CN104194408A - Novel modified titanium dioxide white antirust pigment and preparing method thereof - Google Patents
Novel modified titanium dioxide white antirust pigment and preparing method thereof Download PDFInfo
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- CN104194408A CN104194408A CN201410247313.7A CN201410247313A CN104194408A CN 104194408 A CN104194408 A CN 104194408A CN 201410247313 A CN201410247313 A CN 201410247313A CN 104194408 A CN104194408 A CN 104194408A
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Abstract
The invention discloses novel titanium dioxide white antirust pigment and a preparing method thereof. The method includes adding deionized water into a titanium dioxide crude product not subjected to surface treatment to obtain a slurry material, adding vinyl alkoxy phosphate, an organosilicone coupling agent and an alcohol amine type dispersant into the slurry material, dispersing at a high speed to fully mix the compounds, adjusting the pH value of the slurry material to 6-8, adding deionized water and a nanometer material, dispersing at a high speed to fully mix the compounds, drying the material mixture that is fully mixed, performing oxygen-free calcination at 200-400 DEG C for 3-3.5 h, cooling and smashing to obtain a product. The vinyl alkoxy phosphate, the organosilicone coupling agent and the nanometer material cover titanium dioxide particles. When a metal surface is coated with the pigment, a phosphate coating and a compact organosilicone coupling structure can be formed, thus effectively improving corrosion resistance of the pigment. Acrylate groups and the coupling agent exist on surfaces of the particles, thus effectively improving the dispersion stability of the pigment in an organic medium.
Description
Technical field
The present invention relates to a kind of white pigment and preparation method thereof, be specifically related to a kind of new modified titanium dioxide white rust-stabilising pigment and preparation method thereof.
Background technology
Titanium dioxide is the fields such as a kind of white pigment of excellent performance, widespread use and coating, ink, plastics, papermaking.But himself photochemical activity of the TiO 2 particles of uncoated modification is high, very easily cause the organic medium in application system that chemical bond energy fracture and chemical degradation occur, cause the decline of overall performance, apply limited.Main manifestations on coating and printing ink is efflorescence, loss of gloss, xanthochromia etc.Meanwhile, titanium dioxide surface is very easily hydrophilic, so be the most effective approach that improves its stable dispersion in organic medium to its surperficial modification.Improving the hydrophilic while, the group of introducing some antiseptic property excellences can effectively improve the over-all properties of particle simultaneously.On this basis, the surface modification of titanium dioxide is just seemed to particularly important.
Summary of the invention
First technical problem to be solved by this invention is to provide the new modified titanium dioxide white rust-stabilising pigment of the corrosion-resistant and stably dispersing performance of a kind of effective raising.
For solving the problems of the technologies described above, modifying titanium dioxide white pigment of the present invention comprises the slurry that the weight concentration made by not surface treated titanium dioxide crude product and deionized water is 60～80%, in the weight ratio with not surface treated titanium dioxide crude product, in this slurry, also add following raw materials according:
Vinyl alkoxy phosphoric acid ester: 0.1～4%,
Organo-silicon coupling agent: 0.1～4%
Nano material: 2～10%
Alcamines dispersion agent: 0.1～0.5%.
Described alcamines dispersion agent be α-amino isopropyl alcohol, diethanolamine, trolamine,, N, the one or more combination of N-dimethylethanolamine.
Described organo-silicon coupling agent be γ-aminopropyltrimethoxysilane, methyltrimethoxy silane, aminopropyl triethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, etc. in one or more combination.
The model that vinyl alkoxy phosphoric acid ester is produced by French Rhodia is the vinyl alkoxy phosphoric acid ester of PAM-100.
Described nano material is the one or more combination in nano-calcium carbonate, Nano silica sol and nano silicon etc.
Technique scheme utilizes vinyl alkoxy phosphoric acid ester (organic substance of phosphoric acid group) and organo-silicon coupling agent to be coated TiO 2 particles, make it when application, can be attached to substrate surface and form one deck phosphatize phosphate coat, and make the organosilicon reticulated structure of coating formation densification, thereby can effectively raise the corrosion resistance nature of pigment, titanium dioxide surface has one deck to contain the coating film of propionic ester group simultaneously, effectively raises the stably dispersing performance of pigment in organic medium.
Second technical problem to be solved by this invention is to provide a kind of preparation method of novel modifying titanium dioxide white rust-stabilising pigment, for solving the problems of the technologies described above, the preparation method of the modifying titanium dioxide white rust-stabilising pigment that the present invention is novel is: first by not surface treated titanium dioxide crude product, adding deionized water to make weight concentration is 60～80% slurry, in the weight ratio with not surface treated titanium dioxide crude product, in slurry, add 0.1～4% vinyl alkoxy phosphoric acid ester, 0.1～4% organo-silicon coupling agent and 0.1～0.5% alcamines dispersion agent, high speed dispersion fully mixes it.Then pH value is adjusted to 6-8, then adds 2～10% nano material, high speed dispersion mixes it, by after the drying materials mixing,, carrying out anaerobic calcining 3～3.5 hours at 200～400 ℃, cooling crush obtains product.
Described organo-silicon coupling agent be γ-aminopropyltrimethoxysilane, methyltrimethoxy silane, aminopropyl triethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane, etc. in one or more combination.
Described alcamines dispersion agent is diethanolamine, trolamine, α-amino isopropyl alcohol, N, the one or more combination of N-dimethylethanolamine.
The not surface treated titanium dioxide crude product that the present invention adopts is the not surface treated titanium dioxide making by sulfuric acid process.Sulfuric acid process is that titanium-iron powder and the vitriol oil are carried out to acidolysis reaction production titanous sulfate, generates metatitanic acid, more obtain titanium dioxide product through calcining, pulverizing through hydrolysis.This method can be produced anatase titanium dioxide and rutile titanium dioxide.
The model that vinyl alkoxy phosphoric acid ester is produced by French Rhodia is the vinyl alkoxy phosphoric acid ester of PAM-100.
Described nano material is the one or more combination in nano-calcium carbonate, Nano silica sol and nano silicon etc.
The present invention, by the surface treatment to titanium dioxide, can effectively be covered its surperficial photochemical activity point, can effectively improve the chemical stability of titanium dioxide application system.Utilize vinyl alkoxy phosphoric acid ester to be coated its surface, by bound phosphate groups, the phosphatization complexing action in metallic surface improves antiseptic property on the one hand, meanwhile, make titanium dioxide surface contain acrylate group, can effectively improve its stably dispersing performance in organic medium.Organo-silicon coupling agent can effectively improve the compactness of coating, effectively plays the effect blocking water, thereby improves rustless property, further improves the antiseptic property of whole product, reaches a best effect.
The invention has the advantages that the condition of surface that can effectively improve titanium dioxide, the covered effect of realizing ideal.When improving Investigation of stabilized dispersion of nano, also there is good antiseptic property.Therefore, reduce the usage quantity of pigment, reduced greatly cost.
Embodiment
Example one:
Adopt 65 kilograms of not surface treated titanium dioxide crude products, adding 35 kilograms of deionized waters to make concentration is 65% slurry, the trolamine that adds the PAM-100 of 1 kilogram, 1 kilogram of methyltrimethoxy silane and 0.30 kilogram, utilizes dispersion machine to turn lower high speed dispersion 1500 it is fully mixed.Then PH is adjusted to 7, then adds the nano-calcium carbonate of 5 kilograms, after the powder mixing is dried, carry out anaerobic calcining 3 hours at 350 ℃, then cooling crush obtains efficient corrosion resisting and 72 kilograms of the white pigments that easily disperse.
Example two:
Adopt 70 kilograms of not surface treated titanium dioxide crude products, adding 30 kilograms of deionized waters to make concentration is 70% slurry, the trolamine that adds the PAM-100 of 0.7 kilogram, 0.5 kilogram of methyltrimethoxy silane and 0.20 kilogram, utilizes dispersion machine to turn lower high speed dispersion 1500 it is fully mixed.Then PH is adjusted to 7, then adds the nano silicon of 5 kilograms, after the powder mixing is dried, carry out anaerobic calcining 3 hours at 400 ℃, then cooling crush obtains efficient corrosion resisting and 77 kilograms of the white pigments that easily disperse.
Example three:
Adopt 60 kilograms of not surface treated titanium dioxide crude products, adding 40 kilograms of deionized waters to make concentration is 60% slurry, the trolamine that adds the PAM-100 of 1 kilogram, 1 kilogram of methyltrimethoxy silane and 0.30 kilogram, utilizes dispersion machine to turn lower high speed dispersion 1500 it is fully mixed.Then PH is adjusted to 7, then adds the nano-calcium carbonate of 5 kilograms, after the powder mixing is dried, carry out anaerobic calcining 3 hours at 350 ℃, then cooling crush obtains efficient corrosion resisting and 67 kilograms of the white pigments that easily disperse.
Dispersed detection:
After getting respectively sample that 4 grams of untreated samples and example one to ten obtain and 6 grams of Synolac grinding distribution 300 turning on plain grinding instrument, with Hegman grind gage, detect the fineness of sample, according to the size of fineness, judge the dispersiveness of product, as table one.
Table one: the dispersed data of product
| Sample number into spectrum | Untreated samples | Example one | Example two | Example three |
| Fineness, μ m | 55 | 8 | 10 | 11 |
Antiseptic property detects:
First sample (sample that untreated samples, example one to ten obtain) is obtained to sample paint according to the anticorrosion middle grey base paint formulation of table two.
Table two: anticorrosion middle grey base paint formulation
| Raw material | Sample paint (components by weight percent) |
| Epoxy resin (50%) | 480 |
| Sample | 15 |
| Carbon black | 0.5 |
| Talcum powder | 8 |
| Process white | 12 |
| Organophilic clay | 1.5 |
| Dimethylbenzene | 10 |
| Butanols | 5 |
By above-mentioned sample paint and 200# daiamid epoxy curing agent, (according to weight ratio paint in 6: 1, with general steel plate, make model, 45 ± 3 microns of paint film thickness, detect salt spray resistance, and performance detection data as shown in Table 3.
Table three: product salt spray resistance
| Sample number into spectrum | Salt fog result (h, non-corrosive, non-foaming, do not come off) |
| The sample paint that untreated samples makes | 120 |
| The sample paint that example one makes | 980 |
| The sample paint that example two makes | 1060 |
| The sample paint that example three makes | 880 |
From table one and table three data, can find out, dispersion stabilization and the preservative property of surface treated titanium dioxide are greatly improved, and it is dispersed and rustless property is all very excellent.
Claims (5)
1. a new modified titanium dioxide white rust-stabilising pigment, it is characterized in that: comprise the slurry that the weight concentration made by not surface treated titanium dioxide crude product and deionized water is 60～80%, in the weight ratio with not surface treated titanium dioxide crude product, in this slurry, also add following raw materials according:
Vinyl alkoxy phosphoric acid ester: 0.1～4%,
Organo-silicon coupling agent: 0.1～4%
Nano material: 2～10%
Alcamines dispersion agent: 0.1～0.5%.
2. a kind of new modified titanium dioxide white rust-stabilising pigment according to claim 1, is characterized in that: described organo-silicon coupling agent is the one or more combination in γ-aminopropyltrimethoxysilane, methyltrimethoxy silane, aminopropyl triethoxysilane, 3-glycidyl ether oxygen base propyl trimethoxy silicane, γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three ('beta '-methoxy oxyethyl group) silane, N-β-aminoethyl-γ-aminopropyl methyl dimethoxysilane.
3. the preparation method of an a kind of new modified titanium dioxide white rust-stabilising pigment as claimed in claim 1 or 2, it is characterized in that: first by not surface treated titanium dioxide crude product, adding deionized water to make weight concentration is 60～80% slurry, in the weight ratio with not surface treated titanium dioxide crude product, in slurry, add 0.1～4% vinyl alkoxy phosphoric acid ester, 0.1～4% organo-silicon coupling agent and 0.1～0.5% alcamines dispersion agent, high speed dispersion fully mixes it, the PH of slurry is adjusted to 6-8, add again 2～10% nano material, high speed dispersion mixes it.By after the drying materials mixing, at 200～400 ℃, carry out anaerobic calcining 3～3.5 hours, cooling crush obtains product.
4. the preparation method of a kind of new modified titanium dioxide white rust-stabilising pigment according to claim 3, it is characterized in that: described alcamines dispersion agent is diethanolamine, trolamine, α-amino isopropyl alcohol, N, the one or more combination of N-dimethylethanolamine.
5. the preparation method of a kind of new modified titanium dioxide white rust-stabilising pigment according to claim 3, is characterized in that: described nano material is the one or more combination in nano-calcium carbonate, Nano silica sol and nano silicon.
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| CN201410247313.7A CN104194408A (en) | 2014-06-03 | 2014-06-03 | Novel modified titanium dioxide white antirust pigment and preparing method thereof |
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| CN201410247313.7A CN104194408A (en) | 2014-06-03 | 2014-06-03 | Novel modified titanium dioxide white antirust pigment and preparing method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107384001A (en) * | 2017-08-08 | 2017-11-24 | 海泉风雷新能源发电股份有限公司 | Ester modified ink of UV radiation of a kind of macromolecular chain alkyl phosphoric acid and preparation method thereof |
| CN109306212A (en) * | 2017-07-28 | 2019-02-05 | 李新念 | A kind of method of production of white pigment |
| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
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| JPS62177070A (en) * | 1986-01-30 | 1987-08-03 | Pilot Ink Co Ltd | Coloring solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109306212A (en) * | 2017-07-28 | 2019-02-05 | 李新念 | A kind of method of production of white pigment |
| CN107384001A (en) * | 2017-08-08 | 2017-11-24 | 海泉风雷新能源发电股份有限公司 | Ester modified ink of UV radiation of a kind of macromolecular chain alkyl phosphoric acid and preparation method thereof |
| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
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