CN105623316A - Iron-red-series low-gloss lamellar pigment and preparation method thereof - Google Patents
Iron-red-series low-gloss lamellar pigment and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an iron-red-series low-gloss lamellar pigment and a preparation method thereof, relating to the field of pearlescent pigments. Mica with the particle size of 0.15-5 mu m is used as a substrate, and iron oxide is coated on the substrate to form an iron oxide coating, wherein the coating is formed by carrying out hydrolysis in a ferric iron salt solution. The method comprises the following steps: mixing mica powder and water to form a suspension, adding a crystal grain regulator into the suspension, regulating the pH value, adding the ferric iron salt solution while stirring to perform hydrolysis coating, keeping the pH value of the suspension stable, continuing dropwisely adding the ferric iron salt solution until the a slightly purple red color phase is obtained, stirring, regulating the pH value of the solution, carrying out vacuum filtration, drying, calcining and cooling. Compared with the prior art, the prepared product is approximately spherical, is delicate and smooth, is very skin-friendly, has the advantages of high covering power and low gloss, has the matt effect, and can be widely used in cosmetics, leather, plastics, inks and paints.
Description
Technical field
The present invention relates to pearlescent pigment technical field, especially a kind of iron oxide red series low gloss sheet layer pigment and preparation method thereof.
Background technology
Pearlescent pigment can reproduce graceful gloss and the color that nature Margarita, shell, metal, swimming fish and butterfly have, it relies on and the refraction of light, reflection, projection is created form and aspect and gloss, can give plastic, leather etc. with deep stereovision and special reflecting feel. Why pearlescent pigment has the imparting pearlescent gloss of goods, being because it is with natural muscovite or artificial mica synthesis or glass flake for core, special chemical technology is adopted to form powder pigment at one or more layers metal-oxide of core Surface coating, so that it has a kind of structurally very much like with natural peral sandwich body of plane, complex light can be resolved into various monochromatic light by it as prism, and various different interference colours are formed by interference of light, it is shown that and the pearly luster of beauty and metallic luster.
The main Types of pearlescent pigment has: Muscovitum coating pearlescent pigment, natural indestructible pearl delustering pigment and bismuth oxychloride crystallization pearlescent pigment. Their the base material overwhelming majority adopts Muscovitum, Muscovitum high resilience, flexible, wear resistence and wearability are good, high temperature insulation, it is insoluble in acid-base solution, stable chemical nature, epigranular, so, Muscovitum is a kind of well pearlescent pigment base substrate, and a lot of oxides can be deposited on its surface and embody the pearl effect of uniqueness.
At present, deposit at mica surface and prepare the oxide of pearlescent pigment and have: TiO2, ZrO2, SnO2, Cr2O3, Fe2O3, SiO2 etc. And the invention of current ferrum series pearlescent pigment product and technology for producing are quite ripe at home and abroad, Patents technology also has a lot, and it is widely used in industry-by-industry; Its particle diameter of Muscovitum base material that current ferrum series pearlescent pigment depends on is all more than 10 ��m. And in little particle size range, particularly at D50The trickle particle diameter of=1 ~ 5 ��m rarely has research, firstly, because particle diameter is only small, the pigment productivity doing little particle diameter is low, and energy consumption is high, and the production cycle is long, and difficulty is big, vulnerable to pollution; Secondly, the pigment of Unit Weight, particle diameter is more little, the quantity of particle is more many, then seamed edge quantity is more many, then glossiness is more low, when pearlescent pigment particle diameter is less than 0.15-5 micron, prepared pearlescent pigment glossiness is very low, and its glossiness is in dumb light scope, so pearlescent pigment produces and research worker thinks the necessity do not studied; Again, because substrate used is flake, mainly phyllosilicate class material, by high radius-thickness ratio (diameter/thickness) substrate that wet grinding obtains, its thickness is substantially at 100 ran, namely close to or 1-dimention nano yardstick, it is well known that nano material is due to the quantum effect of superhigh specific surface area, when drying and calcine, being very easy to reunite and formed and have relatively high bond strength, irregular agglomerated particle, so that it loses required laminar pigment performance.
Summary of the invention
One of the technical problem to be solved is to provide a kind of matte effect with uniqueness and great exquisiteness is soft and smooth and the iron oxide red series low gloss sheet layer pigment of pro-skin.
In order to solve the problems referred to above, the technical solution adopted in the present invention is: using particle diameter for the Muscovitum of 0.15��5 ��m as base material, being coated with ferrum oxide on this base material, form iron oxide coated layer, this iron oxide coated layer is hydrolyzed cladding in solubility ferric salt solution.
In technique scheme, technical scheme is it may also is that described ferric salt solution is one or both in iron sulfate, ferric chloride, ferric nitrate more specifically.
Further: the clad ratio of described iron oxide coated layer is 60%��95%.
Further: described Muscovitum is natural mica or synthetic mica.
The preparation method that the two of the technical problem to be solved are to provide the iron oxide red series low gloss sheet layer pigment that a kind of preparation technology is simple, relevance grade is high.
In order to solve the problems referred to above, the technical solution adopted in the present invention is:
Including following making step:
A, take the Muscovitum that particle diameter is 0.15��5 ��m and mix with deionized water and be stirred, stir 30��60 minutes, form the suspension that solid-liquid weight ratio is 1:10��45;
B, put into after crystal grain regulator to described suspension under agitation, gained suspension agitating heating in same rotating speed is warming up to 65��80 DEG C, after continuing stirring 15��40 minutes, regulates the pH value of described suspension, pH value is regulated to 1.5��3.4;
After C, step B complete, being further continued for stirring 15��40 minutes, then in described suspension, a speed dropping ferric salt solution of dripping with 10��25ml/h is hydrolyzed cladding, and instillation alkaline solution maintains stablizing of described suspension pH value simultaneously;
D, by step C drip speed dropping ferric salt solution 0.5��2 hour after, dripping speed and rotating speed raising, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, constant temperature stirs 30��60 minutes again, regulate the pH value of this suspension, be subsequently adding anti-agglomeration agent, continue stirring 30��60min; ;
E, the suspension that D step is formed carry out sucking filtration, drying, calcining, cooling, obtain iron oxide red series low gloss sheet layer pigment.
Further: in step A, described mixing speed is 480r/min; In step C, described ferric salt solution concentration is 60g/l, and described alkaline solution is ammonia spirit, sodium hydroxide solution or carbonate solution, and the concentration of this alkaline solution is 10%; In D step, dripping speed and be increased to 30ml/h, mixing speed is increased to 500 turns/min; In E step, after suspension filtering and washing, being dried by filter cake, described drying temperature is 90��120 DEG C, then calcines, and described calcining heat is 580��800 DEG C.
Further: the 0.001-2% that consumption is described mica powder dry weight of the described anti-agglomeration agent of addition; Described anti-agglomeration agent is soluble inorganic salt and/or dissolved organic matter, and described soluble inorganic salt is phosphate or aluminum soluble salt; Described dissolved organic matter is cationic surface active substances or anion active material.
Further: described phosphate is sodium hexameta phosphate, sodium pyrophosphate or sodium phosphate; Described aluminum soluble salt is aluminum chloride, aluminum nitrate or sodium aluminate; Described cationic surface active substances is chitosan, cation CMC sodium, the CPAM of small-molecular-weight and other water-soluble cationic compound; Described anion active material is stearic acid, oleic acid, dodecyl sodium sulfate and other water dissolvable anionic compound.
Crystal grain regulator of the present invention is used to suppress or promote that metal-oxide hydrolysis regulates oxide particle size, it mainly has organic anion compound, non-ionic compound, cationic compound, the inorganic compound such as chlorate of calcium, magnesium, aluminum, zinc etc., nitrate, carbonate, oxide, hydroxide.
Owing to have employed technique scheme, the present invention compared with prior art has the advantages that
1, the iron oxide red series low gloss sheet layer pigment that the present invention obtains, it is that the Muscovitum of 0.15��5 ��m is as base material owing to being employing particle diameter, coated iron oxide on the substrate, form the special iron oxide red series low gloss sheet layer pigment of a kind of iron oxide red inclined purple phase, owing to pigment particle size is only small, drying with calcination process can form reunion and lose pigment performance, therefore, the hydrolytic process of preparation process adds anti-agglomeration agent and prevents knot grain, the clad ratio of this pigment iron oxides has reached 60%��95%, its product approximate spheres shape, great exquisiteness is soft and smooth, pro-skin effect is fairly obvious, and high covering power, Huang Hong can be prepared, red, the iron oxide red series of products of purplish red various form and aspect, glossiness is low, matte effect is notable.
2, this method preparation technology is simple, and relevance grade is high, adds crystalline controlling agent, the effective size controlling particle, have certain transparency before hydrolysis; Pigment anti-agglomeration agent is added so that the pearlescent pigment particles after cladding is sheet, not easily ties grain, thus having bigger specific surface area, has unglazed or matte effect after hydrolysis.
3, ammonia spirit is used to maintain stablizing of suspension pH value, ammonium chloride is generated after ammonia hydrolysis, owing to pigment particle size is too little, during washing desalination, not easily elimination is clean, it is necessary to the elimination when calcining, again owing to ammonium chloride in a small amount can be decomposed into hydrogen chloride and ammonia between 340-400 degree, so that finished pigment not saliferous, be conducive to application.
Accompanying drawing explanation
Fig. 1 is the surface of pigments TiO that the embodiment of the present invention 1 prepares2The SEM figure of diameter characterization.
Fig. 2 is the surface of pigments TiO that the embodiment of the present invention 2 prepares2The SEM figure of diameter characterization.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and following example are used for further illustrating the present invention, but are not restricted to the present invention:
Embodiment 1:
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take D50=2.17 ��m trickle particle diameter natural mica dried bean noodles weight 22g, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 480r/min, form suspension, add crystal grain regulator Polyethylene Glycol 0.1g, stir 15��40min;
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.2;
After C, step B complete, it is further continued for stirring 30 minutes, then dripping, with the speed of 20ml/h, the liquor ferri trichloridi that concentration is 60g/l in suspension to be hydrolyzed cladding, instillation concentration is that the ammonia spirit of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping liquor ferri trichloridi 1 hour after, liquor ferri trichloridi is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, adds dodecyl sodium sulfate 0.20g, continue stirring 30 minutes after sucking filtration, at 120 DEG C dry;
E, 580 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Embodiment 2
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take D50=3.21 ��m trickle particle diameter natural mica dried bean noodles weight 22g, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 480r/min, form suspension, add crystal grain regulator Polyethylene Glycol 0.1g, stir 15��40min.
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.1;
After C, step B complete, it is stirred for 30 minutes, then dripping, with the speed of 20ml/h, the liquor ferri trichloridi that concentration is 60g/l in suspension to be hydrolyzed cladding, instillation concentration is that the ammonia spirit of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping liquor ferri trichloridi 1 hour after, liquor ferri trichloridi is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, adds dodecyl sodium sulfate 0.20g, continue stirring 30 minutes after sucking filtration, at 120 DEG C dry;
E, 760 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Embodiment 3
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take the synthetic mica dry weight 22g of particle diameter D50=1.51 ��m, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 480r/min, form suspension, add crystal grain regulator CaCl20.5g, stir 15��40min;
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.2;
After C, step B complete, it is further continued for stirring 30 minutes, then dripping, with the speed of 20ml/h, the ferrum sulfuricum oxydatum solutum that concentration is 0.8mol/l in suspension to be hydrolyzed cladding, instillation concentration is that the sodium hydroxide solution of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping ferrum sulfuricum oxydatum solutum 1 hour after, ferrum sulfuricum oxydatum solutum is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, adds chitosan 0.2g, continue stirring 30 minutes after sucking filtration, at 110 DEG C dry;
E, 780 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Embodiment 4
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take the synthetic mica dry weight 25g of particle diameter D50=1.51 ��m, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 480r/min, form suspension, add crystal grain regulator MgCl20.5g, stir 15��40min;
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.2;
After C, step B complete, it is further continued for stirring 30 minutes, then dripping, with the speed of 20ml/h, the iron nitrate solution that concentration is 0.8mol/l in suspension to be hydrolyzed cladding, instillation concentration is that the sodium hydroxide solution of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping iron nitrate solution 1 hour after, iron nitrate solution is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, adds sodium phosphate 0.5g, continue stirring 30 minutes after sucking filtration, at 110 DEG C dry;
E, 780 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Embodiment 5
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take the synthetic mica dry weight 22g of particle diameter D50=3.12 ��m, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 480r/min, form suspension, add crystal grain regulator calcium carbonate 0.5g, stir 15��40min;
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.2;
After C, step B complete, it is further continued for stirring 30 minutes, then dripping, with the speed of 20ml/h, the iron nitrate solution that concentration is 0.8mol/l in suspension to be hydrolyzed cladding, instillation concentration is that the sodium hydroxide solution of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping iron nitrate solution 1 hour after, iron nitrate solution is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, adds aluminum nitrate 0.5g, continue stirring 30 minutes after sucking filtration, at 110 DEG C dry;
E, 780 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Embodiment 6
The preparation method of this iron oxide red series low gloss sheet layer pigment is:
A, take the synthetic mica dry weight 20g of particle diameter D50=4.30 ��m, put into and mix equipped with in the reaction pot of 800ml deionized water, stir 30 minutes with the mixing speed of 500r/min, form suspension, add crystal grain regulator zinc nitrate 0.5g, stir 15��40min;
B, in thermostat water bath, be heated to 75 DEG C after, with open 10% dilute hydrochloric acid regulate suspension pH value to 3.2;
After C, step B complete, it is further continued for stirring 30 minutes, then dripping, with the speed of 20ml/h, the iron nitrate solution that concentration is 0.8mol/l in suspension to be hydrolyzed cladding, instillation concentration is that the sodium hydroxide solution of 10% is to maintain pH of suspension value stabilization in the scope of 3.1��3.2 simultaneously;
D, by step C drip speed dropping iron nitrate solution 1 hour after, iron nitrate solution is dripped with the speed of 30ml/h, rotating speed is increased to 500r/min simultaneously, continuing hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, then constant temperature stirs 30 minutes, add sodium pyrophosphate 0.5g, continue stirring 30 minutes after sucking filtration, do not wash, at 110 DEG C dry;
E, 760 DEG C of temperature lower calcinations 20 minutes, naturally cool to room temperature, obtain the iron oxide red series low gloss sheet layer pigment that outward appearance is reddish tint inclined purple.
Testing result:
One, glossiness detection:
(1) prepared by pigment model: by pigment and resin in 1:10(mass ratio) ratio mix well, and with the film applicator blade coating of 25 �� m-thick on black and white plate colour table, drying 10min at 105 DEG C.
(2) glossiness detecting instrument: BGD515 type three angle glossometer (20 �� 60 �� 85 ��), Guangzhou style reaches experiment
Room instrument articles for use company limited.
(3) detection of glossiness: this instrument is adjusted under 60 �� of angles, experiments of measuring sample gloss value on white base plate.
Embodiment 1-6 is testing result under vancometer, such as table 1:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Glossiness | 6.9 | 9.2 | 3.2 | 3.5 | 9.5 | 10.9 |
Note: glossiness < 20, then belong to dumb light series.
As seen from the above table, the pigment that embodiment 1-6 prepares, matte effect is notable.
Two, surface of pigments TiO2Diameter characterization
Can be seen that from Fig. 1 and Fig. 2, after adding anti-agglomeration agent, the granule in pigment and granule do not bond agglomerating, good dispersion.
Claims (8)
1. an iron oxide red series low gloss sheet layer pigment, it is characterized in that: using particle diameter for the Muscovitum of 0.15��5 ��m as base material, being coated with ferrum oxide on this base material, form iron oxide coated layer, this iron oxide coated layer is hydrolyzed cladding in solubility ferric salt solution.
2. iron oxide red series low gloss sheet layer pigment according to claim 1, it is characterised in that: described ferric salt solution is one or both in iron sulfate, ferric chloride, ferric nitrate.
3. iron oxide red series low gloss sheet layer pigment according to claim 1 and 2, it is characterised in that: the clad ratio of described iron oxide coated layer is 60%��95%.
4. iron oxide red series low gloss sheet layer pigment according to claim 1 and 2, it is characterised in that: described Muscovitum is natural mica or synthetic mica.
5. the method for the iron oxide red series low gloss sheet layer pigment preparing any one in claim 1-4, it is characterised in that include following making step:
A, take the Muscovitum that particle diameter is 0.15��5 ��m and mix with deionized water and be stirred, stir 30��60 minutes, form the suspension that solid-liquid weight ratio is 1:10��45;
B, put into after crystal grain regulator to described suspension under agitation, gained suspension agitating heating in same rotating speed is warming up to 65��80 DEG C, after continuing stirring 15��40 minutes, regulates the pH value of described suspension, pH value is regulated to 1.5��3.4;
After C, step B complete, being further continued for stirring 15��40 minutes, then in described suspension, a speed dropping ferric salt solution of dripping with 10��25ml/h is hydrolyzed cladding, and instillation alkaline solution maintains stablizing of described suspension pH value simultaneously;
D, by step C drip speed dropping ferric salt solution 0.5��2 hour after, dripping speed and rotating speed raising, continue hydrolysis cladding, until stopping reinforced after obtaining reddish tint partially purple form and aspect, constant temperature stirs 30��60 minutes again, regulate the pH value of this suspension, be subsequently adding anti-agglomeration agent, continue stirring 30��60min; ;
E, the suspension that D step is formed carry out sucking filtration, drying, calcining, cooling, obtain iron oxide red series low gloss sheet layer pigment.
6. the preparation method of iron oxide red series low gloss sheet layer pigment according to claim 5, it is characterised in that: in step A, described mixing speed is 480r/min; In step C, described ferric salt solution concentration is 60g/l, and described alkaline solution is ammonia spirit, sodium hydroxide solution or carbonate solution, and the concentration of this alkaline solution is 10%; In D step, dripping speed and be increased to 30ml/h, mixing speed is increased to 500 turns/min; In E step, after suspension filtering and washing, being dried by filter cake, described drying temperature is 90��120 DEG C, then calcines, and described calcining heat is 580��800 DEG C.
7. the preparation method of iron oxide red series low gloss sheet layer pigment according to claim 5, it is characterised in that: the 0.001-2% that consumption is described mica powder dry weight of the described anti-agglomeration agent of addition; Described anti-agglomeration agent is soluble inorganic salt and/or dissolved organic matter, and described soluble inorganic salt is phosphate or aluminum soluble salt; Described dissolved organic matter is cationic surface active substances or anion active material.
8. the preparation method of iron oxide red series low gloss sheet layer pigment according to claim 7, it is characterised in that: described phosphate is sodium hexameta phosphate, sodium pyrophosphate or sodium phosphate; Described aluminum soluble salt is aluminum chloride, aluminum nitrate or sodium aluminate; Described cationic surface active substances is chitosan, cation CMC sodium, the CPAM of small-molecular-weight and other water-soluble cationic compound; Described anion active material is stearic acid, oleic acid, dodecyl sodium sulfate and other water dissolvable anionic compound.
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| CN106280550A (en) * | 2016-07-19 | 2017-01-04 | 浙江凯色丽科技发展有限公司 | Glass flake base anti-corrosion paint and preparation method thereof |
| CN107325588A (en) * | 2017-07-10 | 2017-11-07 | 林中 | A kind of preparation method for the pigment for coating high gorgeous degree iron oxide |
| CN116144199A (en) * | 2022-12-16 | 2023-05-23 | 湖南肆玖科技有限公司 | Preparation method of dyed mica |
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| CN116144199A (en) * | 2022-12-16 | 2023-05-23 | 湖南肆玖科技有限公司 | Preparation method of dyed mica |
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