CN114180639B - Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing - Google Patents

Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing Download PDF

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CN114180639B
CN114180639B CN202111517097.XA CN202111517097A CN114180639B CN 114180639 B CN114180639 B CN 114180639B CN 202111517097 A CN202111517097 A CN 202111517097A CN 114180639 B CN114180639 B CN 114180639B
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crushing
magnesium ferrite
preparing
iron
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程冲
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/62L* (lightness axis)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/63Optical properties, e.g. expressed in CIELAB-values a* (red-green axis)
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values
    • C01P2006/64Optical properties, e.g. expressed in CIELAB-values b* (yellow-blue axis)

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Abstract

The invention provides a method for preparing yellow inorganic nano-oxide pigment by steam drying and crushing, which relates to the field of inorganic pigment, and comprises the following steps: s1: preparing magnesium ferrite slurry: adding an iron source and a magnesium source into water, mixing, stirring and grinding; s2: preparing a magnesium ferrite precursor: drying and crushing the magnesium ferrite slurry prepared in the step S1 to obtain a nanoscale superfine magnesium ferrite precursor; s3: preparing magnesium ferrite: and (3) pyrolyzing the magnesium ferrite precursor obtained in the step (S2), cooling, and crushing to obtain a magnesium ferrite finished product. The method has the advantages of low energy consumption and short reaction time; the appearance of the finished product is uniform, the consistency is high, and the stability is good; the raw materials are easy to obtain, the process is simple, the cost is low, and the industrial production is easy to realize.

Description

Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing
Technical Field
The invention relates to the field of inorganic pigments, in particular to a method for preparing a yellow inorganic nano-oxide pigment by steam drying and crushing.
Background
Iron oxide is the second largest inorganic pigment next to titanium white, and is also the first largest colored inorganic pigment. Iron oxide yellow, also called iron oxyhydroxide, is an alkaline oxide with relatively stable chemical properties, and has a chemical molecular formula of FeOOH or Fe 2O3·H2 O, and can be dehydrated and decomposed to become red at about 177 ℃, so that the application of the common iron oxide yellow pigment in high-temperature occasions such as plastic processing and baking type coating is limited. At present, zinc ferrite is used as a common high-temperature-resistant yellow inorganic pigment, and the zinc ferrite does not change color at 400 ℃, but contains heavy metal zinc, so that the zinc ferrite is harmful to the environment and human health. Magnesium ferrite becomes an excellent substitute for zinc ferrite.
Chinese patent CN102502857 discloses a preparation method of magnesium ferrite pigment, which is characterized in that iron oxide yellow filter cake is mixed with active magnesium oxide, and simultaneously, auxiliary agents with dispersing and anti-sintering functions are added to carry out batching, pulping, high-speed dispersing, suction filtration, drying, roasting reaction and crushing, thus obtaining the orange-yellow high temperature resistant magnesium ferrite pigment. The method has the advantages of single raw material variety, addition of auxiliary agent for reaction, long process flow, long preparation time, incapability of industrial production, darker color and low purity of the product.
Aiming at the problems of single raw material variety, singing process flow, long preparation time and the like of the magnesium ferrite pigment in the prior art, the invention provides a magnesium ferrite pigment with simple process, low raw material requirement, short preparation time and high quality.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides the preparation method of the environment-friendly yellow inorganic nano oxide pigment with simple process, low raw material requirement, short preparation time, bright color, high purity and thermal stability. The method for preparing the material comprises the following steps of,
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for preparing an inorganic nano oxide pigment, which comprises the following steps:
S1: preparing magnesium ferrite slurry: adding an iron source and a magnesium source into water, mixing, stirring and grinding;
S2: preparing a magnesium ferrite precursor: drying and crushing the magnesium ferrite slurry prepared in the step S1 by using steam to obtain a nanoscale superfine magnesium ferrite precursor;
S3: preparing magnesium ferrite: and (3) pyrolyzing the magnesium ferrite precursor obtained in the step (S2), cooling, and crushing to obtain a magnesium ferrite finished product.
Further, the iron source in step S1 includes one or more of iron oxide yellow, iron oxide red, iron oxide black and iron powder, and the magnesium source includes magnesium oxide and/or magnesium hydroxide.
Further, the molar ratio of the iron content in the iron source to the magnesium content in the magnesium source in the step S1 is 1.6-2.4:1.
Further, it is characterized in that: the weight of the water in the step S1 accounts for 80-90% of the weight of the magnesium ferrite slurry.
Further, the stirring frequency in the step S1 is 100-200 revolutions/min.
Further, the grinding time in the step S1 is 1-3h, the grinding is carried out by using a nano grinder, the grinding medium of the nano grinder is zirconia balls with the thickness of 0.3-0.4mm, and the rotating speed is 2000-4000 revolutions per minute.
Further, the steam temperature of the steam drying and crushing in the step S2 is 260-320 ℃, and the steam pressure is 0.8-1.4MPa.
Further, in the step S3, air flow crushing is adopted, and the air pressure is 0.6MPa-0.8MPa. The D50 granularity is controlled between 0.5 and 1 micron.
Further, the pyrolysis in the step S3 is performed under an oxygen or air atmosphere, and the heating rate is 10-15 ℃/min.
Further, the pyrolysis temperature in the step S3 is 800-1000 ℃, and the heat preservation time is 10-60min.
The invention also provides the inorganic nano oxide pigment prepared by the method.
The invention has the technical effects that:
1. The invention adopts the pulping method of the high-speed grinding of the nanometer grinder, so that the particle size and the shape of the raw materials are uniform, various raw materials are quickly and uniformly mixed, the pulping time is saved, and the energy consumption is reduced.
2. The method adopts the main steam crushing dryer to dry and crush, and the prepared precursor is nano fine powder with uniform morphology and higher activity, so that materials are heated uniformly, react uniformly and have short reaction time in the sintering process. The prepared magnesium ferrite has uniform appearance, high consistency and good stability.
3. The scheme of the invention has the advantages of no doping, no impurity introduction, easily available raw materials, simple process, low cost and easy industrial production.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention.
Before the embodiments of the invention are explained in further detail, it is to be understood that the invention is not limited in its scope to the particular embodiments described below; it is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention.
Where numerical ranges are provided in the examples, it is understood that unless otherwise stated herein, both endpoints of each numerical range and any number between the two endpoints are significant both in the numerical range. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It should be noted that the raw materials used in the present invention are all common commercial products, and therefore the sources thereof are not particularly limited.
Example 1
10L of tap water, 1000g of iron oxide yellow and 283g of magnesium oxide (the molar ratio of iron to magnesium in the raw materials is 1.6:1) are sequentially added into a reaction tank, and all the materials are stirred and ground for 1h after being added, so as to obtain evenly mixed magnesium ferrite slurry. The stirring frequency is 100 rpm, the grinding medium of the nano grinder is zirconia balls with the diameter of 0.3-0.4mm, and the rotating speed is 2000 rpm.
And drying and crushing the magnesium ferrite slurry by a steam crusher, wherein the steam temperature is 260 ℃ and the steam pressure is 1.2MPa, and obtaining the magnesium ferrite precursor.
And (3) placing the magnesium ferrite precursor into a high-temperature refractory container, then placing the container into a tube furnace, self-heating to 800 ℃ at 10 ℃/min under the atmosphere of high-purity oxygen, preserving heat for 10min, naturally cooling, and finally crushing by using a jet mill, wherein the jet mill adopts air pressure of 0.8MPa to obtain the magnesium ferrite.
Example 2
10L of tap water, 899g of iron oxide red and 226g of magnesium oxide (the molar ratio of iron to magnesium in the raw materials is 2:1) are sequentially added into a reaction tank, and all materials are stirred and ground for 2 hours after the addition, so as to obtain evenly mixed magnesium ferrite slurry. The stirring frequency is 200 revolutions per minute, the grinding medium of the nano grinder is zirconia balls with the diameter of 0.3-0.4mm, and the rotating speed is 3000 revolutions per minute.
And drying and crushing the magnesium ferrite slurry by a steam crusher, wherein the steam temperature is 280 ℃, and the steam pressure is 1.4MPa, so as to obtain a magnesium ferrite precursor.
And (3) placing the magnesium ferrite precursor into a high-temperature refractory container, then placing the container into a tube furnace, self-heating to 900 ℃ at 10 ℃/min under the atmosphere of high-purity oxygen, preserving heat for 30min, naturally cooling, and finally crushing by using a jet mill, wherein the jet mill adopts air pressure of 0.8MPa to obtain the magnesium ferrite.
Example 3
8L of tap water, 1048g of iron oxide black and 189g of magnesium oxide (the molar ratio of iron to magnesium in the raw materials is 2.4:1) are sequentially added into a reaction tank, and all the materials are stirred and ground for 3 hours after the addition, so as to obtain the uniformly mixed magnesium ferrite slurry. The stirring frequency is 200 revolutions per minute, the grinding medium of the nano grinder is zirconia balls with the diameter of 0.3-0.4mm, and the rotating speed is 4000 revolutions per minute.
And drying and crushing the magnesium ferrite slurry by a steam crusher, wherein the steam temperature is 300 ℃, and the steam pressure is 1.0MPa, so as to obtain a magnesium ferrite precursor.
And (3) placing the magnesium ferrite precursor into a high-temperature refractory container, then placing the container into a tube furnace, self-heating to 1000 ℃ at 12 ℃/min under high-purity oxygen atmosphere, preserving heat for 45min, naturally cooling, and finally crushing by using a jet mill, wherein the jet mill adopts air pressure of 0.6MPa to obtain the magnesium ferrite.
Example 4
8L of tap water, 629g of iron powder and 327g of magnesium hydroxide (the molar ratio of iron to magnesium in the raw materials is 2:1) are sequentially added into a reaction tank, and after all materials are added, stirring and grinding are carried out for 2 hours, so as to obtain the uniformly mixed magnesium ferrite slurry. The stirring frequency is 200 revolutions per minute, the grinding medium of the nano grinder is zirconia balls with the diameter of 0.3-0.4mm, and the rotating speed is 3000 revolutions per minute.
And (3) drying and crushing the magnesium ferrite slurry by a steam crusher, wherein the steam temperature is 320 ℃, and the steam pressure is 0.8MPa, so as to obtain a magnesium ferrite precursor.
And (3) placing the magnesium ferrite precursor into a high-temperature refractory container, then placing the container into a tube furnace, self-heating to 900 ℃ at 15 ℃/min under the atmosphere of high-purity oxygen, preserving heat for 60min, naturally cooling, and finally crushing by using a jet mill, wherein the jet mill adopts air pressure of 0.6MPa to obtain the magnesium ferrite.
Comparative example 1
The raw material proportion is the same as that of the embodiment 1, the beating working section is changed into stirring beating by using a high-speed dispersing machine, the dewatering working section is changed into a plate-frame filter pressing mode, and the sintering and crushing conditions are the same as those of the embodiment 1.
Comparative example 2
The raw material ratio is the same as that of the embodiment 2, the pulping working section is changed to stirring and pulping by using a high-speed dispersing machine, the dewatering working section is changed to a plate-frame filter pressing mode, and the sintering and crushing conditions are the same as those of the embodiment 1.
Comparative example 3
The raw material ratio is the same as that of the embodiment 3, the pulping working section is changed to stirring and pulping by using a high-speed dispersing machine, the dewatering working section is changed to a plate-frame filter pressing mode, and the sintering and crushing conditions are the same as those of the embodiment 1.
Comparative example 4
The raw material proportion is the same as that of the embodiment 4, the beating working section is changed to stirring beating by using a high-speed dispersing machine, the dewatering working section is changed to a plate-frame filter pressing mode, and the sintering and crushing conditions are the same as those of the embodiment 1.
The test method comprises the following steps: performing a chromaticity value test on the magnesium ferrite obtained in each example, and analyzing by a color difference meter to obtain L, a and b; the hiding power test was performed according to national standard GB1726-79 (89), and the results were counted in Table 1.
The results are counted in table 1.
TABLE 1 detection results of magnesium ferrite
Examples L a b Hiding power (%)
Example 1 57.46 33.19 45.31 47.75
Example 2 57.47 33.64 45.65 48.15
Example 3 56.29 33.79 44.31 47.40
Example 4 57.39 33.85 45.99 47.43
Comparative example 1 56.89 34.53 46.18 47.62
Comparative example 2 52.80 35.68 39.73 53.96
Comparative example 3 50.45 38.05 35.46 53.34
Comparative example 4 53.52 34.88 41.33 52.71
The detection result shows that the process has low requirements on raw materials, low production energy consumption, short production period, relatively close chromaticity value and hiding power value, good color phase of the synthesized finished product, stable performance and better reference basis for selecting low-cost raw materials for later production.
Finally, it should be noted that the above description is only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and that the simple modification and equivalent substitution of the technical solution of the present invention can be made by those skilled in the art without departing from the spirit and scope of the technical solution of the present invention.

Claims (8)

1. A method of preparing an inorganic nano-oxide pigment, characterized by: the method comprises the following steps:
S1: preparing magnesium ferrite slurry: adding an iron source and a magnesium source into water, mixing, stirring and grinding;
S2: preparing a magnesium ferrite precursor: drying and crushing the magnesium ferrite slurry prepared in the step S1 by using steam to obtain a nanoscale superfine magnesium ferrite precursor;
s3: preparing magnesium ferrite: pyrolyzing the magnesium ferrite precursor obtained in the step S2, cooling, and crushing to obtain a magnesium ferrite finished product;
the grinding mode in the step S1 is nanometer high-speed grinding, the grinding time is 1-3h, the grinding medium for nanometer high-speed grinding is zirconia balls with the thickness of 0.3-0.4mm, and the rotating speed is 2000-4000 revolutions per minute; the steam temperature of the steam drying and crushing in the step S2 is 260-320 ℃, and the steam pressure is 0.8-1.4MPa; the pyrolysis temperature in the step S3 is 800-1000 ℃, and the heat preservation time is 10-60min.
2. The method according to claim 1, characterized in that: the iron source in step S1 includes one or more of iron oxide yellow, iron oxide red, iron oxide black and iron powder, and the magnesium source includes magnesium oxide and/or magnesium hydroxide.
3. The method according to claim 1, characterized in that: the molar ratio of the content of the iron element in the iron source to the content of the magnesium element in the magnesium source in the step S1 is 1.6-2.4:1.
4. The method according to claim 1, characterized in that: the weight of the water in the step S1 accounts for 80-90% of the weight of the magnesium ferrite slurry.
5. The method according to claim 1, characterized in that: the stirring frequency in the step S1 is 100-200 revolutions/min.
6. The method according to claim 1, characterized in that: in the step S3, the crushing adopts air current crushing, and the air pressure is 0.6MPa-0.8MPa.
7. The method according to claim 1, characterized in that: the pyrolysis in the step S3 is carried out under the atmosphere of oxygen or air, and the heating rate is 10-15 ℃/min.
8. An inorganic nano-oxide pigment prepared by the method of any one of claims 1-7.
CN202111517097.XA 2021-12-08 2021-12-08 Method for preparing yellow inorganic nano oxide pigment by steam drying and crushing Active CN114180639B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102107910A (en) * 2011-03-23 2011-06-29 上海理工大学 Preparation method of nano magnesium ferrite
CN102502857A (en) * 2011-10-21 2012-06-20 南通宝聚颜料有限公司 Formula of high temperature-resistant magnesium ferrite orange-yellow pigment and preparation process thereof
CN103420428A (en) * 2012-09-28 2013-12-04 上海理工大学 Preparation method of magnesium ferrite nano-particles

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102107910A (en) * 2011-03-23 2011-06-29 上海理工大学 Preparation method of nano magnesium ferrite
CN102502857A (en) * 2011-10-21 2012-06-20 南通宝聚颜料有限公司 Formula of high temperature-resistant magnesium ferrite orange-yellow pigment and preparation process thereof
CN103420428A (en) * 2012-09-28 2013-12-04 上海理工大学 Preparation method of magnesium ferrite nano-particles

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
姜山等编.《纳米》.科学普及出版社,2013,第58页. *
杨晓清等编.《包装机械与设备》.国防工业出版社,2009,262-263页. *

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