CN103525131A - Heat-resistant yellow hydrous iron oxide pigment and manufacturing method thereof, and paint and resin composition using same pigment - Google Patents
Heat-resistant yellow hydrous iron oxide pigment and manufacturing method thereof, and paint and resin composition using same pigment Download PDFInfo
- Publication number
- CN103525131A CN103525131A CN201310269881.2A CN201310269881A CN103525131A CN 103525131 A CN103525131 A CN 103525131A CN 201310269881 A CN201310269881 A CN 201310269881A CN 103525131 A CN103525131 A CN 103525131A
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- CN
- China
- Prior art keywords
- ferric oxide
- hydrous ferric
- thermotolerance
- yellow
- oxide pigment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 146
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- GFMIDCCZJUXASS-UHFFFAOYSA-N hexane-1,1,6-triol Chemical compound OCCCCCC(O)O GFMIDCCZJUXASS-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- MOUPNEIJQCETIW-UHFFFAOYSA-N lead chromate Chemical compound [Pb+2].[O-][Cr]([O-])(=O)=O MOUPNEIJQCETIW-UHFFFAOYSA-N 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
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- 238000013507 mapping Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 210000004681 ovum Anatomy 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 229920002401 polyacrylamide Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
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- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
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- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
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- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
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- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
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- 229940083466 soybean lecithin Drugs 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- NVKTUNLPFJHLCG-UHFFFAOYSA-N strontium chromate Chemical compound [Sr+2].[O-][Cr]([O-])(=O)=O NVKTUNLPFJHLCG-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
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- 229940036248 turpentine Drugs 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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Landscapes
- Paints Or Removers (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a yellow hydrous iron oxide pigment with excellent heat resistance and dispersity, and a simple manufacturing method thereof. According to the heat-resistant yellow hydrous iron oxide pigment, the surface of a hydrous iron oxide particle is coated by a mixture containing aluminium silicate and high-molecular compounds, and the pigment can be obtained by adding a mixture, which mainly contains a mixture of inorganic compounds at least mainly containing clay minerals and the high-molecular compounds, to an aqueous dispersion containing hydrous iron oxide particles for processing, and forming an aluminium silicate hydroxide layer.
Description
Technical field
The present invention relates to have excellent thermotolerance and dispersed yellow hydrous ferric oxide pigment (yellow ultramarine being formed by the ferric oxide that comprises crystal water) and easy manufacture method thereof.
Background technology
The coloured material that yellow ultramarine is used as resin, coating, road pavement is used widely.Particularly road bitumen mat formation and coiled material coating in, need the thermotolerance of 250 ℃ of left and right.
As yellow ultramarine, conventionally use the situation of the materials such as lead chromate, strontium yellow, Cadmium Sulfide more.Although just the excellent heat resistance of these materials, toxic, also has carinogenicity, so it uses existing problems.
On the other hand, yellow hydrous ferric oxide pigment is used in the various uses such as resin, coating, ink, due to its nontoxicity, is the material to human-body safety, also very excellent as the material of environmental protection in addition.But, relating to thermotolerance, it is problem russet 230 ℃ of left and right variable colors that existence is followed in the disengaging of 200 ℃ of left and right crystal water.
Therefore, when conventionally in the thermoplastic resins such as the polyethylene of more than 200 ℃ forming process, polypropylene, styrene polymer, polymeric amide, polyolefine, ABS, the coating curing in 200～250 ℃ of left and right or construction, be heated to more than 200 ℃ or the road marking of melting use with being difficult to use yellow hydrous ferric oxide pigment in coating.
As the solution countermeasure of such problem, for example, report has the method (with reference to patent documentation 1) of hydrous ferric oxide particle being carried out hydrothermal treatment consists in autoclave in water or alkali aqueous solution.
In addition, also report has the method (with reference to patent documentation 2,3) of using the coated hydrous ferric oxide particles such as aluminum compound, silicon compound in autoclave.
Also report the surperficial method (with reference to patent documentation 4) of the coated hydrous ferric oxide particle of hydrous oxide that useful Al forms.
Also report the surperficial method (with reference to patent documentation 5,6,7) of the coated hydrous ferric oxide particle of hydrous oxide that useful Fe and Al form.
In addition proposed in autoclave with (AlO),
xpO
4(OH)
x-3the surperficial method (with reference to patent documentation 8) of the aluminum compound coated iron oxide representing.
Prior art document
Patent documentation
Patent documentation 1: Japanese kokai publication sho 50-115698 communique
Patent documentation 2: Japanese kokai publication sho 55-158130 communique
Patent documentation 3: Japanese kokai publication sho 53-034827 communique
Patent documentation 4: Japanese kokai publication hei 9-165531 communique
Patent documentation 5: Japanese kokai publication hei 11-012492 communique
Patent documentation 6: Japanese kokai publication hei 11-012491 communique
Patent documentation 7: TOHKEMY 2000-191938 communique
Patent documentation 8: Japanese kokai publication sho 62-112661 communique
Summary of the invention
Invent problem to be solved
Require the most not use now special device convenient disposal, carry out improved heat resistance processing, yellow hydrous ferric oxide pigment and the manufacture method thereof of the with low uncertainty and excellent dispersion of the form and aspect before and after processing.
That is, utilize above-mentioned (1) method to carry out the yellow hydrous ferric oxide pigment of processing, thermotolerance improves, but the form of particle and size-grade distribution alter a great deal before and after improved heat resistance treatment process,, can there is dispersed problem in its result, and the variation of form and aspect is also large.
The method of above-mentioned (2), (3), (8) is to process in autoclave, can not think easy method.
In addition, the method for above-mentioned (4), (5), (6), any all needs high purityization to process before heat-resisting processing,, needs to adjust the processing of pH or heating before heat-resisting processing that is, processes and needs the plenty of time, can not think easy method.
For solving the method for problem
Above-mentioned technical task, reaches by following the present invention.
That is, the yellow hydrous ferric oxide pigment of a kind of thermotolerance of the present invention, is characterized in that, the particle surface of hydrous ferric oxide particle is by comprising the clay mineral that contains pure aluminium silicate and the mixture coated (the present invention 1) of macromolecular compound.
In addition, the present invention is the yellow hydrous ferric oxide pigment of the thermotolerance described in the present invention 1, and wherein, the content of pure aluminium silicate is 2～50 % by weight (the present invention 2) with respect to hydrous ferric oxide particle.
In addition, the present invention is the yellow hydrous ferric oxide pigment of the thermotolerance described in the present invention 1 or 2, and wherein, the content of macromolecular compound is 0.1～2 % by weight (the present invention 3) with respect to hydrous ferric oxide particle.
In addition, the present invention is the yellow hydrous ferric oxide pigment of a kind of thermotolerance, wherein, the particle surface of hydrous ferric oxide particle is coated by comprising the mixture of the clay mineral that contains pure aluminium silicate and macromolecular compound, then by a kind or two or more compound coated (the present invention 4) being selected from rosin compound, Yelkin TTS, sorbitan acid esters, oleic acid.
In addition, the present invention is the manufacture method of the yellow hydrous ferric oxide pigment of a kind of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in the present invention 1～3, in this manufacture method, in the aqueous dispersions that contains hydrous ferric oxide particle, add and at least mainly contain the mineral compound of clay mineral and the mixture of macromolecular compound is processed, thus, at the particle surface of hydrous ferric oxide particle, form the hydroxide layer (the present invention 5) of pure aluminium silicate.
In addition, the present invention is the manufacture method of the yellow hydrous ferric oxide pigment of a kind of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in the present invention 1～3, in this manufacture method, after in the aqueous dispersions that contains hydrous ferric oxide particle, interpolation at least mainly contains the mineral compound of clay mineral, add macromolecular compound and process, thus, at the particle surface of hydrous ferric oxide particle, form the hydroxide layer (the present invention 6) of pure aluminium silicate.
In addition, the present invention is the manufacture method of the yellow hydrous ferric oxide pigment of a kind of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in the present invention 1～3, in this manufacture method, add macromolecular compound in the aqueous dispersions that contains hydrous ferric oxide particle after, add the mineral compound at least mainly contain clay mineral and process, at the particle surface of hydrous ferric oxide particle, form thus the hydroxide layer (the present invention 7) of pure aluminium silicate.
In addition, the present invention is the manufacture method of the yellow hydrous ferric oxide pigment of a kind of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in the present invention 4, in this manufacture method, the yellow hydrous ferric oxide pigment obtaining for the manufacture method of utilizing the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in the present invention 5～7, use dry mixer, with the one kind or two or more compound being selected from rosin compound, Yelkin TTS, sorbitan acid esters, oleic acid, carry out surface treatment (the present invention 8).
In addition, the present invention is a kind of coating, it is characterized in that, it is (the present invention 9) that form by the yellow hydrous ferric oxide pigment of thermotolerance described in any one coordinate the present invention 1～4 in coating formation base material in.
The present invention is a kind of resin combination, it is characterized in that, its be the application of the invention 1～4 in the yellow hydrous ferric oxide pigment of thermotolerance described in any one carry out painted (the present invention 10) that obtain.
The effect of invention
The yellow hydrous ferric oxide pigment of thermotolerance of the present invention is to have excellent thermotolerance and dispersed yellow hydrous ferric oxide pigment, is suitable as stable on heating yellow ultramarine.
The manufacture method of the yellow hydrous ferric oxide pigment of thermotolerance of the present invention, for not use the easy processing of special device, carry out the processing that improved heat resistance is processed and dispersiveness is improved, the foxy before and after processing is few, and the manufacture method of the yellow hydrous ferric oxide pigment of excellent dispersion.
Embodiment
Be described in more detail technical scheme of the present invention, as follows.
With regard to the yellow hydrous ferric oxide pigment of thermotolerance of the present invention, in the aqueous dispersions of yellow hydrous ferric oxide particle, making at least to take clay mineral is that mineral compound and the macromolecular compound of leading exists, mix and make its reaction, thus, can form at the particle surface of this yellow hydrous ferric oxide particle the layer of the oxyhydroxide of pure aluminium silicate.
Hydrous ferric oxide particle of the present invention be shaped as fusiform, needle-like or grain of rice shape.
The average major axis footpath of hydrous ferric oxide particle of the present invention is 0.1～1.0 μ m, is preferably 0.15～0.6 μ m.In the situation of average major axis footpath less than 0.1 μ m, the surface-area based on being caused by fine particles increases, and intergranular cohesive force increases, difficulties in dispersion in resin combination or vehicle.On the other hand, surpass in the situation of 1.0 μ m, be accompanied by macrobead, be difficult in resin combination or vehicle dispersed.
Hydrous ferric oxide particle of the present invention, average short shaft diameter is 0.01～0.20 μ m, more preferably 0.012～0.15 μ m.In the situation of average short shaft diameter less than 0.01 μ m, the surface-area based on being caused by fine particles increases, and intergranular cohesive force increases, difficulties in dispersion in resin combination or vehicle.On the other hand, surpass in the situation of 0.20 μ m, be accompanied by macrobead, be difficult in resin combination or vehicle dispersed.
Hydrous ferric oxide particle of the present invention, axial ratio (average major axis footpath/average short shaft diameter) is 2～20, more preferably 2.5～18.In the situation of axial ratio less than 2, be difficult to obtain thering is filming of sufficient rigidity.On the other hand, axial ratio surpasses 20, and the entanglement of the particle in vehicle is many, bad dispersibility, and viscosity increases.
The BET specific surface area of hydrous ferric oxide particle of the present invention is 10～180m
2/ g, more preferably 10～150m
2/ g.BET specific surface area is 10～180m preferably
2the reason of/g is identical with the reason of lower value with the average higher limit of short shaft diameter with average major axis footpath.
Clay mineral of the present invention refers to the general name of the silicate minerals that forms clay, refers to the compound that the metal ion of aluminium, sodium, calcium etc. and sheet that silicic acid links can form stratiform.Specifically, can use wilkinite, zeolite, kaolin, polynite, chlorite etc.
Outside these clay minerals, can also add the metal oxides such as calcium oxide, magnesium oxide.
Due to according to their form and aspect of the place of production separately, form and have small difference, so preferably as far as possible for particulate and connect subalbous form and aspect.
In addition, as macromolecular compound of the present invention, preferably there is cationic macromolecular compound.Specifically, the macromolecular compound of preferred polyamine class, Dyhard RU 100 class, polyacrylamide, PMAm class, esters of acrylic acid.The molecular weight of macromolecular compound is generally 100,000～1,000 ten thousand, is preferably 1,000,000～1,000 ten thousand.
The addition of clay mineral, is preferably 2～50 % by weight with respect to hydrous ferric oxide particle, more preferably 10～30 % by weight.The addition of clay mineral is less than in the situation of 2 % by weight, and the thermotolerance of the yellow hydrous ferric oxide pigment obtaining is inadequate, surpasses in the situation of 50 % by weight, and the form and aspect of yellow hydrous ferric oxide pigment change.
The addition of macromolecular compound, is preferably 0.1～2.0 % by weight with respect to hydrous ferric oxide particle, more preferably 0.2～1.0 % by weight.The addition of macromolecular compound is less than in the situation of 0.1 % by weight, and the thermotolerance of the yellow hydrous ferric oxide pigment obtaining is inadequate, surpasses in the situation of 2.0 % by weight, and the amount of moisture of yellow hydrous ferric oxide pigment increases, and form and aspect change.
In addition, the metal oxide adding on the basis of clay mineral, can add 0～10 % by weight left and right with respect to clay mineral.Add and surpass in the situation of 10 % by weight, according to circumstances likely cause foxy.
Heat-resisting processing of the present invention, first, with respect to the aqueous dispersions of 3～10 % by weight concentration of hydrous ferric oxide particle, add and at least take clay mineral as main mineral compound and the mixture of macromolecular compound, make its ℃ reaction about 10 minutes～1 hour in room temperature～80.PH is now 3～11 scope, does not need special adjustment.Reaction finishes rear cool to room temperature, afterwards, adjusts as required the scope of pH to 6～8, then by filtering, dry predetermined processing, can access yellow oxidizing aqueous iron powder body.
Equally, first, with respect to the aqueous dispersions of 3～10 % by weight concentration of hydrous ferric oxide particle, add and at least take clay mineral as main mineral compound, ℃ reaction is after 30 minutes～1 hour in room temperature～80 to make it, and interpolation macromolecular compound, said temperature reaction 30 minutes～1 hour.After reaction finishes, with above-mentioned same, cool to room temperature, filters, dry predetermined processing afterwards, can access yellow oxidizing aqueous iron powder body.
In addition, with respect to the aqueous dispersions of 3～10 % by weight concentration of hydrous ferric oxide particle, add macromolecular compound, make its ℃ reaction after 30 minutes～1 hour in room temperature～80, add and at least take clay mineral as main mineral compound, said temperature reaction 30 minutes～1 hour.After reaction finishes, with above-mentioned same, cool to room temperature, filters, dry predetermined processing afterwards, obtains yellow oxidizing aqueous iron powder body.
Then, the yellow hydrous ferric oxide pigment of thermotolerance of the present invention is described.
Yellow hydrous ferric oxide pigment of the present invention be shaped as fusiform, needle-like or grain of rice shape.
The average major axis footpath of yellow hydrous ferric oxide pigment of the present invention is 0.1～1.0 μ m, is preferably 0.15～0.6 μ m.In the situation of average major axis footpath less than 0.1 μ m, the surface-area based on being caused by fine particles increases, and intergranular cohesive force increases, and is difficult to disperse in resin combination or vehicle.On the other hand, surpass in the situation of 1.0 μ m, be accompanied by macrobead, be difficult in resin combination or vehicle dispersed.
The average short shaft diameter of the yellow hydrous ferric oxide pigment in the present invention is 0.01～0.20 μ m, is preferably 0.012～0.15 μ m.In the situation of average short shaft diameter less than 0.01 μ m, the surface-area based on being caused by fine particles increases, and intergranular cohesive force increases, and is difficult to disperse in resin combination or vehicle.On the other hand, surpass in the situation of 0.20 μ m, be accompanied by macrobead, be difficult in resin combination or vehicle dispersed.
The axial ratio of yellow hydrous ferric oxide pigment of the present invention (average major axis footpath/average short shaft diameter) is 2～20, more preferably 2.5～18.In the situation of axial ratio less than 2, be difficult to obtain thering is filming of sufficient rigidity.On the other hand, axial ratio surpasses in 20 situation, and the entanglement of the particle in vehicle is many, bad dispersibility sometimes, and viscosity can increase.
The BET specific surface area of yellow hydrous ferric oxide pigment of the present invention is 10～180m
2/ g, more preferably 10～150m
2/ g.BET specific surface area is 10～180m preferably
2the reason of/g is identical with the reason of lower value with the average higher limit of short shaft diameter with average major axis footpath.
The thermotolerance of yellow hydrous ferric oxide pigment of the present invention is preferably more than 250 ℃.During 250 ℃ of thermotolerance less thaies, cannot reach object of the present invention.
In addition, thermotolerance of the present invention, according to evaluation method evaluation described later.
The form and aspect of yellow hydrous ferric oxide pigment of the present invention, preferably L* value is that 40～80, a* value is-30～+ 35, b* value is+30～+ 100 scope.L* value, a* value, b* value, in above-mentioned extraneous situation, cannot obtain the yellow ultramarine as the object of the invention.
Yellow hydrous ferric oxide pigment optimization of the present invention is coated processing with the further effects on surface of following material.That is, as for the coated material of processing in surface, can use any or combination separately of rosin compound, Yelkin TTS, sorbitan ester compound, oleic acid.They any can both expect to make the effect that lipophilicity improves, oil number reduces of surface of pigments.As a result of, can reduce the viscosity of coating.
As rosin compound, can use rosin, tallol rosin, modified rosin, rosin ester etc.
As Yelkin TTS, can use soybean lecithin, Ovum Gallus domesticus Flavus lecithin.
As sorbitan ester compound, can use sorbitan monostearate, sorbitan tristearate, sorbitan monolaurate, dehydrated sorbitol mono-fatty acid ester, span 40 etc., there is the compound of a plurality of change gamma values in them.
The surface that utilizes these materials to carry out is coated, with respect to yellow hydrous ferric oxide pigment, is preferably that 0.5～5 % by weight is processed.More preferably 0.5～2 % by weight is processed.
The surface that utilizes these materials to carry out is coated, uses the dry mixers such as Henschel mixer, nauta mixer, mortar mixer to carry out, easy so preferably.In these handlers, add specified amount enforcement resistance to heat treated yellow hydrous ferric oxide pigment, then finish materials directly added or add with the form of dissolving in suitable solvent, carry out the combination treatment of specified time, can access thus the yellow hydrous ferric oxide pigment of thermotolerance of excellent dispersion.
Then, to being combined with the coating of yellow hydrous ferric oxide pigment of the present invention, describe.
The mixing ratio of the yellow hydrous ferric oxide pigment in coating of the present invention, can take and form with respect to coating the scope use that base material 100 weight parts are 0.5～100 weight part.If consider the operability of coating, be preferably 1.0～100 weight parts.
As coating, form base material, coordinate resin, solvent, coordinate as required grease, defoamer, pigment extender, dry promotor, tensio-active agent, curing catalyst, auxiliary agent etc.
As resin, can use solvent based coating with or oiliness printing-ink in modified rosin resin, the petroleum resin etc. such as rosin based resin, maleic acid resin, polyamide resin, Nitrocellulose, ethane-acetic acid ethyenyl ester copolymer resins, rosin modified phenolic resin, Abietyl modified maleic acid resin such as normally used acrylic resin, Synolac, vibrin, urethane resin, epoxy resin, resol, melamine resin, aminoresin, vinyl chloride resin, silicone resin, rosin, limed rosin.As water class coating use, can make water class coating use, the normally used water soluble acrylic resin of water color ink, water-soluble phenylethene-maleic acid resin, water soluble alkyd resin, water-soluble melamine resin, aqurous ployurethane emulsion resin, water-soluble epoxy resin, Polyester Resin Water Soluble etc.
As solvent, can use normally used soybean oil in solvent based coating use, toluene, dimethylbenzene, thinner (thinner), butylacetate, methyl acetate, mibk, methylcyclohexane, ethyl cellosolve, propyl cellosolve, ethylene glycol butyl ether, the glycol ethers solvents such as propylene glycol monomethyl ether, ethyl acetate, butylacetate, the esters solvents such as pentyl acetate, hexane, heptane, the aliphatic hydrocarbon kind solvents such as octane, the clicyclic hydrocarbon kind solvents such as hexanaphthene, the petroleum-type solvents such as mineral turpentine, acetone, the ketones solvents such as methylethylketone, methyl alcohol, ethanol, propyl alcohol, the alcoholic solvents such as butanols, aliphatic hydrocarbon etc.
As water class coating solvent, can with water and water class coating with in the ethylene oxides such as glycol ethers solvent, diethylene glycol, triglycol, polyoxyethylene glycol, dipropylene glycol, tripropylene glycol, polypropylene glycol such as alcoholic solvent, methylcyclohexane, ethyl cellosolve, propyl cellosolve, ethylene glycol butyl ether such as normally used ethanol, propyl alcohol, butanols or propylene oxide addition polymer, ethylene glycol, propylene glycol, 1, the water-miscible organic solvents such as the aklylene glycols such as 2,6-hexanetriol, glycerine, 2-Pyrrolidone mix use.
As grease, can use the stand oil that linseed oil, tung oil, fork oil, the processing of safflower wet goods siccative oil are obtained.
As defoamer, can use Nopco8034(trade(brand)name), SN Defoamer477(trade(brand)name), SN Defoamer5013(trade(brand)name), SN Defoamer247(trade(brand)name), SN Defoamer382(trade(brand)name) (above any be San Nopco Co., Ltd. manufacture), Antifoam08(trade(brand)name), Emulgen903(trade(brand)name) commercially available product of (any is Kao Corp's manufacture above) etc.
Then, the resin combination that contains yellow hydrous ferric oxide pigment of the present invention is described.
The mixing ratio of the yellow hydrous ferric oxide pigment in resin combination of the present invention, is used with the scope of 0.01～200 weight part with respect to 100 parts by weight resin.Consider the operability of resin combination, be preferably 0.05～150 weight part, more preferably 0.1～100 weight part.
As the formation base material in resin combination of the present invention, together with known thermoplastic resin, as required, can coordinate the additives such as lubricant, softening agent, antioxidant, UV light absorber, various stablizers with yellow hydrous ferric oxide pigment.
As resin, can use polyethylene, polypropylene, polybutene, the polyolefine such as polyisobutene, polyvinyl chloride, polymethylpentene, polyethylene terephthalate, polybutylene terephthalate, polystyrene, copolymer in cinnamic acrylic ester, vinylbenzene-vinyl acetate copolymer, acrylonitrile-butadiene-styrene copolymer, vinyl cyanide-EPDM-styrol copolymer, acrylic resin, polymeric amide, polycarbonate, polyacetal, the thermoplastic resins such as urethane, Abietyl modified maleic acid resin, resol, epoxy resin, vibrin, silicone resin, rosin-ester, rosin, natural rubber, synthetic rubber etc.
The amount of additive is below 50% with respect to the summation of yellow hydrous ferric oxide pigment and resin.The content of additive surpasses in the situation of 50 % by weight, and formability reduces.
Resin combination of the present invention, fully hybrid resin raw material and yellow hydrous ferric oxide pigment in advance, then, use mixing roll or forcing machine, under heating, apply strong shearing action, destroy the aggregate of yellow hydrous ferric oxide pigment, dispersed yellow hydrous ferric oxide pigment in resin combination, then forming process is for to be used corresponding to the shape of object.
Resin combination of the present invention also can obtain via masterbatch pellet.
Masterbatch pellet of the present invention, as required using the matrix material resin of the formation base material as coating and resin combination and above-mentioned yellow hydrous ferric oxide pigment, after mixing with mixing machines such as ribbon blender, nauta mixer, Henschel mixer, superhigh speed mixing machines, with mixing, moulding such as known single-screw intermixing extruder or twin-screw mixer forcing machines, cut off afterwards or with Banbury, mixing said mixture such as pressurization kneading machine etc., by the mixing thing pulverizing obtaining or moulding, cut-out, manufacture thus.
Matrix material resin and yellow hydrous ferric oxide pigment, to the supply of mixing roll, can, with the ratio difference weight feed of regulation, also can be supplied with both mixtures.
The average major diameter of masterbatch pellet of the present invention is 1～6mm, preferably the scope of 2～5mm.Average minor axis is 2～5mm, is preferably 2.5～4mm.In the situation of the not enough 1mm of average major diameter, operability when pellet is manufactured is poor and not preferred.Surpass in the situation of 6mm, large by the big or small gap of matrix material resin with dilution, be difficult to abundant dispersion.In addition, its shape can be different shape, can be unsetting and spherical etc. granular, cylindrical, sheet etc.
The matrix material resin using in masterbatch pellet of the present invention, can be used and the same resin of resin-phase for above-mentioned resin combination.
In addition, the composition of the matrix material resin in masterbatch pellet, can be used the resin same with the matrix material resin-phase that dilutes use, also can use different resins, use in the situation of different resins, every characteristic of considering to utilize the intermiscibility between resin to determine decides.
The amount of the yellow hydrous ferric oxide pigment coordinating in masterbatch pellet, is 1～200 weight part with respect to matrix material resin 100 weight parts, is preferably 1～150 weight part, more preferably 1～100 weight part.In the situation of quantity not sufficient 1 weight part of yellow hydrous ferric oxide pigment, melt viscosity when mixing is not enough, and the good distribution of yellow hydrous ferric oxide pigment is mixed difficulty.The amount of yellow hydrous ferric oxide pigment surpasses in the situation of 200 weight parts, matrix material resin-phase is less for yellow hydrous ferric oxide pigment, therefore, yellow hydrous ferric oxide pigment is difficult to dispersing and mixing well, in addition, and due to the small variation of the addition along with masterbatch pellet, the content of the yellow hydrous ferric oxide pigment coordinating in resin combination can significantly change, so, be difficult to be adjusted into required content, so not preferred.In addition, mechanical friction is violent and inappropriate.
<effect>
First, main points of the present invention are: in the aqueous dispersions of yellow hydrous ferric oxide particle, with the form being pre-mixed, add or add respectively separately and at least take clay mineral as main mineral compound and macromolecular compound, in room temperature～80, ℃ make its reaction, thus, at the particle surface of this yellow hydrous ferric oxide particle, form the layer of the oxyhydroxide of pure aluminium silicate, can access the yellow hydrous ferric oxide pigment of thermotolerance.
Main points are in addition: by the surface of the yellow hydrous ferric oxide pigment of the thermotolerance obtaining, any in rosin compound, Yelkin TTS, sorbitan ester compound, oleic acid or composition material are separately coated processing, can access the yellow hydrous ferric oxide pigment of thermotolerance of excellent dispersion.
Embodiment
Below, based on embodiment and comparative example, illustrate in greater detail the present invention.But the present invention is not subject to these any restriction.
The average major axis footpath of particle, average short shaft diameter, by measuring respectively major axis footpath, the short shaft diameter of electron micrograph (* 20000) being expanded as respectively on vertical and horizontal to 350 particles shown in the photo (* 80000) of twice, represent with its mean value.
The specific surface area value value representation of measuring by BET method.
The specific conductivity of product, is used electrical conductivity meter to measure.
The content of the soluble sodium salt of sample, measures: in the Erlenmeyer flask of 300ml, take 5g sample, add the pure water 100ml boiling as follows, heating, keeps boiling state about 5 minutes, afterwards, jump a queue, place and be cooled to normal temperature, add the water that is equivalent to reduction, jump a queue again, mixing vibration 1 minute, standing 5 minutes, afterwards, use the filter paper filtering supernatant liquor of No.5C, use inductively coupled plasma emission spectrophotometer (Seiko Instruments Inc's manufacture) to measure the Na in filtrate
+.
Form and aspect are measured as follows: by Hoover miller (Hoover Muller), 0.5g sample and 0.5ml Viscotrol C is mixing for pasty state, in this paste, add 4.5g varnish (Clear lacquer), mixing, coating, use 150 μ m(6mil) coating machine be coated on cast-coated paper, make paint chips (coating thickness: approximately 30 μ m), to this paint chips, use multiple light courcess spectral photometric colour measuring meter (MSC-IS-2D, SUGA trier (strain) is manufactured) Multi-Spectro-Colour-Meter, by the Lab space of Hunter, measure L* value, a* value, b* value, with according to (the Commission Internationnale de1 ' Eclairage of International Commission on Illumination, CIE) 1976(L* value, a* value, b* value) value representation of even perceptual space.
Thermotolerance is measured by following method: making and using the solvent of the yellow hydrous ferric oxide pigment of thermotolerance is coating, this coating is coated to aluminium sheet (0.8mm * 70mm * 150mm) with the thickness of 20 μ m, be dried, formation is filmed, and evaluates the thermotolerance of this paint chips obtaining thus., each test film is put into electric furnace, the temperature of electric furnace is carried out to various changes, in each temperature, carry out 5 minutes heat treated, use multiple light courcess spectral photometric colour measuring meter (MSC-IS-2D, SUGA trier (strain) is manufactured) form and aspect (the L* value of Multi-spectro-colour-Meter mensuration coated panel before and after each temperature heating, a* value, b* value), the measured value of take before heating is benchmark, obtain the Δ E* that following formula represents, use semilogarithmic plot, take transverse axis as Heating temperature, the longitudinal axis is the mapping of Δ E* value, Δ E* value is just in time reached to the temperature of 1.5 o'clock as the heat resisting temperature of coated film.
ΔE*=((ΔL*)2+(Δa*)2+(Δb*)2)1/2
Δ L* value: the L* value before and after the heat treated of duplicate poor
Δ a* value: the a* value before and after the heat treated of duplicate poor
Δ b* value: the b* value before and after the heat treated of duplicate poor
Oil number, according to JIS K5101, drips linseed oil to sample, mixing with trowel (ヘ ラ), and take becomes a block moment and measure as terminal.
Embodiment 1:
The heat-resisting processing that<mixture by clay mineral class and macromolecular compound carries out>
Using hydrous ferric oxide particle powder 1(major axis average diameter 0.37 μ m, minor axis average diameter 0.062 μ m, axial ratio (major axis footpath/short shaft diameter) 6.0, BET specific surface area 19.3m as starting raw material
2/ g) wet cake suspends in water, prepares the suspension liquid 3000mL of concentration 5 % by weight, then, uses high speed dispersor and vertical ball mill in this suspension liquid, fully to disperse hydrous ferric oxide particle powder.Now the pH of aqueous suspension is 5.6.
In this suspension liquid of 3000mL, slowly add that to be pre-mixed wilkinite 7.5g(be 5 % by weight with respect to hydrous ferric oxide solids component) and macromolecular compound (manufacture of ACCOFLOC C-310:MT AQUAPOLYMER company) 0.3g(with respect to hydrous ferric oxide solids component, be 0.2 % by weight) mixture that obtains, heat to 80 ℃, make it said temperature reaction 30 minutes.The pH of reaction solution is now 3.6.Drop temperature to after room temperature, by suction filter, filter, wash, then, the drying machine inner dryings of 100 ℃ 1 day.
Use mixing and kneading machine (ラ イ カ イ Machine) to pulverize the hydrous ferric oxide particle powder obtaining.The BET specific surface area of the hydrous ferric oxide particle powder obtaining is 18.7m
2/ g.
Creating conditions of the yellow hydrous ferric oxide pigment of thermotolerance is now as shown in table 2, and every characteristic of the yellow hydrous ferric oxide pigment of thermotolerance obtaining is as shown in table 3.
<the solvent that comprises the yellow hydrous ferric oxide pigment of thermotolerance is the modulation of coating>
The yellow hydrous ferric oxide pigment of above-mentioned thermotolerance 10g, amino-alkyd resin and thinner are coordinated with following ratio, add in the vial of 140ml with together with the granulated glass sphere 90g of 3mm Φ, then, in coating wobbler (paint shaker), make time of vibration change into 1 minute, within 3 minutes, 5 minutes, 10 minutes, 30 minutes, 60 minutes, 90 minutes, mix, make each abrasive (mill base).
The relation of time of vibration and form and aspect is as shown in table 5.
The yellow hydrous ferric oxide granular pigments of thermotolerance: 10g
Amino-alkyd resin: 16g
Solvent (thinner): 6g
Granulated glass sphere (3mm Φ): 90g
In the abrasive of making, add 50g amino-alkyd resin, in paint regulator (paint conditioner), vibration is 5 minutes, makes thus coating.
The coating obtaining is coated to aluminium sheet (0.8mm * 70mm * 150mm) with the thickness of 20 μ m, be dried, formation is filmed, and measures the form and aspect of the paint chips obtaining thus.The paint chips that the abrasive that uses vibration to make for 60 minutes obtains, L* value is that 62.0, a* value is that 17.3, b* value is 51.1.
Based on above-described embodiment 1, change various creating conditions, obtain the yellow hydrous ferric oxide particle powder of thermotolerance.
Hydrous ferric oxide 1～4:
As processed particle, prepare the hydrous ferric oxide 1～4 shown in table 1.
<heat-resisting the processing undertaken by clay mineral class and macromolecular compound>
Embodiment 2:
To hydrous ferric oxide particle powder 1(average major axis footpath 0.37 μ m, average short shaft diameter 0.062 μ m, BET specific surface area 19.3m
2the aqueous suspension 3000mL of 5 % by weight concentration/g), adding wilkinite 45g(is 30% with respect to hydrous ferric oxide solids component), heat to 80 ℃, then, add 1.5g(with 1 % by weight) macromolecular compound (ZP-700, HYMO company manufactures), at said temperature, make its reaction 30 minutes, now the pH of reaction solution is 3.4.
After reaction finishes, cool to room temperature, is used suction filter to filter and wash processing, the drying machine inner drying by the filter cake obtaining at 100 ℃.
The average major axis footpath of this particle powder is that 0.39 μ m, average short shaft diameter are that 0.064 μ m, BET specific surface area are 19.7m
2/ g, the L* value of form and aspect is that 61.0, a* value is that 17.0, b* value is 51.0.
In addition, the result of thermal test, heat resisting temperature is 268 ℃.
Embodiment 3:
To hydrous ferric oxide particle powder 2(average major axis footpath 0.35 μ m, average short shaft diameter 0.06 μ m, BET specific surface area 21.1m
2the aqueous suspension 3000mL of 5 % by weight concentration/g), add macromolecular compound (MP-784, the manufacture of HYMO company) 1.2g(is 0.8 % by weight with respect to hydrous ferric oxide solids component), heat to 80 ℃, then, add 30g(with 20 % by weight) zeolite, at said temperature, make its reaction 30 minutes, now the pH of reaction solution is 3.6.
After reaction finishes, cool to room temperature, is used suction filter to filter and wash processing, the drying machine inner drying by the filter cake obtaining at 100 ℃.
The average major axis footpath of this particle powder is that 0.36 μ m, average short shaft diameter are that 0.061 μ m, BET specific surface area are 21.0m
2/ g, the L* value of form and aspect is that 59.1, a* value is that 17.1, b* value is 49.5.
In addition, the result of thermal test, heat resisting temperature is 273 ℃.
Embodiment 4 and 5, comparative example 1 and 2:
Except changing the kind of hydrous ferric oxide particle, the kind and addition of the kind of clay mineral and addition, macromolecular compound, to process with the same method of embodiment.
Mainly create conditions and be shown in table 2 and 3 with every characteristic.
<dispersed raising is processed>
In the Henschel mixer of useful volume 10L, add and implemented above-mentioned resistance to heat treated yellow hydrous ferric oxide particle powder 1kg, add therein the mixture of mixed rosin 10g and ethanol 30g, at 50 ℃, carry out 2 hours combination treatment, after cool to room temperature, take out powder, obtain the yellow hydrous ferric oxide particle powder of processing with rosin.
Change the kind of heat-resisting yellow hydrous ferric oxide particle and the kind for the treatment of agent, treatment capacity, process.
Treatment condition are now shown in table 4.
<dispersed evaluation>
With following ratio, coordinate the yellow hydrous ferric oxide pigment of above-mentioned thermotolerance 10g, amino-alkyd resin and thinner, be added in the vial of 140ml together with 3mm Φ granulated glass sphere 90g, then, in coating wobbler, make time of vibration change into 1 minute, 3 minutes, 5 minutes, 10 minutes, 30 minutes, 60 minutes, 90 minutes, mix, make each abrasive.
The yellow hydrous ferric oxide granular pigments of thermotolerance: 10g
Amino-alkyd resin: 16g
Solvent (thinner): 6g
Granulated glass sphere (3mm Φ): 90g
In the abrasive of making, add 50g amino-alkyd resin, in paint regulator, vibrate 5 minutes, make coating.
The coating obtaining is coated to aluminium sheet (0.8mm * 70mm * 150mm) with the thickness of 20 μ m, be dried, formation is filmed, and measures the form and aspect of the paint chips obtaining thus.
What obtain the results are shown in table 5.
As shown in table 5, the oil number of thermotolerance yellow ultramarine of the present invention (A, B, C, H, I, J and K) is little of below 55, excellent dispersion.Particularly known thermotolerance yellow ultramarine of the present invention (H, I, J, K) is with respect to the pigment before each surface treatment (A, B, C), and the vibration of coating wobbler just can reach the form and aspect that are close with aim colour with the short period of time.In other words, known can dispersion at short notice.
Table 1
Table 2
Table 3
Table 4
Table 5
Industrial utilizability
The yellow hydrous ferric oxide pigment of thermotolerance of the present invention is to have excellent thermotolerance and dispersed yellow hydrous ferric oxide pigment, is suitable as stable on heating yellow ultramarine.
Claims (10)
1. the yellow hydrous ferric oxide pigment of thermotolerance, is characterized in that:
The particle surface of hydrous ferric oxide particle is coated by comprising the mixture of the clay mineral that contains pure aluminium silicate and macromolecular compound.
2. the yellow hydrous ferric oxide pigment of thermotolerance as claimed in claim 1, is characterized in that:
The content of pure aluminium silicate is 2～50 % by weight with respect to hydrous ferric oxide particle.
3. the yellow hydrous ferric oxide pigment of thermotolerance as claimed in claim 1 or 2, is characterized in that:
The content of macromolecular compound is 0.1～2 % by weight with respect to hydrous ferric oxide particle.
4. the yellow hydrous ferric oxide pigment of thermotolerance, is characterized in that:
The particle surface of hydrous ferric oxide particle is coated by comprising the mixture of the clay mineral that contains pure aluminium silicate and macromolecular compound, then by be selected from rosin compound, Yelkin TTS, sorbitan acid esters, oleic acid a kind or two or more compound coated.
5. a manufacture method for the yellow hydrous ferric oxide pigment of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in claim 1～3, and this manufacture method is characterised in that:
By adding in the aqueous dispersions containing hydrous ferric oxide particle, at least mainly contain the mineral compound of clay mineral and the mixture of macromolecular compound is processed, at the particle surface of hydrous ferric oxide particle, to form the hydroxide layer of pure aluminium silicate.
6. a manufacture method for the yellow hydrous ferric oxide pigment of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in claim 1～3, and this manufacture method is characterised in that:
After interpolation at least mainly contains the mineral compound of clay mineral in the aqueous dispersions that contains hydrous ferric oxide particle, add macromolecular compound and process, thus, at the particle surface of hydrous ferric oxide particle, form the hydroxide layer of pure aluminium silicate.
7. a manufacture method for the yellow hydrous ferric oxide pigment of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in claim 1～3, and this manufacture method is characterised in that:
Add macromolecular compound in the aqueous dispersions that contains hydrous ferric oxide particle after, add the mineral compound at least mainly contain clay mineral and process, at the particle surface of hydrous ferric oxide particle, form thus the hydroxide layer of pure aluminium silicate.
8. a manufacture method for the yellow hydrous ferric oxide pigment of thermotolerance, it is for the manufacture of the yellow hydrous ferric oxide pigment of thermotolerance claimed in claim 4, and this manufacture method is characterised in that:
The yellow hydrous ferric oxide pigment obtaining for the manufacture method of utilizing the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in claim 5～7, use dry mixer, with the one kind or two or more compound being selected from rosin compound, Yelkin TTS, sorbitan acid esters, oleic acid, carry out surface treatment.
9. a coating, is characterized in that:
It is to form by the yellow hydrous ferric oxide pigment of thermotolerance described in any one coordinate claim 1～4 in coating formation base material in.
10. a resin combination, is characterized in that:
It is to require the yellow hydrous ferric oxide pigment of the thermotolerance described in any one in 1～4 to carry out painted obtaining by right to use.
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| CN105504882A (en) * | 2015-12-15 | 2016-04-20 | 江苏省常熟环通实业有限公司 | Preparation method for surface-coated modified iron oxide yellow |
| CN105602291A (en) * | 2016-02-17 | 2016-05-25 | 升华集团德清华源颜料有限公司 | Method for improving hue of particle iron oxide yellow pigment |
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| CN114410127A (en) * | 2022-01-21 | 2022-04-29 | 中国科学院兰州化学物理研究所 | Method for efficiently and cleanly preparing clay mineral hybrid bismuth yellow pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPS4829528B1 (en) * | 1969-04-28 | 1973-09-11 | ||
| JPS5757755A (en) * | 1980-09-26 | 1982-04-07 | Toyo Soda Mfg Co Ltd | Improvement on pigment characteristics of yellow iron oxide |
| JPS59120657A (en) * | 1982-12-27 | 1984-07-12 | Lion Corp | Surface-coated pigment |
| JPH07179913A (en) * | 1993-12-24 | 1995-07-18 | Kao Corp | Production of magnetic metal powder and coating film for magnetic recording medium |
| JP3485647B2 (en) * | 1994-10-05 | 2004-01-13 | チタン工業株式会社 | Pigment and its production method |
| JP3214542B2 (en) * | 1995-12-14 | 2001-10-02 | 戸田工業株式会社 | Method for producing heat-resistant yellow iron-containing hydrous pigment |
| JP3480485B2 (en) * | 1997-06-23 | 2003-12-22 | 戸田工業株式会社 | Method for producing heat-resistant yellow iron-containing hydrous pigment |
| JP3509842B2 (en) * | 1997-06-23 | 2004-03-22 | 戸田工業株式会社 | Production method of heat-resistant yellow iron hydroxide hydroxide pigment |
| JP2005290059A (en) * | 2004-03-31 | 2005-10-20 | Toda Kogyo Corp | Red iron oxide pigment, and coating material and resin composition produced by using the same |
| JP5413554B2 (en) * | 2008-04-25 | 2014-02-12 | 戸田工業株式会社 | Coloring pigment for sunlight high reflection paint |
-
2013
- 2013-06-28 JP JP2013137153A patent/JP6217905B2/en active Active
- 2013-06-28 CN CN201310269881.2A patent/CN103525131A/en active Pending
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| CN107090195A (en) * | 2017-05-02 | 2017-08-25 | 湖州师范学院 | A kind of easy dispersing iron oxide yellow pigment of heat resistant type and preparation method thereof |
| CN107033777A (en) * | 2017-05-31 | 2017-08-11 | 江苏精盾节能科技有限公司 | It is a kind of for insulating moulding coating of energy saving door and window and preparation method thereof |
| CN109608909A (en) * | 2018-11-19 | 2019-04-12 | 岳西县邦玉铁系颜料有限公司 | A kind of iron oxide pigment of good dispersion |
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|---|---|
| JP6217905B2 (en) | 2017-10-25 |
| JP2014028947A (en) | 2014-02-13 |
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