CN111892831A - Composite powder for electronic adhesive and preparation method and application thereof - Google Patents

Composite powder for electronic adhesive and preparation method and application thereof Download PDF

Info

Publication number
CN111892831A
CN111892831A CN202010786662.1A CN202010786662A CN111892831A CN 111892831 A CN111892831 A CN 111892831A CN 202010786662 A CN202010786662 A CN 202010786662A CN 111892831 A CN111892831 A CN 111892831A
Authority
CN
China
Prior art keywords
powder
wollastonite
needle
grinding
magnesium hydroxide
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.)
Pending
Application number
CN202010786662.1A
Other languages
Chinese (zh)
Inventor
温声平
宋建强
李海滨
邹检生
彭鹤松
吴维冰
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.)
Jiangxi Guangyuan Chemical Co Ltd
Original Assignee
Jiangxi Guangyuan Chemical 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 Jiangxi Guangyuan Chemical Co Ltd filed Critical Jiangxi Guangyuan Chemical Co Ltd
Priority to CN202010786662.1A priority Critical patent/CN111892831A/en
Publication of CN111892831A publication Critical patent/CN111892831A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/28—Compounds of silicon
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02—Compounds of alkaline earth metals or magnesium
    • C09C1/028—Compounds containing only magnesium as metal
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • C09C3/041—Grinding
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06—Treatment with inorganic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT 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
    • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/19—Oil-absorption capacity, e.g. DBP values
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/32—Thermal properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a composite powder for electronic adhesive, a preparation method and application thereof, and relates to the technical field of fillers for electronic adhesive. The invention provides a preparation method of composite powder for electronic adhesive, which comprises the following steps: mixing the needle-shaped wollastonite coarse powder with a grinding aid, grinding by a dry method, then mixing with a dispersing agent and water to prepare slurry, and grinding, drying, depolymerizing and breaking up by a wet method to obtain needle-shaped wollastonite ultrafine powder; mixing brucite and grinding aid, grinding by dry method, and grading to obtain magnesium hydroxide ultrafine powder; and carrying out mechanochemical compounding on the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder, and then adding a modifier for surface modification to obtain the composite powder for the electronic adhesive. The needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder prepared by the invention have small particle size and narrow particle size distribution, and the obtained composite powder for the electronic adhesive has excellent fluidity, dispersibility, insulativity, thermal conductivity, bonding strength, flame retardant property and compatibility with resin.

Description

Composite powder for electronic adhesive and preparation method and application thereof
Technical Field
The invention relates to the technical field of fillers for electronic adhesives, in particular to a composite powder for electronic adhesives and a preparation method and application thereof.
Background
With the rapid development of science and technology, the requirements of people on the quality of electronic products are continuously improved, the electronic products are updated more and more quickly, the requirements on the performance of materials are higher and higher, the smart phone is in the 5G era, various manufacturers further pursue the reliability and the light weight and the thinness of the smart phone, the configuration change of the 5G smart phone mainly comprises a processor, a radio frequency front end, an antenna, a camera, materials and other devices, and the requirements on the assembly and bonding schemes of the smart phone are severer. The 5G mobile phone is a new generation of high-tech product, the performance of the mobile phone is greatly improved once, and the upgrading of the processor, the 5G baseband and the high-speed flash charging become high heat sources in a narrow space of the mobile phone.
The portability of 5G mobile phones requires that the mobile phones must be light in weight, and the combination of the internal high-heat-generation components and the whole heat dissipation system cannot be separated from the bonding and encapsulation of electronic glue. As communication equipment which is almost never separated, if a fire and an explosion are caused by heating, the health and the safety of people are seriously harmed, and the electronic adhesive for the mobile phone is required to have good insulativity, thermal conductivity, bonding strength and flame retardant property. At present, common powder materials for mobile phone electronic glue are magnesium hydroxide and silicon dioxide, but the powder materials cannot simultaneously meet the requirements of electronic glue in 5G communication equipment on insulativity, thermal conductivity, bonding strength and flame retardance.
Disclosure of Invention
In view of this, the present invention provides a composite powder for electronic glue, and a preparation method and an application thereof. The composite powder for the electronic adhesive, which is prepared by the preparation method provided by the invention, has excellent insulativity, thermal conductivity, bonding strength and flame retardant property and excellent compatibility with resin.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of composite powder for electronic adhesive, which comprises the following steps:
(1) mixing the needle-shaped wollastonite coarse powder with a first grinding aid, and carrying out first dry grinding to obtain needle-shaped wollastonite fine powder;
mixing the needle-shaped wollastonite fine powder, a dispersing agent and water into slurry to obtain wollastonite slurry;
sequentially carrying out wet grinding, drying and depolymerization on the wollastonite slurry to break up the wollastonite slurry to obtain needle-shaped wollastonite ultrafine powder;
(2) mixing the brucite coarse powder with a second grinding aid, carrying out second dry grinding, and then grading to obtain magnesium hydroxide ultrafine powder;
(3) carrying out mechanochemical compounding on the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder, and then adding a modifier for surface modification to obtain composite powder for the electronic adhesive;
the step (1) and the step (2) have no chronological order.
Preferably, in step (1), the first grinding aid comprises sodium polyacrylate, sodium stearate or sodium dodecyl sulfate; the mass of the first grinding aid is 0.5-1% of that of the needle-shaped wollastonite coarse powder;
the particle size of the needle-shaped wollastonite fine powder is 400-600 meshes.
Preferably, in the step (1), the dispersing agent comprises polyethylene glycol fatty acid sodium and/or sodium polyacrylate; the mass of the dispersing agent is 0.4-0.7% of that of the needle-shaped wollastonite fine powder;
the solid content of the wollastonite paste is 60-65%.
Preferably, in the step (1), the wet grinding temperature is 80-85 ℃, and the time is 1-3 h;
the particle size of the needle-shaped wollastonite ultrafine powder is 4000-4500 meshes.
Preferably, in the step (2), the particle size of the brucite coarse powder is 5-10 mm;
the second grinding aid comprises sodium polyacrylate, sodium hexametaphosphate or ammonium polyacrylate; the mass of the second grinding aid is 0.5-1% of the mass of the brucite coarse powder;
the particle size of the magnesium hydroxide ultrafine powder is 4000-4500 meshes.
Preferably, in the step (3), the mass ratio of the needle-shaped wollastonite micropowder to the magnesium hydroxide micropowder is 1: (2-4);
the modifier comprises one or more of disodium sulfosuccinate, potassium monododecyl phosphate and fatty alcohol-polyoxyethylene ether ammonium sulfate;
the mass of the modifier is 0.5-1% of the sum of the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder.
Preferably, in the step (3), the mechanochemical composition is carried out under the condition of high-speed stirring, the rotating speed of the high-speed stirring is 2500-4000 r/min, and the time is 0.5-1 h;
the temperature of the surface modification is 100-140 ℃, and the time is 0.3-0.6 h.
The invention provides composite powder for electronic adhesive, which is prepared by the preparation method in the technical scheme and comprises needle-shaped modified wollastonite ultrafine powder and modified magnesium hydroxide ultrafine powder.
Preferably, the mass ratio of the needle-shaped modified wollastonite micropowder to the modified magnesium hydroxide micropowder is 1: (2-4).
The invention also provides application of the composite powder for the electronic adhesive in the technical scheme in preparation of the electronic adhesive for 5G communication equipment.
The invention provides a preparation method of composite powder for electronic adhesive, which comprises the following steps: (1) mixing the needle-shaped wollastonite coarse powder with a first grinding aid, and carrying out first dry grinding to obtain needle-shaped wollastonite fine powder; mixing the needle-shaped wollastonite fine powder, a dispersing agent and water into slurry to obtain wollastonite slurry; sequentially carrying out wet grinding, drying and depolymerization on the wollastonite slurry to break up the wollastonite slurry to obtain needle-shaped wollastonite ultrafine powder; (2) mixing the brucite coarse powder with a second grinding aid, carrying out second dry grinding, and then grading to obtain magnesium hydroxide ultrafine powder; (3) carrying out mechanochemical compounding on the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder, and then adding a modifier for surface modification to obtain composite powder for the electronic adhesive; the step (1) and the step (2) have no chronological order. According to the invention, needle-shaped wollastonite and a grinding aid are ground in a dry method, a dispersing agent is added for wet grinding, and the particle size of wollastonite is reduced and wollastonite powder is effectively dispersed through a depolymerization and scattering process after drying; the particle size of the magnesium hydroxide ultrafine powder is reduced by carrying out dry grinding and grading on brucite and a grinding aid; wollastonite has the functions of heat conduction, insulation, reinforcement and improvement of precipitation of spherical filler, and has good fluidity, but the flame retardance is not enough, magnesium hydroxide can resist flame, but the bonding strength is not enough, and the thixotropy is good and the fluidity is not good; through surface modification, the activation degree of the composite powder can be improved, the oil absorption value of the composite powder is reduced, the dispersibility and the fluidity are improved, and the compatibility with resin is further improved; meanwhile, the needle-shaped wollastonite ultrafine powder has excellent heat conduction and insulation properties, so that the heat conduction and insulation properties of the electronic adhesive can be obviously improved, and the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder have synergistic effect, so that the flame retardant property of the electronic adhesive can be improved; the compatibility of the modified composite powder filler for the electronic adhesive and resin is greatly improved, and the bonding strength of the composite powder filler for the electronic adhesive is improved. Moreover, the preparation method provided by the invention is simple to operate and suitable for industrial production.
As shown in the test results of the examples, the composite material for the electronic adhesive prepared by the inventionThe whiteness of the powder is more than 93.2, the oil absorption is less than 30mL/100g, and the particle diameter D501.73 to 1.82 μm, D973.12 to 3.58 μm, and a BET specific surface area of 12.29 to 13.45m2(ii)/g, the degree of activation was 93.8% or more, the water content was 0.3% or less, and Fe was not detected2O3、Mn2+、Cr6+、Pb2+And Cd2+Good dispersibility, adhesive strength of 8.5-11.3 MPa, adhesive strength of 19.6-24.5 MPa, thermal conductivity of 0.8-1.2W/m.k, and insulation of 1.03-1.21 kOmega/cm3The flame retardance is 36-48. The composite powder for the electronic adhesive prepared by the embodiment of the invention has the advantages of high glossiness, low oil absorption, low moisture content, high activation degree, extremely low metal content, good dispersibility, resin compatibility, bonding strength, heat conductivity, insulating property and flame retardant property, can meet the strict requirements of the electronic adhesive on heat conductivity, insulation and flame retardant in 5G communication equipment, improves the additional values of wollastonite powder and magnesium hydroxide products, and widens the application field of the electronic adhesive.
Drawings
FIG. 1 is an optical microscope photograph of needle-like wollastonite micropowder prepared in example 4, magnified 500 times;
FIG. 2 is an optical microscope photograph at 900 times magnification of magnesium hydroxide micropowder prepared in example 4;
FIG. 3 is an optical microscope photograph of 1600 times magnification of the composite powder for electronic glue prepared in example 4.
Detailed Description
The invention provides a preparation method of composite powder for electronic adhesive, which comprises the following steps:
(1) mixing the needle-shaped wollastonite coarse powder with a first grinding aid, and carrying out first dry grinding to obtain needle-shaped wollastonite fine powder;
mixing the needle-shaped wollastonite fine powder, a dispersing agent and water into slurry to obtain wollastonite slurry;
sequentially carrying out wet grinding, drying and depolymerization on the wollastonite slurry to break up the wollastonite slurry to obtain needle-shaped wollastonite ultrafine powder;
(2) mixing the brucite coarse powder with a second grinding aid, carrying out second dry grinding, and then grading to obtain magnesium hydroxide ultrafine powder;
(3) carrying out mechanochemical compounding on the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder, and then adding a modifier for surface modification to obtain composite powder for the electronic adhesive;
the step (1) and the step (2) have no chronological order.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
The needle-shaped wollastonite coarse powder and a first grinding aid are mixed and ground by a first dry method to obtain needle-shaped wollastonite fine powder.
In the present invention, the coarse powder of needle-like wollastonite is preferably obtained by washing, drying, screening and coarsely crushing raw needle-like wollastonite ore in this order. In the invention, the whiteness of the needle-shaped wollastonite raw ore is preferably 91.0-93.0, and the purity of the needle-shaped wollastonite raw ore is preferably 95-97%. The frequency of the water washing is not particularly limited, and the dust on the surface of the needle-shaped wollastonite raw ore can be cleaned. In the present invention, the drying manner is preferably air drying. The screening method is not particularly limited, and black blocky impurities can be removed completely. In the present invention, the crushing preferably includes coarse crushing and secondary crushing performed in this order. The mode of the coarse crushing and the secondary crushing is not particularly limited, and the crushing mode known by the technicians in the field can be adopted; in an embodiment of the invention, the crushing is preferably jaw crushing. In the invention, the particle size of the crushed wollastonite particles obtained by coarse crushing is preferably 5-7 cm, more preferably 5.5-6.5 cm, and most preferably 6 cm. In the invention, the particle size of the wollastonite coarse powder is preferably 5 to 10mm, more preferably 6 to 9mm, and most preferably 7 to 8 mm.
In the present invention, the first grinding aid preferably includes sodium polyacrylate, sodium stearate, or sodium lauryl sulfate; the mass of the first grinding aid is preferably 0.5 to 1%, more preferably 0.7 to 0.9%, and most preferably 0.8% of the mass of the wollastonite coarse powder. In the invention, the first grinding aid has the functions of improving grinding efficiency and reducing equipment abrasion.
In the present invention, the mixing is preferably stirring mixing, and the speed and time of the stirring mixing are not particularly limited in the present invention, and the raw materials may be uniformly mixed.
The first dry grinding method is not particularly limited in the present invention, and a dry grinding method known to those skilled in the art may be used.
After the first dry grinding, the invention preferably further comprises sieving and grading the coarse material obtained by the first dry grinding to obtain wollastonite coarse powder. The operation of the sieving and classifying in the present invention is not particularly limited, and the operation of the sieving and classifying known to those skilled in the art may be employed. In the present invention, the particle size of the needle-like wollastonite fine powder is preferably 400 to 600 mesh, more preferably 450 to 550 mesh, and most preferably 500 mesh.
According to the invention, the needle-shaped wollastonite coarse powder is ground to 400-600 meshes by a dry method, so that slurry preparation and wet grinding are facilitated, and the condition that the needle-shaped structure of the wollastonite is damaged due to direct dry grinding of the wollastonite to 4000-4500 meshes can be avoided.
After the needle-shaped wollastonite fine powder is obtained, the needle-shaped wollastonite fine powder, a dispersing agent and water are mixed into slurry to obtain the wollastonite slurry.
In the present invention, the dispersant preferably includes sodium polyethylene glycol fatty acid and/or sodium polyacrylate, more preferably sodium polyethylene glycol fatty acid and sodium polyacrylate; the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate is preferably 1: (3-5), more preferably 1: (3.5-4.5), and most preferably 1: 4. In the present invention, the mass of the dispersing agent is preferably 0.4 to 0.8%, more preferably 0.6 to 0.7% of the mass of the needle-like wollastonite fine powder. In the present invention, the dispersant functions as: the rheological property of the wollastonite slurry is improved, the viscosity of the wollastonite slurry is reduced, and the dispersion stability of wollastonite particles is improved; the impact of the grinding medium on wollastonite particles is improved, the grinding effect is improved, the grinding efficiency is improved, and the grinding cost is reduced; the stability of the wollastonite paste is improved, and wollastonite particles are prevented from flocculating.
The amount of the water is not particularly limited, and the solid content of the wollastonite paste can be 60-65%, and the solid content of the wollastonite paste is more preferably 61-64%, and even more preferably 62-63%.
After wollastonite slurry is obtained, the wollastonite slurry is sequentially subjected to wet grinding, drying, depolymerization and disintegration to obtain needle-shaped wollastonite ultrafine powder.
In the invention, the grinding balls adopted in the wet grinding are preferably zirconia beads; the Mohs hardness of the zirconia beads is preferably 8; the diameter of the zirconia beads is preferably 4-6 mm, more preferably 4.5-5.5 mm, and most preferably 5 mm. In the present invention, the filling rate of the zirconia beads is preferably 20 to 35%, more preferably 20 to 30%, and most preferably 25 to 30%. In the invention, the wet grinding temperature is preferably 80-85 ℃, more preferably 81-84 ℃, and most preferably 82-83 ℃; the time is preferably 1 to 3 hours, more preferably 1.5 to 2.5 hours, and most preferably 2 hours. In the present invention, the wet grinding is preferably performed in a vertical stirring mill.
In the present invention, the drying is preferably performed by flash drying; the temperature of the hot air for flash drying is preferably 180-200 ℃, more preferably 185-195 ℃, and most preferably 200 ℃; the time for flash evaporation drying is preferably 0.3-0.6 h, more preferably 0.3-0.5 h, and most preferably 0.4-0.5 h.
In the invention, the depolymerization and scattering are preferably carried out in a depolymerization and scattering machine, and the dried powder is preferably conveyed to the depolymerization and scattering machine through a screw reamer feeder; the rotating speed of the depolymerization beater is preferably 2000-2500 r/min, more preferably 2100-2400 r/min, and most preferably 2200-2300 r/min; the time for depolymerization and scattering is preferably 15-25 min, more preferably 18-22 min, and most preferably 20 min. The invention can destroy the agglomeration generated by the needle-shaped wollastonite ultrafine powder in the drying process through depolymerization and scattering.
In the invention, the particle size of the needle-shaped wollastonite ultrafine powder is preferably 4000-4500 meshes, more preferably 4100-4400 meshes, and most preferably 4200-4300 meshes. In the invention, the particle size of the needle-shaped wollastonite ultrafine powder is preferably 0.21 to 0.25 μm, and more preferably 0.20 to 0.23 μm. The needle-shaped wollastonite ultrafine powder prepared by the method has small granularity, narrow particle size distribution and good dispersibility.
The brucite coarse powder and a second grinding aid are mixed, ground by a second dry method and classified to obtain the magnesium hydroxide ultrafine powder.
In the invention, the brucite coarse powder is preferably obtained by sequentially washing, drying, screening and crushing brucite. In the invention, the purity of the brucite is preferably equal to or more than 90%, and more preferably 91-92%. The invention has no special limit on the washing times, and can clean the dust on the brucite surface. In the present invention, the drying manner is preferably air drying. The screening method is not particularly limited, and black blocky impurities can be removed completely. The crushing mode is not particularly limited, and the crushing mode known to a person skilled in the art can be adopted; in particular, jaw crushing. In the present invention, the crushing preferably includes coarse crushing and secondary crushing in this order to obtain brucite coarse powder. In the invention, the particle size of the brucite crushed materials obtained by coarse crushing is preferably 5-7 cm, more preferably 5.5-6.5 cm, and most preferably 6 cm. In the invention, the particle size of the brucite coarse powder is preferably 5-10 mm, more preferably 6-9 mm, and most preferably 7-8 mm.
In the present invention, the second grinding aid preferably includes sodium polyacrylate, sodium hexametaphosphate, or ammonium polyacrylate; the mass of the second grinding aid is preferably 0.5 to 1%, more preferably 0.7 to 0.9%, and most preferably 0.8% of the mass of the brucite coarse powder. In the invention, the second grinding aid has the functions of improving grinding efficiency and reducing equipment abrasion.
In the present invention, the mixing is preferably stirring mixing, and the speed and time of the stirring mixing are not particularly limited in the present invention, and the raw materials may be uniformly mixed.
In the invention, the grinding medium adopted by the second dry grinding is preferably a ceramic-coated steel ball steel section; the Mohs hardness of the grinding medium is preferably 8-9; the diameter of the grinding medium is preferably 2-4 cm, more preferably 2.5-3.5 cm, and most preferably 4 cm. In the present invention, the filling rate of the grinding medium is preferably 25 to 45%, more preferably 30 to 40%, and most preferably 35 to 40%. In the present invention, the second dry grinding is preferably performed in a horizontal ceramic-lined ball mill. The invention adopts the ceramic lining ball mill, which can reduce the iron content in the magnesium hydroxide and prevent the reduction of whiteness in the grinding process.
In the invention, the particle size of the powder after the second dry grinding is preferably 800-1000 meshes, more preferably 850-950 meshes, and most preferably 900 meshes.
In the present invention, the classification includes primary classification and secondary classification which are performed in sequence; the granularity of the powder after primary classification is preferably 2000-2500 meshes, more preferably 2100-2400 meshes, and most preferably 2200-2300 meshes; the granularity of the powder material (namely the magnesium hydroxide ultrafine powder) after the secondary classification is preferably 4000-4500 meshes, more preferably 4100-4400 meshes, and most preferably 4200-4300 meshes. In the invention, the primary classification and the secondary classification are preferably carried out by using a classifier, the principle of the classifier is that the rotating speed corresponding to the fineness of 2000-2500 meshes is set by adjusting the rotating speed of a classification wheel, powder reaching the fineness can pass through the classification wheel, powder which cannot reach the fineness can enter a ball mill by wind power to be ground again until the particle size meets the requirement, and the classification is a continuous sieving process. In an embodiment of the invention, the grader is purchased from the Shenyang aircraft industry group.
In the present invention, the particle size distribution of the magnesium hydroxide micropowder is preferably 0.16 to 0.23 μm, and more preferably 0.16 to 0.20 μm. The magnesium hydroxide ultrafine powder prepared by crushing, dry grinding and grading has small particle size, narrow particle size distribution and high grinding efficiency and yield.
After needle-shaped wollastonite ultrafine powder and magnesium hydroxide ultrafine powder are obtained, the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder are subjected to mechanochemical compounding, and then a modifier is added for surface modification to obtain the composite powder for the electronic adhesive.
In the present invention, the mass ratio of the needle-like wollastonite micropowder to the magnesium hydroxide micropowder is preferably 1: (2-4), more preferably 1: (2.5-3.5), and most preferably 1: 3. In the invention, the mechanochemical compounding is preferably carried out under the condition of high-speed stirring, and the rotating speed of the high-speed stirring is preferably 2500-4000 r/min, more preferably 3000-3500 r/min; the time is preferably 0.5-1 h. In the present invention, the mechanochemical compounding is preferably carried out in a high-efficiency powder modifier. The needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder generate interparticle acting force through mechanochemical compounding, the agglomeration and overlapping of particles are reduced, the advantages and the disadvantages of the wollastonite and the magnesium hydroxide after compounding are complementary, and the fluidity and the dispersibility of the needle-shaped wollastonite and the magnesium hydroxide are obviously improved when the needle-shaped wollastonite and the magnesium hydroxide are applied to electronic glue; meanwhile, due to the excellent heat conduction and insulation properties of the wollastonite, the heat conduction and insulation properties of the electronic adhesive are improved, and in addition, the wollastonite synergistically acts to improve the flame retardant property of the magnesium hydroxide.
In the invention, the modifier comprises one or more of disodium sulfosuccinate, potassium monododecyl phosphate and fatty alcohol-polyoxyethylene ether ammonium sulfate. In the invention, when the modifier is a composite modifier, the type of the modifier in the composite modifier is not particularly limited, and any combination can be adopted; the invention has no special limit to the mass ratio of different modifiers, and the modifier can be used in any proportion; in the embodiment of the invention, the composite modifier preferably consists of disodium sulfosuccinate monoester, potassium monododecyl phosphate and fatty alcohol-polyoxyethylene ether ammonium sulfate, and the mass ratio of the disodium sulfosuccinate monoester, the potassium monododecyl phosphate and the fatty alcohol-polyoxyethylene ether ammonium sulfate in the composite modifier is preferably 3:2: 1. In the invention, the mass of the modifier is preferably 0.5-1%, more preferably 0.4-0.8%, and most preferably 0.5-0.6% of the sum of the masses of the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder.
In the invention, the temperature of the surface modification is preferably 100-140 ℃, more preferably 110-130 ℃, and most preferably 120-130 ℃; the time is preferably 0.3 to 0.6h, more preferably 0.3 to 0.5h, and most preferably 0.4 to 0.5 h. In the invention, in the surface modification process, the modifier is melted into a molten state by heating and stirring for heating, the surface of the powder is uniformly coated with the modifier by high-speed stirring, and the modifier and calcium ions and magnesium ions in the powder generate ionic bond action. The activation degree of the composite powder for the electronic adhesive can be improved through surface modification, the higher the activation degree is, the lower the oil absorption value is, the better the dispersibility and the fluidity are, and the stronger the compatibility with resin is.
After the surface modification, the invention preferably also comprises the step of collecting and packaging the modified composite powder to obtain the composite powder for the electronic adhesive. The present invention is not particularly limited to the collection and packaging, and the collection and packaging method known to those skilled in the art may be used.
The invention provides composite powder for electronic adhesive, which is prepared by the preparation method in the technical scheme and comprises needle-shaped modified wollastonite ultrafine powder and modified magnesium hydroxide ultrafine powder.
In the present invention, the ratio by mass of the needle-like modified wollastonite micropowder to the modified magnesium hydroxide micropowder is preferably 1: (2-4) more preferably 1: (2.5-3.5), and most preferably 1: 3.
In the composite powder for the electronic adhesive, the hydroxyl on the surface of the modified magnesium hydroxide ultrafine powder and the calcium in the needle-shaped modified wollastonite ultrafine powder interact with each other through van der Waals force, so that the modified magnesium hydroxide ultrafine powder is adsorbed on the surface of the needle-shaped modified wollastonite ultrafine powder.
The invention also provides application of the composite powder for the electronic adhesive in the technical scheme in preparation of the electronic adhesive for 5G communication equipment.
In the invention, the electronic glue preferably comprises the following preparation raw materials in parts by mass: 30-40 parts of composite powder for electronic adhesive, 30-35 parts of silicon dioxide, 9-11 parts of epoxy resin, 7-9 parts of phenolic resin, 4-6 parts of flame retardant, 1.3-1.7 parts of flame retardant additive and 0.4-0.6 part of accelerator.
The raw materials for preparing the electronic adhesive comprise, by mass, 30-40 parts of the composite powder for the electronic adhesive, preferably 32-38 parts, more preferably 34-36 parts, and most preferably 35 parts.
The composite powder for the electronic adhesive comprises, by mass, 30-35 parts of silicon dioxide, preferably 31-34 parts of silicon dioxide, and more preferably 32-33 parts of silicon dioxide.
The composite powder for the electronic adhesive comprises, by mass, 9-11 parts of epoxy resin, preferably 9.5-10.5 parts, and more preferably 10 parts. In the present invention, the epoxy resin is preferably a bisphenol a type epoxy resin.
The composite powder for the electronic adhesive comprises, by mass, 7-9 parts of phenolic resin, preferably 7.5-8.5 parts of phenolic resin, and more preferably 8 parts of phenolic resin.
The composite powder for the electronic adhesive comprises, by mass, 4-6 parts of a flame retardant, preferably 4.5-5.5 parts, and more preferably 5 parts. In the present invention, the flame retardant is preferably a brominated phenolic.
The composite powder for the electronic adhesive comprises, by mass, 1.3-1.7 parts of a flame retardant additive, preferably 1.4-1.6 parts, and more preferably 1.5 parts. In the present invention, the flame retardant aid preferably includes Sb2O3。
The composite powder for the electronic adhesive comprises, by mass, 0.4-0.6 part of an accelerator, preferably 0.45-0.55 part, and more preferably 0.5 part. In the present invention, the accelerator preferably includes methylimidazole, 2-methylimidazole.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Sequentially washing, airing and screening needle-shaped wollastonite raw ore to remove black blocky impurities, carrying out jaw crushing until the particle size is 5-7 cm, and carrying out secondary jaw crushing to obtain wollastonite coarse powder with the particle size of 5-10 mm;
mixing the wollastonite coarse powder with a first grinding aid, and carrying out first dry grinding to obtain needle-shaped wollastonite fine powder with the granularity of 600 meshes; wherein the mass of the first grinding aid is 0.5 percent of that of the wollastonite coarse powder;
mixing the needle-shaped wollastonite fine powder, polyethylene glycol sodium fatty acid, sodium polyacrylate and water into slurry to obtain wollastonite slurry with the solid content of 60 percent; wherein the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate is 1:3, and the mass of the dispersing agent is 0.4% of that of the needle-shaped wollastonite fine powder;
adding the wollastonite slurry into a vertical stirring mill, carrying out wet grinding for 1h at the temperature of 80 ℃, carrying out flash drying for 0.3h at the temperature of 180 ℃, and then conveying the wollastonite slurry to a depolymerization and scattering machine through a screw reamer feeder to depolymerize and scatter to obtain needle-shaped wollastonite ultrafine powder with the granularity of 4000 meshes; wherein, the grinding balls adopted in the wet grinding are zirconia beads with Mohs hardness of 8 and diameter of 4-6 mm, and the filling rate of the zirconia beads is 20%.
(2) Washing brucite with the purity of more than or equal to 90%, airing and screening to remove black block-shaped impurities in sequence, carrying out jaw crushing until the granularity is 5-7 cm, and carrying out secondary jaw crushing to obtain brucite coarse powder with the granularity of 5-10 mm;
mixing the brucite coarse powder with a second grinding aid, placing the mixture into a horizontal ceramic lining ball mill, grinding the mixture to 800-1000 meshes by a second dry method, and then carrying out primary classification and secondary classification to obtain magnesium hydroxide ultrafine powder with the granularity of 4000 meshes; wherein the mass of the second grinding aid is 0.5 percent of the mass of the brucite coarse powder; the grinding medium for the second dry grinding is a ceramic-coated steel ball rigid section with the Mohs hardness of 8-9 and the diameter of 2-4 cm, and the filling rate of the grinding medium is 25%.
(3) Conveying the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder into a high-efficiency powder modifying machine according to the mass ratio of 1:3, carrying out mechanochemical compounding for 0.5h under the condition of 3000r/min, then adding a compound modifying agent consisting of disodium sulfosuccinate monoester, potassium monododecyl phosphate and fatty alcohol-polyoxyethylene ether ammonium sulfate according to the mass ratio of 3:2:1, carrying out surface modification for 0.3h under the condition of 110 ℃, collecting and packaging to obtain the compound powder for the electronic adhesive; wherein the mass of the composite modifier is 0.6 percent of the sum of the mass of the needle-shaped wollastonite ultrafine powder and the mass of the magnesium hydroxide ultrafine powder.
Example 2
The composite powder for electronic glue was prepared according to the method of example 1, differing from example 1 in that, in step (1): the mass of the first grinding aid is 0.6 percent of that of the wollastonite coarse powder; the mass of the dispersing agent is 0.6 percent of that of wollastonite coarse powder, and the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate in the dispersing agent is 1: 4; the solid content of the wollastonite paste is 60 percent; the temperature of the wet grinding is 80 ℃, the time is 1.5h, and the filling rate of the zirconia beads is 25%.
In the step (2): the mass of the second grinding aid is 0.6 percent of the mass of the brucite coarse powder; the packing fraction of the grinding media was 25%.
In the step (3), the temperature of the surface modification is 115 ℃ and the time is 0.3 h.
Example 3
The composite powder for electronic glue was prepared according to the method of example 1, differing from example 1 in that, in step (1): the mass of the first grinding aid is 0.7 percent of that of the wollastonite coarse powder; the mass of the dispersing agent is 0.5 percent of that of wollastonite coarse powder, and the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate in the dispersing agent is 1: 5; the solid content of the wollastonite paste is 60 percent; the temperature of the wet grinding is 80 ℃, the time is 1.5h, and the filling rate of the zirconia beads is 25%.
In the step (2): the mass of the second grinding aid is 0.7 percent of the mass of the brucite coarse powder; the packing fraction of the grinding media was 30%.
In the step (3), the temperature of the surface modification is 120 ℃, and the time is 0.3 h.
Example 4
The composite powder for electronic glue was prepared according to the method of example 1, differing from example 1 in that, in step (1): the mass of the first grinding aid is 0.8 percent of that of the wollastonite coarse powder; the mass of the dispersing agent is 0.6 percent of that of wollastonite coarse powder, and the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate in the dispersing agent is 1: 4; the solid content of the wollastonite paste is 63 percent; the temperature of the wet grinding is 83 ℃, the time is 2.5h, and the filling rate of the zirconia beads is 28%.
In the step (2): the mass of the second grinding aid is 0.8 percent of the mass of the brucite coarse powder; the packing fraction of the grinding media was 37%.
In the step (3), the temperature of surface modification is 125 ℃, and the time is 0.35 h; the mass of the composite modifier is 0.8 percent of the sum of the mass of the needle-shaped wollastonite ultrafine powder and the mass of the magnesium hydroxide ultrafine powder.
An optical microscope image of the acicular wollastonite micropowder prepared in this example magnified 500 times is shown in FIG. 1. from FIG. 1, it is clear that the wollastonite powder retains a good acicular structure.
An optical microscopic image of the ultrafine magnesium hydroxide powder prepared in this example magnified 900 times is shown in FIG. 2, and it can be seen from FIG. 2 that particle size control of magnesium hydroxide is relatively concentrated.
An optical microscopic image of the composite powder for electronic adhesive prepared in this example magnified 1600 times is shown in FIG. 3, and it is understood from FIG. 3 that wollastonite and magnesium hydroxide are effectively compounded, and magnesium hydroxide powder having a small particle size is adsorbed around wollastonite powder.
Example 5
The composite powder for electronic glue was prepared according to the method of example 1, differing from example 1 in that, in step (1): the mass of the first grinding aid is 0.9 percent of that of the wollastonite coarse powder; the mass of the dispersing agent is 0.7 percent of that of wollastonite coarse powder, and the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate in the dispersing agent is 1: 4; the solid content of the wollastonite paste is 65 percent; the temperature of the wet grinding is 90 ℃, the time is 3.0h, and the filling rate of the zirconia beads is 40%.
In the step (2): the mass of the second grinding aid is 0.9 percent of the mass of the brucite coarse powder; the packing fraction of the grinding media was 40%.
In the step (3), the temperature of surface modification is 130 ℃, and the time is 0.4 h; the mass of the composite modifier is 0.8 percent of the sum of the mass of the needle-shaped wollastonite ultrafine powder and the mass of the magnesium hydroxide ultrafine powder.
Example 6
The composite powder for electronic glue was prepared according to the method of example 1, differing from example 1 in that, in step (1): the mass of the first grinding aid is 1.0 percent of that of the wollastonite coarse powder; the mass of the dispersing agent is 0.8 percent of that of wollastonite coarse powder, and the mass ratio of the polyethylene glycol fatty acid sodium to the sodium polyacrylate in the dispersing agent is 1: 5; the solid content of the wollastonite paste is 65 percent; the temperature of the wet grinding is 95 ℃, the time is 3.0h, and the filling rate of the zirconia beads is 35%.
In the step (2): the mass of the second grinding aid is 1.0 percent of the mass of the brucite coarse powder; the packing fraction of the grinding media was 45%.
In the step (3), the temperature of surface modification is 140 ℃ and the time is 0.4 h; the mass of the composite modifier is 0.8 percent of the sum of the mass of the needle-shaped wollastonite ultrafine powder and the mass of the magnesium hydroxide ultrafine powder.
The performance of the composite powder for electronic adhesive prepared in examples 1 to 6 was measured, and the results are shown in table 1:
TABLE 1 Performance test results of composite powder for electronic adhesive
Figure BDA0002622232630000131
Figure BDA0002622232630000141
As is clear from Table 1, the whiteness of the composite powder for electronic adhesive prepared by the invention is more than 93.2, the oil absorption is less than 30mL/100g, and the particle diameter D501.73 to 1.82 μm, D973.12 to 3.58 μm, and a BET specific surface area of 12.29 to 13.45m2(ii)/g, the degree of activation was 93.8% or more, the water content was 0.3% or less, and Fe was not detected2O3、Mn2+、Cr6+、Pb2+And Cd2+Good dispersibility, adhesive strength of 8.5-11.3 MPa, adhesive strength of 19.6-24.5 MPa, thermal conductivity of 0.8-1.2W/m.k, and insulation of 1.03-1.21 kOmega/cm3The flame retardance is 36-48. Illustrating, an electron prepared by an embodiment of the inventionThe composite powder for glue has high glossiness, low oil absorption, low moisture content, high activation degree, extremely low metal content, and good bonding strength, heat conductivity, insulating property and flame retardant property.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The preparation method of the composite powder for the electronic adhesive is characterized by comprising the following steps of:
(1) mixing the needle-shaped wollastonite coarse powder with a first grinding aid, and carrying out first dry grinding to obtain needle-shaped wollastonite fine powder;
mixing the needle-shaped wollastonite fine powder, a dispersing agent and water into slurry to obtain wollastonite slurry;
sequentially carrying out wet grinding, drying and depolymerization on the wollastonite slurry to break up the wollastonite slurry to obtain needle-shaped wollastonite ultrafine powder;
(2) mixing the brucite coarse powder with a second grinding aid, carrying out second dry grinding, and then grading to obtain magnesium hydroxide ultrafine powder;
(3) carrying out mechanochemical compounding on the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder, and then adding a modifier for surface modification to obtain composite powder for the electronic adhesive;
the step (1) and the step (2) have no chronological order.
2. The method according to claim 1, wherein in the step (1), the first grinding aid comprises sodium polyacrylate, sodium stearate or sodium dodecyl sulfate; the mass of the first grinding aid is 0.5-1% of that of the needle-shaped wollastonite coarse powder;
the particle size of the needle-shaped wollastonite fine powder is 400-600 meshes.
3. The preparation method according to claim 1, wherein in the step (1), the dispersant comprises polyethylene glycol sodium fatty acid and/or sodium polyacrylate; the mass of the dispersing agent is 0.4-0.7% of that of the needle-shaped wollastonite fine powder;
the solid content of the wollastonite paste is 60-65%.
4. The preparation method according to claim 1, wherein in the step (1), the temperature of the wet grinding is 80-85 ℃ and the time is 1-3 h;
the particle size of the needle-shaped wollastonite ultrafine powder is 4000-4500 meshes.
5. The preparation method according to claim 1, wherein in the step (2), the brucite coarse powder has a particle size of 5-10 mm;
the second grinding aid comprises sodium polyacrylate, sodium hexametaphosphate or ammonium polyacrylate; the mass of the second grinding aid is 0.5-1% of the mass of the brucite coarse powder;
the particle size of the magnesium hydroxide ultrafine powder is 4000-4500 meshes.
6. The preparation method according to claim 1, wherein in the step (3), the mass ratio of the needle-like wollastonite micropowder to the magnesium hydroxide micropowder is 1: (2-4);
the modifier comprises one or more of disodium sulfosuccinate, potassium monododecyl phosphate and fatty alcohol-polyoxyethylene ether ammonium sulfate;
the mass of the modifier is 0.5-1% of the sum of the needle-shaped wollastonite ultrafine powder and the magnesium hydroxide ultrafine powder.
7. The preparation method according to claim 1 or 6, wherein in the step (3), the mechanochemical composition is carried out under the condition of high-speed stirring, the rotating speed of the high-speed stirring is 2500-4000 r/min, and the time is 0.5-1 h;
the temperature of the surface modification is 100-140 ℃, and the time is 0.3-0.6 h.
8. The composite powder for electronic adhesive prepared by the preparation method of any one of claims 1 to 7 comprises needle-shaped modified wollastonite micropowder and modified magnesium hydroxide micropowder.
9. The composite powder for electronic adhesive according to claim 7, wherein the weight ratio of the needle-like modified wollastonite micropowder to the modified magnesium hydroxide micropowder is 1: (2-4).
10. The use of the composite powder for electronic adhesive according to any one of claims 8 to 9 in the preparation of electronic adhesive for 5G communication equipment.
CN202010786662.1A 2020-08-07 2020-08-07 Composite powder for electronic adhesive and preparation method and application thereof Pending CN111892831A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010786662.1A CN111892831A (en) 2020-08-07 2020-08-07 Composite powder for electronic adhesive and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202010786662.1A CN111892831A (en) 2020-08-07 2020-08-07 Composite powder for electronic adhesive and preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN111892831A true CN111892831A (en) 2020-11-06

Family

ID=73246033

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202010786662.1A Pending CN111892831A (en) 2020-08-07 2020-08-07 Composite powder for electronic adhesive and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN111892831A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113980490A (en) * 2021-11-16 2022-01-28 江西广源化工有限责任公司 Magnesium hydroxide with high specific surface area, and preparation method and application thereof
CN114481697A (en) * 2022-01-20 2022-05-13 江西广源化工有限责任公司 Brucite composite material and preparation method and application thereof
CN114539812A (en) * 2022-03-02 2022-05-27 江西广源新材料有限公司 Inorganic powder, preparation method thereof and reinforced and toughened polypropylene modified master batch
CN114957795A (en) * 2022-06-16 2022-08-30 江西广源化工有限责任公司 Composite filler and preparation method thereof, and fluororubber composite material and preparation method thereof
CN115010994A (en) * 2022-05-13 2022-09-06 江西广源化工有限责任公司 Modified superfine wollastonite powder and its prepn and application
CN115386140A (en) * 2022-09-01 2022-11-25 江西广源化工有限责任公司 Nano flaky kaolin-wollastonite-hydroxy silicone oil ternary composite powder and preparation method and application thereof
CN116444858A (en) * 2023-03-29 2023-07-18 江西广源化工有限责任公司 Wollastonite/magnesium hydroxide composite inorganic flame retardant and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829912A (en) * 2015-04-21 2015-08-12 蚌埠天光传感器有限公司 Low odor flame retardant silane crosslinked polyethylene cable material and producing method thereof
CN104892980A (en) * 2015-06-05 2015-09-09 葫芦岛首创科技有限公司 Preparation method of nano-CaCO3-coated brucite composite material
CN106397749A (en) * 2016-08-31 2017-02-15 荣盛石化股份有限公司 Synthesis method of high strength and high modulus polyester
CN109651849A (en) * 2018-12-20 2019-04-19 江西广源化工有限责任公司 A kind of preparation method of flame-retardant cable wollastonite surface cladded aluminium hydroxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104829912A (en) * 2015-04-21 2015-08-12 蚌埠天光传感器有限公司 Low odor flame retardant silane crosslinked polyethylene cable material and producing method thereof
CN104892980A (en) * 2015-06-05 2015-09-09 葫芦岛首创科技有限公司 Preparation method of nano-CaCO3-coated brucite composite material
CN106397749A (en) * 2016-08-31 2017-02-15 荣盛石化股份有限公司 Synthesis method of high strength and high modulus polyester
CN109651849A (en) * 2018-12-20 2019-04-19 江西广源化工有限责任公司 A kind of preparation method of flame-retardant cable wollastonite surface cladded aluminium hydroxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曾金波，等: "硅灰石、微囊化红磷/天然水镁石复配阻燃聚丙烯的制备与性能", 《浙江化工》 *

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113980490A (en) * 2021-11-16 2022-01-28 江西广源化工有限责任公司 Magnesium hydroxide with high specific surface area, and preparation method and application thereof
CN114481697A (en) * 2022-01-20 2022-05-13 江西广源化工有限责任公司 Brucite composite material and preparation method and application thereof
CN114481697B (en) * 2022-01-20 2022-12-09 江西广源化工有限责任公司 Brucite composite material and preparation method and application thereof
CN114539812A (en) * 2022-03-02 2022-05-27 江西广源新材料有限公司 Inorganic powder, preparation method thereof and reinforced and toughened polypropylene modified master batch
CN115010994A (en) * 2022-05-13 2022-09-06 江西广源化工有限责任公司 Modified superfine wollastonite powder and its prepn and application
CN115010994B (en) * 2022-05-13 2023-12-05 江西广源化工有限责任公司 Modified superfine wollastonite powder and preparation method and application thereof
CN114957795A (en) * 2022-06-16 2022-08-30 江西广源化工有限责任公司 Composite filler and preparation method thereof, and fluororubber composite material and preparation method thereof
CN115386140A (en) * 2022-09-01 2022-11-25 江西广源化工有限责任公司 Nano flaky kaolin-wollastonite-hydroxy silicone oil ternary composite powder and preparation method and application thereof
CN115386140B (en) * 2022-09-01 2023-08-25 江西广源化工有限责任公司 Nanometer flaky kaolin-wollastonite-hydroxyl silicone oil ternary composite powder and preparation method and application thereof
CN116444858A (en) * 2023-03-29 2023-07-18 江西广源化工有限责任公司 Wollastonite/magnesium hydroxide composite inorganic flame retardant and preparation method thereof

Similar Documents

Publication Publication Date Title
CN111892831A (en) Composite powder for electronic adhesive and preparation method and application thereof
CN110951279A (en) Preparation method of superfine acicular wollastonite modified spherical silicon dioxide composite powder
KR102262637B1 (en) Method for surface modification of submicron silicon micropowder
KR101190938B1 (en) Method for production of raw material for use in the production of sintered ore
CN112210232B (en) Special superfine heavy calcium carbonate for latex gloves and preparation method and application thereof
TWI236393B (en) Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
CN103396681B (en) Composite fine barium sulfate and manufacturing method thereof
CN102888020A (en) Preparation method for brucite inorganic flame retardant
CN109810294B (en) Preparation method of high-end nano calcium carbonate for butyl rubber products
CN101538419B (en) Process for preparing brucite inorganic flame retardant
WO2020043131A1 (en) Spherical graphite used for lithium batteries and preparation method therefor
CN102909383A (en) Method for preparing ultrafine nickel powder or cobalt powder
CN114773752B (en) Steel slag PVC (polyvinyl chloride) calendered film base material and preparation method thereof
CN114395274A (en) Superfine modified magnesium hydroxide, preparation method and application thereof, and flame-retardant polyolefin cable material
CN109748286B (en) High-whiteness high-oil-absorption-value calcined kaolin and preparation method thereof
CN104910646A (en) Preparation method for wet ground heavy calcium carbonate
CN113930112B (en) Preparation process method of powder coating
WO2022233034A1 (en) Method for preparing composite pigment filler for coatings by using coal gasification slag
CN114426781B (en) Superfine heavy calcium carbonate and preparation method thereof
CN115851003A (en) Inorganic flame-retardant composite filler and preparation method and application thereof
JP6036295B2 (en) Pretreatment method of sintering raw materials
CN111892748B (en) Composite mineral powder for reducing plastic size shrinkage rate and preparation method and application thereof
CN114773880A (en) Superfine heavy calcium carbonate and preparation method thereof
CN113831760A (en) Preparation method of modified silica and modified silica
CN113510244A (en) Method and device for producing flaky metal pigment

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
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20201106