CN1609000A - Prepn process of nano filming titanium dioxide colloid - Google Patents
Prepn process of nano filming titanium dioxide colloid Download PDFInfo
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- CN1609000A CN1609000A CN 200310111846 CN200310111846A CN1609000A CN 1609000 A CN1609000 A CN 1609000A CN 200310111846 CN200310111846 CN 200310111846 CN 200310111846 A CN200310111846 A CN 200310111846A CN 1609000 A CN1609000 A CN 1609000A
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Abstract
The preparation process of nano filming titanium dioxide colloid includes dialysis treating titanium compound aqua to obtain solution of nano filming titanium dioxide colloid; reacting the colloid solution with ammonia water to obtain titanium hydroxide and reacting with proper amount of hydrogen peroxide to obtain anatase type nanometer titanium dioxide solution; and vacuum drying to obtain powder of particle size below 100 nm. The preparation process has low cost, simple process, easy application in industrial production and no environmental pollution. The product may be used widely.
Description
Technical field
That the present invention relates to is nano-titanium oxide film forming colloidal preparation method.
Background technology
Nano-titanium oxide was come out in the later stage eighties 20th century., specific surface area very little owing to its particle diameter is big, interface atom proportion has particular performances greatly.For example: excellent photochemical catalysis effect, ultraviolet shielded effect, transparent nontoxic, peculiar colour effect etc., make it promptly enjoy favor once emerging.Want in automotive industry, sun care preparations, high grade paint, wastewater treatment, sterilization, environmental protection, there is wide application prospect aspects such as sorbent material and ceramic material.
The preparation method of nano-anatase titanium oxide that at present many reported in literature arranged mainly contains sol-gel method, vapour deposition process, hydrothermal oxidization method etc.These preparation methods respectively have characteristics, but they also have the deficiency of the relatively poor nano-anatase titanium oxide of resulting mixed crystal type often or degree of crystallinity except that defectives such as cost high technology complexity are arranged.This will obviously reduce the function of nano-titanium oxide.
The invention provides that a kind of cost is low, the preparation method of the simple nano-titanium oxide film forming glue of technology liquid solution, anatase type nano-titanium oxide suspension, powder.
Summary of the invention
The objective of the invention is to realize by following technical solution: the present invention includes following steps:
A: under temperature is lower than 30 ℃ and agitation condition, the preparation titanium compound aqueous solution, the concentration of titanium compound is 0.001～3mol/L
-1
B: with this titanium compound aqueous solution dialysis, up to pH＞4, promptly obtain nano-titanium oxide colloid film-forming soln, its size range is 1～100nm.
Nano-titanium oxide colloidal solution of the present invention is under temperature is lower than 30 ℃ and agitation condition, and the dropping ammonia hybrid reaction obtains slip.Described slip obtains the titanium hydroxide solid, and the specific conductivity of washing water layer with deionized water is no more than 100Ms/CM
-2Described washed titanium hydroxide solid dispersed is in deionized water, add superoxol, titanium hydroxide solid and hydrogen peroxide rub happy than being 1: 0.1～2.5, be heated to 50～150 ℃, after 1～20 hour, cool to room temperature obtains the anatase type nano titanium oxide solution, and its granularity is less than 100nm.
Anatase type nano-titanium oxide of the present invention is being lower than vacuum-drying under 150 ℃ of conditions, obtains anatase type nano-titanium oxide powder, and its granularity is less than 100nm.Add respectively and be equivalent to one times of titanium hydroxide quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants.Described tackifier are carboxymethyl cellulose, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
Titanium compound raw material of the present invention can be titanous chloride TiCl
3, titanium tetrachloride TiCl
4, titanium sulfate Ti (SO
4)
2, contain oxygen titanium sulfate TiOSO
4, titanium oxychloride TiOCl
2Deng.
The present invention can also be with concentration adjustment to 0.01～10% of described nano-titanium oxide colloidal solution, range of viscosities 1～100mPas.Use dip-coating method, rotational method or spraying method be film forming on carriers such as metal, glass or pottery.In the tool membrane carrier that 300～600 ℃ of sintering temperatures obtain, sintering time is 0.1～5 hour, obtains the carrier of the nano oxidized titanium film of tool.Add respectively and be equivalent to one times of titanium compound quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants.Wherein said tackifier are carboxymethyl cellulose, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
Specific implementation method of the present invention:
The preparation of 1 nano-titanium oxide film forming glue liquid solution comprises the steps:
(1) under temperature is lower than 30 ℃ and agitation condition, the preparation titanium compound aqueous solution, the concentration of titanium compound is 0.01～3mol/L
-1
(2) with this titanium compound aqueous solution dialysis, up to pH＞4, promptly obtain nano-titanium oxide colloid film-forming soln, its size range is 1～100nm.
Wherein the titanium compound raw material can be titanous chloride (TiCl3), titanium tetrachloride (TiCl4), titanium sulfate (Ti (SO4) 2), contain oxygen titanium sulfate (TiOSO4), titanium oxychloride (TiOCl2) etc.
The preparation of 2 anatase type nano-titanium oxide suspension comprises the steps:
(1) temperature is lower than that the dropping ammonia hybrid reaction obtains slip (this moment, the amount of used ammonia was suitable with 2 moles times the stoichiometric amounts that titanium-containing compound are converted into the needed ammonia of titanium hydroxide) in the nano-titanium oxide colloidal solution that obtains under 30 ℃ and the agitation condition in preparation 1 step (2) by nano-titanium oxide film forming glue alms bowl solution.
(2) slip obtains titanium hydroxide in the separating step (1), and the specific conductivity of washing water layer with deionized water is no more than 100Ms/CM
-2
(3) with titanium hydroxide solid dispersed washed in the step (2) in deionized water, add superoxol, titanium hydroxide solid and hydrogen peroxide mol ratio are 1: 0.1～2.5, be heated to 50～150 ℃, after 1～20 hour, cool to room temperature obtains the anatase type nano titanium oxide solution, and its granularity is less than 100nm.
The preparation of 3 anatase type nano-titanium oxide powders comprises the steps:
The anatase type nano-titanium oxide that obtains in preparation 2 steps (3) with anatase type nano-titanium oxide suspension is being lower than vacuum-drying under 150 ℃ of conditions, obtains anatase type nano-titanium oxide powder, and its granularity is less than 100nm.
When being used for matrix film forming such as metal, pottery, glass when the nano-titanium oxide film forming glue liquid solution that obtains among the preparation method 1 of above-mentioned nano-titanium oxide film forming glue liquid solution, add respectively and be equivalent to one times of titanium compound quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants.Wherein said tackifier are carboxymethyl cellulose, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
Add respectively among the preparation method 2 of above-mentioned anatase nano-titanium oxide suspension and be equivalent to one times of titanium hydroxide quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants.Wherein said tackifier are carboxymethyl cellulose, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
Nano-titanium oxide film forming glue liquid solution can be applicable to be the lining film forming of base material, to heat-treat then with metal, pottery, glass etc. among the present invention under 300～600C condition, obtains metal, pottery, the glass of the nano oxidized titanium film lining of anatase type.It has the organism in the deodorization of decomposing greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, antirust, anti-algae, plant effluent, decolouring, the purification atmosphere.Be widely used in hospital, aerospace apparatus, school, restaurant, food processing plant, bathroom lavatory, restaurant, automobile, indoor and outdoor, KTV box, various mechanicalss etc.
Anatase type nano-titanium oxide suspension is harmless among the present invention, can be coated with multiple substrate material (as metal, pottery, glass, plastics, wood, stone, fiber, cloth, paper), can carry out blending with fiber, cloth etc., can mix, can be mixed and made into antibiotic self-cleaning coating, also can directly make sprays with coating with paper pulp.The seasoning at normal temperatures of anatase type nano-titanium oxide suspension can be kept permanent effect.Organism in the deodorization of decomposing greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, antirust, anti-algae, plant effluent, decolouring, the purification atmosphere is arranged.Be widely used in hospital, school, restaurant, food processing plant, bathroom lavatory, restaurant, automobile, indoor and outdoor, KTV box, various mechanicalss etc.
The nano oxidized attitude powder body material of anatase type can be used for preparing anatase type nano-titanium oxide suspension, is prepared into nano ceramics, also can connects to join and decompose greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, antirust, anti-algae, the deodorization of plant effluent, decolouring, in the mechanicalss such as atmospheric cleaning among the present invention.
The preparation method of nano-titanium oxide film forming glue liquid solution of the present invention, anatase titanium oxide suspension, powder has following advantage:
(1) raw material of Cai Yonging is cheap and easy to get, so preparation cost is low.
(2) technology is simple, easily amplifies.
(3) to environment and human body without any harmful part.
Do not need pyroprocessing when (4) anatase type nano-titanium oxide suspension uses.
(5) anatase type nano suspending liquid or diameter of particle are little, less than 100nm.
The invention will be further described below in conjunction with embodiment, but not with any pattern restriction the present invention.
Embodiment 1
Under temperature is lower than 30 ℃ and agitation condition, the preparation titanium tetrachloride aqueous solution, concentration is 0.05mol/L
-1With this titanium salt aqueous solution dialysis,, promptly obtain nano-titanium oxide film forming glue liquid solution up to pH＞4.The tensio-active agent sodium phosphate and the tackifier carboxymethyl cellulose that add each 0.3 milligram/gram titanium oxide.Use dip-coating method, rotational method or spraying method are after film forming on the carriers such as glass or pottery, 300～600 ℃ of sintering temperatures 0.1～5 hour, obtain the carrier of the nano oxidized titanium film of tool anatase type, has the intensive photocatalysis characteristic, can be used for decomposing greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, plant effluent is handled.
Embodiment 2
Under temperature is lower than 30 ℃ and agitation condition, the preparation titanium tetrachloride aqueous solution, concentration is 0.05mol/L
-1With this titanium salt aqueous solution dialysis, up to pH＞4, the dropping ammonia hybrid reaction obtains the slip amount of used ammonia (this moment to be converted into the stoichiometric amount of the needed ammonia of titanium hydroxide suitable with 2 moles times the titanium salt that will contain).Separate slip and obtain the titanium hydroxide solid, the specific conductivity of washing water layer with deionized water is no more than 100Ms/CM
-2Titanium hydroxide solid dispersed washed in inciting somebody to action again is in deionized water, add superoxol, titanium hydroxide solid and hydrogen peroxide rub happy than being 1: 0.1～2.5, be heated to 50～150 ℃, after 1～20 hour, cool to room temperature obtains the anatase type nano titanium oxide solution, and its granularity is less than 100nm.
Embodiment 3
The tensio-active agent sodium phosphate and the tackifier carboxymethyl cellulose that add each 0.3 milligram/gram titanium oxide among the embodiment 2 in the suspension of gained.Can be coated with multiple substrate material (as metal, pottery, glass, plastics, wood, stone, fiber, cloth, paper), can carry out blending with fiber, cloth etc., can mix, can be mixed and made into antibiotic self-cleaning coating, also can directly make in sprays or the adding makeup with coating with paper pulp.Anatase type nano-titanium oxide suspension is harmless, and seasoning at normal temperatures can be kept permanent effect.Organism in the deodorization of decomposing greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, antirust, anti-algae, plant effluent, decolouring, the purification atmosphere is arranged, absorb ultraviolet function.
Embodiment 4
The anatase type nano-titanium oxide vacuum-drying under 80 ℃ of conditions that obtains among the embodiment 2 obtains anatase type nano-titanium oxide powder, and its granularity is less than 100nm.Can be used for preparing anatase type nano-titanium oxide suspension, be prepared into nano ceramics, also can connect to join and decompose greasy dirt, mildew-resistant, deodorizing, sterilization, automatically cleaning, antirust, anti-algae, the deodorization of plant effluent, decolouring, in the mechanicalss such as atmospheric cleaning, makeup.
Claims (12)
1, a kind of nano-titanium oxide film forming colloidal preparation method is characterized in that it comprises the steps:
A: under temperature is lower than 30 ℃ and agitation condition, the preparation titanium compound aqueous solution, the concentration of titanium compound is 0.001～3mol/L
-1
B: with this titanium compound aqueous solution dialysis, up to pH＞4, promptly obtain nano-titanium oxide colloid film-forming soln, its size range is 1～100nm.
2, nano-titanium oxide film forming colloidal preparation method according to claim 1 is characterized in that described nano-titanium oxide colloidal solution under temperature is lower than 30 ℃ and agitation condition, and the dropping ammonia hybrid reaction obtains slip.
3, nano-titanium oxide film forming colloidal preparation method according to claim 2 is characterized in that described slip obtains the titanium hydroxide solid, and the specific conductivity of washing water layer with deionized water is no more than 100Ms/CM
-2
4, nano-titanium oxide film forming colloidal preparation method according to claim 3, it is characterized in that described washed titanium hydroxide solid dispersed is in deionized water, add superoxol, titanium hydroxide solid and hydrogen peroxide rub happy than being 1: 0.1～2.5, be heated to 50～150 ℃, after 1～20 hour, cool to room temperature, obtain the anatase type nano titanium oxide solution, its granularity is less than 100nm.
5, nano-titanium oxide film forming colloidal preparation method according to claim 4 is characterized in that described anatase type nano-titanium oxide is being lower than vacuum-drying under 150 ℃ of conditions, obtains anatase type nano-titanium oxide powder, and its granularity is less than 100nm.
6, nano-titanium oxide film forming colloidal preparation method according to claim 5, it is characterized in that adding respectively and be equivalent to one times of titanium hydroxide quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants.
7, nano-titanium oxide film forming colloidal preparation method according to claim 6 is characterized in that described tackifier are carboxymethyl cellulose, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
8, nano-titanium oxide film forming colloidal preparation method according to claim 1 is characterized in that described titanium compound raw material can be titanous chloride TiCl
3, titanium tetrachloride TiCl
4, titanium sulfate Ti (SO
4)
2, contain oxygen titanium sulfate TiOSO
4, titanium oxychloride TiOCl
2Deng.
9, nano-titanium oxide film forming colloidal preparation method according to claim 1 is characterized in that concentration adjustment to 0.01～10% of described nano-titanium oxide colloidal solution, range of viscosities 1～100mPas.
10, nano-titanium oxide film forming colloidal preparation method according to claim 9 is characterized in that using dip-coating method, and rotational method or spraying method be film forming on carriers such as metal, glass or pottery.
11, nano-titanium oxide film forming colloidal preparation method according to claim 10 is characterized in that the tool membrane carrier that 300～600 ℃ of sintering temperatures obtain, and sintering time is 0.1～5 hour, obtains the carrier of the nano oxidized titanium film of tool.
12, nano-titanium oxide film forming colloidal preparation method according to claim 11, the preparation method who it is characterized in that described nano-titanium oxide film forming glue liquid solution, it is characterized in that adding respectively and be equivalent to one times of titanium compound quality to ten thousand/tensio-active agent and tackifier doubly, wherein said tensio-active agent is a carboxylate salt, sulfuric ester or phosphate anion tensio-active agent or polyethylene glycols or multivalence alcohol surfactants, wherein said tackifier are carboxymethyl celluloses, ethyl cellulose, montmorillonite, methylcellulose gum or acrylic acid or the like tackifier.
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| CN 200310111846 CN1609000A (en) | 2003-10-17 | 2003-10-17 | Prepn process of nano filming titanium dioxide colloid |
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| CN 200310111846 CN1609000A (en) | 2003-10-17 | 2003-10-17 | Prepn process of nano filming titanium dioxide colloid |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100395188C (en) * | 2005-12-02 | 2008-06-18 | 北京宇极科技发展有限公司 | Method for preparing titanium oxide colloid and correlates thereof |
| CN100484880C (en) * | 2005-09-22 | 2009-05-06 | 中国科学院理化技术研究所 | Low-temperature crystallized nano titanium dioxide powder and synthesis method of sol |
| CN103343456A (en) * | 2013-07-23 | 2013-10-09 | 北京纳琦环保科技有限公司 | Method for processing fiber product with antibacterial and deodorant properties |
| CN103341356A (en) * | 2013-07-23 | 2013-10-09 | 北京纳琦环保科技有限公司 | Processing method of water purifying agent of ceramic tourmaline-loaded titanium dioxide film |
| CN103386300A (en) * | 2013-07-23 | 2013-11-13 | 北京纳琦环保科技有限公司 | Processing method of ceramic honeycomb plate air purifying agent |
| CN103482885A (en) * | 2013-07-23 | 2014-01-01 | 北京纳琦环保科技有限公司 | Processing method for sintering and film-formation of self-cleaning glass with photocatalytic performance |
| CN104549198A (en) * | 2014-11-05 | 2015-04-29 | 华文蔚 | Preparation method of TiO2 catalyst |
| CN107837802A (en) * | 2017-11-03 | 2018-03-27 | 盛槿滺 | A kind of composite photo-catalyst and preparation method thereof |
-
2003
- 2003-10-17 CN CN 200310111846 patent/CN1609000A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100484880C (en) * | 2005-09-22 | 2009-05-06 | 中国科学院理化技术研究所 | Low-temperature crystallized nano titanium dioxide powder and synthesis method of sol |
| CN100395188C (en) * | 2005-12-02 | 2008-06-18 | 北京宇极科技发展有限公司 | Method for preparing titanium oxide colloid and correlates thereof |
| CN103343456A (en) * | 2013-07-23 | 2013-10-09 | 北京纳琦环保科技有限公司 | Method for processing fiber product with antibacterial and deodorant properties |
| CN103341356A (en) * | 2013-07-23 | 2013-10-09 | 北京纳琦环保科技有限公司 | Processing method of water purifying agent of ceramic tourmaline-loaded titanium dioxide film |
| CN103386300A (en) * | 2013-07-23 | 2013-11-13 | 北京纳琦环保科技有限公司 | Processing method of ceramic honeycomb plate air purifying agent |
| CN103482885A (en) * | 2013-07-23 | 2014-01-01 | 北京纳琦环保科技有限公司 | Processing method for sintering and film-formation of self-cleaning glass with photocatalytic performance |
| CN104549198A (en) * | 2014-11-05 | 2015-04-29 | 华文蔚 | Preparation method of TiO2 catalyst |
| CN107837802A (en) * | 2017-11-03 | 2018-03-27 | 盛槿滺 | A kind of composite photo-catalyst and preparation method thereof |
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