CN1300804A - Active oxide coated porous powder and its preparing process and application - Google Patents

Active oxide coated porous powder and its preparing process and application Download PDF

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Publication number
CN1300804A
CN1300804A CN99126362A CN99126362A CN1300804A CN 1300804 A CN1300804 A CN 1300804A CN 99126362 A CN99126362 A CN 99126362A CN 99126362 A CN99126362 A CN 99126362A CN 1300804 A CN1300804 A CN 1300804A
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oxide
silicide
weight
porous powder
mixture
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CN99126362A
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CN1095487C (en
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宋广智
张敬杰
杨岩峰
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Institute of Photographic Chemistry of CAS
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Institute of Photographic Chemistry of CAS
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Abstract

A porous powder coated by high-activity oxide is prepared from the mixture of two or more chosen from nm-class TiO2, alumina, Cr2O3, nickel oxide, and iron oxide (25-65%), alkali-earth metal oxide (5-60%), and silicial and/or bromide and/or rare-earth oxide (5-45%) through mixing them with water, high-moleccular polymer and acid, homogenizing and further processing. Said powder can be used to preparing paint to clean air, deodour, and resist bacteria, photocatalytic ink, printed paint and co-filler. It has improved dispersity, durability and weatherability.

Description

Porous powder material that activating oxide coats and its production and use
The invention belongs to nano inorganic powder material technology field, particularly porous powder material, especially the nano level TiO of high activity oxide coating 2Powder body material that coats and its production and use.
Up to now, the powder body material that contains coated by titanium dioxide, not only can be coated in paper, plastics, timber and metallic surface and play pearly-lustre or interception, and because its particle diameter is very little, specific surface is big, contain air again, its density is reduced, when it and some special auxiliary agent combine, can make the function (as photocatalytic activity) of coating obtain unconventional performance.
Disclosed clad nano level oxide powder normally adopts wet chemistry methods such as coprecipitation method, calpis method and hydrothermal method, be prepared into fine powder earlier, can make meticulous coating micro-capsule powder body material through emulsion polymerization, interfacial polymerization, simple coacervation and dry bath method again.The powder body material of these coatings has high reactivity and big specific surface, but has also produced very easily adsorbed gas and liquid, and powder is easily reunited and the shortcoming that causes its due performance to be difficult to bring into play.The report of this respect is referring to the article of " modern chemical industry " magazine 1999 the 19th volumes the 9th phase the 50th page article and 1999 the 5th volumes of " Chinese powder technology " magazine the 5th phase 18-20 page or leaf.
The objective of the invention is to overcome the shortcoming of above-mentioned technology, the porous powder material, especially the nano level TiO that provide high activity oxide to coat 2Powder body material that coats and its production and use.The powder body material that this oxide compound coats, because the extraordinary form on its surface, its dispersiveness, weather resistance, weathering resistance are improved, and then improve its surfactivity, make its surface possess new physics, chemistry, optical characteristics, adapting to different application requiring, thereby improve the added value of the powder body material that this technology of employing makes greatly.
The object of the present invention is achieved like this:
The porous powder that high activity oxide provided by the invention coats, its composition (weight percent) contains: Nano titanium dioxide, Nano titanium dioxide and alumina in Nano level or with the nano level chromium sesquioxide or with nano level nickel oxide or the mixture formed with nanometer ferro oxide, or any two or more the compound in Nano titanium dioxide and alumina in Nano level, nano level chromium sesquioxide, nano level nickel oxide and the nanometer ferro oxide is by the mixture of any part by weight composition: 25%～65%;
Alkaline earth metal oxide: 5%～60%;
Silicide, or silicide and boride or the mixture formed with rare earth oxide, or the mixture of silicide and boride and rare earth oxide composition, wherein silicide accounts for the over half of mixture weight:
5％～45％。Wherein alkaline earth metal oxide is BaO, CaO or MgO etc.; Silicide is SiO 2Or Na 2SiO 3Deng; Boride is B 2O 3, H 3BO 3Or Na 2B 4O 7Deng; Rare earth oxide is La 2O 3Or CeO 2Deng.
The preparation method of the porous powder that high activity oxide provided by the invention coats carries out according to the following steps:
Add Nano titanium dioxide or alumina in Nano level or nano level chromium sesquioxide or nano level nickel oxide or nanometer ferro oxide earlier, or above-claimed cpd with two or more by any part by weight blended mixture, the add-on of wherein said compound or mixture is weight percentage 10%～25%; Weight percent is that 10%～30% alkaline earth metal oxide and weight percent are 40%～65% water, stirs; Add silicide again, or silicide and boride or the mixture formed with rare earth oxide, or the mixture formed of silicide and boride and rare earth oxide, the add-on of wherein said silicide or mixture is weight percentage 0.5%～10%, and described silicide accounts for the over half of mixture weight; Weight percent is 0.1%～5% high molecular weight water soluble polymer, weight percent is 0～10% mineral acid or organic acid, stir through abundant down at 50～90 ℃, to becoming meticulous homogeneous slurry, wherein grinding medium is the zirconium dioxide bead more than 1 hour in grinding; Adopt conventional drying process then, meticulous homogeneous slurry is processed into granular powder; Through 500 ℃ to 1200 ℃ high temperature sinterings 0.01～3 minute, promptly obtain the porous powder carrier then; Then the porous powder carrier behind the sintering is put in the aqueous solution that contains oxide compound, fully stirred after 10 minutes～30 minutes again drying or handle, can obtain the porous powder material that high activity oxide coats through 500 ℃～1200 ℃ high temperature sinterings;
Wherein said component and the weight percent content that contains the aqueous solution of oxide compound is:
Nano titanium dioxide 2%～10%;
Titanium compound 0～15%;
Soluble alkaline earth salt 5%～30%;
Boride 0～10%;
Silicide 0～10%;
Water 65%～90%.
Wherein
Alkaline earth metal oxide is BaO, CaO or MgO etc. in the described meticulous homogeneous slurry; Silicide is SiO 2Or Na 2SiO 3Deng; Boride is B 2O 3, H 3BO 3Or Na 2B 4O 7Deng; Rare earth oxide is La 2O 3Or CeO 2Deng; High molecular weight water soluble polymer is polyvinyl alcohol (PVA), polyoxyethylene glycol (PEG), polyoxyethylene (PEO), methylcellulose gum (MC), carboxymethyl cellulose (CMC) or carboxyethyl cellulose (EC); Described mineral acid or organic acid are hydrochloric acid, nitric acid, acetic acid or oxalic acid etc.
The drying process of described routine is air stream drying, spraying drying or fluidized drying.
Soluble alkaline earth salt is nitrate of baryta, magnesium nitrate, calcium chloride or magnesium chloride in the described aqueous solution that contains oxide compound; Described titanium compound is a tetrabutyl titanate; Described boride is a boric acid; Described silicide is silicic acid or aerosil.
Purposes of the present invention: but can be used for the coating of production environment purifying air, self-cleaning, deodorization, antibiotic and antiscale and have the printing ink of a series of special uses of photocatalysis characteristic and the stopping composition auxiliary agent of printing coatings by the coated porous powder of high activity oxide provided by the present invention.
Advantage of the present invention: the powder body material that oxide compound of the present invention coats, because the extraordinary form on its surface, its dispersiveness, weather resistance, weathering resistance are improved and improve, and then improve its surfactivity, make its surface possess new physics, chemistry, optical characteristics, adapting to different application requiring, thereby improve the added value of the powder body material that this technology of employing makes greatly.
The present invention is described in detail below in conjunction with example: but described embodiment limits protection scope of the present invention absolutely not.
Embodiment 1:
Nano titanium dioxide 20% (weight)
BaO 20% (weight)
SiO 25% (weight)
Polyvinyl alcohol (PVA) 2% (weight)
Water 50% (weight)
Hydrochloric acid 3% (weight)
Earlier add Nano titanium dioxide, BaO and water according to the above ratio, stir, add SiO again 2, polyvinyl alcohol (PVA), hydrochloric acid, 50 ℃ down through fully stirring, grinds 3 hours extremely meticulous homogeneous slurry, wherein grinding medium is the zirconium dioxide bead.Adopt air stream drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 25 μ m.Through 500 ℃ of high temperature sinterings 3 minutes, promptly obtain the porous powder carrier then.Porous powder carrier behind the sintering is put in the aqueous solution that concentration expressed in percentage by weight is 5% titanium dioxide and 10% nitrate of baryta then, fully stir drying and 500 ℃ of high temperature sinterings processing again after 30 minutes, can obtain median size is the coated porous powder body material of high activity oxide of 26 μ m.Contained component and weight percent are: Nano titanium dioxide 50%; BaO40%; SiO 210%.
Embodiment 2
Alumina in Nano level 23% (weight)
CaO 20% (weight)
SiO 2And B 2O 35% (weight)
SiO wherein 2And B 2O 3Weight ratio 3: 2
Polyoxyethylene (PEO) 0.2% (weight)
Water 50% (weight)
Mineral acid or organic acid 1.8% (weight)
Earlier add alumina in Nano level, CaO and water according to the above ratio, stir, add other component again, became meticulous homogeneous slurry in 2 hours through fully stirring, grinding down at 60 ℃, wherein grinding medium is the zirconium dioxide bead.Under 115 ℃ of conditions, slurries are carried out spraying drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 30 μ m.Through 800 ℃ of high temperature sinterings 2 minutes, promptly obtain the porous powder carrier then.Then the porous powder carrier behind the sintering is put into that to contain weight percent be that 3% Nano titanium dioxide and weight percent are 5% calcium chloride and in the aqueous solution of homogenization treatment, fully stirred after 10 minutes and can obtain the coated porous powder body material of high activity oxide that diameter is 30.5 μ m particle diameters 120 ℃ of dryings again; Contained component and weight percent are: Nano titanium dioxide 5.9%, alumina in Nano level 45.1%, CaO39.2%, SiO 2And B 2O 39.8%.
Embodiment 3
Nano level chromium sesquioxide 25% (weight)
MgO 15% (weight)
Na 2SiO 35% (weight)
Polyoxyethylene glycol (PEG) 1% (weight)
Water 54% (weight)
Earlier add nano level chromium sesquioxide, MgO and water according to the above ratio, stir, add Na again 2SiO 3And polyglycol (PEG), became meticulous homogeneous slurry in 1.5 hours through fully stirring, grinding down at 80 ℃, wherein grinding medium is the zirconium dioxide bead.Under 120 ℃ of conditions, slurries are carried out spraying drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 20 μ m.Through 1000 ℃ of high temperature sinterings 1 minute, promptly obtain the porous powder carrier then.Then the porous powder carrier behind the sintering is put into and contained Nano titanium dioxide 6% (weight percent), magnesium chloride 5% (weight percent) and boric acid 5% (weight percent) and in the aqueous solution of homogenization treatment, fully stir after 20 minutes and can obtain the coated porous powder body material of high activity oxide that median size is 21 μ m particle diameters 120 ℃ of dryings again.Contained component and weight percent are: Nano titanium dioxide 11.8%, nano level chromium sesquioxide 49.0%, MgO29.4%, Na 2SiO 39.8%.
Embodiment 4
Nano level nickel oxide 20% (weight)
BaO 15% (weight)
Na 2SiO 3, La 2O 3And Na 2B 4O 7, 10% (weight)
Its weight ratio is Na 2SiO 3: La 2O 3: Na 2B 4O 7=3: 1: 1;
Carboxymethyl cellulose (CMC) 2% (weight)
Water 53% (weight)
Earlier add nano level nickel oxide, BaO and water according to the above ratio, stir, add Na again 2SiO 3, and La 2O 3, Na 2B 4O 7, carboxymethyl cellulose (CMC) and acetic acid, became meticulous homogeneous slurry in 3 hours through fully stirring, grinding down at 90 ℃, wherein grinding medium is the zirconium dioxide bead.Under 120 ℃ of conditions, slurries are carried out spraying drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 30 μ m.1200 ℃ of high temperature sinterings are 0.02 minute then, promptly obtain the porous powder carrier.Then the porous powder carrier behind the sintering is put into and contained Nano titanium dioxide 10% (weight percent), nitrate of baryta 15% (weight percent) and silicic acid 5% (weight percent) and in the aqueous solution of homogenization treatment, fully stir after 30 minutes and can obtain the coated porous powder body material of high activity oxide that median size is 30 μ m particle diameters 120 ℃ of dryings again, contained component and weight percent are: Nano titanium dioxide 18.2%, nano level nickel oxide 36.4%, BaO27.3%, Na 2SiO 3, and La 2O 3, Na 2B 4O 718.1%.
Embodiment 5
Nanometer ferro oxide 20% (weight)
CaO 20% (weight)
SiO 25% (weight)
Carboxyethyl cellulose (EC) 2% (weight)
Water 51% (weight)
Nitric acid 2% (weight)
Earlier add nanometer ferro oxide, CaO and water according to the above ratio, stir, add SiO again 2, poly-carboxyethyl cellulose (EC) and nitric acid, became meticulous homogeneous slurry in 4 hours through fully stirring, grinding down at 70 ℃, wherein grinding medium is the zirconium dioxide bead.Under 120 ℃ of conditions, slurries are carried out spraying drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 8 μ m.Through 900 ℃ of high temperature sinterings 1 minute, promptly obtain the porous powder carrier then.Then the porous powder carrier behind the sintering is put into and contained Nano titanium dioxide 10% (weight percent), tetrabutyl titanate 3% (weight percent), magnesium chloride 10% (weight percent), boric acid 5% (weight percent) and silicic acid 2% (weight percent) and in the aqueous solution of homogenization treatment, fully stir after 30 minutes and can obtain the coated porous powder body material of high activity oxide that diameter is 9 μ m particle diameters 120 ℃ of dryings again, contained component and weight percent are: Nano titanium dioxide 18.2%, nanometer ferro oxide 36.4%, CaO36.4%, SiO 29.1%.
Embodiment 6
The mixture of Nano titanium dioxide and aluminum oxide and nickel oxide, wherein titanium dioxide is 10% (weight),
Aluminum oxide is that 5% (weight) nickel oxide is 3% (weight) 18% (weight)
Ba0 20% (weight)
SiO 25% (weight)
Carboxymethyl cellulose (CMC) 2% (weight)
Water 53% (weight)
Hydrochloric acid 2% (weight)
Add earlier mixture, BaO and the water of Nano titanium dioxide and aluminum oxide and nickel oxide according to the above ratio, stir, add SiO again 2Carboxymethyl cellulose (CMC) and hydrochloric acid became meticulous homogeneous slurry in 3 hours through fully stirring, grinding down at 90 ℃, and wherein grinding medium is the zirconium dioxide bead.Under 120 ℃ of conditions, slurries are carried out spraying drying then, meticulous homogeneous slurry is processed into the granular powder that median size is 35 μ m.Through 1200 ℃ of high temperature sinterings 0.02 minute, promptly obtain the porous powder carrier then.Then the porous powder carrier behind the sintering is put into and contained Nano titanium dioxide 10% (weight percent), nitrate of baryta 5% (weight percent) and silicic acid 5% (weight percent) and in the aqueous solution of homogenization treatment, fully stir after 30 minutes and can obtain the coated porous powder body material of high activity oxide that median size is 36 μ m particle diameters 120 ℃ of dryings again, contained component and weight percent are: the mixture 52.8% of Nano titanium dioxide and aluminum oxide and nickel oxide, BaO37.7%, SiO 29.4%.

Claims (7)

1. the porous powder material that coats of an activating oxide is characterized in that comprising that following component and weight percentage are:
Nano titanium dioxide; Nano titanium dioxide and alumina in Nano level or with the nano level chromium sesquioxide or with nano level nickel oxide or the mixture formed with nanometer ferro oxide; Or the mixture 25%～65% formed by any part by weight of any two or more the compound in Nano titanium dioxide and alumina in Nano level, nano level chromium sesquioxide, nano level nickel oxide and the nanometer ferro oxide;
Alkaline earth metal oxide 5%～60%;
Silicide: or silicide and boride or the mixture formed with rare earth oxide, or the mixture of silicide and boride and rare earth oxide composition, wherein silicide accounts for the over half of mixture weight
5％～45％。
2. the porous powder material that activating oxide as claimed in claim 1 coats is characterized in that described alkaline earth metal oxide is BaO, CaO or MgO; Described silicide is SiO 2Or Na 2SiO 3Described boride is B 2O 3, H 3BO 3Or Na 2B 4O 7Described rare earth oxide is La 2O 3Or CeO 2
3. as the porous powder preparation methods of the described a kind of activating oxide coating of claim 1-2, it is characterized in that:
Add Nano titanium dioxide or alumina in Nano level or nano level chromium sesquioxide or nano level nickel oxide or nanometer ferro oxide earlier, or above-claimed cpd with two or more by any part by weight blended mixture, the add-on of wherein said compound or mixture is weight percentage 10%～25%; Weight percent is that 10%～30% alkaline earth metal oxide and weight percent are 40%～65% water, stirs; Add silicide again, or silicide and boride or the mixture formed with rare earth oxide, or the mixture formed of silicide and boride and rare earth oxide, the add-on of wherein said silicide or mixture is weight percentage 0.5%～10%, and described silicide accounts for the over half of mixture weight; Weight percent is 0.1%～5% high molecular weight water soluble polymer, weight percent is 0～10% mineral acid or organic acid, stir through abundant down at 50～90 ℃, to becoming meticulous homogeneous slurry, wherein grinding medium is the zirconium dioxide bead more than 1 hour in grinding; Adopt conventional drying process then, meticulous homogeneous slurry is processed into granular powder; Through 500 ℃ to 1200 ℃ high temperature sinterings 0.01～3 minute, promptly obtain the porous powder carrier then; Then the porous powder carrier behind the sintering is put in the aqueous solution that contains oxide compound, fully stirred after 10 minutes～30 minutes again drying or handle, can obtain the porous powder material that high activity oxide coats through 500 ℃～1200 ℃ high temperature sinterings;
Wherein said component and the weight percent content that contains the aqueous solution of oxide compound is:
Nano titanium dioxide 2%～10%
Titanium compound 0～15%
Soluble alkaline earth salt 5%～30%
Boride 0～10%
Silicide 0～10%
Water 65%～90%.
4. the porous powder preparation methods that activating oxide as claimed in claim 3 coats, the drying process that it is characterized in that described routine is air stream drying, spraying drying or fluidized drying.
5. the porous powder preparation methods that activating oxide as claimed in claim 3 coats is characterized in that alkaline earth metal oxide is BaO, CaO or MgO in the described meticulous homogeneous slurry, and described silicide is SiO 2Or Na 2SiO 3, described boride is B 2O 3, H 3BO 3Or Na 2B 4O 7, described rare earth oxide is La 2O 3Or CeO 2, described high molecular weight water soluble polymer is polyvinyl alcohol, polyoxyethylene glycol, polyoxyethylene, methylcellulose gum, carboxymethyl cellulose or carboxyethyl cellulose.
6. the porous powder preparation methods that activating oxide as claimed in claim 3 coats is characterized in that soluble alkaline earth salt is nitrate of baryta, magnesium nitrate, calcium chloride or magnesium chloride in the described aqueous solution that contains oxide compound; Described titanium compound is a tetrabutyl titanate; Described boride is a boric acid; Described silicide is silicic acid or aerosil.
7. the purposes of the porous powder material that coats as the described a kind of activating oxide of claim 1-2, but it is characterized in that being used for the coating of production environment purifying air, self-cleaning, deodorization, antibiotic and antiscale and have the printing ink of a series of special uses of photocatalysis characteristic and the stopping composition auxiliary agent of printing coatings.
CN99126362A 1999-12-17 1999-12-17 Active oxide coated porous powder and its preparing process and application Expired - Fee Related CN1095487C (en)

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CN100444952C (en) * 2006-04-30 2008-12-24 天津南开戈德集团有限公司 Supported nanometer crystalline titania photocatalyst and its prepn process
CN101070197B (en) * 2006-05-09 2011-04-20 北京化工大学 Method for preparing porous glass ball with optical catalytic activity
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CN102702571A (en) * 2012-05-23 2012-10-03 沈阳化工大学 Preparation method of flame-retardant antibiotic composite material of magnesium hydrate/titanium dioxide
CN102924979A (en) * 2012-11-05 2013-02-13 昆明理工大学 Method for preparing inorganic and organic coating titanium dioxide
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CN107683257A (en) * 2015-03-30 2018-02-09 谢珀德颜色公司 The composite of nanocrystal is absorbed containing UV
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CN101070197B (en) * 2006-05-09 2011-04-20 北京化工大学 Method for preparing porous glass ball with optical catalytic activity
CN101322497B (en) * 2008-07-08 2012-07-25 西南科技大学 Active stephanoporate mineral TiO2-doped composite catalytic antimicrobial material preparation and using method
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CN107683257A (en) * 2015-03-30 2018-02-09 谢珀德颜色公司 The composite of nanocrystal is absorbed containing UV
CN106082291A (en) * 2016-06-22 2016-11-09 江西鑫陶科技股份有限公司 A kind of preparation method of activated alumina desiccant
CN106082291B (en) * 2016-06-22 2017-09-12 江西鑫陶科技股份有限公司 A kind of preparation method of activated alumina desiccant
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