CN102352134B - 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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- CN102352134B CN102352134B CN201110241647.XA CN201110241647A CN102352134B CN 102352134 B CN102352134 B CN 102352134B CN 201110241647 A CN201110241647 A CN 201110241647A CN 102352134 B CN102352134 B CN 102352134B
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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 a large class nano material of Recent study exploitation.Red iron oxide is nontoxic, tasteless, has higher heatproof (over 300 ℃), resistance to marquis, special (5 grades) property of acid and alkali-resistance and ultraviolet ray is had to shielding; And the ferric oxide of nanostructure is due to the high tinting strength of nano effect (>=95%), high transparent, compared with features such as pure color pools, it is widely used in paint class coating, building material industry, plastics, food and medicine field etc.
The dispersiveness of nano-powder in medium determined the performance of its excellent properties, and solve the dispersed best bet of nanometer split, is exactly that the particle surface of nano-powder is modified and modification, 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 before reuniting, nanoparticle protect to reach the object of eliminating hard aggregation.
The method of nano powder surface modification is at present a lot, its ultimate principle is all to carry out corresponding physics and chemistry processing on the surface of nano-powder, parcel surface adsorption, surface are coated, surface grafting etc., and all finishinges or modification are all 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 conventional ionic has sodium carbonate, Sodium Tetraborate, sodium acrylate, ammonium polyacrylate etc.; Conventional steric hindrance type dispersion agent has polyvinyl butyral acetal, polyvinyl alcohol, polyacrylic acid etc.
Aspect the application at coating industry and preservation transportation, need to prepare water miscible nanometer ferric oxide powder.But, with conventional centrifugal method, be difficult to be isolated; And make its precipitation by regulating pH to reduce its Zeta potential, then the dry powder of preparing, can be difficult to redispersion because there is hard aggregation.
Summary of the invention
Primary and foremost purpose of the present invention is to overcome above-mentioned the deficiencies in the prior art, and the preparation method of the water-soluble powder of a kind of nanometer ferric oxide is provided.
Object of the present invention realizes by following technical proposals:
A preparation method for the water-soluble powder of nanometer ferric oxide, comprises the steps:
(1) by the synthetic method of hydro-thermal low temperature, prepare 100mL nanometer ferric oxide colloid;
(2) above-mentioned ferric oxide colloid is added to 10 ~ 20%(volumetric concentration) coating, then under magnetic stirring apparatus, stir 2h;
(3) in above-mentioned solution, add flocculation agent to stir 20mins, then centrifugal under 3000 ~ 4500 rev/min, then use 50ml solvent wash four times, finally dry 6h in vacuum drying oven, obtains the coated water-soluble powder of nanometer ferric oxide of coating.
Preferably, the synthetic method of the hydro-thermal low temperature that step (1) is described is that to take titanium dioxide industry by product green vitriol be raw material, and the nanometer ferric oxide that synthesizes is colloid-stabilised, good dispersity and narrow diameter distribution.
Preferably, the coating adding described in step (2) can be tensio-active agent sodium polyacrylate, polyoxyethylene glycol, polyvinyl alcohol etc.Concentration range 10 ~ 20% (volumetric concentration).
Preferably, the described flocculation agent of step (3) can be polyacrylamide, the aqueous solution of cationic starch etc. or ethanolic soln.Concentration range 0 ~ 50%(volumetric concentration).
The present invention compared with prior art tool has the following advantages and beneficial effect:
(1) solved the hard aggregation in nanometer ferric oxide colloid drying process;
(2) than pigment dyestuff, the weathering resistance that the product of gained has had and thermostability;
(3) uv absorption property of this water-soluble powder is stronger, and ruddiness is absorbed hardly, presents purer redness.
accompanying drawing explanation
Fig. 1 is the size distribution figure after the dry rear redispersion of embodiment 1 colloid mixture;
Fig. 2 is the transmission electron microscope picture of embodiment 1 coated rear nanometer ferric oxide.
Embodiment
Below in conjunction with specific embodiment, the present invention is more specifically described in detail, but embodiments of the present invention are not limited to this.
The water adopting is tap water, and nanometer ferric oxide colloid solid content is 1%.The detection means adopting is: transmission electron microscope TEM, dynamic light scattering DLS.
The preparation process of nanometer ferric oxide colloid is as follows: take green vitriol as raw material, be mixed with the solution that concentration is 0.1 ~ 0.5 mol/L, then this solution is carried out to oxide treatment and obtain Fe
2(SO
4)
3solution; By above-mentioned Fe
2(SO
4)
3solution is heated to boiling, and adding alkali to make pH value of solution is 7 ~ 10, and reaction generates Fe (OH)
3, then cooling; By cooled Fe (OH)
3carry out being distributed in 1000 ml water after centrifuge washing, make Fe (OH)
3concentration be 0.1 ~ 0.5 mol/L, be then heated to boiling, stir, the reaction times is 5 h, finally makes red nano iron trioxide water-soluble colloid.
embodiment 1
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.
From accompanying drawing one, can find out, the size distribution of coated rear gained powder redispersion is 118nm, and Zeta potential is-88mV.
From accompanying drawing two, can find out, nanometer ferric oxide disperses very even, there is no obvious reunion.
embodiment 2
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then add the polyvinyl alcohol of 10mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then add the sodium polyacrylate of 10mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
In this experiment, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 10mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then add the polyoxyethylene glycol of 10mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyvinyl alcohol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then add the polyvinyl alcohol of 20mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the sodium polyacrylate that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then add the sodium polyacrylate of 20mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide solution 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide solution of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 15mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch aqueous solution 20mL, stir 20mins, centrifugal under 4500 rev/min, use again the cationic starch solution washing four times of 50ml, last dry 6h in vacuum drying oven, the nanometer ferric oxide colloid after being coated 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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add polyacrylamide ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the polyacrylamide ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 15mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then the polyoxyethylene glycol that adds 20mL, then under magnetic stirring apparatus, stir 2h, add cationic starch ethanolic soln 20mL, stir 20mins, centrifugal under 4500 rev/min, with the cationic starch ethanolic soln of 50ml, wash four times more at every turn, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.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, first get the homemade nanometer ferric oxide colloid of 100ml, then add the polyoxyethylene glycol of 20mL, then under magnetic stirring apparatus, stir 2h, centrifugal under 4500 rev/min, finally in vacuum drying oven, be dried 6h, the nanometer ferric oxide colloid after being coated.The characteristic of this water-soluble powder and embodiment's 1 is basic identical, can be referring to embodiment 1.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (2)
1. a preparation method for the water-soluble powder of nanometer ferric oxide, is characterized in that, comprises the steps:
(1) prepare nanometer ferric oxide colloid: take green vitriol as raw material, be mixed with the solution that concentration is 0.1～0.5mol/L, then this solution is carried out to oxide treatment and obtain Fe
2(SO
4)
3solution; By above-mentioned Fe
2(SO
4)
3solution is heated to boiling, and adding alkali to make pH value of solution is 7～10, and reaction generates Fe (OH)
3, then cooling; By cooled Fe (OH)
3carry out being distributed in 1000ml water after centrifuge washing, make Fe (OH)
3concentration be 0.1～0.5mol/L, be then heated to boiling, stir, the reaction times is 5h, finally makes red nano iron trioxide water-soluble colloid;
(2) to the coating that adds colloid volume 10～20% in above-mentioned ferric oxide colloid, then under magnetic stirring apparatus, stir 2h, described coating is sodium polyacrylate, polyoxyethylene glycol or polyvinyl alcohol;
(3) in above-mentioned solution after coated, add flocculation agent, 50% of addition≤colloid volume of flocculation agent, stir 20mins, centrifugal under 3000～4500rev/min condition, with flocculation agent, wash again, finally dry in vacuum drying oven, obtain the coated water-soluble powder of nanometer ferric oxide of coating.
2. the preparation method of the water-soluble powder of nanometer ferric oxide according to claim 1, it is characterized in that the aqueous solution, the ethanolic soln of polyacrylamide, the ethanolic soln of the aqueous solution of cationic starch or cationic starch that the described flocculation agent of step (3) is polyacrylamide.
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