CN102585570A - Water-soluble non-combustible ceramic anti-radiation coating and preparation method thereof - Google Patents

Water-soluble non-combustible ceramic anti-radiation coating and preparation method thereof Download PDF

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CN102585570A
CN102585570A CN2012100064911A CN201210006491A CN102585570A CN 102585570 A CN102585570 A CN 102585570A CN 2012100064911 A CN2012100064911 A CN 2012100064911A CN 201210006491 A CN201210006491 A CN 201210006491A CN 102585570 A CN102585570 A CN 102585570A
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water
coating
fire
agent
soluble
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CN102585570B (en
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黄健
宋雪峰
马保国
蹇守卫
赵子强
殷海波
段超群
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武汉理工大学
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Abstract

The invention relates to a water-soluble non-combustible ceramic anti-radiation coating and a preparation method thereof. The coating comprises an active material, an inorganic filler, a shrinkage reducing agent, a thickening agent, a flame retardant, a silicate binder, a reflection reinforcing agent and an aid in a mass ratio of (2-2.8):(0.5-1):0.40:(0.01-0.04):(0.4-0.8):2.13:(0.067-0.2):0.3. The coating is formed by fully mixing the components uniformly and can be used for painting or spraying, and a layer of modified fluoro-silicone emulsion is painted on the surface of the coating after the coating is surface-dried. The coating can be used as an exterior wall coating (base coat), and also can be used as a protective coating for the surfaces of an exterior wall thermal insulation plate, mortar, a sintered brick and a building enclosure structure; and the water-soluble ceramic coating has the characteristics of high durability, light weight, high strength, high efficiency, flame retardance, fire resistance, controllable quality, water resistance, alkali resistance, freezing and thawing resistance, cracking resistance, falling resistance and the like.

Description

A kind of water-soluble ceramic radiation shielding coating and preparation method thereof that do not fire
Technical field
The present invention relates to a kind of water-soluble ceramic radiation shielding coating and preparation method thereof that do not fire, mainly be used as the supercoat of outer wall material, material of construction and architectural exterior-protecting construction.
Background technology
Most of organic coatings have added human body and the deleterious starting material of environment in process of production; In production, construction and the use of coating, all can give off a large amount of harmful waste waters and waste gas; Environment is caused severe contamination, and organic coating burns very easily, it makes flame spread rapidly in combustion processes; Produce a large amount of inflammable and toxic gases, caused huge potential safety hazard.For this reason, low pollution of exploitation or free of contamination environment-friendly type coating have been subjected to extensive attention.
At present, the base-material of domestic inorganic paint is silicon sol, water glass or white cement mostly, and other solid material mixes as auxiliary material, play effects such as filling or modification, but volume is very limited.Active ground slag, activated grammite can be reduced cost, protect environment as the base-material of inorganic paint, have great importance.Pulverized slag powder and silicon ash generally are pearl, and lighter color is convenient to adjust the system color as the base-material of inorganic paint.In addition, compare with other gelling material, the chemically reactive of breeze and silicon ash is higher, and the physicals of coating is better and controlled behind hydration reaction.But the speed of response of ground slag is very fast, just can generate fine and close aluminate in the several minutes, is coated on the ground slag particle surface; Stop hydration reaction further to carry out, so, necessary admixture alkali-activator in coating; Destroy the formation of aluminate, hydration reaction could normally carry out.Active breeze and activated grammite are during as the base-material of inorganic paint, and its process of setting needs the certain humidity and the length of time, if in outdoor thin layer brushing, dope layer be easy to as yet not aquation before because of phenomenons such as ftractureing, peel off appear in dehydration.Therefore, the necessary an amount of admixture of admixture of coating system prevents coating cracking or cubic deformation.
In addition, along with the progressively raising of energy conservation standard, adopt the thickness of flammable organic insulation material constantly to increase, the problem of external wall fire and fire spread is more outstanding.So; The use that has added the inorganic paint of efficient expansion type flame retardant can effectively reduce the probability of buildings presence of fire, can effectively protect the uses of combustible material in External Thermal Insulation System such as polystyrene foam for example commonly used and hard-foam polyurethane.
Therefore no matter, have the coating of the high feature of environmental protection, high-durability, high flame retardant type and complex heat-preservation effect, be aspect fire safety, still aspect exterior wall composite thermal insulation, can both satisfy the requirement of country, and practical applications is had important and practical meanings.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of not fire ceramic radiation shielding coating to above-mentioned prior art with high-efficiency environment friendly, high-durability and high security inorganic water-soluble; It is when making full use of the asepsis environment-protecting material; Fire protection flame retarding is combined with radioprotective, obtained more high-grade inorganic paint.
The present invention solves its technical problem and adopts following technical scheme: a kind of water-soluble ceramic radiation shielding coating that do not fire; It is characterized in that its component and component concentration thereof count by mass ratio: active material: mineral filler: economization agent: thickening material: fire retardant: silicate bond: reflection enhancement agent: auxiliary agent=2~2.8: 0.5~1: 0.40: 0.01-0.04: 0.4~0.8: 2.13: 0.067~0.2: 0.3; Wherein, Described reflection enhancement agent is a gas phase nano silicon-dioxide; Described fire retardant is the modification expansible black lead, and described silicate bond is a water glass, and its modulus n is 2.2~2.5; Described economization agent is a redispersible latex powder, and described thickening material is a hydroxyethylmethyl-cellulose.
Press such scheme, described active material is the mixture of breeze and silicon ash, and the mass ratio of breeze and silicon ash is not less than 5: 1.
Press such scheme, described mineral filler is any one or the multiple mixing in talcum powder, mica powder and the pigment, and wherein said pigment is any one or the multiple mixing in white titanium pigment, zinc barium powder, chromate or the iron oxide pigment.
Press such scheme, described modification Preparation of Expansible Graphite method is that crystalline flake graphite, ydrogen peroxide 50 and nitrosonitric acid are mixed, and in ice-water bath, stirs rapidly; To reaction mild after with this reaction system constant temperature at 25 ℃, washing, suction filtration drip acetic acid soln and constantly stir; Reaction 60~120min, washing, suction filtration; Oven dry gets the modification expansible black lead.
Press such scheme, described modification Preparation of Expansible Graphite method is than crystalline flake graphite: KMnO according to quality 4=1: 0.2~0.4 ratio adds KMnO in crystalline flake graphite 4, stir, add HClO 3Solution also keeps 35 ℃ of intermittently stirring reaction 60~120min, washing then, and suction filtration, oven dry can obtain the modification expansible black lead.
Press such scheme, described auxiliary agent is that the silok7110 water-based wetting dispersing agent and the vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid of silok company is that mixing in 2: 1.3 is formed according to mass ratio.
Water-soluble preparation method of not firing ceramic radiation shielding coating; It is characterized in that including following steps: with active material: mineral filler: economization agent: thickening material: fire retardant: silicate bond: reflection enhancement agent: auxiliary agent=2~2.8: 0.5~1: 0.40: 0.01-0.04: 0.4~0.8: 2.13: 0.067~0.2: 0.3 thorough mixing can be brushed or sprayed after evenly; Behind the coating surface drying at its external coating one deck modified fluoro-silicone emulsion; Wherein, described reflection enhancement agent is a gas phase nano silicon-dioxide, and described fire retardant is the modification expansible black lead; Described silicate bond is a water glass; Its modulus n is 2.2~2.5, and described thickening material is a hydroxyethylmethyl-cellulose, and described economization agent is a redispersible latex powder.
The acting as of each main raw material(s) among the present invention:
Water glass, gelling material, its effect is to form stable fine and close silica network layer and hydrated calcium silicate resist with active base-material breeze;
Gas phase nano silicon-dioxide has huge specific surface area, active greatly, can when coating is dry, form reticulated structure; Increase the intensity and the smooth finish of coating simultaneously; And improved the suspension of pigment, can keep coating do not fade for a long time, not stratified, have thixotropy, sag prevention, to execute formula functional, especially anti-ly stain metachromia and can improve greatly; Has good automatically cleaning ability and sticking power; And has extremely strong uv-absorbing, infrared external reflection characteristic, the thermal insulation and the weather resistance of increase coating;
Mineral filler such as talcum powder, mica powder is filled in gelling material inside and plays the effect that improves intensity;
The modification expansible black lead; Be expansion type flame retardant, its effect is under comparatively high temps, can produce volume to expand significantly or produce foam-like material and be covered in the surface, forms stable heat insulation coating; Play secluding air, effectively insulating effect; Thereby reach fire-retardant purpose, according to the difference of binding substance, also can produce CO simultaneously because of being heated 2, NH 3, H 2Non-flammable gases such as O, the inflammable gas that the high molecular polymer decomposes is discharged is diluted and reach fire-retardant effect;
Additive such as redispersible latex powder, hydroxyethylmethyl-cellulose, adhesive property, the rheological property of adjustment gelling material improve volume stability;
The water-based wetting dispersing agent, a kind of inorganic paint auxiliary agent is applicable to the moistening dispersion of inorganic paint, keeps the good dispersiveness of slip and mobile, the color development power and the gloss of raising coating that can be bigger;
Vinylformic acid double cyclopentenyl oxygen ethyl ester, a kind of film coalescence aid of inorganic paint can reduce the second-order transition temperature of coating; Under film forming environment, carry out polymerization and crosslinked automatically; Become the composition part of film, can reach than better hardness of former coating film forming and gloss, itself does not cause the pollution to environment; Non-volatile, and have permanent stability after in being fitted on coating.
It is a kind of environment-friendly type, nontoxic, the low pollution that gained of the present invention water-soluble do not fired ceramic radiation shielding coating; Volatile Organic Compound (VOC) value is 0, fire resistance is the inorganic paint of A level; Describedly water-solublely do not fire that ceramic radiation shielding coating thickness can be 0.7~3mm, has high durable impervious waterproof, highly effective flame-retardant fire prevention, efficient radioprotective and the incorporate inorganic paint of composite thermal insulation; This coating can be used as exterior coating (primary coat), can be used as also that outer wall board heat preservation plate material surface, mortar are surperficial, the supercoat of vitrified brick, enclosure of buildings structure.
Described process of the present invention does, base treatment → water-soluble is not fired the water-soluble brushing of not firing ceramic radiation shielding coating of the preparation of ceramic radiation shielding coating → in basic unit, carry out or spraying → at its external coating one deck modified fluoro-silicone emulsion.
It is described that water-soluble not fire ceramic radiation shielding coating surface drying time be 1.65h.
Water-soluble cohesive strength of not firing ceramic coating is >=0.57MPa.
Water-soluble do not fire ceramic coating through water-fast test (500h), alkaline-resisting test (300h), freeze-thaw cycle test (10 times) after, do not have softening, do not have and bubble, do not have peeling phenomenon, do not have powder phenomenon-tion, do not have obvious variable color.
The present invention compared with prior art has following main advantage:
1. the high durable and feature of environmental protection: utilize material prepn environment-friendly type, nontoxic, low pollutions such as blast-furnace cinder micro-powder, Volatile Organic Compound (VOC) value is 0, fire resistance is the inorganic paint of A level, the Si (OH) of water glass solution formation in the coating 4The Ca (OH) that can form with breeze vitreum alkalization 2Reaction generates the fine and close cancellated hydrated calcium silicate gel of silica, and the system that makes has higher cohesive strength and low-heat seepage flow coefficient more; The gas phase nano silicon-dioxide that adds can effectively play radioprotective, function such as anti-aging.Have quality controllable, anti-water, alkaline-resisting, freeze-thawing resistant, lightweight, cracking resistance, anti-hollowing, anti-performance characteristics such as come off, improved the weather resistance of coating.
2. high-grade flame retardant resistance: coating system has added the modification expansible black lead; This efficient flame-retarding agent have strong resistance to pressure, snappiness, plasticity-and self lubricity, extremely strong anti-high and low temperature, anticorrosive, radioprotective characteristic, extremely strong shock-resistance features and electric conductivity, extremely strong anti-aging, anti-twist characteristic, nontoxic, do not contain any carcinogens; And the fusing that can resist various metals and the characteristics of infiltration are arranged; Can under comparatively high temps, can produce volume and expand significantly or produce foam-like material, be covered in coatingsurface, form stable heat insulation coating; Play secluding air, effectively insulating effect; Thereby reach fire-retardant purpose,, also can produce CO because of being heated according to the difference of binding substance 2, NH 3, H 2Non-flammable gases such as O, the inflammable gas that high-temperature heating decompose to be discharged is diluted and reach fire-retardant effect.
3. efficient radioprotective and complex heat-preservation effect: in coating system, added efficient radiation-resistant gas phase nano silicon-dioxide; Has extremely strong uv-absorbing; The infrared external reflection characteristic; And weakened thermal-radiating transmission greatly and reduced hot seep effect, use the effect that can play complex heat-preservation simultaneously with the insulation body material.
Embodiment:
Below in conjunction with embodiment the present invention is described further, but not only is confined to following embodiment.
Embodiment 1:
1) modification Preparation of Expansible Graphite: crystalline flake graphite, ydrogen peroxide 50 and nitrosonitric acid are mixed, in ice-water bath, stir rapidly, to reaction mild after with this reaction system constant temperature at 25 ℃; Behind washing, suction filtration, drip the acetic acid soln of content >=99.5% and constantly stir reaction 60min; Washing; Suction filtration, oven dry must not have sulphur and does not have ash content modification expansible black lead; Expanding volume is 300-350ml/g, and wherein the ratio of crystalline flake graphite, nitrosonitric acid, ydrogen peroxide 50, acetate is 5 (g): 12 (ml): 1 (ml): 5 (ml);
2) particle diameter of each solid material control: with breeze, silicon ash, talcum powder, mica powder, redispersible latex powder, hydroxyethylmethyl-cellulose etc. levigate to particle size distribution at 10~40 μ m; Particle is slick and sly, and macrobead is with less with the particle of sharp-pointed water caltrop;
3) water-soluble preparation of not firing ceramic radiation shielding coating: with active material, mineral filler, redispersible latex powder, hydroxyethylmethyl-cellulose, modification expansible black lead, water glass, gas phase nano silicon-dioxide, auxiliary agent according to mass ratio 2.67: 0.7: 0.4: 0.03: 0.53: 2.13: 0.07: 0.3 thorough mixing promptly got the water-soluble ceramic radiation shielding coating that do not fire after evenly.Wherein: described active material is that breeze and silicon ash are formed according to mass ratio at 5.675: 1; Described mineral filler is that talcum powder and mica powder are that mixing in 2: 1 is formed by mass ratio; Said auxiliary agent is that silok7110 water-based wetting dispersing agent and vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid are that mixing in 2: 1.3 is formed according to mass ratio.
All the other each main raw material chemical ingredientss of the present invention, physicals are seen table 1-7 respectively.
Above-mentioned water-soluble physicals of not firing ceramic radiation shielding coating material is used, and experimental result is seen table 8.
Embodiment 2:
1) modification Preparation of Expansible Graphite: according to quality than crystalline flake graphite: KMnO 4=1: 0.3 ratio adds KMnO in crystalline flake graphite 4, stir, add 70% HClO 3Solution, to keep solid-to-liquid ratio be that 1: 4 ratio keeps 35 ℃ of intermittently stirring reaction 90min, after washing, and suction filtration, oven dry can obtain the modification expansible black lead, and expanding volume is 550ml/g;
2) particle diameter of each solid material control: with breeze, silicon ash, talcum powder, mica powder, zinc barium powder, redispersible latex powder, hydroxyethylmethyl-cellulose etc. levigate to particle size distribution at 10~40 μ m; Particle is slick and sly, and macrobead is with less with the particle of sharp-pointed water caltrop;
3) water-soluble preparation of not firing ceramic radiation shielding coating: with active material, mineral filler, redispersible latex powder, hydroxyethylmethyl-cellulose, modification expansible black lead, water glass, gas phase nano silicon-dioxide, auxiliary agent by mass ratio 2.66: 0.77: 0.4: 0.033: 0.47: 2.13: 0.1: 0.3 thorough mixing promptly got the water-soluble ceramic radiation shielding coating that do not fire after evenly.Wherein: described active material is that breeze and silicon ash are formed according to mass ratio at 7: 1; Described mineral filler is that talcum powder, mica powder and zinc barium powder are that mixing in 1: 0.5: 2 is formed by mass ratio; Said auxiliary agent is that silok7110 water-based wetting dispersing agent and vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid are that mixing in 2: 1.3 is formed according to mass ratio.
Embodiment 3:
1) modification Preparation of Expansible Graphite: according to quality than crystalline flake graphite: KMnO 4=1: 0.35 ratio adds KMnO in crystalline flake graphite 4, stir, add 70% HClO 3Solution, to keep solid-to-liquid ratio be that 1: 4 ratio keeps 35 ℃ of intermittently stirring reaction 90min, after washing, and suction filtration, oven dry can obtain the modification expansible black lead, and expanding volume is 550ml/g;
2) particle diameter of each solid material control: with breeze, silicon ash, talcum powder, mica powder, white titanium pigment, redispersible latex powder, hydroxyethylmethyl-cellulose etc. levigate to particle size distribution at 10~40 μ m; Particle is slick and sly, and macrobead is with less with the particle of sharp-pointed water caltrop.
3) water-soluble preparation of not firing ceramic radiation shielding coating: with active material, mineral filler, redispersible latex powder, hydroxyethylmethyl-cellulose, modification expansible black lead, water glass, gas phase nano silicon-dioxide, auxiliary agent according to mass ratio 2.4: 0.7: 0.4: 0.033: 0.8: 2.13: 0.2: 0.3 thorough mixing promptly got the water-soluble ceramic radiation shielding coating that do not fire after evenly.Wherein: described active material is that breeze and silicon ash are formed according to mass ratio at 7.9: 1; Described mineral filler is that talcum powder, mica powder and white titanium pigment are that mixing in 3: 1: 1 is formed by mass ratio; Said auxiliary agent is that silok7110 water-based wetting dispersing agent and vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid are that mixing in 2: 1.3 is formed according to mass ratio.
Embodiment 4:
1) modification Preparation of Expansible Graphite: with crystalline flake graphite, ydrogen peroxide 50, nitrosonitric acid, in ice-water bath, stir rapidly, to reaction mild after with this reaction system constant temperature at 25 ℃; Behind washing, suction filtration, drip the acetic acid soln of content >=99.5% and constantly stir reaction 60min; Washing; Suction filtration, oven dry must not have sulphur and does not have ash content modification expansible black lead; Expanding volume is 300-350ml/g, and wherein the ratio of crystalline flake graphite, nitrosonitric acid, ydrogen peroxide 50, acetate is 5 (g): 12 (ml): 1 (ml): 5 (ml);
2) particle diameter of each solid material control: with breeze, silicon ash, talcum powder, zinc barium powder, ferric oxide yellow pigment, redispersible latex powder, hydroxyethylmethyl-cellulose etc. levigate to particle size distribution at 10~40 μ m; Particle is slick and sly, macrobead with the less talcum powder of the particle of sharp-pointed water caltrop, zinc barium powder and ferric oxide yellow pigment;
3. water-soluble preparation of not firing ceramic radiation shielding coating: with active material, mineral filler, redispersible latex powder, hydroxyethylmethyl-cellulose, modification expansible black lead, water glass, gas phase nano silicon-dioxide, auxiliary agent by mass ratio 2.6: 0.77: 0.4: 0.033: 0.4: 2.13: 0.15: 0.3 thorough mixing promptly got the water-soluble ceramic radiation shielding coating that do not fire after evenly.Wherein: described active material is that breeze and silicon ash are formed according to mass ratio at 10: 1; Described mineral filler is that talcum powder, zinc barium powder and ferric oxide yellow pigment are that mixing in 3: 1: 1 is formed by mass ratio; Said auxiliary agent is that silok7110 water-based wetting dispersing agent and vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid are that mixing in 2: 1.3 is formed according to mass ratio.
Subordinate list
Chemical analysis/the Wt% of table 1 breeze
Chemical analysis/the Wt% of table 2 silicon ash
The physical parameter of table 3 silicon ash
Table 4 gas phase nano silicon-dioxide parameter
Table 5 redispersible latex powder physicals
Table 6silok7110 water-based wetting dispersing agent parameter
Table 7 vinylformic acid double cyclopentenyl oxygen ethyl ester parameter
Table 8 experimental result

Claims (7)

1. one kind does not water-solublely fire ceramic radiation shielding coating; It is characterized in that its component and component concentration thereof count by mass ratio: active material: mineral filler: economization agent: thickening material: fire retardant: silicate bond: reflection enhancement agent: auxiliary agent=2 ~ 2.8:0.5 ~ 1:0.40:0.01-0.04:0.4 ~ 0.8:2.13:0.067 ~ 0.2:0.3; Wherein, described reflection enhancement agent is a gas phase nano silicon-dioxide, and described fire retardant is the modification expansible black lead; Described silicate bond is a water glass; Its modulus n is 2.2 ~ 2.5, and described economization agent is a redispersible latex powder, and described thickening material is a hydroxyethylmethyl-cellulose.
2. by the described water-soluble ceramic radiation shielding coating that do not fire of claim 1, it is characterized in that described active material is the mixture of breeze and silicon ash, and the mass ratio of breeze and silicon ash is not less than 5:1.
3. by claim 1 or the 2 described water-soluble ceramic radiation shielding coatings that do not fire; It is characterized in that described mineral filler is any one or the multiple mixing in talcum powder, mica powder and the pigment, wherein said pigment is any one or the multiple mixing in white titanium pigment, zinc barium powder, chromate or the iron oxide pigment.
4. by the described water-soluble ceramic radiation shielding coating that do not fire of claim 3, it is characterized in that described modification Preparation of Expansible Graphite method is that crystalline flake graphite, ydrogen peroxide 50 and nitrosonitric acid are mixed, and in ice-water bath, stir rapidly; To reaction mild after with this reaction system constant temperature at 25 ℃, washing, suction filtration drip acetic acid soln and constantly stir; Reaction 60 ~ 120min, washing, suction filtration; Oven dry gets the modification expansible black lead.
5. by the described water-soluble ceramic radiation shielding coating that do not fire of claim 3, it is characterized in that described modification Preparation of Expansible Graphite method is than crystalline flake graphite: KMnO according to quality 4The ratio of=1:0.2 ~ 0.4 adds KMnO in crystalline flake graphite 4, stir, add HClO 3Solution also keeps 35 ℃ of intermittently stirring reaction 60 ~ 120min, washing then, and suction filtration, oven dry can obtain the modification expansible black lead.
6. by claim 4 or the 5 described water-soluble ceramic radiation shielding coatings that do not fire, it is characterized in that described auxiliary agent is that silok7110 water-based wetting dispersing agent and the vinylformic acid double cyclopentenyl oxygen ethyl ester film coalescence aid of silok company is that 2:1.3 mixes and forms according to mass ratio.
7. each described water-soluble preparation method of not firing ceramic radiation shielding coating of claim 1-6; It is characterized in that including following steps: with active material: mineral filler: economization agent: thickening material: fire retardant: silicate bond: reflection enhancement agent: auxiliary agent=2 ~ 2.8:0.5 ~ 1:0.40:0.01-0.04:0.4 ~ 0.8:2.13:0.067 ~ 0.2:0.3 thorough mixing can be brushed or sprayed after evenly; Behind the coating surface drying at its external coating one deck modified fluoro-silicone emulsion; Wherein, described reflection enhancement agent is a gas phase nano silicon-dioxide, and described fire retardant is the modification expansible black lead; Described silicate bond is a water glass; Its modulus n is 2.2 ~ 2.5, and described thickening material is a hydroxyethylmethyl-cellulose, and described economization agent is a redispersible latex powder.
CN201210006491.1A 2012-01-09 2012-01-09 Water-soluble non-combustible ceramic anti-radiation coating and preparation method thereof CN102585570B (en)

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