CN102352134A - Method for preparing nanometer ferric oxide water-soluble powder - Google Patents
Method for preparing nanometer ferric oxide water-soluble powder Download PDFInfo
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- CN102352134A CN102352134A CN201110241647XA CN201110241647A CN102352134A CN 102352134 A CN102352134 A CN 102352134A CN 201110241647X A CN201110241647X A CN 201110241647XA CN 201110241647 A CN201110241647 A CN 201110241647A CN 102352134 A CN102352134 A CN 102352134A
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Abstract
The invention discloses a method for preparing nanometer ferric oxide water-soluble powder, which comprises the following steps of: (1) preparing 100 ml of nanometer ferric oxide colloid by using the low temperature hydrothermal synthesis method; (2) adding a coating agent into the ferric oxide colloid, and stirring the coating agent and the ferric oxide colloid through a magnetic stirring apparatus; and (3) adding a flocculating agent into the solution, stirring the solution for 29 min at 4500 rev/min, washing the solution for four times by using 50 ml of flocculating agent, and finally drying the product in a vacuum drying oven for 6 h to obtain the nanometer ferric oxide water-soluble powder coated by the coating agent. The nanometer ferric oxide powder prepared by the method has strong ultraviolet absorption property, hardly absorbs red light and forms pure red color. The nanometer ferric oxide powder can be applied to the industries of water-based paints or water-based ink and the water-soluble colloid is stable.
Description
Technical field
The present invention relates to the preparation method of the water-soluble powder of a kind of nanometer ferric oxide, belong to coating and pigment production technical field.
Background technology
Nanometer iron oxide red (α-Fe
2O
3) be one big type of nano material of Recent study exploitation.Red iron oxide is nontoxic, tasteless, has special (5 grades) property of higher heatproof (above 300 ℃), anti-marquis, acid and alkali-resistance and ultraviolet ray is had shielding; And the ferric oxide of nanostructure because the high tinting strength of nano effect (>=95%), high transparent, than characteristics such as pure color pools, it is widely used in a lacquer type coating, building material industry, plastics, food and medicine field or the like.
The dispersiveness of nano-powder in medium determined the performance of its excellent properties, is exactly that the particle surface of nano-powder is modified and modification and solve the dispersed best bet of nanometer split, can improve its dispersiveness in medium on the one hand; Also can improve its use properties on the other hand, for example: catalytic, wettability and electronics performance etc.Thereby also can, nanoparticle protect the purpose of eliminating hard aggregation to reach before reuniting.
The method of nano powder surface modification at present is a lot; Its ultimate principle all is to carry out corresponding physics and chemical treatment on the surface of nano-powder; Parcel surface adsorption, surface coating, surface grafting etc., all finishinges or modification all are to carry out on the surface of nanoparticle.The dispersion agent that is commonly used to modification can be divided into: ionic dispersant and steric hindrance type dispersion agent.The dispersion agent of ionic commonly used has yellow soda ash, Sodium Tetraborate, sodium acrylate, ammonium polyacrylate etc.; Steric hindrance type dispersion agent commonly used has polyvinyl butyral acetal, polyvinyl alcohol, polyacrylic acid etc.
For the application of coating industry and preserve transportation aspect, need prepare water miscible nanometer ferric oxide powder.But, be difficult to its separation with conventional centrifugal method; And making its deposition through regulating its Zeta potential of pH reduction, drying is prepared powder then, can be difficult to redispersion because of hard aggregation takes place.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome the deficiency of above-mentioned prior art, and the preparation method of the water-soluble powder of a kind of nanometer ferric oxide is provided.
The object of the invention is realized through following technical proposals:
The preparation method of the water-soluble powder of a kind of nanometer ferric oxide comprises the steps:
(1) prepares 100mL nanometer ferric oxide colloid with the cryogenic synthesis method of hydro-thermal;
(2) with the coating of above-mentioned ferric oxide colloid adding 10 ~ 20% (volumetric concentrations), under magnetic stirring apparatus, stir 2h then;
(3) in above-mentioned solution, add flocculation agent and stir 20mins, centrifugal under 3000 ~ 4500 rev/min then, use the 50ml solvent wash again four times, dry 6h in vacuum drying oven obtains the water-soluble powder of nanometer ferric oxide that coating coats at last.
Preferably, the cryogenic synthesis method of the described hydro-thermal of step (1) is to be raw material with titanium dioxide industry by product green vitriol, and the nanometer ferric oxide that synthesizes is colloid-stabilised, good dispersity and narrow diameter distribution.
Preferably, the coating of the said adding of step (2) can be the tensio-active agent sodium polyacrylate, polyoxyethylene glycol, polyvinyl alcohol etc.Concentration range 10 ~ 20% (volumetric concentration).
Preferably, the said flocculation agent of step (3) can be a polyacrylamide, the aqueous solution of cationic starch etc. or ethanolic soln.Concentration range 0 ~ 50% (volumetric concentration).
The present invention compared with prior art has following advantage and beneficial effect:
(1) solved hard aggregation in the nanometer ferric oxide colloid drying process;
(2) than pigment dyestuff, the product of gained has good weathering resistance and thermostability;
(3) uv absorption property of this water-soluble powder is stronger, and ruddiness is absorbed hardly, presents purer redness.
Description of drawings
Fig. 1 is the size distribution figure behind the redispersion after the embodiment 1 colloid mixture drying;
Fig. 2 is the transmission electron microscope picture that embodiment 1 coats back nanometer ferric oxide.
Embodiment
Below in conjunction with specific embodiment the present invention is done further concrete detailed description the in detail, but embodiment of the present invention is not limited thereto.
The water that is adopted is tap water, and nanometer ferric oxide colloid solid content is 1%.The detection means that adopts is: transmission electron microscope TEM, dynamic light scattering DLS.
Nanometer ferric oxide colloidal preparation process is following: with the green vitriol is raw material, is mixed with the solution that concentration is 0.1 ~ 0.5 mol/L, then this solution is carried out oxide treatment and obtains Fe
2(SO
4)
3Solution; With above-mentioned Fe
2(SO
4)
3Solution is heated to boiling, and it is 7 ~ 10 that adding alkali makes pH value of solution, and reaction generates Fe (OH)
3, cooling then; With cooled Fe (OH)
3Carry out being distributed in the 1000 ml water behind the centrifuge washing, make Fe (OH)
3Concentration be 0.1 ~ 0.5 mol/L, be heated to boiling then, stir, the reaction times is 5 h, finally makes the water-soluble colloid of red nano ferric oxide.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.
Can find out that from accompanying drawing one size distribution that coats back gained powder redispersion is 118nm, Zeta potential is-88mV.
Can find out that from accompanying drawing two the nanometer ferric oxide disperses very even, does not have obvious reunion.
Embodiment 2
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 3
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 4
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 6
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 7
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 8
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 9
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the polyvinyl alcohol of 10mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 11
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 12
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 13
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 14
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 16
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 17
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 18
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the sodium polyacrylate of 10mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 19
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 21
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 22
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 23
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 24
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 26
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 10mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 27
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the polyoxyethylene glycol of 10mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 28
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 29
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 30
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 31
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 32
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 33
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 34
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 35
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyvinyl alcohol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
?
Embodiment 36
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the polyvinyl alcohol of 20mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 37
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 38
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 39
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 40
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 41
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 42
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 43
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 44
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The sodium polyacrylate that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 45
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the sodium polyacrylate of 20mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 46
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 47
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide solution of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 48
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 15mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 49
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch aqueous solution 20mL, stir 20mins; Centrifugal under 4500 rev/min; Use the cationic starch solution washing four times of 50ml again, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating at every turn.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 50
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 51
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add polyacrylamide ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the polyacrylamide ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 52
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 15mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1
Embodiment 53
In this experiment; At first get the homemade nanometer ferric oxide colloid of 100ml; The polyoxyethylene glycol that adds 20mL then; Under magnetic stirring apparatus, stir 2h then, add cationic starch ethanolic soln 20mL, stir 20mins; Centrifugal under 4500 rev/min; Again at every turn with the cationic starch ethanolic soln of 50ml washing four times, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Embodiment 54
In this experiment, at first get the homemade nanometer ferric oxide colloid of 100ml, add the polyoxyethylene glycol of 20mL then; Under magnetic stirring apparatus, stir 2h then; Centrifugal under 4500 rev/min, dry 6h in vacuum drying oven at last, the nanometer ferric oxide colloid after obtaining coating.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. the preparation method of the water-soluble powder of nanometer ferric oxide is characterized in that, comprises the steps:
(1) preparation nanometer ferric oxide colloid;
(2) coating of adding colloid volume 10 ~ 20% in above-mentioned ferric oxide colloid stirs 2h then under magnetic stirring apparatus;
(3) flocculation agent of adding colloid volume 0 ~ 50% in the solution after above-mentioned coating; When the addition of flocculation agent is non-vanishing; Stir 20mins; Centrifugal under 3000 ~ 4500 rev/min conditions; Wash with flocculation agent again; Dry in vacuum drying oven at last, obtain the water-soluble powder of nanometer ferric oxide that coating coats; When the addition of flocculation agent is zero, centrifugal under 3000 ~ 4500 rev/min conditions, dry in vacuum drying oven at last, obtain the water-soluble powder of nanometer ferric oxide that coating coats.
2. according to the preparation method of the water-soluble powder of the said nanometer ferric oxide of claim 1, it is characterized in that the said nanometer ferric oxide of step (1) colloidal preparation method adopts the cryogenic synthesis method of hydro-thermal.
3. according to the preparation method of the water-soluble powder of the said nanometer ferric oxide of claim 1, it is characterized in that the said coating of step (2) is a tensio-active agent.
4. according to the preparation method of the water-soluble powder of the said nanometer ferric oxide of claim 3, it is characterized in that said tensio-active agent is sodium polyacrylate, polyoxyethylene glycol or polyvinyl alcohol.
5. according to the preparation method of the water-soluble powder of the said nanometer ferric oxide of claim 1, it is characterized in that the said flocculation agent of step (3) is the aqueous solution or the ethanolic soln of polyacrylamide or cationic starch.
6. the water-soluble powder of nanometer ferric oxide is characterized in that, this water-soluble powder is by any said method preparation of claim 1 ~ 5.
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