalline Cellulose composite powder.
2) preparation of 3-M2BOL acetic ester composite solution:
The weight percent of each raw material used is: dioctyl phthalate (DOP) 5%, propyl carbinol 5%, polyvinyl alcohol 5%, Potassium Persulphate 0.16%, 3-M2BOL acetic ester 46%, and surplus is water;
First dioctyl phthalate (DOP) is mixed with propyl carbinol, stir and make it dissolve, form solution first stand-by;
Added by water in a container, be heated to 80 DEG C, under agitation add polyvinyl alcohol, be warming up to 95 DEG C, insulation is to all dissolving; After to be dissolved, stop heating making temperature be down to 68 ~ 70 DEG C, under agitation add 3-M2BOL acetic ester, form solution second stand-by;
By solution first and the mixing of solution second, add Potassium Persulphate, be uniformly mixed, be warmed up between 65 ~ 70 DEG C, stop 1-2 hour, obtain 3-M2BOL acetic ester composite solution, stand-by;
3) washing fastness coated material preparation: wherein the weight percent of each composition is: above-mentioned titaniferous Microcrystalline Cellulose composite powder 20%, slag powder 12%, urethane 0.15%, titanium dioxide 2%, silicon sol 0.1%, silica powder 3%, surplus is above-mentioned 3-M2BOL acetic ester composite solution.Each composition is put into container stir.
Wherein, the particle diameter of slag powder is 80-100 μm; Titanium dioxide has fineness 80-100 μm; The particle diameter of titaniferous Microcrystalline Cellulose composite powder is 80-100nm, and the particle diameter of silica powder is 0.5-0.8mm.
Embodiment two:
Step 1) in liquid A and solution B be 1:1.4 in mass ratio;
Step 3) weight percent of each composition is in coating material: nano level titaniferous Microcrystalline Cellulose composite powder 25%, slag powder 16%, urethane 0.2%, titanium dioxide 5%, silicon sol 0.5%, silica powder 5%, all the other are 3-M2BOL acetic ester composite solution.
Other preparation process is with embodiment one.
Embodiment three:
Step 1) in liquid A and solution B be 1:1.5 in mass ratio;
Step 3) weight percent of each composition is in coating material: nano level titaniferous Microcrystalline Cellulose composite powder 23%, slag powder 14%, urethane 0.17%, titanium dioxide 4%, silicon sol 0.3%, silica powder 4%, all the other are 3-M2BOL acetic ester composite solution.
Other preparation process is with embodiment one.
Embodiment four: proportioning components is not in scope of design of the present invention.
Step 1) in liquid A and solution B be 1:1 in mass ratio;
Step 3) weight percent of each composition is in coating material: nano level titaniferous Microcrystalline Cellulose composite powder 18%, slag powder 10%, urethane 0.12%, titanium dioxide 1%, silicon sol 0.05%, silica powder 2%, all the other are 3-M2BOL acetic ester composite solution.
Other preparation process is with embodiment one.
Embodiment five: proportioning components is not in scope of design of the present invention.
Step 1) in liquid A and solution B be 1:1.8 in mass ratio;
Step 3) weight percent of each composition is in coating material: nano level titaniferous Microcrystalline Cellulose composite powder 30%, slag powder 18%, urethane 0.3%, titanium dioxide 6%, silicon sol 0.6%, silica powder 6%, all the other are 3-M2BOL acetic ester composite solution.
Other preparation process is with embodiment one.
Test:
In coated material of the present invention, 3-M2BOL acetic ester composite solution is caking agent, does not very fewly have solvent action, too much can dilute coating; Urethane and silicon sol are the caking agent enhancement component in coating, very fewly do not have bonding effect, too much can dilute insulation particle and solvent; Titaniferous Microcrystalline Cellulose composite powder, silica powder, titanium dioxide and slag powder are aggregate, very fewly do not have heat insulation and enhancement, too much can reduce the bonding effect of caking agent.
Claims (5)
1. a washing fastness coated material, is characterized in that, in this coated material, the weight percent of each composition is:
Titaniferous Microcrystalline Cellulose composite powder 20-25%, slag powder 12-16%, urethane 0.15-0.2%, titanium dioxide 2-5%, silicon sol 0.1-0.5%, silica powder 3-5%, all the other are 3-M2BOL acetic ester composite solution;
Wherein in slag powder, the weight percent of each composition is: CaO 36-40%, Al2O3 13-15%, MgO 6-9%, FeO 0.3-0.5%, and all the other are SiO2; The particle diameter of slag powder is 80-100 μm; The fineness 80-100 μm of titanium dioxide; The particle diameter of titaniferous Microcrystalline Cellulose composite powder is 80-100nm, and the particle diameter of silica powder is 0.5-0.8mm;
The concrete preparation process of described titaniferous Microcrystalline Cellulose composite powder is as follows: under ice-water bath, titanium tetrachloride is slowly added dropwise in Virahol, concentrated hydrochloric acid is added in solution, stir, drip ammoniacal liquor again, form solution A, wherein the volume ratio of titanium tetrachloride, Virahol, concentrated hydrochloric acid and ammoniacal liquor is 90:420:4.8:135;
By Microcrystalline Cellulose and the vitriol oil with 1: 20 weight ratio mix, at ultrasonic frequency 50kHz, in 50-55 DEG C of supersound process 1h under power 400W, obtain milk-white coloured suspension B, stand-by; Wherein the particle diameter of Microcrystalline Cellulose is 70-75nm;
By aforesaid liquid A with solution B in mass ratio for 1:1.3-1.5 mixes, at ultrasonic frequency 50kHz after mixing, power is in 50-55 DEG C of ultrasonic agitation 1-2h under 400W; Then by gained mixed solution at 95 DEG C of rotary evaporation in vacuo, obtain solid gel, then 115-125 DEG C of drying, is milled into powder, obtains titaniferous Microcrystalline Cellulose composite powder; Wherein, the mass percentage concentration of concentrated hydrochloric acid is 37%; The mass percentage concentration 28% of ammoniacal liquor; The mass percentage concentration of concentrated sulfuric acid solution is 50%; The rotating speed 1000r/min of rotary evaporation in vacuo;
The concrete preparation process of described 3-M2BOL acetic ester composite solution is as follows:
The weight percent of each raw material used is: dioctyl phthalate (DOP) 4-6%, propyl carbinol 1-2%, polyvinyl alcohol 5-6%, Potassium Persulphate 0.15-0.19%, 3-M2BOL acetic ester 45-50%, and surplus is water; First dioctyl phthalate (DOP) is mixed with propyl carbinol, stir and make it dissolve, form solution first stand-by; Added by water in a container, be heated to 80 DEG C, under agitation add polyvinyl alcohol, be warming up to 95 DEG C, insulation is to all dissolving; After to be dissolved, stop heating making temperature be down to 68 ~ 70 DEG C, under agitation add 3-M2BOL acetic ester, form solution second stand-by; By solution first and the mixing of solution second, add Potassium Persulphate, be uniformly mixed, be warmed up between 65 ~ 70 DEG C, stop 1-2 hour, obtain 3-M2BOL acetic ester composite solution.
2. a preparation method for washing fastness coated material, the method comprises the following steps:
1) preparation of titaniferous Microcrystalline Cellulose composite powder:
Under ice-water bath, be slowly added dropwise in Virahol by titanium tetrachloride, add concentrated hydrochloric acid, stir, then drip ammoniacal liquor in solution, form solution A, wherein the volume ratio of titanium tetrachloride, Virahol, concentrated hydrochloric acid and ammoniacal liquor is 90:420:4.8:135;
By Microcrystalline Cellulose and the vitriol oil with 1: 20 weight ratio mix, at ultrasonic frequency 50kHz, in 50-55 DEG C of supersound process 1h under power 400W, obtain milk-white coloured suspension B, stand-by; Wherein the particle diameter of Microcrystalline Cellulose is 70-75nm;
By aforesaid liquid A with solution B in mass ratio for 1:1.3-1.5 mixes, at ultrasonic frequency 50kHz after mixing, power is in 50-55 DEG C of ultrasonic agitation 1-2h under 400W; Then by gained mixed solution at 95 DEG C of rotary evaporation in vacuo, obtain solid gel, then 115-125 DEG C of drying, is milled into powder, obtains titaniferous Microcrystalline Cellulose composite powder;
2) preparation of 3-M2BOL acetic ester composite solution:
The weight percent of each raw material used is: dioctyl phthalate (DOP) 4-6%, propyl carbinol 1-2%, polyvinyl alcohol 5-6%, Potassium Persulphate 0.15-0.19%, 3-M2BOL acetic ester 45-50%, and surplus is water; First dioctyl phthalate (DOP) is mixed with propyl carbinol, stir and make it dissolve, form solution first stand-by; Added by water in a container, be heated to 80 DEG C, under agitation add polyvinyl alcohol, be warming up to 95 DEG C, insulation is to all dissolving; After to be dissolved, stop heating making temperature be down to 68 ~ 70 DEG C, under agitation add 3-M2BOL acetic ester, form solution second stand-by; By solution first and the mixing of solution second, add Potassium Persulphate, be uniformly mixed, be warmed up between 65 ~ 70 DEG C, stop 1-2 hour, obtain 3-M2BOL acetic ester composite solution, stand-by;
3) washing fastness coated material preparation: wherein the weight percent of each composition is: titaniferous Microcrystalline Cellulose composite powder 20-25%, slag powder 12-16%, urethane 0.15-0.2%, titanium dioxide 2-5%, silicon sol 0.1-0.5%, silica powder 3-5%, all the other are 3-M2BOL acetic ester composite solution, each composition is put into container and stirs;
The particle diameter of described slag powder is 80-100 μm; Titanium dioxide has fineness 80-100 μm; The particle diameter of titaniferous Microcrystalline Cellulose composite powder is 80-100nm, and the particle diameter of silica powder is 0.5-0.8mm.
3. the preparation method of washing fastness coated material according to claim 2, is characterized in that: step 1) described in the mass percentage concentration of concentrated hydrochloric acid be 37%.
4. the preparation method of washing fastness coated material according to claim 2, is characterized in that: step 1) described in ammoniacal liquor mass percentage concentration be 28%.
5. the preparation method of washing fastness coated material according to claim 2, is characterized in that: step 1) described in the vitriol oil to be mass percentage concentration be 50% concentrated sulfuric acid solution.
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| CN201310029421.2A CN103073959B (en) | 2013-01-25 | 2013-01-25 | Washable coating material and preparation method thereof |
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| CN201310029421.2A CN103073959B (en) | 2013-01-25 | 2013-01-25 | Washable coating material and preparation method thereof |
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| CN104194531B (en) * | 2014-08-20 | 2016-05-11 | 南京信息工程大学 | A kind of solvent resistance environment protecting water-based paint and preparation method |
| CN104804166B (en) * | 2015-04-28 | 2017-10-03 | 中科院广州化学有限公司南雄材料生产基地 | A kind of flame retardant polyurethane nano-cellulose composite and its preparation method and application |
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| JP4758872B2 (en) * | 2006-11-22 | 2011-08-31 | 独立行政法人産業技術総合研究所 | Method for producing barium titanate powder |
| CN101338101A (en) * | 2008-08-14 | 2009-01-07 | 广州市星冠化工涂料有限公司 | Nanometer interior wall coating g |
| CN101709160A (en) * | 2009-12-16 | 2010-05-19 | 东北大学 | Inorganic antibacterial coating with titaniferous blast furnace slag and preparation method thereof |
| CN102399483A (en) * | 2011-12-22 | 2012-04-04 | 华南理工大学 | Organic/inorganic composite heat-insulating heat-preserving water-based building coating and preparation method thereof |
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