CN104692400A - Preparation method of water-soluble inorganic nanometer material - Google Patents
Preparation method of water-soluble inorganic nanometer material Download PDFInfo
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Abstract
The invention discloses a preparation method of a water-soluble inorganic nanometer material. The preparation method comprises the following steps in sequence: dispersing an inorganic nanometer material in an organic solution, adding a treating agent A and reacting to obtain a suspension solution; separating and drying the suspension solution to obtain a separated and dried product; dispersing the separated and dried product in a nitric acid solution and collecting the suspension solution in the upper layer; separating and drying the suspension solution in the upper layer to obtain the separated and dried product, measuring the content of a solid phase in the separated and dried product and diluting by using the nitric acid solution to obtain a diluted solution; adding a treating agent B and a treating agent C into the diluted solution to react and then adding a treating agent D to react to obtain a reaction suspension solution; neutralizing and separating the reaction suspension solution and then performing constant-temperature drying to obtain a final product. The preparation method disclosed by the invention is simple, easy to understand, convenient to operate, accurate in results, low in cost and capable of being used for fundamentally solving the dispersion problem of the inorganic nanometer material in water.
Description
Technical field
The invention belongs to Surface Modification of Nanosized Materials technical field, relate to the preparation method of nano material, particularly relate to a kind of preparation method of water-soluble inorganic nano material.
Background technology
The structure of nano material has specificity, such as small-size effect, quantum size effect, surface effects and macro quanta tunnel effect etc., therefore in the various fields such as catalyzer, biotechnology, oil drilling engineering, demonstrates application prospect widely.
At present, the technology of preparing of nano material has been tending towards ripe, but carries out modification and process also there is great difficulty for difference use medium, different use occasion to nano-material surface.Such as, the outward appearance of nano material silicon-dioxide is amorphous white powder, and particle size range is at 1-100nm, and microtexture is spherical, presents cotton-shaped and netted grain pattern.It is one of ultra tiny New Inorganic Materials of extremely important high-tech, there is the excellent specific properties such as particle diameter is very little, specific surface area is large, superficial attractive forces is strong, surface energy is large, chemical purity is high, dispersing property is good, also there is satisfactory stability, reinforcing, thickening property and thixotropy.But the feature of the high-specific surface area of nano material, high surface energy, makes it flocculation very easily occur in water or reunite, is not easy dispersion, makes nano material lose meaning in water.
In oil gas drilling engineering field, usually use dispersion agent (as Sodium hexametaphosphate 99) to improve the dispersiveness of inorganic nano material in water, but dispersion agent can lose efficacy under the hot environment of Oil/gas Well depths, and the composite of drilling fluid can be affected.If itself carry out modification, grafting soluble groups to inorganic nano material surface, the scattering problem of inorganic nano material in water fundamentally can be solved.
Usual employing redox initiation method is to inorganic nano material modifying surface, and the method can initiated polymerization in a mild condition.Redox initiator can cause alcohol, amine, aldehyde, ketone, acid, mercaptan and vinyl monomer (as vinyl cyanide and acrylamide) and copolyreaction occurs.The successful graft polymerization reaction causing vinyl monomer and silica sphere in milk sap of redox initiator, such as styrene methyl methacrylate on aerosil surface, NIPA at nanometer silicon dioxide particle surface, acrylamide at the graft polymerization reaction of superfine silicon dioxide particle surface.So far, also nobody utilizes redox initiator that water soluble sulfonated monomer (as vinyl sulfonic acid or its esters) is grafted to the surface of functionalization inorganic nano material.Therefore, be badly in need of the preparation method of a kind of water-soluble inorganic nano material of exploitation, to realize the modification of himself, and then solve its problem easily occurring to reunite in water.
Summary of the invention
For solving problems of the prior art, the invention provides a kind of preparation method of water-soluble inorganic nano material, it comprises the following steps according to sequencing:
Step one: inorganic nano material is dispersed in organic solution, and add treatment agent A, be obtained by reacting suspension;
Step 2: carried out by suspension being separated, dry, obtains being separated desciccate;
Step 3: separation desciccate is dispersed in salpeter solution, and collect upper strata suspension;
Step 4: carried out by upper strata suspension being separated, dry, obtains being separated desciccate, and measures its solid load, then adopt salpeter solution dilution, obtain diluting soln;
Step 5: add treatment agent B and treatment agent C reacts in diluting soln, then adds treatment agent D and reacts, obtain reaction suspension;
Step 6: carried out neutralizing and being separated by reaction suspension, then freeze-day with constant temperature, obtains final product.
The preparation method of water-soluble inorganic nano material of the present invention, at the surface grafting hydrophilic radical of particulate inorganic nano material, to improve the water-soluble of particulate inorganic nano material, can make it in water, play the advantage of nano material, expands its Application Areas.By the method, also can improve the high temperature resistance of the inorganic nano material aqueous solution, avoid the composite problem of solution caused owing to adding dispersion agent simultaneously.
Preferably, in described step one, inorganic nano material is any one in silicon-dioxide, titanium dioxide, zinc oxide, ferric oxide, calcium carbonate.
In above-mentioned either a program preferably, in described step one, organic solution is any one in ethanol, toluene, methyl alcohol, ether, trichloromethane.
In above-mentioned either a program preferably, in described step one, treatment agent A is surface-modifying agent.
The present invention utilizes the group in treatment agent A (siloxy) to react with the surface group (hydroxyl) of particulate inorganic nano material, treatment agent A is grafted to the surface of inorganic nano material, obtain the inorganic nano material of functionalized (aminopropyl-functional), thus create more graft site on the surface of inorganic nano material.
In above-mentioned either a program preferably, described surface-modifying agent is silane coupling agent.
The surface of inorganic nano material can produce good consistency with organism after coupling agent treatment.Coupling agent molecule must possess two kinds of groups, a kind ofly carries out chemical reaction with the surface of inorganic nano material, and another kind of (organo-functional group) and organism react or compatible.The mechanism of action of coupling agent is, is hydrolyzed to form bonding between inorganic and organic interface, promotes interface fusion, strengthen the property.The siliceous part of silane coupling agent can provide the powerful keyed jointing to base material.
In above-mentioned either a program preferably, described silane coupling agent is any one in 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-aminopropyl triethoxysilane, 3-(methacryloxypropyl) propyl trimethoxy silicane.
In above-mentioned either a program preferably, in described step one, by the mode of mechanical stirring and/or ultrasonic vibration, inorganic nano material is dispersed in organic solution.
In step one, be dispersed in organic solution by churned mechanically mode by inorganic nano material, use agitator, rotating speed is 300rpm, mechanical stirring 20min; Inorganic nano material is dispersed in organic solution by the mode also by ultrasonic vibration, ultrasonic vibration 20min; Inorganic nano material is dispersed in organic solution by the mode also combined with ultrasonic vibration by mechanical stirring, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.Churned mechanically effect is that inorganic nano material is dispersed in organic solution, and makes the two mix; The effect of ultrasonic vibration inorganic nano material is activated and fragmentation by vibration, makes it to mix further with organic solution.
In above-mentioned either a program preferably, in described step one, the temperature of reaction of inorganic nano material and treatment agent A is 80-85 DEG C, and the reaction times is 20-30h.The present invention is bright through a large amount of confirmatory test, and in this temperature of reaction and reaction time range, the group in treatment agent A and the surface group of inorganic nano material can fully react.More preferably 82 DEG C, 24h.
In above-mentioned either a program preferably, in the reaction process of described inorganic nano material and treatment agent A, nitrogen protection is passed into.
In above-mentioned either a program preferably, in the reaction process of described inorganic nano material and treatment agent A, carry out mechanical stirring, make the two fully reaction, and reaction evenly, reaction contact area is large, and graft site is many.The rotating speed of agitator is 300rpm, Keep agitation in reaction process.
In above-mentioned either a program preferably, in described step 2, suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min, and with this understanding, suspension can abundant separating-purifying.
In above-mentioned either a program preferably, the drying temperature of described suspension is 75-85 DEG C, and time of drying is 10-20h.The present invention proves through lot of experiments, under this drying conditions, in suspension more than 95% hygroscopic water (moisture or other volatile liquid components) effusion of can vaporizing, to obtain the desciccate of regulation water capacity.Preferred drying conditions is 82 DEG C, 12h.
In above-mentioned either a program preferably, in described step 2, being separated desciccate is functionalized inorganic nano material, i.e. the inorganic nano material of aminopropyl-functional.
In above-mentioned either a program preferably, in described step 3, by the mode of mechanical stirring and/or ultrasonic vibration, separation desciccate is dispersed in salpeter solution.
In step 3, be dispersed in salpeter solution by churned mechanically mode by separation desciccate, use agitator, rotating speed is 300rpm, mechanical stirring 20min; Separation desciccate is dispersed in salpeter solution by the mode also by ultrasonic vibration, ultrasonic vibration 20min; Also the mode combined by mechanical stirring and ultrasonic vibration is dispersed in salpeter solution by being separated desciccate, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.
In above-mentioned either a program preferably, in described step 3, separation desciccate is dispersed in dilute nitric acid solution.Dilute nitric acid solution has satisfactory stability, and its concentration is 0.14mol/L.
In above-mentioned either a program preferably, in described step 4, upper strata suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min, and with this understanding, upper strata suspension can abundant separating-purifying.
In above-mentioned either a program preferably, the drying temperature of described upper strata suspension is 75-85 DEG C, and time of drying is 10-20h.The present invention proves through lot of experiments, under this drying conditions, in the suspension of upper strata more than 95% hygroscopic water (moisture or other volatile liquid components) effusion of can vaporizing, to obtain the desciccate of regulation water capacity.Preferred drying conditions is 80 DEG C, 15h.
In above-mentioned either a program preferably, in described step 4, the mass percent of the separation desciccate in diluting soln is 0.2-0.5%.In step 4, obtain being separated desciccate, measure that its solid load is inorganic nano material raw materials quality 1/3.
In above-mentioned either a program preferably, in described step 5, treatment agent B is tensio-active agent.
In above-mentioned either a program preferably, described tensio-active agent is any one in Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, polyacrylic acid, polyacrylate.Described polyacrylate is sodium polyacrylate or polyacrylic acid potassium.
In above-mentioned either a program preferably, in described step 5, treatment agent C is vinyl monomer.
In above-mentioned either a program preferably, described vinyl monomer is vinyl sulfonic acid or vinylsulfonate.Described vinylsulfonate is sodium vinyl sulfonate.
In above-mentioned either a program preferably, in described step 5, treatment agent D is redox initiator.
In above-mentioned either a program preferably, described redox initiator is any one in ceric ammonium nitrate, ammonium persulphate, Potassium Persulphate.
The present invention utilizes the redox initiation for the treatment of agent D, the graft site on activated particle shape inorganic nano material surface, makes the group generation copolyreaction in graft site and treatment agent C, obtains water-soluble inorganic nano material.In reaction process, use treatment agent B to disperse reactant, control grafting amount.
In above-mentioned either a program preferably, in described step 5, the temperature of reaction of diluting soln and treatment agent B, treatment agent C and treatment agent D is 75-85 DEG C, and the reaction times is 20-30h.The present invention proves through lot of experiments, in this Reaction conditions range, the redox initiation for the treatment of agent D, the dissemination for the treatment of agent B can give full play of, and make the abundant copolymerization of group in graft site and treatment agent C, the performance of the water-soluble inorganic nano material obtained is more stable.Preferred reaction conditions is 80 DEG C, 24h.
In above-mentioned either a program preferably, in the reaction process of described diluting soln and treatment agent B, treatment agent C and treatment agent D, nitrogen protection is passed into.
In above-mentioned either a program preferably, in the reaction process of described diluting soln and treatment agent B, treatment agent C and treatment agent D, carry out mechanical stirring, react fully and carry out.The rotating speed of agitator is 300rpm, Keep agitation in reaction process.
In above-mentioned either a program preferably, in described step 6, in reaction suspension, add sodium hydroxide solution neutralize, obtain neutralized reaction product.The amount adding sodium hydroxide is 3%.
In above-mentioned either a program preferably, in neutralized reaction product, add acetone soln, obtain separating out product.The present invention need add excessive acetone soln.
In above-mentioned either a program preferably, described precipitation product is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min, and with this understanding, separating out product can abundant separating-purifying.
In above-mentioned either a program preferably, the drying temperature of described precipitation product is 75-85 DEG C, and time of drying is 10-20h.The present invention proves through lot of experiments, under this drying conditions, separates out hygroscopic water (moisture or other volatile liquid components) effusion of can vaporizing of in product more than 95%, to obtain the desciccate of regulation water capacity.Preferred drying conditions is 80 DEG C, 15h.
In above-mentioned either a program preferably, in described step 6, final product is water-soluble inorganic nano material.
The preparation method of water-soluble inorganic nano material of the present invention, first utilize treatment agent A by the surface functionalization of particulate inorganic nano material, manufacture graft site, then graft site produces free radical under the initiation for the treatment of agent D, there is copolyreaction with solubility treatment agent C, generate final product water-soluble inorganic nano material.Carry out assay by testing experiment: infrared scan test result shows, treatment agent C is successfully grafted to the surface of inorganic nano material; Testing graininess result shows, the inorganic nano material of this preparation method synthesis has good solubility and stability in water.Preparation method of the present invention is easily understood, simple operation, result is accurate, cost is low, fundamentally can solve the scattering problem of inorganic nano material in water.
Accompanying drawing explanation
Fig. 1 is a preferred embodiment schema of the preparation method according to water-soluble inorganic nano material of the present invention;
Fig. 2 is the infrared scan test result schematic diagram embodiment illustrated in fig. 1 of the preparation method according to water-soluble inorganic nano material of the present invention;
Fig. 3 is the testing graininess result schematic diagram embodiment illustrated in fig. 1 of the preparation method according to water-soluble inorganic nano material of the present invention.
Embodiment
In order to further understand summary of the invention of the present invention, elaborate the present invention below in conjunction with specific embodiment.
Embodiment one:
As shown in Figure 1, a kind of preparation method of water-soluble inorganic nano material, it comprises the following steps according to sequencing:
Step one: inorganic nano material is dispersed in organic solution, and add treatment agent A, be obtained by reacting suspension;
Step 2: carried out by suspension being separated, dry, obtains being separated desciccate;
Step 3: separation desciccate is dispersed in salpeter solution, and collect upper strata suspension;
Step 4: carried out by upper strata suspension being separated, dry, obtains being separated desciccate, and measures its solid load, then adopt salpeter solution dilution, obtain diluting soln;
Step 5: add treatment agent B and treatment agent C reacts in diluting soln, then adds treatment agent D and reacts, obtain reaction suspension;
Step 6: carried out neutralizing and being separated by reaction suspension, then freeze-day with constant temperature, obtains final product.
In step one, particulate inorganic nano material is silicon-dioxide, and organic solution is ethanol, and treatment agent A is surface-modifying agent.Described surface-modifying agent is silane coupling agent, and described silane coupling agent is 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane.Inorganic nano material is dispersed in organic solution by the mode combined with ultrasonic vibration by mechanical stirring, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.The temperature of reaction of inorganic nano material and treatment agent A is 82 DEG C, and the reaction times is 24h, passes into nitrogen protection in reaction process, and carries out mechanical stirring, and the rotating speed of agitator is 300rpm.
In step 2, suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of suspension is 82 DEG C, and time of drying is 12h.Being separated desciccate is functionalized inorganic nano material, i.e. the inorganic nano material of aminopropyl-functional.
In step 3, the mode combined by mechanical stirring and ultrasonic vibration is dispersed in dilute nitric acid solution by being separated desciccate, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.The concentration of dust technology is 0.14mol/L.
In step 4, upper strata suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of upper strata suspension is 80 DEG C, and time of drying is 15h.Obtain being separated desciccate, measure that its solid load is inorganic nano material raw materials quality 1/3.The mass percent of the separation desciccate in diluting soln is 0.2%.
In step 5, treatment agent B is tensio-active agent, and described tensio-active agent is Sodium dodecylbenzene sulfonate; Treatment agent C is vinyl monomer, and described vinyl monomer is vinyl sulfonic acid; Treatment agent D is redox initiator, and described redox initiator is ceric ammonium nitrate.The temperature of reaction of diluting soln and treatment agent B, treatment agent C and treatment agent D is 80 DEG C, and the reaction times is 24h, passes into nitrogen protection in reaction process, and carries out mechanical stirring, and the rotating speed of agitator is 300rpm.
In step 6, the sodium hydroxide solution adding 3% in reaction suspension neutralizes, and obtains neutralized reaction product.In neutralized reaction product, add excessive propanone solution, obtain separating out product.Separate out product to be separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of separating out product is 80 DEG C, and time of drying is 15h.Final product is water-soluble inorganic nano material.
Carry out assay by testing experiment: as shown in Figure 2, infrared scan test result shows, treatment agent C is successfully grafted to the surface of inorganic nano material; As shown in Figure 3, testing graininess result shows, the inorganic nano material of this preparation method synthesis has good solubility and stability in water.The preparation method of the present embodiment is easily understood, simple operation, fundamentally can solve the scattering problem of inorganic nano material in water.
Embodiment two:
A preparation method for water-soluble inorganic nano material, its step, reaction mechanism, beneficial effect etc. are identical with embodiment one, unlike:
In step one, particulate inorganic nano material is titanium dioxide, and organic solution is toluene, and treatment agent A is 3-aminopropyl triethoxysilane.Inorganic nano material is dispersed in organic solution by the mode combined with ultrasonic vibration by mechanical stirring, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.The temperature of reaction of inorganic nano material and treatment agent A is 80 DEG C, and the reaction times is 30h.
In step 2, suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of suspension is 75 DEG C, and time of drying is 20h.Being separated desciccate is functionalized inorganic nano material.
In step 3, be dispersed in dilute nitric acid solution by churned mechanically mode by separation desciccate, the rotating speed of agitator is 300rpm, mechanical stirring 20min.The concentration of dust technology is 0.14mol/L.
In step 4, upper strata suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of upper strata suspension is 75 DEG C, and time of drying is 20h.The mass percent of the separation desciccate in diluting soln is 0.5%.
In step 5, treatment agent B is sodium lauryl sulphate; Treatment agent C is sodium vinyl sulfonate; Treatment agent D is ammonium persulphate.The temperature of reaction of diluting soln and treatment agent B, treatment agent C and treatment agent D is 75 DEG C, and the reaction times is 30h.
In step 6, the sodium hydroxide solution adding 3% in reaction suspension neutralizes, and obtains neutralized reaction product.In neutralized reaction product, add excessive propanone solution, obtain separating out product.Separate out product to be separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of separating out product is 75 DEG C, and time of drying is 20h.Final product is water-soluble inorganic nano material.
Embodiment three:
A preparation method for water-soluble inorganic nano material, its step, reaction mechanism, beneficial effect etc. are identical with embodiment one, unlike:
In step one, particulate inorganic nano material is zinc oxide, and organic solution is trichloromethane, and treatment agent A is 3-(methacryloxypropyl) propyl trimethoxy silicane.Inorganic nano material is dispersed in organic solution by the mode combined with ultrasonic vibration by mechanical stirring, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.The temperature of reaction of inorganic nano material and treatment agent A is 85 DEG C, and the reaction times is 20h.
In step 2, suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of suspension is 85 DEG C, and time of drying is 10h.Being separated desciccate is functionalized inorganic nano material.
In step 3, be dispersed in dilute nitric acid solution by the mode of ultrasonic vibration by separation desciccate, the rotating speed of agitator is 300rpm, mechanical stirring 20min.The concentration of dust technology is 0.14mol/L.
In step 4, upper strata suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of upper strata suspension is 85 DEG C, and time of drying is 10h.The mass percent of the separation desciccate in diluting soln is 0.3%.
In step 5, treatment agent B is polyacrylic acid; Treatment agent C is sodium vinyl sulfonate; Treatment agent D is Potassium Persulphate.The temperature of reaction of diluting soln and treatment agent B, treatment agent C and treatment agent D is 85 DEG C, and the reaction times is 20h.
In step 6, the sodium hydroxide solution adding 3% in reaction suspension neutralizes, and obtains neutralized reaction product.In neutralized reaction product, add excessive propanone solution, obtain separating out product.Separate out product to be separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of separating out product is 85 DEG C, and time of drying is 10h.Final product is water-soluble inorganic nano material.
Embodiment four:
A preparation method for water-soluble inorganic nano material, its step, reaction mechanism, beneficial effect etc. are identical with embodiment one, unlike:
In step one, particulate inorganic nano material is ferric oxide, and organic solution is methyl alcohol, and treatment agent A is 3-(methacryloxypropyl) propyl trimethoxy silicane.Be dispersed in organic solution by churned mechanically mode by inorganic nano material, the rotating speed of agitator is 300rpm, mechanical stirring 20min.The temperature of reaction of inorganic nano material and treatment agent A is 83 DEG C, and the reaction times is 22h.
In step 2, suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of suspension is 78 DEG C, and time of drying is 15h.Being separated desciccate is functionalized inorganic nano material.
In step 3, the mode combined by mechanical stirring and ultrasonic vibration is dispersed in dilute nitric acid solution by being separated desciccate, the ultrasonic vibration again of first mechanical stirring, and the rotating speed of agitator is 300rpm, mechanical stirring 20min, ultrasonic vibration 20min.The concentration of dust technology is 0.14mol/L.
In step 4, upper strata suspension is separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of upper strata suspension is 82 DEG C, and time of drying is 12h.The mass percent of the separation desciccate in diluting soln is 0.4%.
In step 5, treatment agent B is sodium polyacrylate; Treatment agent C is vinyl sulfonic acid; Treatment agent D is ceric ammonium nitrate.The temperature of reaction of diluting soln and treatment agent B, treatment agent C and treatment agent D is 82 DEG C, and the reaction times is 26h.
In step 6, the sodium hydroxide solution adding 3% in reaction suspension neutralizes, and obtains neutralized reaction product.In neutralized reaction product, add excessive propanone solution, obtain separating out product.Separate out product to be separated in centrifuges, in Vacuumdrier, carry out drying.The rotating speed of whizzer is 5000rpm, and centrifugation time is 30min.The drying temperature of separating out product is 82 DEG C, and time of drying is 12h.Final product is water-soluble inorganic nano material.
Those skilled in the art are understood that, the preparation method of water-soluble inorganic nano material of the present invention comprises the summary of the invention of the invention described above specification sheets and the arbitrary combination of embodiment part and each several part shown by accompanying drawing, as space is limited and not have each scheme of these combination formations to describe one by one for making specification sheets simple and clear.Within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. a preparation method for water-soluble inorganic nano material, it comprises the following steps according to sequencing:
Step one: inorganic nano material is dispersed in organic solution, and add treatment agent A, be obtained by reacting suspension;
Step 2: carried out by suspension being separated, dry, obtains being separated desciccate;
Step 3: separation desciccate is dispersed in salpeter solution, and collect upper strata suspension;
Step 4: carried out by upper strata suspension being separated, dry, obtains being separated desciccate, and measures its solid load, then adopt salpeter solution dilution, obtain diluting soln;
Step 5: add treatment agent B and treatment agent C reacts in diluting soln, then adds treatment agent D and reacts, obtain reaction suspension;
Step 6: carried out neutralizing and being separated by reaction suspension, then freeze-day with constant temperature, obtains final product.
2. the preparation method of water-soluble inorganic nano material as claimed in claim 1, it is characterized in that: in described step one, inorganic nano material is any one in silicon-dioxide, titanium dioxide, zinc oxide, ferric oxide, calcium carbonate.
3. the preparation method of water-soluble inorganic nano material as claimed in claim 1, it is characterized in that: in described step one, organic solution is any one in ethanol, toluene, methyl alcohol, ether, trichloromethane.
4. the preparation method of water-soluble inorganic nano material as claimed in claim 1, it is characterized in that: in described step one, treatment agent A is surface-modifying agent.
5. the preparation method of water-soluble inorganic nano material as claimed in claim 4, is characterized in that: described surface-modifying agent is silane coupling agent.
6. the preparation method of water-soluble inorganic nano material as claimed in claim 5, it is characterized in that: described silane coupling agent is 3-(2,3-epoxy third oxygen) propyl trimethoxy silicane, 3-aminopropyl triethoxysilane, 3-(methacryloxypropyl) any one in propyl trimethoxy silicane.
7. the preparation method of water-soluble inorganic nano material as claimed in claim 1, be is characterized in that: in described step one, is dispersed in organic solution by inorganic nano material by the mode of mechanical stirring and/or ultrasonic vibration.
8. the preparation method of water-soluble inorganic nano material as claimed in claim 1, it is characterized in that: in described step one, the temperature of reaction of inorganic nano material and treatment agent A is 80-85 DEG C, and the reaction times is 20-30h.
9. the preparation method of water-soluble inorganic nano material as claimed in claim 8, is characterized in that: in the reaction process of described inorganic nano material and treatment agent A, pass into nitrogen protection.
10. the preparation method of water-soluble inorganic nano material as claimed in claim 9, is characterized in that: in the reaction process of described inorganic nano material and treatment agent A, carries out mechanical stirring.
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