CN115537040B - Superfine magnesium hydroxide and preparation method and application thereof - Google Patents

Superfine magnesium hydroxide and preparation method and application thereof Download PDF

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Publication number
CN115537040B
CN115537040B CN202211044367.4A CN202211044367A CN115537040B CN 115537040 B CN115537040 B CN 115537040B CN 202211044367 A CN202211044367 A CN 202211044367A CN 115537040 B CN115537040 B CN 115537040B
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brucite
concentrate
magnesium hydroxide
bin
superfine
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CN115537040A (en
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张晓明
邓鹏�
宋波
吴维冰
万江霖
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Henan Nanzhao New Guangyuan Material Co ltd
Jiangxi Guangyuan Chemical Co Ltd
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Henan Nanzhao New Guangyuan Material Co ltd
Jiangxi Guangyuan Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/028Compounds containing only magnesium as metal
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041Grinding
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/38Coatings with pigments characterised by the pigments
    • D21H19/385Oxides, hydroxides or carbonates
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/44Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/64Inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/19Oil-absorption capacity, e.g. DBP values

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Disintegrating Or Milling (AREA)

Abstract

The invention belongs to the technical field of papermaking, and provides superfine magnesium hydroxide and a preparation method and application thereof. The preparation method provided by the invention adopts the brucite concentrate with a lamellar structure and the fiber brucite concentrate as the brucite concentrate, and after superfine grinding, the lamellar structure and the fiber structure are mutually piled up, so that larger pores exist among powder particles, and the oil absorption value of superfine magnesium hydroxide is greatly improved. The data of the examples show that the oil absorption value of the obtained superfine magnesium hydroxide is 60-80 mL/100g. When the superfine magnesium hydroxide is applied to the thermal paper precoat, the color development effect of the thermal paper can be improved; in addition, because the superfine magnesium hydroxide has better heat conductivity, the heat of the printing head can be quickly conducted, the phenomenon that the coating is heated and melted due to local heat concentration is relieved, and the accumulation condition of the coating dirt of the printing head is relieved.

Description

Superfine magnesium hydroxide and preparation method and application thereof
Technical Field
The invention relates to the technical field of papermaking, in particular to superfine magnesium hydroxide and a preparation method and application thereof.
Background
Thermal paper is a specialty paper that is specially used in thermal printers and thermal fax machines, and generally comprises a base paper substrate, a precoat layer, and a thermally sensitive color-developing layer. The main fillers currently used in precoating of thermal paper are calcined kaolin, talc and light calcium carbonate.
With the development of technology, paper printing speed is increasing. When the thermal paper is printed at a high speed, certain chemical substances (such as leuco dye, color developing agent and the like) in the surface coating of the paper are heated and melted locally at the moment, so that the printing head can be attached with coating dirt, the heat conductivity of the printing head is further influenced, and the color development sensitivity of the coating and the color development density of the recording layer are reduced. Thus, the precoat layer of thermal paper requires a relatively high oil absorption value for the filler selected, typically over 50mL/100 g. The filler with high oil absorption can enhance the absorbability of the thermal paper on molten substances, thereby reducing the accumulation of dirt on the coating of the printing head.
The heat-sensitive precoat is added with partial heat-conducting filler to avoid the local aggregation of heat, thereby avoiding the phenomena of melting and sticking of substances such as color developing agent and the like. Magnesium hydroxide is a white filler with good heat conductivity, and is commonly applied to heat-conducting nylon and various electronic heat dissipation devices. The current deep processing technology of superfine magnesium hydroxide filler mainly comprises a brucite chemical precipitation method and a mineral method. The chemical precipitation method comprises the following steps: magnesium nitrate with a certain concentration and absolute ethyl alcohol (or PEG 6000) are placed in a closed round-bottom flask and stirred uniformly, and a certain temperature is maintained through a constant-temperature water bath. Under the condition of mechanical stirring, 10mL of strong ammonia water is slowly dripped into a three-neck flask by a dripping funnel, reacted for a period of time, filtered in vacuum, washed three times by deionized water and absolute ethyl alcohol respectively, dried in vacuum at 100 ℃ for 1 hour, and ground to obtain a sample. Although the obtained superfine magnesium hydroxide can be used as a precoating filler of thermal paper, the process is complex, the reaction condition is harsh, and the application cost is high. The mineral method is generally an air flow pulverizer, a ball mill or a wet stirring mill, so that the mineral method is simple to operate, but the oil absorption of the superfine magnesium hydroxide obtained by the mineral method is low, generally 30-50 mL/100g, and the superfine magnesium hydroxide cannot be applied to thermal paper.
Disclosure of Invention
In view of the above, the present invention aims to provide an ultrafine magnesium hydroxide, and a preparation method and application thereof. The superfine magnesium hydroxide obtained by the preparation method provided by the invention has high oil absorption.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of superfine magnesium hydroxide, which comprises the following steps:
sequentially crushing, grinding and deironing brucite concentrate to obtain brucite coarse powder;
mixing the brucite coarse powder with a grinding aid, and carrying out superfine grinding to obtain brucite fine powder;
classifying the brucite fine powder to obtain the superfine magnesium hydroxide;
the brucite concentrate comprises brucite concentrate with a lamellar structure and fiber brucite concentrate.
Preferably, the mass ratio of the brucite concentrate with the lamellar structure to the fiber brucite concentrate is 1: 5-5: 1.
preferably, the grinding aid comprises a mixture of sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer and glycerol; the weight molecular weight of the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer is 3500-4500; the mass ratio of the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer to the glycerol in the grinding aid is 1:1 to 1:5.
preferably, the addition amount of the grinding aid is 1.2-2.0% of the mass of brucite coarse powder.
Preferably, the superfine grinding is performed in a ball mill, the ball mill is a two-bin ball mill, the inner wall of the two-bin ball mill is a full ceramic lining plate, the two-bin ball mill comprises a front bin and a rear bin, and filling media of the front bin and the rear bin are alumina ceramic balls; the mass ratio of the filling medium in the front bin to the filling medium in the rear bin is 1:2; the density of the alumina ceramic balls is 3.2-4.0 g/cm 3
Preferably, the filling medium of the front bin is alumina ceramic balls with the particle size of 40mm, alumina ceramic balls with the particle size of 30mm and alumina ceramic balls with the particle size of 20mm, and the mass ratio is 1: (3-6): (0.8-1.5); the filling medium of the rear bin is alumina ceramic balls with the particle size of 15mm and alumina ceramic balls with the particle size of 8mm, and the mass ratio is 1:2.
Preferably, the total time of the superfine grinding is 40-60 min.
Preferably, the rotational speed of the classification is 3600 to 4000rpm, the classification is performed in a classifier, and the surfaces of the blades of the classifier are coated with a ceramic wear layer.
The invention also provides the superfine magnesium hydroxide obtained by the preparation method of the technical scheme, and the oil absorption value of the superfine magnesium hydroxide is 60-80 mL/100g.
The invention also provides application of the superfine magnesium hydroxide in the technical scheme as precoating filler in thermal paper.
The invention provides a preparation method of superfine magnesium hydroxide, which comprises the following steps: sequentially crushing, grinding and deironing brucite concentrate to obtain brucite coarse powder; mixing the brucite coarse powder with a grinding aid, and carrying out superfine grinding to obtain brucite fine powder; classifying the brucite fine powder to obtain the superfine magnesium hydroxide; the brucite concentrate comprises brucite concentrate with a lamellar structure and fiber brucite concentrate. The preparation method provided by the invention adopts the brucite concentrate with a lamellar structure and the fiber brucite concentrate as the brucite concentrate, and after superfine grinding, the lamellar structure and the fiber structure are mutually piled up, so that larger pores exist among powder particles, and the oil absorption value of superfine magnesium hydroxide is greatly improved. The data of the examples show that the oil absorption value of the obtained superfine magnesium hydroxide is 60-80 mL/100g. When the superfine magnesium hydroxide is applied to the thermal paper precoat, the color development effect of the thermal paper can be improved; in addition, because the superfine magnesium hydroxide has better heat conductivity, when the superfine magnesium hydroxide is applied to the thermosensitive precoat, the heat of the printing head can be quickly conducted, the phenomenon that the coating is heated and melted due to local heat concentration is slowed down, and the accumulation condition of dirt on the coating of the printing head is lightened.
Further, the invention selects the mixture of sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer and glycerin as the superfine grinding aid, wherein the glycerin can prolong the residence time of the magnesium hydroxide material in the ball mill and improve the grinding fineness; the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer not only can improve the grinding efficiency, but also has a C3-C6 hydrophobic skeleton, so that the agglomeration of superfine magnesium hydroxide powder can be avoided, the sodium lignin sulfonate component can also enhance the compatibility of superfine magnesium hydroxide and paper, and the rosin glyceride component can improve the smoothness and the fluid permeation resistance of the thermal paper.
Furthermore, the two-bin ball mill can realize superfine grinding of brucite concentrate and improve grinding efficiency through the use of the two-bin ball mill, grading of grinding media and setting of filling quantity.
Drawings
FIG. 1 is a flow chart of a preparation method provided by the invention;
FIG. 2 is a scanning electron micrograph of the ultra-fine magnesium hydroxide obtained in example 1.
Detailed Description
The invention provides a preparation method of superfine magnesium hydroxide, which comprises the following steps:
sequentially crushing, grinding and deironing brucite concentrate to obtain brucite coarse powder;
mixing the brucite coarse powder with a grinding aid, and carrying out superfine grinding to obtain brucite fine powder;
classifying the brucite fine powder to obtain the superfine magnesium hydroxide;
the brucite concentrate comprises brucite concentrate with a lamellar structure and fiber brucite concentrate.
In the present invention, the raw materials used in the present invention are preferably commercially available products unless otherwise specified.
Brucite concentrate is crushed, ground and deironied in turn to obtain brucite coarse powder.
In the invention, the brucite concentrate comprises brucite concentrate with a lamellar structure and fiber brucite concentrate; the mass ratio of the brucite concentrate with the lamellar structure to the fiber brucite concentrate is preferably 1: 5-5: 1. in the invention, the mass content of magnesium hydroxide in the brucite concentrate with the lamellar structure is preferably more than or equal to 96%, and the mass content of magnesium hydroxide in the fiber brucite concentrate is preferably more than or equal to 96%. In the invention, the lamellar structure brucite concentrate is preferably lamellar structure brucite concentrate from Liaoning wide meadow area; the fibrous brucite concentrate is preferably from Shaanxi black forest region.
In the present invention, the brucite concentrate preferably further comprises a separate pretreatment before crushing, and the pretreatment preferably comprises a screening and a washing performed sequentially. In the present invention, the screening preferably includes magnetic separation and manual separation; the magnetic separation and the manual separation are not particularly limited, and magnetic separation operation and manual separation operation well known to those skilled in the art can be adopted. In the invention, the screening can remove the sundry stones. In the present invention, the ore washing preferably includes the steps of: and flushing the screened brucite by adopting a high-pressure water gun. In the invention, the ore washing can remove sediment and the like on the surface of brucite.
In the present invention, the crushing is preferably jaw crushing, which refers to crushing in a jaw crusher. In the present invention, the particle size of the crushed material is preferably 1 to 3mm.
In the present invention, the grinding is preferably performed in a ring roller mill. In the present invention, the particle size of the material obtained by the milling is preferably 100 to 200 mesh.
In the present invention, the iron removal is preferably performed in an electromagnetic iron remover. In the invention, the iron removal can reduce the influence of iron impurities on whiteness.
In the present invention, the brucite coarse powder preferably has a particle size of 200 to 300 mesh.
After brucite coarse powder is obtained, the brucite coarse powder is mixed with a grinding aid, and superfine grinding is carried out to obtain brucite fine powder.
In the present invention, the grinding aid preferably comprises a mixture of sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer and glycerin. In the present invention, the weight molecular weight of the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer is preferably 3500 to 4500. In the invention, the mass ratio of the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer and the glycerol in the grinding aid is preferably 1:1 to 1:5. in the present invention, the addition amount of the grinding aid is preferably 1.2 to 2.0% by mass, more preferably 1.4 to 1.8% by mass, and still more preferably 1.5 to 1.6% by mass of the brucite coarse powder. In the invention, the feeding speed of the grinding aid is preferably 3-4 Hz. In the present invention, the feeding speed of the brucite coarse powder is preferably 5-6 Hz.
In the present invention, the ultra-fine grinding is preferably performed in a ball mill, which is preferably a two-bin ball mill. In the invention, the inner wall of the two-bin ball mill is preferably an all-ceramic lining plate. In the invention, the two-bin ball mill comprises a front bin and a rear bin, wherein the filling medium of the front bin and the rear bin is preferably alumina ceramic balls, and the density of the alumina ceramic balls is preferably 3.2-4.0 g/cm 3 Further preferably 3.6g/cm 3 . In the invention, the mass ratio of the filling medium in the front bin to the filling medium in the rear bin is preferably 1:2.
in the invention, the filling medium of the front bin is preferably alumina ceramic balls with the particle size of 40mm, alumina ceramic balls with the particle size of 30mm and alumina ceramic balls with the particle size of 20mm, and the mass ratio of the alumina ceramic balls is 1: (3-6): the mixed system of (0.8 to 1.5) is more preferably 1:4: 1.2.
In the invention, the filling medium of the rear bin is preferably alumina ceramic balls with the particle size of 15mm and alumina ceramic balls with the particle size of 8mm, and the mass ratio is 1:2.
In the present invention, the total time of the ultra-fine grinding is preferably 40 to 60 minutes.
In the present invention, the average particle diameter of the brucite fine powder is preferably 1.0 to 2.0 μm.
After brucite fine powder is obtained, the brucite fine powder is classified to obtain the superfine magnesium hydroxide.
In the present invention, the rotational speed of the classification is preferably 3600 to 4000rpm, more preferably 3700 to 3900rpm. In the present invention, the classification is preferably performed in a classifier whose surface of the blade is covered with a ceramic wear layer. According to the invention, the ceramic wear-resistant layer is coated on the surface of the blade of the classifier, so that the introduction of scrap iron impurities can be prevented, and the influence of scrap iron on whiteness can be reduced.
After the classification, the invention preferably also comprises carrying out iron removal, preferably in an electromagnetic iron remover.
Fig. 1 is a flow chart of a preparation method provided by the invention.
The invention also provides the superfine magnesium hydroxide obtained by the preparation method. In the invention, the oil absorption value of the superfine magnesium hydroxide is 60-80 mL/100g, and the particle size is 1-2 mu m.
The invention also provides application of the superfine magnesium hydroxide in the technical scheme as precoating filler in thermal paper. When the superfine magnesium hydroxide is applied to the thermal paper, the dosage of the superfine magnesium hydroxide is not particularly limited, and can be set by a person skilled in the art according to actual needs.
The ultra-fine magnesium hydroxide, the preparation method and the application thereof, which are provided by the present invention, are described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide-pudding area and fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in Shaanxi black forest area, screening and washing, and then, according to the mass ratio of 5:1, crushing the mixture by a jaw crusher, grinding the mixture by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed is 5.8Hz, adding a grinding aid accounting for 1.2% of the mass of the brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3800) and the mass ratio of glycerin is 1:1, a mixture of two or more of the above-mentioned materials; controlling the feeding speed of the grinding aid to be 3.5Hz; grinding brucite coarse powder in a two-bin ball mill for 45min to obtain brucite fine powder.
Two-bin ball millThe whole size is 2.2mX7.5 m, the installed power is 380kW, and the inner wall is a full ceramic lining plate; the mass ratio of the filling medium in the front bin to the filling medium in the rear bin of the two-bin ball mill is 1:2, the filling medium has a density of 3.6g/cm 3 Alumina ceramic balls of (a); the size of the alumina ceramic balls filled in the front bin is 40mm, 30mm and 20mm, and the mass ratio is 1:4:1.2; the size of the alumina ceramic ball filled in the rear bin is 15mm and the size of the alumina ceramic ball filled in the rear bin is 8mm, and the mass ratio is 1:2.
the brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.56 mu m, and the oil absorption is 61mL/100g.
Example 2
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide-pudding area and fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in Shaanxi black forest area, screening and washing, and then, according to the mass ratio of 3:1, crushing the mixture by a jaw crusher, grinding the mixture by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.5Hz; adding a grinding aid accounting for 1.2% of the mass of brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3850) and the mass ratio of glycerin is 1:1, the feeding speed of the grinding aid is 3.5Hz, so that brucite coarse powder is ground for 50min in a two-bin ball mill, and brucite fine powder is obtained.
The parameters of the two-bin ball mill were the same as in example 1.
Delivering brucite fine powder into a classifier by an induced draft fan, collecting the particle size reaching the standard part by a collector, removing iron and packaging, wherein the rotating speed of the classifier is 3800 rpm;
the average particle diameter of the finished product is 1.65 mu m, and the oil absorption is 65mL/100g.
Example 3
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide-pudding area and fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in Shaanxi black forest area, screening and washing, and then, according to the mass ratio of 1:1, crushing the mixture by a jaw crusher, grinding the mixture by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.8Hz; adding a grinding aid with the mass of 1.5% of brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3800) and the mass ratio of glycerin is 1:1, the feeding speed of the grinding aid is 3.5Hz, so that brucite coarse powder is ground for 50min in a two-bin ball mill, and brucite fine powder is obtained.
The parameters of the two-bin ball mill were the same as in example 1.
The brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.69 mu m, and the oil absorption is 72mL/100g.
Example 4
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide-pudding area and fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in Shaanxi black forest area, screening and washing, and then, according to the mass ratio of 1:2, after being compounded, crushing the mixture by a jaw crusher, and then grinding the mixture by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.2Hz; adding a grinding aid with the mass of 1.5% of brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3850) and the mass ratio of glycerin is 1:1, the feeding speed of the grinding aid is 3.5Hz, so that brucite coarse powder is ground for 48min in a two-bin ball mill, and brucite fine powder is obtained.
The parameters of the two-bin ball mill were the same as in example 1.
The brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.78 mu m, and the oil absorption is 67mL/100g.
Example 5
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide-pudding area and fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in Shaanxi black forest area, screening and washing, and then, according to the mass ratio of 1:3, after being compounded, crushing the mixture by a jaw crusher, and then grinding the mixture by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.6Hz; adding a grinding aid with the mass of 1.4% of brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3800) and the mass ratio of glycerin is 1:1, the feeding speed of the grinding aid is 3.5Hz, so that brucite coarse powder is ground for 50min in a two-bin ball mill, and brucite fine powder is obtained.
The parameters of the two-bin ball mill were the same as in example 1.
The brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.56 mu m, and the oil absorption is 64mL/100g.
Comparative example 1
Selecting brucite concentrate (magnesium hydroxide content is more than or equal to 96%) with lamellar structure in Liaoning wide puddle area, screening, washing, crushing by a jaw crusher, grinding by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.6Hz; adding a grinding aid with the mass of 1.4% of brucite coarse powder, wherein the grinding aid is sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3800) and the mass ratio of glycerin is 1:1, a mixture of two or more of the above-mentioned materials; the feed rate of the grinding aid was 3.5Hz, so that brucite coarse powder was ground in a two-bin ball mill for 50min to obtain brucite fine powder.
The parameters of the two-bin ball mill were the same as in example 1.
The brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.51 mu m, and the oil absorption is 44mL/100g.
Comparative example 2
Selecting fiber brucite concentrate (magnesium hydroxide content is more than or equal to 96%) in the black forest area of Shaanxi, screening and washing, crushing by a jaw crusher, grinding by a ring roller mill, and removing iron to obtain 200-300 mesh brucite coarse powder.
Conveying brucite coarse powder into a two-bin ball mill through a belt for superfine grinding, wherein the feeding speed of the brucite coarse powder is 5.6Hz; adding a grinding aid accounting for 1.4% of the mass of brucite coarse powder, wherein the grinding aid is a mixture of sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer (the weight molecular weight is 3800) and glycerin with the mass ratio of 1:1, and the feeding speed of the grinding aid is 3.5Hz, so that the brucite coarse powder is ground in a two-bin ball mill for 50min, and brucite fine powder is obtained.
The parameters of the two-bin ball mill were the same as in example 1.
The brucite fine powder is delivered into a classifier by an induced draft fan, the rotating speed of the classifier is 3800rpm, and the particle size reaching the standard is collected by a collector, deironing and packaging.
The average particle diameter of the finished product is 1.63 mu m, and the oil absorption is 48mL/100g.
Comparative example 3
Similar to example 1, the difference is: the filling medium of the front bin is ceramic balls with the size of 40mm, 30mm and 20mm, and the mass ratio is 1:5:1.5 alumina ceramic balls, the filling medium of the rear bin is 15mm in size and 8mm in mass ratio of 1:4 alumina ceramic balls.
The average particle diameter of the finished product is 1.92 mu m, and the oil absorption is 56mL/100g.
Table 1 shows the indexes of the superfine magnesium hydroxide obtained in examples 1 to 5 and comparative examples 1 to 3.
TABLE 1 relevant indicators of ultra-fine magnesium hydroxide obtained in examples 1 to 5 and comparative examples 1 to 2
FIG. 2 is a scanning electron micrograph of the ultra-fine magnesium hydroxide obtained in example 1, as can be seen from FIG. 2: the lamellar structure and the fibrous structure magnesium hydroxide are mutually stacked, so that larger pores exist among powder particles, and the oil absorption value of the superfine magnesium hydroxide can be greatly improved.
The foregoing is merely a preferred embodiment of the present invention and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.

Claims (6)

1. The preparation method of the superfine magnesium hydroxide is characterized by comprising the following steps of:
sequentially crushing, grinding and deironing brucite concentrate to obtain brucite coarse powder;
mixing the brucite coarse powder with a grinding aid, and carrying out superfine grinding to obtain brucite fine powder;
classifying the brucite fine powder to obtain the superfine magnesium hydroxide;
the brucite concentrate comprises brucite concentrate with a lamellar structure and fiber brucite concentrate;
the grinding aid comprises a mixture of sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer and glycerol;
the superfine grinding is carried out in a ball mill, the ball mill is a two-bin ball mill, the inner wall of the two-bin ball mill is a full ceramic lining plate, the two-bin ball mill comprises a front bin and a rear bin, and filling media of the front bin and the rear bin are oxygenAluminum ceramic balls; the mass ratio of the filling medium in the front bin to the filling medium in the rear bin is 1:2; the density of the alumina ceramic balls is 3.2-4.0 g/cm 3
The filling medium of the front bin is alumina ceramic balls with the grain diameter of 40mm, alumina ceramic balls with the grain diameter of 30mm and alumina ceramic balls with the grain diameter of 20mm, and the mass ratio is 1: (3-6): (0.8-1.5); the filling medium of the rear bin is alumina ceramic balls with the particle size of 15mm and alumina ceramic balls with the particle size of 8mm, and the mass ratio is 1:2.
2. The preparation method according to claim 1, wherein the mass ratio of the lamellar structure brucite concentrate to the fiber brucite concentrate is 1: 5-5: 1.
3. the preparation method according to claim 1, wherein the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer has a weight molecular weight of 3500 to 4500; the mass ratio of the sodium lignin sulfonate-hydroxypropyl acrylate-rosin glyceride copolymer to the glycerol in the grinding aid is 1:1 to 1:5.
4. the preparation method according to claim 1 or 3, wherein the addition amount of the grinding aid is 1.2 to 2.0% of the mass of brucite coarse powder.
5. The method according to claim 1, wherein the total time of the ultra-fine grinding is 40 to 60 minutes.
6. The method according to claim 1, wherein the classification is performed in a classifier having a surface of a blade coated with a ceramic wear layer at a rotational speed of 3600 to 4000 rpm.
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