CN103145168A - Particle-size-controllable nano and sub-micron CeO2 preparation method - Google Patents
Particle-size-controllable nano and sub-micron CeO2 preparation method Download PDFInfo
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- CN103145168A CN103145168A CN201310063928XA CN201310063928A CN103145168A CN 103145168 A CN103145168 A CN 103145168A CN 201310063928X A CN201310063928X A CN 201310063928XA CN 201310063928 A CN201310063928 A CN 201310063928A CN 103145168 A CN103145168 A CN 103145168A
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Abstract
The invention relates to a particle-size-controllable nano and sub-micron CeO2 preparation method which is characterized by comprising the following steps: by taking cerium nitrate as a solution, adding high molecular surface composite dispersant into the solution, heating the solution to 70-100 DEG C, adding a precipitant solution while stirring in the solution, filtering the precipitate, and then firing at 400-550 DEG C to obtain CeO2 having different particle sizes. The invention has the following advantages: the nano and sub-micron CeO2 prepared by controlling the concentration of the cerium nitrate and controlling the combination and addition of the composite dispersant based on a chemical precipitation method through precipitating, filtering and firing can achieve particle size controllability; the method omits water washing and drying operations; and the preparation method is simple in related equipment and steps, low in cost, low in energy consumption, simple to operate and controllable in particle size.
Description
Technical field:
The present invention relates to the controlled preparation nanometer of a kind of granularity and submicron CeO
2Method, belong to nanocrystalline rare earth oxides system standby field.
Background technology:
Nanometer and submicron CeO
2Be a kind of functional materials of excellent performance, purposes is very wide, can be used on electronic ceramics, radioresistive glass, glass polishing, luminescent material, high temperature oxygen sensitive material, sensing material, solid oxide fuel cell electrode material; Nanometer and submicron CeO
2Have superior oxygen function and the quick oxygen of the high temperature room diffusibility stored, be used in redox reaction and the purifying vehicle exhaust material; Nano Ce O
2Because of its absorb and the scatters ultraviolet ability strong, be used in the fields such as sunlight screening skin-protecting product, fiber, coating, plastics, rubber.
Prepare at present nanometer and submicron CeO
2Method vapor phase process, solid phase method and liquid phase method are arranged, the sol-gel processing in liquid phase method, chemical precipitation method, spray reaction, micro emulsion method, hydrothermal method are preparation nanometer and submicron Ce0
2Main method, wherein the chemical precipitation method processing unit is simple, process is easy to control, cost is low, is fit to suitability for industrialized production.The present invention prepares nanometer and submicron CeO with chemical precipitation method
2Granularity can be reached controlled.
Chinese patent CN1215981C discloses with the precipitator method and has prepared nano Ce O
2The operational path of powder, its preparation process divided for 7 steps carried out, and (1) is mixed with cerous nitrate-ethanolic soln take cerous nitrate, cerium dichloride or cerium dioxide as raw material, and wherein cerous nitrate concentration is 0.2mol/L～0.4mol/L; (2) precipitation agent is ammoniacal liquor-ethanolic soln, and wherein ammonia concn is 1mol/L～3mol/L; (3) in 25 ℃～40 ℃, cerous nitrate-ethanolic soln is added drop-wise in precipitation agent, pH is 9～12, forms gel; (4) gel ageing 12～24 hours in mother liquor; (5) filter, use deionized water wash; (6) in 80 ℃～120 ℃ dryings 5～10 hours; (7) in 400 ℃～550 ℃ roastings 2～5 hours, obtain nano Ce O
2
Chinese patent CN1607180A adopts the micro emulsion homogeneous precipitation method, take cerous carbonate as raw material, through salpeter solution, filtration, add slow release precipitator in solution after filtration, through newborn precipitation from homogeneous solution (PFHS), obtain adding again dispersion agent after presoma, utilize ultrasonic oscillation, carry out the micro emulsion ultrasonic washing, filtration, oven dry obtain oxide nano rare earth.
The preparation method of a Chinese patent CN1821314A super fine cerium oxide for polishing, preparation contains the salts solution of ion, then add tensio-active agent in this solution, contact with a kind of alkaline matter, control the pH value of reaction suspended substance, generate throw out, transform with oxalic acid, control the pH value, filtration, washing, drying, 600 ℃～1000 ℃ lower calcinations, obtain fine cerium oxide.
In the preparation method of Chinese patent CN1215981C, Chinese patent CN1821314A and CN1607180A, technique is precipitation, filtration, washing, dry, calcination, complex operation, and cost is high, and the nano-oxide of preparation is easily reunited, and is wayward.And its preparation process of the present invention is precipitation, filtration, calcination, has saved washing and drying process, controls cerous nitrate concentration, controls composite dispersing agent combination and add-on, through precipitation, filtration, calcination, the nano Ce O for preparing
2Reach granularity controlled.
Summary of the invention:
The objective of the invention is for present preparation nano Ce O
2The uppity shortcoming of granularity provides a kind of low for equipment requirements, controlled preparation nanometer of granularity that technique is simple, easy and simple to handle, cost is low and submicron CeO
2Method, make CeO
2Granularity can reach D
50:＜50nm, D
50: 50nm～100nm, D
50: 100nm～150nm, D
50: the product of four class of 150nm～200nm.
The controlled preparation nanometer of a kind of granularity of the present invention and submicron CeO
2Method, adopt following steps to realize:
(1) be by the CeO that finally prepares in 0.1mol/L～2.0 mol/L cerous nitrate solutions in the concentration for preparing
2Weight 0.1%～5% add composite dispersing agent, form A solution;
(2) precipitation agent is water-soluble, being mixed with concentration is the B solution of 2mol/L～3mol/L;
(3) A solution is heated to 70 ℃～100 ℃, then B solution is added dropwise to carries out chemical reaction in A solution, in 3 minutes～180 minutes reaction times, controlling reaction end pH value is 7～10;
(4) step 3 stirred 10 minutes～60 minutes after forming throw out again;
(5) throw out with step 4 filters out, and this throw out is presoma C;
(6) with presoma C 400 ℃～550 ℃ lower calcinations 2 hours～4 hours, the calcination process is after heating up with the heat-up rate of per hour 100 ℃～2000 ℃, to keep temperature, obtains nanometer and submicron CeO
2Product.
Composite dispersing agent described in step (1) is the mixing of two or more nonionogenic tenside;
Described nonionogenic tenside is styroyl phenol Soxylat A 25-7, polyacrylamide, polyoxyethylene glycol or polyvinyl alcohol;
Precipitation agent described in step (2) is a kind of in bicarbonate of ammonia, volatile salt.
The present invention has the following advantages:
The present invention utilizes chemical precipitation method to control the concentration of cerous nitrate, the combination of control composite dispersing agent and add-on, through precipitation, filtration, calcination, the nanometer of preparing and submicron CeO
2Reach granularity controlled.The technique of this method has been saved washing and dry, and equipment and the step that the preparation method relates to is simple, cost is low, energy consumption is low, easy and simple to handle, and granularity is controlled.
Embodiment:
Below in conjunction with embodiment, the present invention is done into a detailed description, but embodiments of the present invention are not limited to this.
Embodiment 1: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, be mixed with the 0.55mol/L cerous nitrate solution, get the cerous nitrate solution of this concentration of 10L, add polyacrylamide 1.18g, polyvinyl alcohol 1.18g, polyoxyethylene glycol 1.18g, styroyl phenol Soxylat A 25-7 1.18g to become A solution, get the NH of 7.68L2.5mol/L
4HCO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered out, then 400 ℃ of lower calcinations 4 hours, 100 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 9 nm.
Embodiment 2: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, be mixed with the 0.85mol/L cerous nitrate solution, get the cerous nitrate solution of this concentration of 8L, add styroyl phenol Soxylat A 25-7 3.90g, polyacrylamide 3.90g, polyoxyethylene glycol 3.90g to become A solution, get the NH of 9.49L2.5mol/L
4HCO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered, then 450 ℃ of lower calcinations 4 hours, 500 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 89 nm.
Embodiment 3: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, being mixed with the 1.05mol/L cerous nitrate solution, getting the cerous nitrate solution of this concentration of 6L, adding polyvinyl alcohol 8.13g, polyacrylamide 8.13g to become A solution, getting the NH of 8.79L2.5mol/L
4HCO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered, then 550 ℃ of lower calcinations 2 hours, 2000 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 102nm.
Embodiment 4: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, being mixed with the 1.55mol/L cerous nitrate solution, getting the cerous nitrate solution of this concentration of 4L, adding polyoxyethylene glycol 10.66g, polyvinyl alcohol 10.66g to become A solution, getting the NH of 8.66L2.5mol/L
4HCO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered, then 550 ℃ of lower calcinations 4 hours, 1000 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 179nm.
Embodiment 5: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, be mixed with the 0.1mol/L cerous nitrate solution, get the cerous nitrate solution of this concentration of 50L, add polyacrylamide 0.29g, polyvinyl alcohol 0.29g, 0.29 one-tenth A solution of polyoxyethylene glycol, get (the NH of 6.98L2.5mol/L
4)
2CO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered out, then 400 ℃ of lower calcinations 4 hours, 100 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 21nm.
Embodiment 6: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, be mixed with the 1.0mol/L cerous nitrate solution, get the cerous nitrate solution of this concentration of 5.8L, add styroyl phenol Soxylat A 25-7 9.98g, polyoxyethylene glycol 9.98g, polyvinyl alcohol 9.98g to become A solution, get (the NH of 8.1L2.5mol/L
4)
2CO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered out, then 400 ℃ of lower calcinations 4 hours, 500 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 79 nm.
Embodiment 7: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, be mixed with the 1.35mol/L cerous nitrate solution, get the cerous nitrate solution of this concentration of 4.3L, add polyoxyethylene glycol 19.97g, styroyl phenol Soxylat A 25-7 19.97g to become A solution, get (the NH of 8.1L2.5mol/L
4)
2CO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered out, then 550 ℃ of lower calcinations 4 hours, 1000 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 136 nm.
Embodiment 8: use the nitric acid dissolve cerous carbonate or use the water dissolution cerous nitrate, being mixed with the 2.0mol/L cerous nitrate solution, getting the cerous nitrate solution of this concentration of 2.8L, adding polyacrylamide 24.1g, polyoxyethylene glycol 24.1g to become A solution, getting (the NH of 7.8L2.5mol/L
4)
2CO
3Solution becomes B solution, and A solution is heated to 70 ℃～100 ℃, then B solution is added drop-wise to A solution, generates white precipitate, control pH value 7～10, then stirred this precipitation 10 minutes, throw out is filtered out, then 550 ℃ of lower calcinations 4 hours, 2000 ℃/hour of heat-up rates, product were nano Ce O
2, its laser particle analyzer test granularity D
50Be 167 nm.
Claims (4)
1. the controlled preparation nanometer of granularity and submicron CeO
2Method, it is characterized in that: preparation process is as follows:
(1) be by the CeO that finally prepares in 0.1mol/L～2.0 mol/L cerous nitrate solutions in the concentration for preparing
2Weight 0.1%～5% add composite dispersing agent, form A solution;
(2) precipitation agent is water-soluble, being mixed with concentration is the B solution of 2mol/L～3mol/L;
(3) A solution is heated to 70 ℃～100 ℃, then B solution is added dropwise to carries out chemical reaction in A solution, in 3 minutes～180 minutes reaction times, controlling reaction end pH value is 7～10;
(4) step 3 stirred 10 minutes～60 minutes after forming throw out again;
(5) throw out with step 4 filters out, and this throw out is presoma C;
(6) with presoma C 400 ℃～550 ℃ lower calcinations 2 hours～4 hours, the calcination process is after heating up with the heat-up rate of per hour 100 ℃～2000 ℃, to keep temperature, obtains nanometer and submicron CeO
2Product.
2. the controlled preparation nanometer of granularity according to claim 1 and submicron CeO
2Method, it is characterized in that: the composite dispersing agent described in step (1) is the mixing of two or more nonionogenic tenside.
3. the controlled preparation nanometer of granularity according to claim 2 and submicron CeO
2Method, it is characterized in that: described nonionogenic tenside is styroyl phenol Soxylat A 25-7, polyacrylamide, polyoxyethylene glycol or polyvinyl alcohol.
4. the controlled preparation nanometer of granularity according to claim 1 and submicron CeO
2Method, it is characterized in that: the precipitation agent described in step (2) is a kind of in bicarbonate of ammonia, volatile salt.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641146A (en) * | 2013-12-04 | 2014-03-19 | 内蒙古科技大学 | Preparation method of uniformly dispersed fusiform cerium carbonate particles |
| CN108002422A (en) * | 2018-01-31 | 2018-05-08 | 益阳鸿源稀土有限责任公司 | A kind of preparation method of high-purity sub-micron white ceric oxide |
| CN108637925A (en) * | 2018-04-24 | 2018-10-12 | 安徽禾臣新材料有限公司 | A kind of precision optics polishing damping cloth and preparation method thereof |
| CN112340766A (en) * | 2020-11-27 | 2021-02-09 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112675850A (en) * | 2020-12-23 | 2021-04-20 | 江苏广域化学有限公司 | Nickel catalyst, preparation method thereof and synthesis method of pyrimidine derivatives |
| CN115403064A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
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| CN1785815A (en) * | 2005-08-28 | 2006-06-14 | 内蒙古科技大学 | Preparation method of high specific surface area nano-cerium oxide |
| CN1837053A (en) * | 2006-04-12 | 2006-09-27 | 中南大学 | Process for preparing mesoporous ceria |
| CN101898787A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Method for synthesizing submicron cerium oxide by using liquid cerium chloride as raw material |
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2013
- 2013-02-28 CN CN201310063928XA patent/CN103145168A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1785815A (en) * | 2005-08-28 | 2006-06-14 | 内蒙古科技大学 | Preparation method of high specific surface area nano-cerium oxide |
| CN1837053A (en) * | 2006-04-12 | 2006-09-27 | 中南大学 | Process for preparing mesoporous ceria |
| CN101898787A (en) * | 2009-05-25 | 2010-12-01 | 甘肃稀土新材料股份有限公司 | Method for synthesizing submicron cerium oxide by using liquid cerium chloride as raw material |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103641146A (en) * | 2013-12-04 | 2014-03-19 | 内蒙古科技大学 | Preparation method of uniformly dispersed fusiform cerium carbonate particles |
| CN103641146B (en) * | 2013-12-04 | 2015-08-19 | 内蒙古科技大学 | A kind of preparation method of homodisperse fusiformis cerous carbonate particle |
| CN108002422A (en) * | 2018-01-31 | 2018-05-08 | 益阳鸿源稀土有限责任公司 | A kind of preparation method of high-purity sub-micron white ceric oxide |
| CN108637925A (en) * | 2018-04-24 | 2018-10-12 | 安徽禾臣新材料有限公司 | A kind of precision optics polishing damping cloth and preparation method thereof |
| CN108637925B (en) * | 2018-04-24 | 2020-08-04 | 安徽禾臣新材料有限公司 | Damping cloth for polishing precision optical device and preparation method thereof |
| CN112340766A (en) * | 2020-11-27 | 2021-02-09 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112340766B (en) * | 2020-11-27 | 2022-02-01 | 重庆大学 | Cerium oxide modified microwave hydrothermal carbon and preparation method and application thereof |
| CN112675850A (en) * | 2020-12-23 | 2021-04-20 | 江苏广域化学有限公司 | Nickel catalyst, preparation method thereof and synthesis method of pyrimidine derivatives |
| CN115403064A (en) * | 2022-09-20 | 2022-11-29 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
| CN115403064B (en) * | 2022-09-20 | 2023-10-13 | 中国科学院长春应用化学研究所 | Cerium oxide and preparation method thereof |
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Application publication date: 20130612 |