CN100431813C - Nano pulp composition and its preparation method - Google Patents
Nano pulp composition and its preparation method Download PDFInfo
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- CN100431813C CN100431813C CNB2004100248963A CN200410024896A CN100431813C CN 100431813 C CN100431813 C CN 100431813C CN B2004100248963 A CNB2004100248963 A CN B2004100248963A CN 200410024896 A CN200410024896 A CN 200410024896A CN 100431813 C CN100431813 C CN 100431813C
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Abstract
The present invention discloses a nano slurry composition and a preparation method thereof. The present invention has a technical process that titanium tetrachloride and alkali solution react to prepare a titanium oxide colloid which is washed to an ion without impurities by adding alkali to carry out neutralization, and a high-speed dispersion machine is used for washing a product to be prepared into 1 to 25% of suspension. Silicon oxides, aluminum oxides and titanium oxides are compounded and are washed to an ion without impurities, and the high-speed dispersion machine is used for washing the product to be prepared into 1 to 30% of suspension. Formed nano slurry comprises nano material components and water, wherein nano materials are the titanium oxides or a composition of the titanium oxides and the silicon oxides or the aluminum oxides, and the weight percentage concentration of the nano materials is from 1 to 30%. The nano slurry obtained in the method has good dispersivity and stability, the use of a dispersion agent is avoided in a productive process, and an obtained product has the advantages of no poison, no corrosion and no pollution. Productive cost is decreased, and the present invention is favorable for environmental protection and has extensive market prospects.
Description
Technical field
The present invention relates to field of nanometer material technology, refer more particularly to a kind of composition and method of making the same of nano pulp.
Background technology
In the nano material, the special construction of high concentration crystal boundary and crystal boundary atom causes the change of mechanical property, magnetic, dielectricity, superconductivity, optics and even the thermodynamic property of material.Because the nanoparticle surface atomicity increases, the not enough and high surface of surface atom ligancy can, make that these atoms are easy to combine with other atom and settle out, so have very high chemism.Just because of this specific character of nano material makes nano material obtain paying close attention to widely at pottery, microelectronics, bioengineering, photoelectric field, chemical field etc.But because the surface area atomicity of nano material is many, specific area is big, very easily reunite, and the especially manufacturing of nano pulp, because the existence of water, in the nano material forming process, the dispersion of nano material becomes the key that whether can effectively obtain nano pulp.Chinese patent 01128271.1 discloses a kind of production method of nano zinc oxide slurry, and it to the effect that under the condition that dispersant participates in, makes nano zinc oxide slurry by high speed dispersion, ball milling.Thereby obtained a kind of nano pulp of high concentration dispersion.Yet this preparation method must have the existence of dispersant, and many dispersants are phosphoric acid salts, or adopt the dispersant of some imports, not only cost an arm and a leg, and many dispersants are important pollution sources of water body, just very easily cause the rising of the BOD value of water body as phosphoric acid salt.
Summary of the invention
The subject matter that the present invention will solve is the forming process that adopts the regulation and control nano material, realizes the decentralised control of nano pulp forming process, thereby avoids the use of dispersant, realizes the nuisancelessization production of nano pulp.
The objective of the invention is to realize by following manner:
A kind of preparation method of nano pulp, its technical process is:
The formation of a, colloid: react by titanium tetrachloride and aqueous slkali and to make titanium oxide colloid;
B, neutralization: add the alkali neutralization, the pH value of the hierarchy of control is 6-8;
C, washing: the sediment that obtains is washed to the free from admixture ion;
D, formulated suspension: the suspension that washed product is mixed with 1-25% with high speed dispersor;
A, silica or aluminium oxide, or silica and aluminium oxide and titanium oxide is compound: after the titanium oxide suspension of 1-25% fully disperses, add silicate or aluminate, or silicate and aluminate, form nano-titanium oxide, the perhaps nano-complex of titanium oxide and silica or aluminium oxide, the perhaps nano-complex of titanium oxide and silica, aluminium oxide, adding acid again, to be neutralized to pH value be 6-8;
B, washing: the sediment that obtains is washed to the free from admixture ion;
E, formulated suspension: the suspension that washed product is mixed with the nano material of 1-30% with high speed dispersor.
In order to guarantee the abundant of course of reaction, the concentration range of used titanium tetrachloride aqueous solution should be limited in the 5-50%, and aluminate or aqueous silicate solution concentration limits fix in the 2-20% scope.
Another purpose of the present invention provides a kind of nano pulp, this slurry has comprised nano material component and water, wherein nano material is a titanium oxide, the perhaps compound of titanium oxide and silica or aluminium oxide, the perhaps compound of titanium oxide and silica, aluminium oxide, the nano material weight percent concentration is 1-30%.
When nano material was composition, the content of titanium oxide was 1-30%, silica 0-25%, the aluminium oxide 0-25% of gross weight, and surplus is a water.
The particle size of nano material is 5-100nm.
The production method of above-described nano pulp, all kinds of nanometer oxide materials can be combined effectively, the nano pulp dispersiveness and the good stability that are obtained have had the feature of all kinds of nano-oxides simultaneously, and have avoided the use of dispersant in process of production, nontoxic, the no burn into of products obtained therefrom is pollution-free, both reduced production costs, helped environmental protection again, and easy to use, applied widely, have vast market prospect.
The specific embodiment
Embodiment 1: by 100ml concentration is that 5% titanium tetrachloride aqueous solution hydro-oxidation sodium water solution gets titanium oxide hydrate, and make titanium tetrachloride aqueous solution excessive slightly, obtain the titanium oxide colloid of positively charged, added thermal agitation 2 hours, adding concentration is 8% sodium hydrate aqueous solution, the pH value of regulating whole system is 7, and ageing is 2 hours again.The sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour, be mixed with concentration and be 1% suspension through high speed dispersor.
Embodiment 2: by 100ml concentration is that 40% titanium tetrachloride aqueous solution adds ammoniacal liquor and gets titanium oxide hydrate, and makes titanium tetrachloride aqueous solution excessive slightly, obtains the titanium oxide colloid of positively charged, added thermal agitation 1 hour, adding concentration is 10% ammoniacal liquor, and the pH value of regulating whole system is 7, and ageing is 2 hours again.The sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour, be mixed with concentration and be 5% suspension through high speed dispersor.After heating fully disperses, in suspension, drip sodium silicate aqueous solution, fully stirring after half an hour the hydrochloric acid of Dropwise 5 % to the pH value of system is 7 again, ageing half an hour again, the sediment that obtains is washed to the free from admixture ion, sediment after the washing is added pure water, disperse half an hour, be mixed with concentration and be 15% suspension through high speed dispersor.
Embodiment 3: by 100ml concentration is that 10% titanium tetrachloride aqueous solution hydro-oxidation aqueous solutions of potassium gets titanium oxide hydrate, and make titanium tetrachloride aqueous solution excessive slightly, obtain the titanium oxide colloid of positively charged, added thermal agitation 1 hour, adding concentration is 2% potassium hydroxide aqueous solution, the pH value of regulating whole system is 8, and ageing is 2 hours again.The sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour, be mixed with concentration and be 8% suspension through high speed dispersor.After heating fully disperses, dripping 30ml concentration in suspension is 2% sodium aluminate aqueous solution, fully stir after half an hour the hydrochloric acid of Dropwise 5 % again, the pH value that makes system is 7, again ageing half an hour, the sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour through high speed dispersor, be mixed with concentration and be 10% suspension.
Embodiment 4: by 100ml concentration is that 50% titanium tetrachloride aqueous solution hydro-oxidation sodium water solution gets titanium oxide hydrate, and make titanium tetrachloride aqueous solution excessive slightly, obtain the titanium oxide colloid of positively charged, added thermal agitation 1 hour, adding concentration is 15% sodium hydrate aqueous solution, the pH value of regulating whole system is 8, and ageing is 2 hours again.The sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour, be mixed with concentration and be 5% suspension through high speed dispersor.After heating fully disperses, dripping 100ml concentration in suspension is 10% sodium silicate aqueous solution, fully stirring after half an hour again, Dropwise 5 0ml concentration is 10% sodium aluminate aqueous solution, dripping concentration then and be 5% hydrochloric acid to the pH value of system is 6, again ageing half an hour, the sediment that obtains is washed to the free from admixture ion, the sediment after the washing is added pure water, disperse half an hour through high speed dispersor, be mixed with concentration and be 30% suspension.
Claims (6)
1. the preparation of compositions method of a nano pulp is characterized in that its technical process is:
The formation of c, colloid: react by titanium tetrachloride and aqueous slkali and to make titanium oxide colloid;
D, neutralization: add the alkali neutralization, the pH value of the hierarchy of control is 6-8;
E, washing: the sediment that obtains is washed to the free from admixture ion;
F, formulated suspension: the suspension that washed product is mixed with 1-25% with high speed dispersor;
G, silica or aluminium oxide, or silica and aluminium oxide and titanium oxide is compound: after the titanium oxide suspension of 1-25% fully disperses, add silicate or aluminate, or silicate and aluminate, form nano-titanium oxide, the perhaps nano-complex of titanium oxide and silica or aluminium oxide, the perhaps nano-complex of titanium oxide and silica, aluminium oxide, adding acid again, to be neutralized to pH value be 6-8;
H, washing: the sediment that obtains is washed to the free from admixture ion;
I, formulated suspension: the suspension that washed product is mixed with the nano material of 1-30% with high speed dispersor.
2. the preparation of compositions method of a kind of nano pulp as claimed in claim 1, the concentration range that it is characterized in that used titanium tetrachloride aqueous solution is 5-50%.
3. the preparation of compositions method of a kind of nano pulp as claimed in claim 1 is characterized in that used aluminate or aqueous silicate solution concentration range are 2-20%.
4. nano pulp composition, comprise nano material component and water, it is characterized in that described nano material is a titanium oxide, perhaps the compound of titanium oxide and silica or aluminium oxide, the perhaps compound of titanium oxide and silica, aluminium oxide, the nano material weight percent concentration is 1-30%.
5. a kind of nano pulp composition as claimed in claim 4, the content that it is characterized in that titanium oxide are 1-30%, silica 0-25%, the aluminium oxide 0-25% of gross weight, and surplus is a water.
6. as claim 4 or 5 described a kind of nano pulp compositions, the particle size that it is characterized in that described nano material is 5-100nm.
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CN100431813C true CN100431813C (en) | 2008-11-12 |
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CN100547037C (en) * | 2007-11-13 | 2009-10-07 | 攀枝花学院 | A kind of composite envelope titanium white powder and preparation method thereof |
EP3257816A1 (en) * | 2016-06-14 | 2017-12-20 | Kronos International, Inc. | Production of nano-particulate titanium dioxide |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4298718A (en) * | 1968-11-25 | 1981-11-03 | Montecatini Edison S.P.A. | Catalysts for the polymerization of olefins |
US4495338A (en) * | 1968-11-21 | 1985-01-22 | Montecatini Edison S.P.A. | Components of catalysts for the polymerization of olefins |
CN1323743A (en) * | 2000-05-12 | 2001-11-28 | 中国科学院大连化学物理研究所 | Process of preparing titania sol from titanium tetrachloride |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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US4495338A (en) * | 1968-11-21 | 1985-01-22 | Montecatini Edison S.P.A. | Components of catalysts for the polymerization of olefins |
US4298718A (en) * | 1968-11-25 | 1981-11-03 | Montecatini Edison S.P.A. | Catalysts for the polymerization of olefins |
CN1323743A (en) * | 2000-05-12 | 2001-11-28 | 中国科学院大连化学物理研究所 | Process of preparing titania sol from titanium tetrachloride |
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