CN110317068B - Dispersing agent and application thereof - Google Patents

Dispersing agent and application thereof Download PDF

Info

Publication number
CN110317068B
CN110317068B CN201910654846.XA CN201910654846A CN110317068B CN 110317068 B CN110317068 B CN 110317068B CN 201910654846 A CN201910654846 A CN 201910654846A CN 110317068 B CN110317068 B CN 110317068B
Authority
CN
China
Prior art keywords
dispersing agent
dispersant
main component
ferrite
magnetic material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910654846.XA
Other languages
Chinese (zh)
Other versions
CN110317068A (en
Inventor
李玉平
包大新
何震宇
杨武国
吴云飞
李军华
金志洪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hengdian Group DMEGC Magnetics Co Ltd
Original Assignee
Hengdian Group DMEGC Magnetics Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hengdian Group DMEGC Magnetics Co Ltd filed Critical Hengdian Group DMEGC Magnetics Co Ltd
Priority to CN201910654846.XA priority Critical patent/CN110317068B/en
Publication of CN110317068A publication Critical patent/CN110317068A/en
Application granted granted Critical
Publication of CN110317068B publication Critical patent/CN110317068B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/26Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/632Organic additives
    • C04B35/634Polymers
    • C04B35/63404Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • C04B35/63444Nitrogen-containing polymers, e.g. polyacrylamides, polyacrylonitriles, polyvinylpyrrolidone [PVP], polyethylenimine [PEI]
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
    • H01F1/10Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
    • H01F1/11Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

Abstract

The invention relates to the technical field of magnetic materials, in particular to a dispersing agent and application thereof. The dispersing agent comprises a main component and an auxiliary component, wherein the content of the main component in the dispersing agent is 70-95 wt%, and the content of the auxiliary component in the dispersing agent is 5-30 wt%, so that a good dispersing effect can be realized, ferrite powder agglomeration and agglomeration are avoided, the magnetic performance of the ferrite magnetic material is improved, excessive gas harmful to the structure of the ferrite magnetic material can be generated in the sintering process, the qualification rate of the ferrite magnetic material is ensured, in addition, the required using amount is less, a good dispersing effect can be generated, and the material cost can be further saved.

Description

Dispersing agent and application thereof
Technical Field
The invention relates to the technical field of magnetic materials, in particular to a dispersing agent and application thereof.
Background
The ferrite permanent magnet material has the advantages of low price, high temperature resistance and corrosion resistance, so that the ferrite permanent magnet material is widely applied to the fields of motors, engines, sensors and the like. With the development of miniaturization and light weight of motors and generators, the market requires further improvement of the magnetic performance of ferrite permanent magnets. Generally, there are two methods for improving the magnetic performance of sintered ferrite permanent magnet materials, one is to optimize the material components and improve the saturation magnetization and magnetocrystalline anisotropy constant of the magnetic phase (M phase); the other method is to improve the preparation process, optimize the microstructure of the magnet and improve the remanence and the coercive force of the magnet.
The magnetic property of the ferrite is improved by adjusting the material components, the most effective is the combined substitution of La-Co ions, and in the early research, people adopt La3+Substituted moiety Sr2+By Co2+By substitution of part of Fe2+Finally form a film having Sr1-xLaxFe12-yCoyO19SrLaCo ferrite of structure, whichThe highest magnetic performance can reach Br>4500Gs,Hcj>4500 Oe. In recent years, Ca has been adopted2+Substituted moiety Sr2+And further improve La3+And Co2+In such an amount that the material has properties up to Br>4700Gs,Hcj>4800Oe。
The microstructure of the material is optimized by adjusting the preparation process, wherein one effective method is to refine the microstructure of the material so that the average grain size is controlled below 1 μm. To achieve this, it is not only necessary to control the sintering temperature of the subsequent material, but also to prepare ferrite powder particles of sufficiently fine particle size in a ball milling process at the front end. However, as the ferrite powder is made finer, electrostatic force between particles becomes larger, and the powder particles are easily agglomerated. This phenomenon makes it difficult not only to continue the refinement of the powder but also to subsequently orient it under a magnetic field, thus making it difficult to obtain a high-performance ferrite product. The most effective method for solving the problem is to add a small amount of dispersing agent during ball milling, and to reduce the agglomeration of the powder by utilizing the charge repulsion or the polymer blocking effect of the dispersing agent. According to relevant documents and practical application, organic compounds such as calcium gluconate, gluconic acid, sorbitol, ascorbic acid and the like are found to be effective for improving the magnetic performance of the material. However, the above dispersant is easily decomposed during high-temperature sintering to generate CO2And water vapor, which easily causes micro-cracks in the product during release, and finally causes the reduction of the product yield.
A magnet powder, a sintered magnet, a manufacturing process thereof, a bonded magnet, a motor, and an invention patent application for a magnetic recording medium, which are disclosed by the Chinese patent office on 22.12.1999, application publication No. CN1239578A, wherein the magnet powder has at least two different Curie temperatures, the two different Curie temperatures existing in the range of 400 to 480 ℃, and the absolute value of the difference therebetween is 5 ℃ or more, is a hexagonal ferrite main phase containing A, Co and R (wherein A represents Sr, Ba, or Ca, and R represents at least one element selected from the group consisting of rare earth elements (including Y) and Bi). In the technical scheme, the volume of calcium gluconate, gluconic acid, sorbitol, ascorbic acid, lactobionic acid, tartaric acid and the like is effective for improving the performance of the material, but the patent also indicates that the product is cracked due to the addition of too much dispersing agent.
The Chinese patent office discloses an invention patent application of a dispersant for ceramic ink and a preparation method thereof on 27.8.2014, and the application publication number is CN 104004413A; the Chinese patent office discloses an invention patent authorization of a ceramic dispersant and a preparation method thereof in 2018, 12 and 21, and the authorization publication number is CN 106188443B. The above technical solutions all disclose dispersants for ceramics, but in actual use, it was found that the ceramic dispersants are detrimental to the magnetic properties of ferrite magnetic materials, including problems of easy introduction of impurity components unnecessary for the magnet and difficulty in removal, and the above solutions also have problems of lowering the yield of the magnet product.
Zhongpeng [1], high-benefit people [1,2], Ninji [1,2], et al, a study on the influence of a dispersant on the dispersion behavior of a certain bentonite ore [ J ] silicate report, 2018, a document also describes that although the inorganic dispersants sodium pyrophosphate and sodium hexametaphosphate do not influence the qualification rate of products, the adoption of the inorganic dispersants such as sodium pyrophosphate and/or sodium hexametaphosphate does not influence the qualification rate of products because the inorganic dispersants contain phosphorus elements which are not needed by ferrite permanent magnet materials, but can cause the magnetic performance of the ferrite permanent magnet materials to be seriously reduced.
Disclosure of Invention
The invention provides a dispersing agent and application thereof, aiming at solving the problems that when the existing dispersing agent is used for preparing a ferrite magnetic material, the existing dispersing agent is easy to decompose during high-temperature sintering, the dispersing effect is poor, even most dispersing agents cannot generate the dispersing effect, the dispersing agent capable of generating the dispersing effect can generate and release various gases including carbon dioxide and water vapor after decomposition, the released gases are difficult to discharge and are surrounded by ferrite powder, and the prepared ferrite magnetic material product generates cavities, defects and microcracks, so that the whole product yield and quality are reduced. It firstly achieves the following purposes: firstly, the qualified rate of products is ensured, and the problems of product cracking and qualified rate reduction caused by the production of a large amount of gas, incapability of discharging and the like are avoided; secondly, ferrite powder particles can be well dispersed, and the particle size of the ferrite powder can be controlled; and thirdly, the magnetic property of the ferrite magnetic material can be improved.
In order to achieve the purpose, the invention adopts the following technical scheme.
A dispersing agent for the mixture of water and oil,
the dispersant comprises a main component;
the molecular formula of the main component is shown as the following formula 1:
formula 1:
Figure GDA0002540621270000021
in formula 1: n is more than or equal to 2 and less than or equal to 9, M1Is hydrogen or a monovalent or divalent metal, M2Is an amino compound.
The main component can be obtained by polymerizing methyl silanetriol, methanol, monovalent or divalent metal base (such as sodium hydroxide, calcium hydroxide, etc.) and inorganic ammonia salt. The specific preparation process comprises the steps of proportioning, controlling the molar ratio of methyl silanetriol to methanol and univalent or divalent metal alkali to be 1: (0.2-1): (0-1.2), the molar ratio of ammonium ions in the methyl silanetriol and the inorganic ammonia salt is 1: (0.8-1.2), then heating and preserving heat in a protective atmosphere, continuously stirring while heating and preserving heat, adjusting the pH value to be alkalescent after heat preservation is finished, and separating the upper layer in the product to obtain the main component.
In the structure of the main component, it is mainly the carbon-silicon chain structure thereof, i.e. [ CH ]2Si(OM1)2]nAnd (4) partial. The dispersing agent is usually mixed with ferrite powder before ball milling, and during ball milling, ferrite powder particles are cracked under the impact of steel balls to generate fresh surfaces, and OM formed by oxygen cooperating with hydrogen or monovalent or divalent metal is used1The radicals can produce a "sucker" like effect, adsorbing on the fresh surface newly produced by the ferrite powder, and OM1The groups are connected with a silicon-carbon chain structure, and the carbon-silicon chain structure can be used as a touch hand to pull away ferrite powder particles so as to realize isolation and separationFurther, an OM comprising oxygen and an amino compound is connected to one end of the silicon-carbon chain structure2Radical, OM2The radicals can also produce a "sucker" like effect to adsorb on the freshly produced fresh surface of the ferrite powder, while being pulled away by the silicon-carbon chain structure, passing through the OM1Radical and OM2The adsorption effect of the groups is combined with the silicon-carbon chain structure, so that the ferrite powder can be well separated and dispersed, and the agglomeration phenomenon caused by the mutual approach of the newly generated ferrite powder is effectively avoided.
Further, the length of the silicon carbon chain structure in the main component needs to be controlled, and when n < 2, the silicon carbon chain structure does not act as a "tentacle" to pull the ferrite powder apart, and when n > 9, the silicon carbon chain structure is too long, which easily entangles itself, causing agglomeration of the ferrite powder, and also failing to produce a good dispersing effect.
In terms of components, the main component of the dispersing agent reduces carbon elements by adding silicon elements, the silicon elements are not gasified during sintering, the generation of gas can be reduced, the defects of cavities, micro cracks and the like of products caused by gasification are avoided, and the addition of the silicon elements can also improve the mechanical property, the magnetic responsiveness, the biocompatibility and the like of the ferrite magnetic materials of the products to a certain extent.
As a preference, the first and second liquid crystal compositions are,
n in the molecular formula of the main component is 3-5;
m in the molecular formula of the main component1Is any one or more of hydrogen, sodium and potassium.
When n is 3 to 5, the chain length is moderate, so that a good dispersing effect can be achieved, the phenomena of entanglement of silicon-carbon chain structures and the like can be avoided, the silicon-carbon chain structures with the length can be effectively pulled out of the ferrite powder to achieve the dispersing effect, and the stability of the dispersing effect is ensured. The components such as hydrogen, sodium and potassium are easy to discharge, the magnetic performance of the ferrite magnetic material of the final product cannot be reduced, and the adsorption effect is excellent, so that the optimal technical effect can be produced by selecting any one or more of hydrogen, sodium and potassium.
As a preference, the first and second liquid crystal compositions are,
the dispersing agent also comprises an accessory ingredient;
the accessory ingredient is one or more of silicate, carbonate and borate of monovalent or divalent metal.
The auxiliary component is mainly soluble salt which can be dissociated into an ionic state after being matched with the main component to form the dispersing agent, so that the self dispersion of the main component can be promoted, and the main component is more uniform to generate a better dispersion effect.
As a preference, the first and second liquid crystal compositions are,
the content of the main component in the dispersing agent is 70-95 wt%;
the content of the auxiliary components in the dispersing agent is 5-30 wt%.
If the content of the main component is too low, the dispersion effect is poor, and if the content of the main component is low, the content of the accessory component is high, salts in the accessory component are easy to precipitate and impurities are generated; when the content of the subcomponent is less than 5% by weight, the effect of reinforcing the main component is hardly exerted. Within this component ratio range, the main component and the subcomponent can produce a good synergistic effect, thereby achieving good dispersion of the ferrite powder.
The application of a dispersing agent is disclosed,
the dispersing agent is used for preparing ferrite magnetic materials.
The dispersing agent can generate a particularly outstanding dispersing effect on the dispersion of ferrite powder, can realize uniform dispersion of the ferrite powder particularly in the process of ball milling of the ferrite powder, and improves the magnetic performance of the prepared ferrite magnetic material on the premise of not reducing the qualification rate of the ferrite magnetic material product.
As a preference, the first and second liquid crystal compositions are,
the concrete steps of the dispersant used for preparing the ferrite magnetic material comprise:
1) adding a dispersant into the ferrite powder to obtain a mixture;
2) performing wet ball milling on the mixture to obtain slurry after ball milling;
3) placing the slurry in a magnetic field, pumping water and pressing to form a blank;
4) and sintering the blank to obtain the ferrite magnetic material.
The steps for preparing the ferrite magnetic material by using the dispersing agent are simple and efficient, the ferrite magnetic material can be quickly prepared by mixing, ball milling, pressing and sintering, and in the sintering process, the problems that a large amount of gas generated by decomposition of the dispersing agent cannot be discharged, and a product generates micro cracks when a cavity is formed in a blank or the gas is discharged are solved.
As a preference, the first and second liquid crystal compositions are,
the dispersant added in the step 1) is 0.2-1.5 wt% of the total mass of the ferrite powder.
The good dispersing effect can be realized by adding a small amount of the dispersing agent, the material cost can be further saved, and the defect of the blank caused by gas generated in the sintering process can be avoided.
The invention has the beneficial effects that:
1) the good dispersion effect can be realized, and the agglomeration and caking of ferrite powder are avoided, so that the magnetic property of the ferrite magnetic material is improved;
2) excessive gas harmful to the structure of the ferrite magnetic material can be generated in the sintering process, and the qualification rate of the ferrite magnetic material is ensured;
3) the dosage is less, good dispersion effect can be produced, and material cost can be saved.
Detailed Description
The present invention will be described in further detail with reference to specific examples. Those skilled in the art will be able to implement the invention based on these teachings. Moreover, the embodiments of the present invention described in the following description are generally only some embodiments of the present invention, and not all embodiments. Therefore, all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Unless otherwise specified, the raw materials used in the examples of the present invention are all commercially available or available to those skilled in the art; unless otherwise specified, the methods used in the examples of the present invention are all those known to those skilled in the art.
Example 1
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol, sodium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 1.5, the molar ratio of sodium hydroxide to methyl silanetriol is 2: 1, and simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 120 ℃ under the protection of nitrogen, preserving heat for 20min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 3, i.e. chemical formula of H (CH)2Si(ONa)2)3CH2ONH4
Example 2
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol, sodium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 2.5, the molar ratio of sodium hydroxide to methyl silanetriol is 2: 1, and simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 120 ℃ under the protection of nitrogen, preserving heat for 20min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 5, i.e. chemical formula of H (CH)2Si(ONa)2)5CH2ONH4
Example 3
Synthesis of the dispersant principal Components
Placing methyl silanetriol, methanol, sodium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 1.5, the molar ratio of sodium hydroxide to methyl silanetriol is 2: 1, and simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 110 ℃ under the protection of nitrogen, preserving heat for 25min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 3, i.e. chemical formula of H (CH)2Si(ONa)2)3CH2ONH4
Example 4
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol, magnesium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 1.5, the molar ratio of the magnesium hydroxide to the methyl silanetriol is 2: 1, and simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 120 ℃ under the protection of nitrogen, preserving heat for 20min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 3, i.e. chemical formula of H (CH)2SiO2Mg)3CH2ONH4
Example 5
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol, sodium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 1.5, the molar ratio of sodium hydroxide to methyl silanetriol is 2: 1, and simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 125 ℃ under the protection of nitrogen, preserving heat for 15min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 3, i.e. the product is obtainedThe chemical formula is H (CH)2Si(ONa)2)3CH2ONH4
Example 6
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol, potassium hydroxide and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: 1.5, the molar ratio of potassium hydroxide to methyl silanetriol is 2: 1, simultaneously controlling the molar ratio of ammonium sulfate to methyl silanetriol to be 0.5: 1, heating to 125 ℃ under the protection of nitrogen, preserving heat for 15min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 3, i.e. chemical formula of H (CH)2Si(OK)2)3CH2ONH4
Example 7
Synthesis of main components of the dispersant:
placing methyl silanetriol, methanol and ammonium chloride into a reaction kettle, and controlling the molar ratio of the methanol to the methyl silanetriol to be 1: and 5, simultaneously controlling the molar ratio of ammonium chloride to methyl silanetriol to be 1: 1, heating to 125 ℃ under the protection of nitrogen, preserving heat for 15min, continuously stirring the mixed solution in the reaction kettle during the heating and heat preservation periods, discharging and collecting the solution in the reaction kettle after the heat preservation is finished, adjusting the pH value of the solution to be within the range of 7-8, and separating and collecting the upper white emulsion to obtain a main component;
the obtained main component has n of 9, i.e. chemical formula of H (CH)2Si(OH)2)3CH2ONH4
In summary, the main components of the dispersants prepared in examples 1 to 7 are shown in Table 1 below.
TABLE 1 main components of dispersants obtained in examples 1 to 7.
Example numbering n M1 M2
Example 1 3 Na+ NH4 +
Example 2 5 Na+ NH4 +
Example 3 3 Na+ NH4 +
Example 4 3 Mg2+ NH4 +
Example 5 3 Na+ NH4 +
Examples6 3 K+ NH4 +
Example 7 9 H+ NH4 +
Example 8
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 1, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 0.2 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.85 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4245Gs, coercive force Hcj3792.7Oe, maximum magnetic energy product (BH)max4.425MGOe and the yield reaches 88.5 percent.
Example 9
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 2, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 0.2 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.83 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4265Gs, coercive force Hcj3893.0Oe, maximum magnetic energy product (BH)max4.490MGOe and the yield reaches 86.7%.
Example 10
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 3, the main component and the auxiliary component are respectively 80 wt% and 20 wt% in the dispersing agent, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 0.2 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.92 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4208Gs, coercive force Hcj3752.5Oe, maximum magnetic energy product (BH)max4.310MGOe, and the yield reaches 88.9%.
Example 11
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 4, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 0.2 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.85 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4238Gs, coercive force Hcj3852.5Oe, maximum magnetic energy product (BH)max4.410MGOe, and the yield reaches 88.6%.
Example 12
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 5, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 1.0 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.80 μm;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4275Gs, coercive force Hcj3992.5Oe, maximum magnetic energy product (BH)max4.615MGOe, and the yield reaches 88.1%.
Example 13
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 6, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 1.5 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.81 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4270Gs, coercive force Hcj3965.0Oe, maximum magnetic energy product (BH)max4.560MGOe and the yield reaches 87.9%.
Example 14
Preparing the main component of the prepared dispersant into the dispersant, and preparing the dispersant for the ferrite magnetic material:
1) mixing a main component and an auxiliary component to prepare a dispersing agent, wherein the main component is prepared in example 7, the dispersing agent comprises 95 wt% of the main component and 5 wt% of the auxiliary component according to the mass ratio, the prepared dispersing agent is mixed with ferrite powder, and the addition amount of the dispersing agent is 0.2 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.86 μm;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4242Gs, coercive force Hcj3788.9Oe, maximum magnetic energy product (BH)max4.413MGOe, and the yield reaches 88.7%.
Comparative example 1
Preparing a ferrite magnetic material:
1) directly placing ferrite powder in a ball milling tank for wet ball milling for 20h to obtain slurry, and taking a small amount of slurry to only test the particle size;
2) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
3) sintering the blank to obtain a ferrite magnetic material;
4) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 1.15 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4170Gs, coercive force Hcj3612.0Oe, maximum magnetic energy product (BH)max4.060MGOe, and a yield of 88.9%.
Comparative example 2
Preparing a ferrite magnetic material:
1) mixing a dispersing agent and ferrite powder by taking calcium gluconate as the dispersing agent, wherein the addition amount of the dispersing agent is 1.0 wt% of the total mass of the ferrite powder to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.81 mu m;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr4270Gs, coercive force Hcj3897.0Oe, maximum magnetic energy product (BH)max4.760MGOe, and the yield is only 68.9%.
Comparative example 3
Preparing a ferrite magnetic material:
1) mixing a dispersing agent and ferrite powder by taking sodium hexametaphosphate as the dispersing agent, wherein the addition amount of the dispersing agent is 1.0 wt% of the total mass of the ferrite powder, so as to obtain a mixture;
2) placing the mixture in a ball milling tank for ball milling for 20 hours by a wet method, obtaining slurry after ball milling, and taking a small amount of slurry to only test the particle size;
3) placing the slurry in a magnetic field, and pumping water to perform compression molding to obtain a blank;
4) sintering the blank to obtain a ferrite magnetic material;
5) and (4) carrying out magnetic performance test and yield analysis on the ferrite magnetic material obtained by sintering.
After testing and analysis, the following results were obtained:
the median particle size (D50) of the slurry in the step 2) is 0.88 μm;
the remanence B of the ferrite magnetic material prepared in the step 4) is detectedr3897Gs, coercivity Hcj3502.3Oe, maximum magnetic energy product (BH)max3.976MGOe, and a yield of 88.5%.
The results of comparison with comparative examples 1 to 3 in combination with examples 8 to 14 are shown in Table 2 below.
Table 2 comparison of the indexes.
Figure GDA0002540621270000111
Figure GDA0002540621270000121
From the above results, it is obvious that the dispersant of the present invention, when used for preparing ferrite magnetic materials, can not only reduce the particle size of the powder and improve the magnetic properties, but also ensure the yield, and has excellent technical effects.

Claims (5)

1. A dispersant is characterized in that the dispersant is a mixture of,
the dispersant comprises a main component;
the molecular formula of the main component is shown as the following formula 1:
formula 1:
Figure FDA0002540621260000011
in formula 1: n is more than or equal to 2 and less than or equal to 9, M1Is hydrogen or a mono-or divalent metal, M2Is an amino compound;
the dispersing agent also comprises an accessory ingredient;
the accessory ingredient is one or more of silicate, carbonate and borate of monovalent or divalent metal;
the content of the main component in the dispersing agent is 70-95 wt%;
the content of the auxiliary components in the dispersing agent is 5-30 wt%.
2. A dispersant according to claim 1,
n in the molecular formula of the main component is 3-5;
m in the molecular formula of the main component1Is any one or more of hydrogen, sodium and potassium.
3. Use of a dispersant as claimed in claim 1 or 2,
the dispersing agent is used for preparing ferrite magnetic materials.
4. Use of a dispersant according to claim 3,
the concrete steps of the dispersant used for preparing the ferrite magnetic material comprise:
1) adding a dispersant into the ferrite powder to obtain a mixture;
2) performing wet ball milling on the mixture to obtain slurry after ball milling;
3) placing the slurry in a magnetic field, pumping water and pressing to form a blank;
4) and sintering the blank to obtain the ferrite magnetic material.
5. Use of a dispersant according to claim 4,
the dispersant added in the step 1) is 0.2-1.5 wt% of the total mass of the ferrite powder.
CN201910654846.XA 2019-07-19 2019-07-19 Dispersing agent and application thereof Active CN110317068B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910654846.XA CN110317068B (en) 2019-07-19 2019-07-19 Dispersing agent and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910654846.XA CN110317068B (en) 2019-07-19 2019-07-19 Dispersing agent and application thereof

Publications (2)

Publication Number Publication Date
CN110317068A CN110317068A (en) 2019-10-11
CN110317068B true CN110317068B (en) 2020-10-23

Family

ID=68124020

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910654846.XA Active CN110317068B (en) 2019-07-19 2019-07-19 Dispersing agent and application thereof

Country Status (1)

Country Link
CN (1) CN110317068B (en)

Family Cites Families (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5342430A (en) * 1993-07-28 1994-08-30 Grocela Kathe Teresa A Passivation of methylchlorosilane fines
KR100600630B1 (en) * 1998-04-24 2006-07-13 쇼쿠바이가세고교 가부시키가이샤 Coating liquid for forming a silica-based film having low dielectric constant and substrate having film of low dielectric constant coated thereon
ATE394437T1 (en) * 1998-12-11 2008-05-15 Henkel Kgaa USE OF DISPERSIONS OF SILYL-TERMINATED POLYMERS AS SEALANTS
SG101990A1 (en) * 2000-08-11 2004-02-27 Nippon Catalytic Chem Ind Cement dispersant and cement composition comprising this
US6949604B2 (en) * 2001-06-29 2005-09-27 Brown University Polyurethane ionomer blends and methods for their preparation and formation
EP2546308B1 (en) * 2004-11-10 2014-07-16 Kaneka Corporation Curable composition
WO2006124264A1 (en) * 2005-05-12 2006-11-23 Lubrizol Limited Dispersants and compositions thereof
WO2007102911A2 (en) * 2005-12-15 2007-09-13 Lubrizol Limited Novel dispersant and compositions thereof
CN100482743C (en) * 2006-11-30 2009-04-29 许富安 Preparation process of polymer powder capable of redispersing with improved water risisting viscosity and application thereof
CN104446519B (en) * 2014-12-16 2016-08-24 湖南航天磁电有限责任公司 A kind of dispersant improving permanent-magnet ferrite magnetic property and method

Also Published As

Publication number Publication date
CN110317068A (en) 2019-10-11

Similar Documents

Publication Publication Date Title
CN102050619B (en) Method for preparing permanent magnet oxysome material
CN112679207B (en) Permanent magnetic ferrite material and preparation method thereof
CN104609859B (en) Introduce from climing combustion the method that sintering of nano-material auxiliary agent low-temperature sintering is prepared 0-3 magnetoelectric ceramic
CN101205137A (en) Method for manufacturing dry-pressing formed sintered permanent ferrite
US11767432B2 (en) Method for mechanochemical preparation of high-performance iron red/clay mineral hybrid pigment
CN108774005B (en) Vitreous additive, preparation method and application in preparation of ferrite permanent magnet material
CN110156452B (en) M-type strontium ferrite and preparation method thereof
CN102249658A (en) Rare earth permanent ferrite material and preparation method thereof
CN115312283B (en) High-compaction-density injection magnetic powder and preparation method thereof
CN111704452A (en) Permanent magnetic ferrite material and preparation method thereof
JP2005505944A (en) Economical and improved properties of ferrite-type magnets
CN110317068B (en) Dispersing agent and application thereof
CN111362686A (en) Hexagonal magnetoplumbite permanent magnetic ferrite material and preparation method thereof
CN108285348B (en) Method for manufacturing magnetic powder for dry-pressed anisotropic permanent magnet ferrite
CN105732017B (en) A kind of additive and method improving permanent-magnet ferrite magnetic property
CN102129906B (en) Permanent ferrite material additive and preparation method and application thereof
CN110330326A (en) A kind of multielement permanent-magnet ferrite and its preparation method and application
JP2007123511A (en) Ferrite sintered magnet
CN114907130A (en) Additive for preparing permanent magnetic strontium ferrite material and application thereof
WO2005073147A1 (en) Method for producing ferrite sintered compact
CN105236950A (en) High-performance strontium permanent magnetic ferrite preparation method
CN106024238A (en) Gadolinium/yttrium-ion-implanted zinc-plated neodymium-iron-boron magnet and preparation method thereof
CN111196720A (en) Improved high-performance strontium ferrite for magnetic ring and preparation method thereof
TWI691471B (en) Method of fabricating modified ferrite magnetic powder and ferrite magnet
CN113200741B (en) 5g applied low-loss soft magnetic ferrite material and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
PE01 Entry into force of the registration of the contract for pledge of patent right

Denomination of invention: A dispersant and its application

Effective date of registration: 20220621

Granted publication date: 20201023

Pledgee: Dongyang Branch of China Construction Bank Co.,Ltd.

Pledgor: HENGDIAN GROUP DMEGC MAGNETICS Co.,Ltd.

Registration number: Y2022330001027

PE01 Entry into force of the registration of the contract for pledge of patent right