CN109593575A - A kind of preparation method of cerium based nano-material - Google Patents
A kind of preparation method of cerium based nano-material Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
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- C10L1/10—Liquid carbonaceous fuels containing additives
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- C10L1/1233—Inorganic compounds oxygen containing compounds, e.g. oxides, hydroxides, acids and salts thereof
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
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- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
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Abstract
The invention discloses a kind of preparation method of cerium based nano-material, which is prepared by micro passage reaction, which includes at least I section, II section, III section, IV section be sequentially connected along solution flow direction；The preparation method in I section the following steps are included: carry out precipitation reaction；Oxidation reaction is carried out in II section；Dispersed in III section；It is modified and oily molten that long chain organic acid is carried out in IV section；Finally collect the reaction solution in micro passage reaction, stratification takes oily phase to obtain the final product.The present invention carries out reaction controlling using micro passage reaction, can be realized continous way generation, and shortens reaction time (residence time of the solution in reactor is 40-110s), improves the stability of technique；Precipitation solid object is dispersed by dispersing agent simultaneously, avoids sediment in micro passage reaction formation blocking in conjunction with the control of flow rate of liquid.
Description
Technical field
The invention belongs to fuel oil additive fields, and in particular to a kind of to carry out the addition of cerium base diesel oil using micro passage reaction
The preparation method of agent.
Background technique
Diesel engine causes to pollute owner in its tail gas because of diesel oil oxygen-enriched and non-uniform combustion characteristic in the combustion chamber
It to be nitrogen oxides and PM particulate matter.It include pour-point depressant, stabilizer, emulsifier, detersive, cetane number improver using addition
All kinds of diesel fuel additives products common in the market inside can improve oil plant quality and promote burning, improve fuel economy, but right
It is smaller that exhaust pollutant discharges actual influence.Nano-cerium oxide (CeO2) in cerium valence state it is variable, there is good storage oxygen/put oxygen
Ability, can be catalyzed carbon-smoke combustion reduces reaction temperature.Cerium base diesel fuel additives can reduce diesel motor exhaust PM particulate matter row
It puts, prevents the enrichment of grain catcher of the PM in exhaust aftertreatment pipeline, reduce tail gas pipeline vapour lock, to reach reduction oil
The energy-saving effect of consumption.In Europe and north America region, it has been widely applied nearly 20 years.External product has the Envirox of Britain, France
The products such as the Eolys of Rhodia and the Pt Plus of U.S.Clean diesel oil company.China is in this product scope, still category blank.
Particle concentration in tail gas can be reduced into diesel oil by directlying adopt the addition of organic acid cerium salt, but it is not suitable in bavin
The practical use demand stored for a long time in oil.Chinese patent CN102101691B is reported a kind of prepared using hypergravity equipment and existed
The nano-cerium oxide of stable dispersion can be formed in non-polar oil, but the big equipment investment of its batch inventory is high, land occupation is big
Energy consumption is high.Foreign patent WO 03/040270A2 and US7459484B2, which are disclosed, prepares metal oxygen using multistep batch process
Change the method for nano material diesel fuel additives, but its step more times are long, production efficiency is lower.
Intermolecular reaction mass transfer velocity is accelerated in micro passage reaction and reaction temperature control is more accurate, enhances mass transfer and heat transfer
Reaction time to second or minute grade can be greatly reduced in process, and when avoiding in tank reactor reactant concentration with reaction
Between the shortcomings that changing, process stabilizing, product batches stability is high.But it is solid due to being had in the preparation process of cerium based nano-material
Body precipitating generates, and be easy to cause micro passage reaction pipeline blockage using micro passage reaction.
Summary of the invention
The purpose of the present invention is to solve defect existing in the prior art, provide one kind can continous way production, instead
It is short between seasonable, and the preparation process of the controllable cerium base diesel fuel additives of process stabilizing.
In order to achieve the above object, the present invention provides a kind of preparation method of cerium based nano-material, the cerium base nanometer materials
Material is prepared by micro passage reaction, which includes at least I section be sequentially connected, II along solution flow direction
Section, III section, IV section；The preparation method specifically includes the following steps:
(1) aqueous solution of soluble cerium salt and alkaline aqueous solution settling step: are pumped into microchannel by I sections of inlet respectively
Precipitation reaction is carried out in I section of reactor, controls the aqueous solution and the alkaline aqueous solution mixing that are pumped into speed and make cerium salt of solution
Journey time of the solution afterwards in I section is 5-35s, and controlling the reaction temperature in I section is 0-50 DEG C；
(2) oxidation step: oxidant is pumped into II section of inlet of micro passage reaction, it is intended to which general+trivalent cerium is oxidized to+4
Valence,；
(3) dispersion steps: dispersant solution is pumped into III section of inlet of micro passage reaction；
(4) the molten step of oil: changed in the oil-phase solution that IV section of inlet of micro passage reaction is pumped into long chain organic acid
Property reaction, the speed that is pumped into for controlling oil-phase solution makes journey time of the mixed solution in IV section be 15-55s, and controls
Reaction temperature in IV section of system is 50-90 DEG C；
(5) reaction solution in micro passage reaction is collected, 12-24h, layering are stood, gained oil is mutually cerium base nanometer
Material solution.
Aqueous solution, the alkaline aqueous solution of soluble cerium salt in step (1), the oxidant in step (2), in step (3)
Dispersing agent, the oil-phase solution of the long chain organic acid in step (4) is persistently pumped into, until preparation process terminates.
Wherein, control solution in each step is pumped into speed so that the soluble cerium salt being pumped into the unit time, dispersion
The molar ratio of agent is 100:5-80.
Further, control solution in each step is pumped into speed, so that the soluble cerium salt being pumped into the unit time, oxygen
Agent, dispersing agent, long chain organic acid molar ratio be 100:45-55:5-80:35-80, preferred molar ratio 100:50:63:
70。
Wherein, soluble cerium salt uses cerous nitrate or cerous acetate (concentration 0.01-1.5mol/L, preferred concentration 0.1-
0.7mol/L)；Alkaline aqueous solution uses ammonium hydroxide or sodium hydrate aqueous solution (concentration 0.01-2mol/L, preferred concentration 0.1-
0.7mol/L)；Oxidant uses hydrogen peroxide or hypochlorite；Dispersing agent use neopelex, acetic acid, molecular weight for
One of the polyethylene glycol of 800-2000, ethanol amine or a variety of mixing；Long chain organic acid uses the saturated fatty acid of C8-C18；
Oil-phase solution uses long-chain fat hydrocarbon solvent D60 or D80.Preferably, long chain organic acid in the oil-phase solution of long chain organic acid
Concentration is 5wt%.
Further, the temperature in step (1) in I section is preferably controlled in 10-20 DEG C；II section of temperature control in step (2)
System is at 25-35 DEG C；The temperature that (3) III sections of step controls in 25-35 DEG C；IV section of temperature is preferably controlled in 70- in step (4)
80℃。
Preferably, when being pumped into the stroke that speed makes mixed solution in II section of oxidant is controlled in step (2)
Between be 5-15s；The speed that is pumped into of control dispersant solution makes journey time of the mixed solution in III section in step (3)
For 5-15s.
The present invention has the advantage that compared with prior art
The present invention carries out reaction controlling using micro passage reaction, when can be realized continous way generation, and shortening reaction
Between (total residence time of the solution in reactor be 40-110s), improve the stability of technique.
The present invention disperses precipitation solid object by dispersing agent, avoids sediment to micro- logical in conjunction with the control of flow rate of liquid
The blocking of road reactor；The nanometer cerium hydroxide being prepared after precipitating and oxidation is changed using long chain organic acid simultaneously
Property, it can be stable in the presence of in oil-phase solution.
The cerium based nano-material oil-phase solution that the present invention is prepared can be used for diesel fuel additives, can effectively be catalyzed reduction bavin
The initiation temperature of oil, effectively reduces the discharge of particulate matter in diesel motor exhaust, and can stablize oily solution after storage 1.5 years
Soilless sticking precipitating.
Detailed description of the invention
The transmission electron microscope photo of cerium based nano-material in the oiliness sample that Fig. 1 is prepared for the embodiment of the present invention 1；
The particle diameter distribution test chart of cerium based nano-material in the oiliness sample that Fig. 2 is prepared for the embodiment of the present invention 1；
The XRD diagram for the powder that the oiliness sample that Fig. 3 is the embodiment of the present invention 1, embodiment 2 is prepared obtains after being evaporated；
Fig. 4 be various embodiments of the present invention prepare after gained oiliness sample is evaporated obtained powder after the finely ground mixing of carbon dust
The comparison spectrogram of temperature programmed oxidation under oxygen-argon composite atmosphere；
In Fig. 4, summit temperature is oxygen consumption peak when mixing carbon burning in sample, i.e. carbon and the mixed ignition temperature of cerium oxide
Degree；
Fig. 5 is that (Ce element contains in diesel oil after 1 gained oiliness sample of the embodiment of the present invention is mixed with commercially available state five No. 0 diesel oil
Measure 15ppm) and ordinary diesel oil motor exhaust smoke intensity contrast schematic diagram (filter paper smoke meter, engine speed 2800r/min conduct
Experimental test operating condition).
Specific embodiment
The present invention is described in detail combined with specific embodiments below.
The interior caliber of micro passage reaction used is 0.1-6mm in following embodiment.
Embodiment 1
Settling step: by 0.15mol/L cerous acetate aqueous solution, 0.2mol/L ammonium hydroxide respectively with 18ml/min, 49ml/min
Constant flow rate, be pumped into the I section of micro passage reaction mixing and carry out precipitation reaction.Journey time of the mixed solution in I sections
For 7.2s, 15 DEG C of reaction temperature, system pH 8 after reaction.
Oxidation step: 10wt% hydrogen peroxide solution, flow velocity 0.5ml/min are pumped into II section of micro passage reaction.Pump
Entering journey time of the total mixed solution after hydrogen peroxide in II section is 7.1s, and controlling the temperature in II section is 30 DEG C.
Dispersion steps: 1mol/L aqueous acetic acid, flow velocity 1.7ml/min are pumped into III section of micro passage reaction.Pump
Entering journey time of the total mixed solution after acetic acid in III section is 6.9s, and controlling the temperature in III section is 30 DEG C.
The molten step of oil: being pumped into the D80 boat coal solution of isooctyl acid into IV section of micro passage reaction, and concentration 5wt% is pumped into
Speed is 6.8ml/min.It is pumped into journey time 25.3s of the total mixed solution after organic acid in IV section, and controls IV section
In reaction temperature be 75 DEG C.
Raw material in each step is persistently pumped into according to predetermined flow rate, until the product cerium base of preparation amount needed for the production phase
The corresponding raw material of nano material is all pumped into completion.
Collect micro passage reaction mixed solution after the reaction was completed, gained mixed solution is stood 16h liquid separation, in oily phase
It can be used for diesel fuel additives containing cerium based nano-material.
In the embodiment, the soluble cerium salt that is pumped into the unit time, oxidant, dispersing agent, long chain organic acid mole
Than for 100:50:63:70.
The molar content of Ce is 0.053g/mL in final oil phase product.
The oily phase sample for taking the embodiment to be prepared carries out the detection of cerium based nano-material: from the transmission electron microscope photo of Fig. 1
As can be seen that the partial size substantially 8-15nm of gained cerium based nano-material.Fig. 2 show 1 gained cerium based nano-material of embodiment
Particle diameter distribution test chart, average grain diameter 14nm.
From Fig. 1, Fig. 2 it is comprehensive known in the oily phase sample of gained cerium sill partial size be Nano grade, and even particle size distribution,
It concentrates, without obvious agglomeration.
Embodiment 2
Settling step: by 0.4mol/L cerous nitrate aqueous solution, 0.1mol/L ammonium hydroxide respectively with 3ml/min, 48ml/min's
Constant flow rate is pumped into mixing in the I section of micro passage reaction and carries out precipitation reaction.Journey time of the mixed solution in I sections be
28.2s, 0 DEG C of reaction temperature, system pH 10 after reaction.
Oxidation step: the aqueous sodium hypochlorite solution of 0.5mol/L, flow velocity are pumped into II section of micro passage reaction
1.2ml/min.Being pumped into journey time of the total mixed solution after sodium hypochlorite in II section is 9.2s, and is controlled in II section
Temperature is 15 DEG C.
Dispersion steps: 0.2mol/L aqueous ethanolamine, flow velocity 2.7ml/ are pumped into III section of micro passage reaction
min.Being pumped into journey time of the total mixed solution after ethanol amine in III section is 8.7s, and controlling the temperature in III section is 45
℃。
In the molten step of oil: it is pumped into the D80 boat coal solution of ten tetra-carbonics into IV section of micro passage reaction, concentration 5wt%,
Being pumped into speed is 4.4ml/min.It is pumped into journey time 48.6s of the total mixed solution after organic acid in IV section, and is controlled
Reaction temperature in IV section is 55 DEG C.
Raw material in each step is persistently pumped into according to predetermined flow rate, until the product cerium base of preparation amount needed for the production phase
The corresponding raw material of nano material is all pumped into completion.
Collect micro passage reaction mixed solution after the reaction was completed, gained mixed solution is stood 13h liquid separation, in oily phase
It can be used for diesel fuel additives containing cerium based nano-material.
In the embodiment, the soluble cerium salt that is pumped into the unit time, oxidant, dispersing agent, long chain organic acid mole
Than for 100:50:45:65.
The molar content of Ce is 0.036g/mL in final oil phase product.
The oily phase sample for taking the embodiment to be prepared carries out the detection of cerium based nano-material: can from transmission electron microscope picture
Out, cerium based nano-material particle diameter distribution is in 13-23nm；From particle size distribution measuring as can be seen that cerium based nano-material average grain diameter
For 20nm.
Cerium sill partial size is Nano grade, and even particle size distribution, collection in the oily phase sample that the embodiment is prepared
In, without obvious agglomeration.
Embodiment 3
Settling step: by 0.7mol/L cerous nitrate aqueous solution, 0.7mol/L ammonium hydroxide respectively with 10ml/min, 34.5ml/min
Constant flow rate, be pumped into the I section of micro passage reaction mixing and carry out precipitation reaction.Journey time of the mixed solution in I sections
For 10.8s, 45 DEG C of reaction temperature, system pH 7 after reaction.
Oxidation step: the hydrogen peroxide solution of 10wt%, flow velocity 1.2ml/min are pumped into II section of micro passage reaction.
Being pumped into journey time of the total mixed solution after hydrogen peroxide in II section is 10.5s, and controlling the temperature in II section is 45 DEG C.
Dispersion steps: being pumped into the sodium dodecyl benzene sulfonate aqueous solution of 10wt% into III section of micro passage reaction, stream
Fast 2.2ml/min.Being pumped into journey time of the total mixed solution after dispersing agent in III section is 10s, and is controlled in III section
Temperature is 15 DEG C.
In the molten step of oil: it is pumped into the D80 boat coal solution of isostearic acid into IV section of micro passage reaction, concentration 5wt%,
Being pumped into speed is 26.4ml/min.It is pumped into journey time 19.4s of the total mixed solution after organic acid in IV section, and is controlled
Reaction temperature in IV section is 85 DEG C.
Raw material in each step is persistently pumped into according to predetermined flow rate, until the product cerium base of preparation amount needed for the production phase
The corresponding raw material of nano material is all pumped into completion.
Collect micro passage reaction mixed solution after the reaction was completed, gained mixed solution is stood 16h liquid separation, in oily phase
It can be used for diesel fuel additives containing cerium based nano-material.
In the embodiment, the soluble cerium salt that is pumped into the unit time, oxidant, dispersing agent, long chain organic acid mole
Than for 100:50:10:53.
The molar content of Ce is 0.035g/mL in final oil phase product.
The oily phase sample for taking the embodiment to be prepared carries out the detection of cerium based nano-material: can from transmission electron microscope picture
Out, cerium based nano-material particle diameter distribution is in 20-31nm；From particle size distribution measuring as can be seen that cerium based nano-material average grain diameter
For 28nm.
Cerium sill partial size is Nano grade, and even particle size distribution, collection in the oily phase sample that the embodiment is prepared
In, without obvious agglomeration.
Embodiment 4
Settling step: by 0.1mol/L cerous acetate aqueous solution, 0.1mol/L sodium hydroxide respectively with 10ml/min,
The constant flow rate of 31.3ml/min is pumped into mixing in the I section of micro passage reaction and carries out precipitation reaction.Mixed solution is in I sections
Journey time be 23.2s, 40 DEG C of reaction temperature, system pH 8.5 after reaction.
Oxidation step: the hydrogen peroxide solution of 10wt%, flow velocity 0.2ml/min are pumped into II section of micro passage reaction.
Being pumped into journey time of the total mixed solution after hydrogen peroxide in II section is 11.6s, and controlling the temperature in II section is 30 DEG C.
Dispersion steps: the ethyl alcohol of the polyethylene glycol (molecular weight 800) of 20wt% is pumped into III section of micro passage reaction
Solution, flow velocity 1.4ml/min.Being pumped into journey time of the total mixed solution after dispersing agent in III section is 11.2s, and is controlled
Temperature in III section is 30 DEG C.
In the molten step of oil: being pumped into the D60 boat coal solution of isooctyl acid, concentration 5wt%, pump into IV section of micro passage reaction
Entering speed is 1.6ml/min.It is pumped into journey time 32.4s of the total mixed solution after organic acid in IV section, and controls IV
Reaction temperature in section is 85 DEG C.
Raw material in each step is persistently pumped into according to predetermined flow rate, until the product cerium base of preparation amount needed for the production phase
The corresponding raw material of nano material is all pumped into completion.
Collect micro passage reaction mixed solution after the reaction was completed, gained mixed solution is stood 20h liquid separation, in oily phase
It can be used for diesel fuel additives containing cerium based nano-material.
In the embodiment, the soluble cerium salt that is pumped into the unit time, oxidant, dispersing agent, long chain organic acid mole
Than for 100:50:35:45.
The molar content of Ce is 0.083g/mL in final oil phase product.
Take the embodiment that oily phase sample is prepared and carry out the detection of cerium based nano-material: from transmission electron microscope picture as can be seen that
Cerium based nano-material particle diameter distribution is in 25-40nm；From particle size distribution measuring as can be seen that cerium based nano-material average grain diameter is
33nm。
Cerium sill partial size is Nano grade, and even particle size distribution, collection in the oily phase sample that the embodiment is prepared
In, without obvious agglomeration.
Effect example
Gained oiliness sample obtains ceria oxide powder after being evaporated at 500 DEG C in Example 1,2.Embodiment 1,2 oil samples pair
The powder X-ray RD spectrogram answered, is shown in Fig. 3.Illustrate that cerium oxide can be formed after cerium based nano-material oil sample obtained by the method for the present invention is heated,
In, XRD peak shape wideization obviously illustrates that this cerium oxide is nanoscale cerium.
After taking in each embodiment oil sample to be evaporated gained nano-cerium oxide powder with certain carbon dust is finely ground mix after (mixed proportion is
4:1) in oxygen argon (O2/ Ar, 10%) under mixed atmosphere temperature programmed oxidation spectrogram (being compared with pure carbon powder), such as Fig. 4 institute
Show.Wherein peak shape corresponds to carbon dust burning oxygen consumption, and summit temperature corresponds to carbon and the mixed initiation temperature of cerium oxide.Illustrate the present invention
Gained oiliness sample energy catalysis oxidation reduces carbon dust initiation temperature, and optimal with 1 products obtained therefrom effect of the embodiment of the present invention.
After 1 gained oiliness sample of embodiment is mixed with commercially available state five No. 0 diesel oil (Ce constituent content 15ppm in diesel oil) and
Ordinary diesel oil motor exhaust smoke intensity compares (filter paper smoke meter, engine speed 2800r/min is as experimental test operating condition), such as
Shown in Fig. 5.Illustrating oil product obtained by the present invention as diesel fuel additives can effectively reduce particulate matter in diesel motor exhaust
Discharge.
Claims (7)
1. a kind of preparation method of cerium based nano-material, it is characterised in that: the cerium based nano-material passes through micro passage reaction system
Standby, which includes at least I section, II section, III section, IV section be sequentially connected along solution flow direction；The preparation
Method the following steps are included:
(1) settling step: the aqueous solution of soluble cerium salt and alkaline aqueous solution are pumped into microchannel plate by I sections of inlet respectively and answered
Precipitation reaction is carried out in I section of device, the speed that is pumped into for controlling solution makes the aqueous solution of soluble cerium salt and alkaline aqueous solution mixed
Journey time of the solution in I section after conjunction is 5-35s, and controlling the reaction temperature in I section is 0-50 DEG C；
(2) oxidation step: oxidant is pumped into II section of inlet of micro passage reaction；
(3) dispersion steps: dispersant solution is pumped into III section of inlet of micro passage reaction；
(4) it the molten step of oil: is modified instead in the oil-phase solution that IV section of inlet of micro passage reaction is pumped into long chain organic acid
It answers, the speed that is pumped into for controlling oil-phase solution makes journey time of the mixed solution in IV section be 15-55s, and controls IV
Reaction temperature in section is 50-90 DEG C；
(5) reaction solution in micro passage reaction is collected, 12-24h, layering are stood, gained oil is mutually cerium based nano-material
Solution；
Aqueous solution, the alkaline aqueous solution of soluble cerium salt in the step (1), the oxidant in step (2), in step (3)
Dispersing agent, the oil-phase solution of the long chain organic acid in step (4) is persistently pumped into, until preparation process terminates.
2. preparation method according to claim 1, it is characterised in that: control solution in each step is pumped into speed, so that
Soluble cerium salt, the molar ratio of dispersing agent being pumped into unit time are 100:5-80.
3. preparation method according to claim 2, it is characterised in that: control solution in each step is pumped into speed, so that
The soluble cerium salt that is pumped into unit time, oxidant, dispersing agent, long chain organic acid molar ratio be 100:45-55:5-80:
35-80。
4. preparation method according to claim 3, it is characterised in that: control solution in each step is pumped into speed, so that
The soluble cerium salt that is pumped into unit time, oxidant, dispersing agent, long chain organic acid molar ratio be 100:50:63:70.
5. preparation method according to any one of claims 1 to 4, it is characterised in that: the solubility cerium salt uses cerous nitrate
Or cerous acetate；The alkaline aqueous solution uses ammonium hydroxide or sodium hydrate aqueous solution；The oxidant uses hydrogen peroxide or hypochlorous acid
Salt；The dispersing agent uses neopelex, acetic acid, molecular weight in the polyethylene glycol of 800-2000, ethanol amine
One or more mixing；The long chain organic acid uses the saturated fatty acid of C8-C18；The oil-phase solution uses long-chain fat
Hydrocarbon solvent D60 or D80.
6. preparation method according to claim 5, it is characterised in that: the temperature control in the step (1) in I section exists
10-20℃；II section of temperature is controlled at 25-35 DEG C in the step (2)；The temperature of (3) III sections of the step is controlled in 25-35
In DEG C；IV section of temperature is controlled at 70-80 DEG C in the step (4).
7. preparation method according to claim 6, it is characterised in that: control oxidant is pumped into speed in the step (2)
Degree is so that journey time of the mixed solution in II section is 5-15s；Control dispersant solution is pumped into the step (3)
Speed makes journey time of the mixed solution in III section be 5-15s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811571252.4A CN109593575B (en) | 2018-12-21 | 2018-12-21 | Preparation method of cerium-based nano material |
Applications Claiming Priority (1)
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| CN114524450A (en) * | 2022-03-21 | 2022-05-24 | 南京科技职业学院 | Preparation method of nano cerium oxide ultraviolet absorbent |
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