CN1434078A - Method for synthesizing nano red iron oxide - Google Patents
Method for synthesizing nano red iron oxide Download PDFInfo
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- CN1434078A CN1434078A CN 03111879 CN03111879A CN1434078A CN 1434078 A CN1434078 A CN 1434078A CN 03111879 CN03111879 CN 03111879 CN 03111879 A CN03111879 A CN 03111879A CN 1434078 A CN1434078 A CN 1434078A
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- iron oxide
- red iron
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Abstract
The method for synthesizing nano red iron oxide includes the following steps: adding soluble ferric salt solution in a reactor with stirring device, stirring-heating and pumping soluble alkaline substance into the reactor, raising pH value, mixing them and dispersing, filtering and washing to remove impurity, drying, roasting and pulverizing so as to obtain the nano red iron oxide product with small grain size, narrow distribution of particle size, good dispersion property and strong colour-covering power and tinctorial power.
Description
(1) technical field: the present invention relates to a kind of method of synthetic hematite, relate in particular to a kind of method of synthesis of nano red iron oxide.
(2) background technology: shortcoming can only be used in common industrial use to conventional oxidation iron oxide red product because particle diameter is big, the granularity issue is wide, bad dispersibility, tinting strength are weak etc., when it is used in the industry that high-grade paint, printing ink etc. have higher requirements to product granularity, dispersiveness, also must be through one or several grinding step, to improve its dispersiveness, so just make production process complexity, energy consumption height, can't guarantee its stability; And the purposes aspect of requirements at the higher level (0.5 μ m following) being arranged for pigment particles, conventional oxidation iron oxide red product can't use.Nanometer iron oxide red owing to adopt the nano material technology preparation, advantage is clearly arranged at aspects such as product granularity, dispersing property, color and lusters, be the top grade product in the red iron oxide, and nontoxic, can be used for industries such as medicine, food, high-grade paint, high-grade paint, printing ink.
The preparation method of red iron oxide in the past, two kinds of dry method and wet methods are arranged in industrial production: dry production is with ferrous sulfate or other ferrous salts process crystallisation by cooling, dehydrate and calcine and make, utilize the granularity of the product of this method production to be difficult to control, and color and luster is bad; Wet production is that with atmospheric oxidation, the generation nucleus constantly deposits ferric oxide and makes after adding the acid dissolving with the metal iron filings, and this method products obtained therefrom purity is low, the product color instability.And some present nanometer iron oxide red preparation methods often exist complex process, raw materials cost height, introduce shortcomings such as other impurity, nanometer iron oxide red preparation method mainly contains: sol-gel method, this method steps is loaded down with trivial details, and has introduced deleterious organic solvent; Solvent evaporated method, this method preparation cost height, energy utilization rate is low; Hydrolysis method, this method raw materials cost height.
(3) summary of the invention: the objective of the invention is to overcome the deficiency of above-mentioned prior art and provide a kind of step simple, workable, cost is low, nontoxic, be difficult for to introduce the method for the synthesis of nano red iron oxide of other impurity,, narrow particle size distribution little, good dispersity, color opacifying power and strong coloring force with the nanometer iron oxide red particle diameter of this method synthetic.
Purpose of the present invention can reach by following measure: a kind of method of synthesis of nano red iron oxide, it comprises the steps:
A, in the reactor of whipping appts is housed, add the solubility ferric salt solution, this solution is heated to 20-140 ℃;
B, having under the stirring condition, pump into solubility alkalescence material in the solubility ferric salt solution, the rising pH value makes it to generate the slurry that contains ferric oxide nanometer particle;
C, add an amount of sulfonate surfactant, the slurry that blending dispersion generated with relevant nature according to output;
D, will disperse the slurries filtration that is generated and wash to inclusion-free;
E, with above-mentioned material 50-150 ℃ of oven dry, 300-800 ℃ roasting 0.5-2.5 hour, pulverize and promptly to get nanometer iron oxide red product.
In order to further specify purpose of the present invention, the solubility ferric salt solution described in the above-mentioned steps a is a kind of metallic impurity ionic industrial effluent such as nickel, manganese, calcium, magnesium that contain.
In order to further specify purpose of the present invention, the solubility alkalescence material described in the above-mentioned steps b is a kind of in sodium hydroxide, yellow soda ash, the ammoniacal liquor.
In order to further specify purpose of the present invention, the concentration of above-mentioned solubility ferric salt solution is 0.1-5.0M, and the concentration of solubility alkalescence material is 0.1-5.0M, and the mole proportioning of solubility alkalescence material and solubility ferric salt solution is 1-5.
In order to further specify purpose of the present invention, the flow control when pumping into solubility alkalescence material among the above-mentioned steps b is 200-3500L/h, and the variation of the pH value in the lasting observing response still, become 1.5-9.5 up to pH value, and keep stablely, and stop to pump into alkaline matter, keep stirring.
In order to further specify purpose of the present invention, what use among the above-mentioned steps c is the tensio-active agent of 0.1-10%, and this tensio-active agent can be the octadecyl sodium sulfonate.
In order to further specify purpose of the present invention, adopt high-pressure filteration among the above-mentioned steps d, and wash to the inclusion-free ion with pure water and to exist.
The present invention can produce following positively effect compared with the prior art: the present invention adopts liquid-phase precipitation method synthesis of nano red iron oxide, it is precipitation from homogeneous solution in solution under the effect of crystal control agent by solubility trivalent iron salt and alkaline matter, all disperseed nanometer iron oxide red through washing and filtering, oven dry, roasting, this method steps is simple, workable, cost is low, and is nontoxic, is the nanometer iron oxide red method of ideal industrial production.
The liquid-phase precipitation method that is used for synthesizing nano-particle, generally be described to: in metal salt solution, add certain material, make it in solution, to react, long-pending long-pending when the concentration of precipitation particles above sedimentary equilibrium concentration, will generate throw out lentamente, throw out is through repetitive scrubbing, the impurity that removal is sneaked into, dehydration becomes precursor then, and presoma passes through last handling process again, can obtain needed uniform particles, nano material that purity is high.
In general, size of particles and size issue, crystallization parameters, crystalline structure and dispersity can be controlled by reaction kinetics.The factor that influences speed of reaction comprises reaction solution concentration, temperature of reaction, pH value, and reactant is added to the sequential scheduling in the solution, the foreign ion that removes in the reaction is to realize in different pH value deposit by different ions, therefore must be controlled the homogeneity and the metering property of chemistry.The methods such as spraying drying, lyophilize that utilization changes presoma into powder can be avoided being separated and improving the homogeneity of molecular level in the liquid deposition, but because its cost height, energy consumption is big, must seek a kind of more suitably mode and be separated.
Red iron oxide has good color opacifying power and tinting strength, and heat-resisting, anti-solvent, acid and alkali-resistance, nontoxic, antirust, be that first-selected product in the mineral dye can be used for coating, rubber, printing ink, plastics, cement, also can be used for aspects such as makeup, food, tape, tamanori, purposes is very extensive.Nanometer iron oxide red owing to adopt the nano material technology preparation, the fine quality that not only has red iron oxide, and clearly advantage is arranged at aspects such as product granularity, dispersing property, color and lusters, be the top grade product in the red iron oxide, and nontoxic, can be used for industries such as medicine, food.Because particle diameter is tiny, nanometer iron oxide red can shielding ultraviolet rays; The surface is big, can its ageing resistance and intensity be significantly improved in the very fast formation network structure of coating drying process; Also can improve silicon rubber and other kind rubber intensity, elasticity and wear resistance.
The invention provides a kind of method of synthesis of nano red iron oxide---liquid-phase precipitation method, utilize this method synthetic is nanometer iron oxide red to have the following advantages:
(1) the little and narrowly distributing of granularity: the granularity of product is 80-110nm, and about median size 90nm, particle is tiny, and is thinner more than 50 times than common red iron oxide.
(2) strong coloring force: in pigment coloration, the more little tinting strength of granularity is strong more, and its tinting strength improves a lot.
(3) the stably dispersing performance is good: because this method is handled the dispersiveness of product in process of production, guarantee that particle just keeps good dispersion state period beginning formation, and can keep this state, adding special hydrophilic and oleophylic performance handles, make product keep good dispersiveness in water or in the organic solvent, and stable existence.
(4) bright in colour and pure: the product pellet granularity is distributed in the minimum scope, its reflection and absorption light wave narrow range, and the purity height, bright in colour and pure, do not have variegated.
(5) oil number is moderate: nanometer iron oxide red with this method synthetic, oil number is 20g/100g, is highly suitable for high-quality coating.
Utilize the nanometer iron oxide red product of this method synthetic to adopt the transmissioning electric mirror determining product cut size, adopt X-ray diffraction to measure crystal formation, adopt the analyses product purity, adopt appearance method to measure color, adopt the refractive index method to measure opacifying power, adopt gravimetric determination density, obtain following result:
Fe
2O
3Content: 99.0%
Crystal formation: α-Fe
2O
3
Size-grade distribution: 80-100nm
Median size: 90nm
Outward appearance: scarlet powder
Density: 0.2g/cm
3
Opacifying power: 3g/m
2
Relative color strength: 200-300% (common relatively red iron oxide national standard sample)
Oil number: 20g/100g
105 ℃ of volatile matters: " 0.3%
Aqeous suspension pH value: 6.0-8.0
Chromic acid: feminine gender
(4) embodiment: following the specific embodiment of the present invention is elaborated:
Embodiment 1: whipping appts is being housed, have in the reactor of chuck, the solubility ferric salt solution that adds 500 liters of 0.5mol/L, this solubility ferric salt solution is a kind of nickel that contains that the shadow mask industry produces, manganese, calcium, metallic impurity ionic industrial effluent such as magnesium, this solution is heated to 20 ℃ under stirring condition, pump into the 1.5mol/L ammonia soln, flow is 200L/h, continue the variation of the pH value in the observing response still, become 1.5 up to pH value, stop to pump into ammonia soln, keep stirring, add the tensio-active agent octadecyl sodium sulfonate of 0.1% relevant nature according to output, carry out blending dispersion, then back synthetic slurry is filtered by frame, and wash to the existence of inclusion-free ion, 50 ℃ of oven dry then with pure water, 300 ℃ of roastings 0.5 hour are pulverized and are promptly got nanometer iron oxide red product.
Embodiment 2: whipping appts is being housed, have in the reactor of chuck, the solubility ferric salt solution that adds 500 liters of 1.0mol/L, this solubility ferric salt solution is a kind of nickel that contains that the shadow mask industry produces, manganese, calcium, metallic impurity ionic industrial effluent such as magnesium, this solution is heated to 80 ℃ under stirring condition, pump into the 3.5mol/L sodium hydroxide solution, flow is 1600L/h, continue the variation of the pH value in the observing response still, become 5.5 up to pH value, stop to pump into sodium hydroxide solution, keep stirring, the tensio-active agent octadecyl sodium sulfonate that adds 4.5% relevant nature according to output, carry out blending dispersion, then back synthetic slurry is filtered by frame, and wash to the existence of inclusion-free ion, 100 ℃ of oven dry then with pure water, 500 ℃ of roastings 1.5 hours are pulverized and are promptly got nanometer iron oxide red product.
Embodiment 3: whipping appts is being housed, have in the reactor of chuck, the solubility ferric salt solution that adds 500 liters of 2.0mol/L, this solubility ferric salt solution is a kind of nickel that contains that the shadow mask industry produces, manganese, calcium, metallic impurity ionic industrial effluent such as magnesium, this solution is heated to 140 ℃ under stirring condition, pump into the 5.0mol/L sodium carbonate solution, flow is 3500L/h, continue the variation of the pH value in the observing response still, become 9.5 up to pH value, stop to pump into sodium carbonate solution, keep stirring, add the sulfonate surfactant of 10% relevant nature according to output, carry out blending dispersion, then back synthetic slurry is filtered by frame, and wash to the existence of inclusion-free ion, 150 ℃ of oven dry then with pure water, 800 ℃ of roastings 2.5 hours are pulverized and are promptly got nanometer iron oxide red product.
Claims (8)
1, a kind of method of synthesis of nano red iron oxide, it comprises the steps:
A, in the reactor of whipping appts is housed, add the solubility ferric salt solution, this solution is heated to 20-140 ℃;
B, having under the stirring condition, pump into solubility alkalescence material in the solubility ferric salt solution, the rising pH value makes it to generate the slurry that contains ferric oxide nanometer particle;
C, add an amount of sulfonate surfactant, the slurry that blending dispersion generated with relevant nature according to output;
D, will disperse the slurries filtration that is generated and wash to inclusion-free;
E, with above-mentioned material 50-150 ℃ of oven dry, 300-800 ℃ roasting 0.5-2.5 hour, pulverize and promptly to get nanometer iron oxide red product.
2, the method for a kind of synthesis of nano red iron oxide according to claim 1 is characterized in that the solubility ferric salt solution described in the described step a is a kind of metallic impurity ionic industrial effluent such as nickel, manganese, calcium, magnesium that contain.
3, the method for a kind of synthesis of nano red iron oxide according to claim 1 is characterized in that the solubility alkalescence material described in the described step b is a kind of in sodium hydroxide, yellow soda ash, the ammoniacal liquor.
4, according to the method for claim 1 or 2 or 3 described a kind of synthesis of nano red iron oxides, the concentration that it is characterized in that described solubility ferric salt solution is 0.1-5.0M, the concentration of solubility alkalescence material is 0.1-5.0M, and the mole proportioning of solubility alkalescence material and solubility ferric salt solution is 1-5.
5, the method for a kind of synthesis of nano red iron oxide according to claim 1, flow control when it is characterized in that pumping into solubility alkalescence material among the described step b is 200-3500L/h, and the variation of the pH value in the lasting observing response still, become 1.5-9.5 up to pH value, and keep stable, stop to pump into alkaline matter, keep stirring.
6, the method for a kind of synthesis of nano red iron oxide according to claim 1, what it is characterized in that using among the described step c is the tensio-active agent of 0.1-10%.
7,, it is characterized in that described tensio-active agent is the octadecyl sodium sulfonate according to the method for claim 1 or 6 described a kind of synthesis of nano red iron oxides.
8, the method for a kind of synthesis of nano red iron oxide according to claim 1 is characterized in that adopting high-pressure filteration in the described steps d, and washs to the inclusion-free ion with pure water and to exist.
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| CN 03111879 CN1434078A (en) | 2003-02-21 | 2003-02-21 | Method for synthesizing nano red iron oxide |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696208B (en) * | 2004-05-14 | 2010-09-01 | 朗盛德国有限责任公司 | Pure-coloured, readily dispersible iron oxide red pigments with high grinding stability |
| CN112047384A (en) * | 2020-08-13 | 2020-12-08 | 桂林理工大学 | Method for preparing nano iron oxide negative electrode material for lithium ion battery by using tin ore tailing sulfuric acid leaching solution |
| CN114854278A (en) * | 2022-04-25 | 2022-08-05 | 铜陵同达兴实业有限责任公司 | Preparation process of nano iron oxide coating dispersion system |
| CN116768279A (en) * | 2022-06-02 | 2023-09-19 | 恒升元(深圳)新材料科技有限公司 | Iron oxide red powder and preparation method thereof |
-
2003
- 2003-02-21 CN CN 03111879 patent/CN1434078A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1696208B (en) * | 2004-05-14 | 2010-09-01 | 朗盛德国有限责任公司 | Pure-coloured, readily dispersible iron oxide red pigments with high grinding stability |
| CN112047384A (en) * | 2020-08-13 | 2020-12-08 | 桂林理工大学 | Method for preparing nano iron oxide negative electrode material for lithium ion battery by using tin ore tailing sulfuric acid leaching solution |
| CN114854278A (en) * | 2022-04-25 | 2022-08-05 | 铜陵同达兴实业有限责任公司 | Preparation process of nano iron oxide coating dispersion system |
| CN116768279A (en) * | 2022-06-02 | 2023-09-19 | 恒升元(深圳)新材料科技有限公司 | Iron oxide red powder and preparation method thereof |
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