CN1302832A - Surface treating process for modifying nm-class oxide powder - Google Patents
Surface treating process for modifying nm-class oxide powder Download PDFInfo
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- CN1302832A CN1302832A CN 01102115 CN01102115A CN1302832A CN 1302832 A CN1302832 A CN 1302832A CN 01102115 CN01102115 CN 01102115 CN 01102115 A CN01102115 A CN 01102115A CN 1302832 A CN1302832 A CN 1302832A
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Abstract
A process for modifying the surface of nm oxide powder uses TiOSO4, ZrOCl2, AlCl3, MgCl2, or the ethyl silicate (25%) and crystal aluminium chloride (75%) as raw materials, and includes such steps as adding ammonia water or urea as precipitant to the solution, adding high-molecular surfactant (octylphenol polyoxyvinethene, polyvinyl alcohol or polyacrylic acid), deposition, water washing, drying and calcining. Its advantages are high dispersity and low cost. It can be used to prepare high-performance structural ceramic or functional ceramic.
Description
The present invention relates to a kind of surface treating process for modifying nm-class oxide powder.Belong to the nano powder surface treatment technology.
Over nearly more than 20 years, along with the high-performance ceramic preparation science and the flourish of research that use of the new technology, high-purity, the high reactivity and the super-refinement research boom of ceramic raw material also arise at the historic moment.But the super-refinement of powder reach nano level (1～100nm) time, cause the reunion (or even hard aggregation) of ultrafine particle easily, from and influence the performance of advantages such as its high reactivity.TiO with the wet chemistry method preparation
2, ZrO
2, MgO-Al
2O
3-SiO
2During etc. system's nm-class oxide powder or nanoparticle coating composite powder, in order to prevent to reunite, many both at home and abroad employing ethanol dehydrations, the capillary measure of reduction ultrafine particle, perhaps adopting expensive alkoxide is the colloidal sol-gel process of raw material, all receives effect preferably.But in scale production, adopt above-mentioned measure complex process, cost height.
A kind of surface treating process for modifying nm-class oxide powder that the object of the present invention is to provide.This method prepares nm-class oxide powder with wet chemistry method, and process is simple, preparation cost is low.
In order to achieve the above object, the present invention is achieved by the following technical solutions.With the soluble inorganic salt is main raw material, adopt co-precipitation, parcel precipitation or homogeneous depositing technology, the product that obtains after the precipitin reaction makes the nm-class oxide powder or the nanoparticle coating composite granule of surface modification through washing and postorder thermal treatment again, it is characterized in that, with TiOSO
4, ZrOCl
2, AlCl
3, MgCl
2Solution or be that crystal aluminum chloride solution is reaction solution with 1/4 ethyl silicate (TEOS) and 3/4; The concentration of reaction solution is 0.2～0.8mol/L, and solvent is mainly deionized water; Precipitation agent is ammoniacal liquor or urea; In reaction solution, add polyoxyethylene octylphenol ether (OP-10) or the polyvinyl alcohol (PVA) of 2～5wt% or polyacrylic acid (PAA) high molecular type surfactant of 0.5～1.5wt% of 2～5wt%; Temperature of reaction is 40～70 ℃; Polyoxyethylene glycol (PEG is further added in throw out washing back
600-1540) or polyoxyethylene octylphenol ether, and carry out drying at 80～120 ℃, promptly get desired product at 500～1000 ℃ temperature lower calcination at last.
Below the present invention is further described again.
The key of the technology of the present invention is to establish the suitable consumption and the interpolation process of high molecular type surfactant, its objective is to reduce the ultrafine particle surface tension and increase the potential barrier effect of interparticle space.Add OP-10, PVA, PAA in the precipitin reaction process, the amount ranges of OP-10 and PVA is 2～5wt%, and wherein the consumption of PAA is that 0.5～1.5wt% is better; Precipitation begin to reaction solution be final quantity 1/2 during, the solution of tensio-active agent added successively finish, to guarantee its anti-agglomeration effect in the proper concn scope.OP-10, PVA can compoundly add, and its consumption reduces by half separately, and the interpolation process is the same.Because throw out is removed Cl through washing
-Tensio-active agent also runs off thereupon in the time of harmful ions such as ion, in order to prevent that the gel particles surface directly contacts and forms hard aggregation in drying and calcination process, also needs further to add PEG
600～1540Or OP-10.
The invention will be further described with embodiment more below.Embodiment one: nanoparticle TiO
2The preparation 1 of the composite granule of coating coated talc powder) in the Glass Containers of 500ml, add 100ml deionized water and 8g talcum powder, PAA0.05g, stir and became uniform suspension in 15 minutes; 2) in beaker, add 100ml water and 15g titanyl sulfate raw material and 10g urea, be mixed with the transparent reaction liquid of pH＜2; 3) reaction solution is slowly added in the suspension, stirred 10 minutes, be heated to 70～80 ℃ then, continue 1 hour; 4) above-mentioned reaction precipitation thing is separated, washes, suction filtration obtains filter cake again; 5) take by weighing 0.05g OP-10, add the 10ml deionized water, make behind the solution and above-mentioned filter cake uniform mixing; 6) with behind the above-mentioned filtration cakes torrefaction, in electric furnace, calcine, 600～650 ℃ following 1 hour, obtain the good nanoparticle coating TiO of free-running property
2/ talcum powder wrapper (being composite granule).Embodiment two: Al
2O
3-SiO
2The preparation 1 of system's composite oxides nano-powder) in the Glass Containers of 500ml, add 30ml ethanol and 10ml TEOS, stir 5 powder clocks and become homogeneous solution (L1); , 2) and in beaker, add 150ml water and 33g crystal aluminum chloride raw material stirring is dissolved into clear solution (L2); L2 liquid is made an addition in the L1 liquid, be heated to 70 ℃, stirred 2 hours, impel TEOS prehydrolysis; 3) with 0.5g PEG
1540Make an addition in the said hydrolyzed liquid, after the stirred for several minute, drop to pH=8.0～8.5, continue to stir and obtain the precipitin reaction thing half an hour with 6N ammoniacal liquor; 4) above-mentioned reaction precipitation thing is separated, washes, suction filtration obtains filter cake again; 5) take by weighing 0.05g OP-10, add the 10ml deionized water, make behind the solution and above-mentioned filter cake uniform mixing; 6) with behind the above-mentioned filtration cakes torrefaction, calcine in electric furnace, 800～1000 ℃ following 1 hour.Cooling back ball milling obtained the good nanometer Al of free-running property in 2 hours
2O
3-SiO
2Composite oxide powder.
Advantage of the present invention, raw material sources are extensive; Preparation technology is simple; Gained powder good dispersion does not have and reunites, and can extensively use In preparation high performance structure ceramic and function ceramics.
Claims (1)
1. surface treating process for modifying nm-class oxide powder, with the soluble inorganic salt is main raw material, adopt co-precipitation, parcel precipitation or homogeneous depositing technology, the product that obtains after the precipitin reaction makes the nm-class oxide powder or the nanoparticle coating composite granule of surface modification through washing and postorder thermal treatment again, it is characterized in that: with TiOSO
4, ZrOCl
2, AlCl
3, MgCl
2Solution or be reaction solution with 1/4 ethyl silicate and 3/4 crystal aluminum chloride solution, the concentration of reaction solution is 0.2～0.8mol/L, solvent is mainly deionized water; Precipitation agent is ammoniacal liquor or urea; In reaction solution, add the polyoxyethylene octylphenol ether of 2～5wt%, or the polyvinyl alcohol of 2～5wt%, or the polyacrylic acid high molecular type surfactant of 0.5～1.5wt%; Temperature of reaction is 40～70 ℃; Polyoxyethylene glycol (PEG is further added in throw out washing back
600-1540) or polyoxyethylene octylphenol ether, and carry out drying at 80～120 ℃, promptly get desired product at 500～1000 ℃ temperature lower calcination at last.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011021152A CN1141341C (en) | 2001-01-21 | 2001-01-21 | Surface treating process for modifying nm-class oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011021152A CN1141341C (en) | 2001-01-21 | 2001-01-21 | Surface treating process for modifying nm-class oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1302832A true CN1302832A (en) | 2001-07-11 |
| CN1141341C CN1141341C (en) | 2004-03-10 |
Family
ID=4652484
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011021152A Expired - Fee Related CN1141341C (en) | 2001-01-21 | 2001-01-21 | Surface treating process for modifying nm-class oxide powder |
Country Status (1)
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| CN (1) | CN1141341C (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303167C (en) * | 2003-12-19 | 2007-03-07 | 上海电瓷厂 | Composite nano insulating paint processing method and coating method on zinc oxide valve plate |
| CN100457833C (en) * | 2005-10-26 | 2009-02-04 | 太原理工大学 | Nanometer SiO2 powder dispersion method |
| CN102660261A (en) * | 2012-04-19 | 2012-09-12 | 中国科学技术大学 | Preparation method of silicon oxynitride fluorescent powder |
| CN105254921A (en) * | 2015-10-13 | 2016-01-20 | 广东盛朗白石工业有限公司 | Water-soluble polymer complex lipid powder surface treating agent |
| CN107118519A (en) * | 2017-05-11 | 2017-09-01 | 安徽春辉仪表线缆集团有限公司 | A kind of instrument and meter polyester resin composite material |
| CN113817978A (en) * | 2021-09-23 | 2021-12-21 | 南京金鲤新材料有限公司 | Plasma spraying Al2O3-TiO2Method for preparing composite powder |
| CN114479506A (en) * | 2022-02-11 | 2022-05-13 | 豪宗（海口）新材料节能技术工程有限公司 | Antibacterial material for air conditioner and manufacturing method thereof |
-
2001
- 2001-01-21 CN CNB011021152A patent/CN1141341C/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1303167C (en) * | 2003-12-19 | 2007-03-07 | 上海电瓷厂 | Composite nano insulating paint processing method and coating method on zinc oxide valve plate |
| CN100457833C (en) * | 2005-10-26 | 2009-02-04 | 太原理工大学 | Nanometer SiO2 powder dispersion method |
| CN102660261A (en) * | 2012-04-19 | 2012-09-12 | 中国科学技术大学 | Preparation method of silicon oxynitride fluorescent powder |
| CN102660261B (en) * | 2012-04-19 | 2014-10-22 | 中国科学技术大学 | Preparation method of silicon oxynitride fluorescent powder |
| CN105254921A (en) * | 2015-10-13 | 2016-01-20 | 广东盛朗白石工业有限公司 | Water-soluble polymer complex lipid powder surface treating agent |
| CN107118519A (en) * | 2017-05-11 | 2017-09-01 | 安徽春辉仪表线缆集团有限公司 | A kind of instrument and meter polyester resin composite material |
| CN113817978A (en) * | 2021-09-23 | 2021-12-21 | 南京金鲤新材料有限公司 | Plasma spraying Al2O3-TiO2Method for preparing composite powder |
| CN114479506A (en) * | 2022-02-11 | 2022-05-13 | 豪宗（海口）新材料节能技术工程有限公司 | Antibacterial material for air conditioner and manufacturing method thereof |
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| Publication number | Publication date |
|---|---|
| CN1141341C (en) | 2004-03-10 |
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