CN109235139A - A kind of preparation method of high-strength insulating high temperature resistant mica paper - Google Patents

A kind of preparation method of high-strength insulating high temperature resistant mica paper Download PDF

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CN109235139A
CN109235139A CN201811078543.XA CN201811078543A CN109235139A CN 109235139 A CN109235139 A CN 109235139A CN 201811078543 A CN201811078543 A CN 201811078543A CN 109235139 A CN109235139 A CN 109235139A
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parts
temperature
paper
mixed
mica paper
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刘菊花
蒋东明
王素香
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Foshan Chao Hung New Mstar Technology Ltd
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Foshan Chao Hung New Mstar Technology Ltd
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    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H27/00Special paper not otherwise provided for, e.g. made by multi-step processes
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21BFIBROUS RAW MATERIALS OR THEIR MECHANICAL TREATMENT
    • D21B1/00Fibrous raw materials or their mechanical treatment
    • D21B1/02Pretreatment of the raw materials by chemical or physical means
    • D21B1/021Pretreatment of the raw materials by chemical or physical means by chemical means
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/38Coatings with pigments characterised by the pigments
    • D21H19/385Oxides, hydroxides or carbonates
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/38Coatings with pigments characterised by the pigments
    • D21H19/40Coatings with pigments characterised by the pigments siliceous, e.g. clays
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/44Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/52Cellulose; Derivatives thereof
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/36Coatings with pigments
    • D21H19/44Coatings with pigments characterised by the other ingredients, e.g. the binder or dispersing agent
    • D21H19/64Inorganic compounds

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Paper (AREA)
  • Compositions Of Oxide Ceramics (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention relates to a kind of preparation methods of high-strength insulating high temperature resistant mica paper, belong to mica paper technical field.The present invention successively impregnates bamboo plate in acid solution, lye, separate the bamboo fibre in bamboo plate, take out the cell and tissue fluid in bamboo fibre, it recycles highly pressured hydrolysis to decompose the cellulose in bamboo fibre, lignin and generates organic acid, furfural substance, bamboo fibre itself has certain toughness, metal oxide is introduced by surface, the toughness of bamboo fibre, mechanical strength is made to be further strengthened;The present invention will be modified resulting bamboo fibre and mix with ethyl orthosilicate, deionized water is added when impregnating the scraps of paper makes ethyl orthosilicate reaction generate silica, silica-bonded bamboo fibre and mica powder, to utilize bamboo fibre and the good mechanical property of silica, insulating properties and high temperature resistance, toughness, insulating properties and the high-temperature stability for improving mica paper, have broad application prospects.

Description

A kind of preparation method of high-strength insulating high temperature resistant mica paper
Technical field
The present invention relates to a kind of preparation methods of high-strength insulating high temperature resistant mica paper, belong to mica paper technical field.
Background technique
Mica is the general name of a kind of hydrous alumino silicates class, and mica paper is using the high-quality muscovite in Sichuan as raw material, through thermalization It learns or waterpower stripping point is crushed and copy paper is slurried, then cut into continuous roll web or sheet-fed.Mica has insulation, high temperature resistant etc. excellent Good characteristic has in coating, paint, fire-fighting and electric utility and is widely applied very much.It is mesh that mica paper wherein, which is made, in mica One of preceding widest application approach of mica.
Currently, mica paper has had the corresponding whole kinds of mica splitting product.It is industrial mainly to utilize the exhausted of mica paper The insulating materials of edge and heat resistance and anti acid alkali performance affected electrical equipment and electrotechnical apparatus.But directly by mica sheet The mechanical strength and toughness of mica paper obtained are all bad, are not able to satisfy multi-field industrial application.
Mica paper is that tiny mica sheet is that primary raw material is manufactured paper with pulp the paper-based insulation material being prepared through modern paper wet process, It is shaped mainly by the Van der Waals force and electrostatic force between mica sheet, thus the mechanical strength for leading into paper is smaller, makes It is insufficient to obtain mica paper easy fracture, shock resistance, it is difficult to meet requirement and production efficiency is low.
In order to improve the mechanical strength of mica paper, and guarantee its insulation performance, the reinforcement of current use is mainly Using meta-aramid fibers as the reinforcing material of mica paper, this is also the important directions of high-quality combined mica paper insulation development. Existing patent introduction is to improve mica paper to a certain extent using the method for meta-aramid fibers enhancing mica paper Mechanical performance or dielectric strength, however, long-term use temperature is since the heat resistance of meta-aramid fibers ontology is limited 200 DEG C, it is difficult to reach the requirement of C class B insulation grade and the above material, it is difficult to meet the use of high-end field.With large-size machine Develop to miniaturization, especially the equipment such as wind-powered electricity generation, nuclear power, high-speed rail traction electric machine require that motor volume is small, dielectric strength Height, long service life, safe and reliable, to mica paper, higher requirements are also raised.
Therefore, inventing a kind of high mechanical strength, good insulating and mica paper resistant to high temperature has mica paper technical field Positive effect.
Summary of the invention
The technical problems to be solved by the invention: for current mica paper mechanical strength deficiency cause mica paper easy fracture, Shock resistance is insufficient, while being directed to mica paper heat resistance, the defect of poor insulativity, provides a kind of resistance to height of high-strength insulating The preparation method of warm mica paper.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:
A kind of preparation method of high-strength insulating high temperature resistant mica paper, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, it weighs in 7~9 parts of bamboo plates, 22~25 parts of hydrochloric acid and 2~4 parts of malic acid investment beakers, often Temperature is lower to be stood, and filter residue is obtained by filtration after standing, wash with distilled water filter residue 3~5 times, filter residue and sodium hydroxide solution are pressed quality Than single-necked flask being placed in constant temperature boiling in water-bath, filter cake is obtained by filtration, wash with distilled water in 1:20 investment single-necked flask Filter cake 3~5 times;
(2) above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle, with distilled water immersion filter residue, increases air pressure and temperature in kettle, it is permanent Warm constant pressure stands reaction, and filtrate is obtained by filtration after reaction, according to parts by weight, weigh 25~27 parts of filtrates, 2~3 parts of magnesium chlorides, In 1.8~2.2 parts of calcium sulfate and 4.5~4.8 parts of aluminium chloride investment beakers, it is mixed with blender, mixed liquor is made;
(3) sodium hydroxide solution is added dropwise into above-mentioned beaker, adjusts pH value to 10~11, is mixed with blender, after stirring Modified filter residue is obtained by filtration, modified filter residue is placed in baking oven dry 5~6h and obtains desciccate, desciccate is placed in Muffle In furnace, in-furnace temperature is increased under nitrogen atmosphere, and calcined product is made in calcining at constant temperature;
(4) according to parts by weight, above-mentioned 3~5 parts of calcined products, 3~4 parts of ethyl orthosilicates, 6~8 parts of 1,3- rings penta 2 are weighed It is mixed in pure and mild 15~18 parts of dehydrated alcohols investment reaction kettle, mixed glue solution is made, weighs mixed glue solution quality 50~60% Mica flake investment grinder in cross 50 meshes obtain crushed material, by mixed serum and crushed material 5:1 in mass ratio investment burn It is mixed in cup and mixed serum is made;
(5) it chooses and is laid in hot press with a thickness of the scraps of paper of 2~3mm, by 70~80min of above-mentioned mixed serum impregnated sheets of paper, The deionized water of mixed serum quality 30~40% is added after dipping, high temperature suppresses the scraps of paper, the scraps of paper are put into roll squeezer after compacting Moisture removal is removed in roll-in, and the scraps of paper after roll-in are put into drying in baking oven and are discharged to get high-strength insulating high temperature resistant mica paper.
The mass fraction of hydrochloric acid as described in step (1) is 8~12%, and time of repose is 4~6h, sodium hydroxide under room temperature The mass fraction of solution is 20~22%, and the bath temperature in water-bath is 80~90 DEG C, and the constant temperature boiling time is 3~4h.
In high-pressure hydrothermal reaction kettle described in step (2), air pressure is increased to 1.5~1.8MPa, and temperature is increased to 280~ 320 DEG C, constant temperature and pressure stands the reaction time as 60~70min, and the stirring rate of the blender in beaker is 600~700r/ Min, mixing time are 60~70min.
The mass fraction of sodium hydroxide solution described in step (3) is 18~20%, the revolving speed of blender is 500~ 550r/min, mixing time are 40~50min, and the temperature in baking oven is 105~110 DEG C, and drying time is 5~6h, horse Not temperature is increased to 300~330 DEG C in furnace, and the calcining at constant temperature time is 30~40min.
Speed of agitator in reaction kettle described in step (4) is 700~800r/min, mixing time is 40~ 50min。
Compacting pressure in hot press described in step (5) is 16~18MPa, and temperature is 90~100 DEG C, suppresses the scraps of paper Time is 15~20min, and the temperature in baking oven is 110~120 DEG C.
The method have the benefit that:
(1) present invention first first impregnates bamboo plate in acid solution, and boiling is heated in lye, filter is obtained by filtration after boiling Filter residue is then put into high pyrohydrolysis in high-pressure hydrothermal reaction kettle by slag, while being put into magnesium chloride, calcium sulfate, aluminium chloride and being mixed and stir Mixing obtains mixed liquor, and then into mixed liquor, dropwise addition lye adjusting pH value is to alkalinity, the obtained calcined product of drying calcining after filtering, Calcined product and ethyl orthosilicate are mixed to get mixed glue solution, then puts into mica flake powder and obtained mixing slurry is mixed Liquid finally impregnates the scraps of paper in mixed serum, hot pressing after immersion, and drying discharges up to high-strength insulating high temperature resistant cloud after hot pressing Female paper, the present invention successively impregnate bamboo plate in acid solution, lye, separate the bamboo fibre in bamboo plate, and it is fine to take out bamboo Cell and tissue fluid in dimension recycle highly pressured hydrolysis to decompose the cellulose in bamboo fibre, lignin and generate organic acid, chaff Aldehyde material, enable bamboo fibre and the calcium ion, aluminium ion and magnesium ion that are then added formed chelation, covalent bond with And lone pair electrons pairing, by sodium hydroxide is added dropwise, makes calcium, aluminium, magnesium to introduce a large amount of metal ion on bamboo fibre surface Ionic reaction generates respective hydroxide, after high-temperature calcination, is adsorbed in the metal hydroxides reaction on bamboo fibre surface Metal oxide is generated, metal oxide is embedded in bamboo fibre, so that it is improved the heat resistance of bamboo fibre, simultaneous oxidation The insulation performance of magnesium, calcium oxide and aluminium oxide is good, helps to improve the insulation performance of mica paper, and bamboo fibre itself has one Fixed toughness introduces metal oxide by surface, so that the toughness of bamboo fibre, mechanical strength is further strengthened, to mention The mechanical strength of high mica paper;
(2) present invention mixes modified resulting bamboo fibre with ethyl orthosilicate, and deionized water is added when impregnating the scraps of paper to be made just Silester reaction generates silica, silica-bonded bamboo fibre and mica powder, and the mica of sheet surface is made by hot pressing Bamboo fibre and silica are evenly dispersed in layer, to utilize bamboo fibre and the good mechanical property of silica, insulation Property and high temperature resistance, improve the toughness, insulating properties and high-temperature stability of mica paper, have broad application prospects.
Specific embodiment
According to parts by weight, 7~9 parts of bamboo plates, 22~25 parts of mass fractions are weighed as 8~12% hydrochloric acid and 2~4 parts Malic acid is put into beaker, and 4~6h is stood under room temperature, filter residue is obtained by filtration after standing, and filter residue 3~5 times wash with distilled water will The sodium hydroxide solution 1:20 in mass ratio that filter residue and mass fraction are 20~22% is put into single-necked flask, and single-necked flask is set Be in 80~90 DEG C of water-bath in bath temperature, filter cake is obtained by filtration in constant temperature 3~4h of boiling, wash with distilled water filter cake 3~ 5 times;Above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle, with distilled water immersion filter residue, increase in kettle air pressure to 1.5~ 1.8MPa improves temperature in the kettle to 280~320 DEG C, and constant temperature and pressure stands 60~70min of reaction, and filtrate is obtained by filtration after reaction, According to parts by weight, 25~27 parts of filtrates, 2~3 parts of magnesium chlorides, 1.8~2.2 parts of calcium sulfate and 4.5~4.8 parts of chlorinations are weighed Aluminium is put into beaker, and 60~70min is mixed with the revolving speed of 600~700r/min with blender, mixed liquor is made;To above-mentioned The sodium hydroxide solution that mass fraction is 18~20% is added dropwise in beaker, adjusts pH value to 10~11, with blender with 500~ 40~50min is mixed in the revolving speed of 550r/min, and modified filter residue is obtained by filtration after stirring, and modified filter residue is placed in baking oven, Dry 5~6h obtains desciccate under conditions of temperature is 105~110 DEG C, desciccate is placed in Muffle furnace, in nitrogen In-furnace temperature is increased under atmosphere to 300~330 DEG C, calcined product is made in 30~40min of calcining at constant temperature;According to parts by weight, claim Above-mentioned 3~5 parts of calcined products, 3~4 parts of ethyl orthosilicates, 6~8 parts of 1,3- cyclopentadienyl alcohols and 15~18 parts of dehydrated alcohols are taken to throw Enter in reaction kettle, 40~50min is mixed under conditions of speed of agitator is 700~800r/min, mixed glue solution is made, claims It takes the mica flake of mixed glue solution quality 50~60% to put into 50 meshes excessively in grinder and obtains crushed material, by mixed serum and powder The 5:1 in mass ratio that minces, which puts into be mixed in beaker, is made mixed serum;It chooses and is laid in heat with a thickness of the scraps of paper of 2~3mm In press, by 70~80min of above-mentioned mixed serum impregnated sheets of paper, the deionization of mixed serum quality 30~40% is added after dipping Water is then 16~18MPa in compacting pressure, and temperature suppresses 15~20min of the scraps of paper under conditions of being 90~100 DEG C, after compacting The scraps of paper are put into roll-in in roll squeezer and remove moisture, the scraps of paper after roll-in are put into baking oven, are 110~120 DEG C in temperature Under the conditions of drying discharging to get high-strength insulating high temperature resistant mica paper.
According to parts by weight, 7 parts of bamboo plates, the hydrochloric acid that 22 parts of mass fractions are 8% and 2 parts of malic acid are weighed and put into beaker In, 4h is stood under room temperature, filter residue is obtained by filtration after standing, wash with distilled water filter residue 3 times, is 20% by filter residue and mass fraction Sodium hydroxide solution 1:20 in mass ratio investment single-necked flask in, it is 80 DEG C of water-bath that single-necked flask, which is placed in bath temperature, In, filter cake is obtained by filtration, wash with distilled water filter cake 3 times in constant temperature boiling 3h;Above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle In, with distilled water immersion filter residue, increases air pressure in kettle and improve temperature in the kettle to 280 DEG C, constant temperature and pressure stands reaction to 1.5MPa Filtrate is obtained by filtration in 60min after reaction, according to parts by weight, weigh 25 parts of filtrates, 2 parts of magnesium chlorides, 1.8 parts of calcium sulfate and In 4.5 parts of aluminium chloride investment beakers, 60min is mixed with the revolving speed of 600r/min with blender, mixed liquor is made;To above-mentioned The sodium hydroxide solution that mass fraction is 18% is added dropwise in beaker, adjusts pH value to 10, is mixed with blender with the revolving speed of 500r/min Stirring 40min is closed, modified filter residue is obtained by filtration after stirring, modified filter residue is placed in baking oven, under conditions of temperature is 105 DEG C Dry 5h obtains desciccate, and desciccate is placed in Muffle furnace, and raising in-furnace temperature is permanent to 300 DEG C under nitrogen atmosphere Calcined product is made in temperature calcining 30min;According to parts by weight, above-mentioned 3 parts of calcined products, 3 parts of ethyl orthosilicates, 6 part 1 are weighed, In 3- cyclopentadienyl alcohol and 15 parts of dehydrated alcohol investment reaction kettles, it is mixed under conditions of speed of agitator is 700r/min Mixed glue solution is made in 40min, weighs 50 meshes excessively in the mica flake investment grinder of mixed glue solution quality 50% and is crushed Mixed serum is made by being mixed in mixed serum and crushed material 5:1 in mass ratio investment beaker in object;It chooses with a thickness of 2mm The scraps of paper be laid in hot press, by above-mentioned mixed serum impregnated sheets of paper 70min, mixed serum quality 30% is added after dipping Deionized water is then 16MPa in compacting pressure, suppresses scraps of paper 15min under the conditions of at a temperature of 90 °C, put the scraps of paper after compacting Enter roll-in in roll squeezer and remove moisture, the scraps of paper after roll-in are put into baking oven, are dried out under conditions of temperature is 110 DEG C Material is to get high-strength insulating high temperature resistant mica paper.
According to parts by weight, 8 parts of bamboo plates, the hydrochloric acid that 24 parts of mass fractions are 10% and 3 parts of malic acid are weighed and put into beaker In, 5h is stood under room temperature, filter residue is obtained by filtration after standing, wash with distilled water filter residue 4 times, is 21% by filter residue and mass fraction Sodium hydroxide solution 1:20 in mass ratio investment single-necked flask in, it is 85 DEG C of water-bath that single-necked flask, which is placed in bath temperature, In, filter cake is obtained by filtration, wash with distilled water filter cake 4 times in constant temperature boiling 3.5h;Above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle In, with distilled water immersion filter residue, increases air pressure in kettle and improve temperature in the kettle to 300 DEG C, constant temperature and pressure stands reaction to 1.7MPa Filtrate is obtained by filtration in 65min after reaction, according to parts by weight, weigh 26 parts of filtrates, 2 parts of magnesium chlorides, 2.0 parts of calcium sulfate and In 4.7 parts of aluminium chloride investment beakers, 65min is mixed with the revolving speed of 650r/min with blender, mixed liquor is made;To above-mentioned The sodium hydroxide solution that mass fraction is 19% is added dropwise in beaker, adjusts pH value to 11, is mixed with blender with the revolving speed of 520r/min Stirring 45min is closed, modified filter residue is obtained by filtration after stirring, modified filter residue is placed in baking oven, under conditions of temperature is 107 DEG C Dry 5.5h obtains desciccate, and desciccate is placed in Muffle furnace, increases in-furnace temperature under nitrogen atmosphere to 315 DEG C, Calcined product is made in calcining at constant temperature 35min;According to parts by weight, above-mentioned 4 parts of calcined products, 3 parts of ethyl orthosilicates, 7 parts are weighed In 1,3- cyclopentadienyl alcohol and 17 parts of dehydrated alcohol investment reaction kettles, it is mixed under conditions of speed of agitator is 750r/min Mixed glue solution is made in 45min, weighs 50 meshes excessively in the mica flake investment grinder of mixed glue solution quality 55% and is crushed Mixed serum is made by being mixed in mixed serum and crushed material 5:1 in mass ratio investment beaker in object;It chooses with a thickness of 2mm The scraps of paper be laid in hot press, by above-mentioned mixed serum impregnated sheets of paper 75min, mixed serum quality 35% is added after dipping Deionized water is then 17MPa in compacting pressure, and temperature suppresses scraps of paper 17min under conditions of being 95 DEG C, puts the scraps of paper after compacting Enter roll-in in roll squeezer and remove moisture, the scraps of paper after roll-in are put into baking oven, are dried out under conditions of temperature is 115 DEG C Material is to get high-strength insulating high temperature resistant mica paper.
According to parts by weight, 9 parts of bamboo plates, the hydrochloric acid that 25 parts of mass fractions are 12% and 4 parts of malic acid are weighed and put into beaker In, 6h is stood under room temperature, filter residue is obtained by filtration after standing, wash with distilled water filter residue 5 times, is 22% by filter residue and mass fraction Sodium hydroxide solution 1:20 in mass ratio investment single-necked flask in, it is 90 DEG C of water-bath that single-necked flask, which is placed in bath temperature, In, filter cake is obtained by filtration, wash with distilled water filter cake 5 times in constant temperature boiling 4h;Above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle In, with distilled water immersion filter residue, increases air pressure in kettle and improve temperature in the kettle to 320 DEG C, constant temperature and pressure stands reaction to 1.8MPa Filtrate is obtained by filtration in 70min after reaction, according to parts by weight, weigh 27 parts of filtrates, 3 parts of magnesium chlorides, 2.2 parts of calcium sulfate and 4.8 part aluminium chloride is put into beaker, 70min is mixed with the revolving speed of 700r/min with blender, mixed liquor is made;To above-mentioned The sodium hydroxide solution that mass fraction is 20% is added dropwise in beaker, adjusts pH value to 11, is mixed with blender with the revolving speed of 550r/min Stirring 50min is closed, modified filter residue is obtained by filtration after stirring, modified filter residue is placed in baking oven, under conditions of temperature is 110 DEG C Dry 6h obtains desciccate, and desciccate is placed in Muffle furnace, and raising in-furnace temperature is permanent to 330 DEG C under nitrogen atmosphere Calcined product is made in temperature calcining 40min;According to parts by weight, above-mentioned 5 parts of calcined products, 4 parts of ethyl orthosilicates, 8 part 1 are weighed, In 3- cyclopentadienyl alcohol and 18 parts of dehydrated alcohol investment reaction kettles, it is mixed under conditions of speed of agitator is 800r/min Mixed glue solution is made in 50min, weighs 50 meshes excessively in the mica flake investment grinder of mixed glue solution quality 60% and is crushed Mixed serum is made by being mixed in mixed serum and crushed material 5:1 in mass ratio investment beaker in object;It chooses with a thickness of 3mm The scraps of paper be laid in hot press, by above-mentioned mixed serum impregnated sheets of paper 80min, mixed serum quality 40% is added after dipping Deionized water is then 18MPa in compacting pressure, and temperature suppresses scraps of paper 20min under conditions of being 100 DEG C, by the scraps of paper after compacting It is put into roll-in in roll squeezer and removes moisture, the scraps of paper after roll-in are put into baking oven, are dried out under conditions of temperature is 120 DEG C Material is to get high-strength insulating high temperature resistant mica paper.
Comparative example is as a comparison case made the present invention with the high-strength insulating high temperature resistant mica paper that Kunshan company produces High-strength insulating high temperature resistant mica paper and comparative example in high-strength insulating high temperature resistant mica paper carry out performance detection, detection knot Fruit is as shown in table 1:
Test method:
Tensile strength and shrinking percentage test are detected according to the method for national standard GB/T13022-91.
Toughness test: the mica paper in 1~3 comparative example of example is subjected to bend test, crooked radian is greater than 45 degree and is less than It 80 degree, sees whether to be broken.
Dielectric strength test is detected using dielectric breakdown strength tester.
Resistivity measurement is detected using resistivity tester.
Heat resistance test is indicated using long-term use temperature, and measures the tensile strength after long term high temperature use.
1 mica paper performance measurement result of table
According to above-mentioned detection data high-strength insulating high temperature resistant mica paper tensile strength produced by the present invention reach 60MPa with On, show that mica paper provided by the invention has very high mechanical strength, when crooked radian is greater than 45 degree less than 80 degree without disconnected Appearance is split, shows it with good toughness, shock resistance is good, and dielectric strength is high, and resistivity is high, good insulating, heat-resisting temperature Degree is high, heat-resist, has broad application prospects.

Claims (6)

1. a kind of preparation method of high-strength insulating high temperature resistant mica paper, it is characterised in that specific preparation step are as follows:
(1) according to parts by weight, it weighs in 7~9 parts of bamboo plates, 22~25 parts of hydrochloric acid and 2~4 parts of malic acid investment beakers, often Temperature is lower to be stood, and filter residue is obtained by filtration after standing, wash with distilled water filter residue 3~5 times, filter residue and sodium hydroxide solution are pressed quality Than single-necked flask being placed in constant temperature boiling in water-bath, filter cake is obtained by filtration, wash with distilled water in 1:20 investment single-necked flask Filter cake 3~5 times;
(2) above-mentioned filter residue is placed in high-pressure hydrothermal reaction kettle, with distilled water immersion filter residue, increases air pressure and temperature in kettle, it is permanent Warm constant pressure stands reaction, and filtrate is obtained by filtration after reaction, according to parts by weight, weigh 25~27 parts of filtrates, 2~3 parts of magnesium chlorides, In 1.8~2.2 parts of calcium sulfate and 4.5~4.8 parts of aluminium chloride investment beakers, it is mixed with blender, mixed liquor is made;
(3) sodium hydroxide solution is added dropwise into above-mentioned beaker, adjusts pH value to 10~11, is mixed with blender, after stirring Modified filter residue is obtained by filtration, modified filter residue is placed in baking oven dry 5~6h and obtains desciccate, desciccate is placed in Muffle In furnace, in-furnace temperature is increased under nitrogen atmosphere, and calcined product is made in calcining at constant temperature;
(4) according to parts by weight, above-mentioned 3~5 parts of calcined products, 3~4 parts of ethyl orthosilicates, 6~8 parts of 1,3- rings penta 2 are weighed It is mixed in pure and mild 15~18 parts of dehydrated alcohols investment reaction kettle, mixed glue solution is made, weighs mixed glue solution quality 50~60% Mica flake investment grinder in cross 50 meshes obtain crushed material, by mixed serum and crushed material 5:1 in mass ratio investment burn It is mixed in cup and mixed serum is made;
(5) it chooses and is laid in hot press with a thickness of the scraps of paper of 2~3mm, by 70~80min of above-mentioned mixed serum impregnated sheets of paper, The deionized water of mixed serum quality 30~40% is added after dipping, high temperature suppresses the scraps of paper, the scraps of paper are put into roll squeezer after compacting Moisture removal is removed in roll-in, and the scraps of paper after roll-in are put into drying in baking oven and are discharged to get high-strength insulating high temperature resistant mica paper.
2. a kind of preparation method of high-strength insulating high temperature resistant mica paper according to claim 1, it is characterised in that: step (1) mass fraction of the hydrochloric acid described in is 8~12%, and time of repose is 4~6h, the quality point of sodium hydroxide solution under room temperature Number is 20~22%, and the bath temperature in water-bath is 80~90 DEG C, and the constant temperature boiling time is 3~4h.
3. a kind of preparation method of high-strength insulating high temperature resistant mica paper according to claim 1, it is characterised in that: step (2) in the high-pressure hydrothermal reaction kettle described in, air pressure is increased to 1.5~1.8MPa, and temperature is increased to 280~320 DEG C, and constant temperature is permanent It is 60~70min that pressure, which stands the reaction time, and the stirring rate of the blender in beaker is 600~700r/min, when mixing Between be 60~70min.
4. a kind of preparation method of high-strength insulating high temperature resistant mica paper according to claim 1, it is characterised in that: step (3) mass fraction of the sodium hydroxide solution described in is 18~20%, and the revolving speed of blender is 500~550r/min, and mixing is stirred Mixing the time is 40~50min, and the temperature in baking oven is 105~110 DEG C, and drying time is 5~6h, and temperature is increased in Muffle furnace 300~330 DEG C, the calcining at constant temperature time is 30~40min.
5. a kind of preparation method of high-strength insulating high temperature resistant mica paper according to claim 1, it is characterised in that: step (4) speed of agitator in reaction kettle described in is 700~800r/min, and mixing time is 40~50min.
6. a kind of preparation method of high-strength insulating high temperature resistant mica paper according to claim 1, it is characterised in that: step (5) compacting pressure in the hot press described in is 16~18MPa, and temperature is 90~100 DEG C, the compacting scraps of paper time is 15~ 20min, the temperature in baking oven are 110~120 DEG C.
CN201811078543.XA 2018-09-17 2018-09-17 A kind of preparation method of high-strength insulating high temperature resistant mica paper Withdrawn CN109235139A (en)

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CN110407480A (en) * 2019-06-21 2019-11-05 刘其云 A kind of preparation method of high light transmission high tenacity antireflective film
CN110747673A (en) * 2019-09-23 2020-02-04 西南科技大学 Bi/Mo/Co2O4/CO2Method for catalytically purifying Si impurities on surface layer of pulping bamboo chip
CN112522986A (en) * 2020-11-27 2021-03-19 山东鲁阳节能材料股份有限公司 Adsorption type inorganic combined fiber paper and preparation method thereof
CN113493209A (en) * 2020-03-20 2021-10-12 广州昊吉生物科技有限公司 Coating method of low-fluorine fluorophlogopite
CN114808508A (en) * 2022-03-21 2022-07-29 华南理工大学 Insulating paste and preparation method thereof

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CN106189779A (en) * 2016-08-05 2016-12-07 宁波高新区斯汀环保科技有限公司 A kind of preparation method of high-temperature resistant and antistatic coating
CN107134329A (en) * 2017-04-26 2017-09-05 晶锋集团(天长)高分子材料有限公司 A kind of preparation method of insulation mica tape
CN107286772A (en) * 2017-06-30 2017-10-24 常州市日臣艺术装饰材料有限公司 A kind of finishing agent and preparation method thereof

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CN106189779A (en) * 2016-08-05 2016-12-07 宁波高新区斯汀环保科技有限公司 A kind of preparation method of high-temperature resistant and antistatic coating
CN107134329A (en) * 2017-04-26 2017-09-05 晶锋集团(天长)高分子材料有限公司 A kind of preparation method of insulation mica tape
CN107286772A (en) * 2017-06-30 2017-10-24 常州市日臣艺术装饰材料有限公司 A kind of finishing agent and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110407480A (en) * 2019-06-21 2019-11-05 刘其云 A kind of preparation method of high light transmission high tenacity antireflective film
CN110747673A (en) * 2019-09-23 2020-02-04 西南科技大学 Bi/Mo/Co2O4/CO2Method for catalytically purifying Si impurities on surface layer of pulping bamboo chip
CN110747673B (en) * 2019-09-23 2021-01-19 西南科技大学 Bi/Mo/Co2O4/CO2Method for catalytically purifying Si impurities on surface layer of pulping bamboo chip
CN113493209A (en) * 2020-03-20 2021-10-12 广州昊吉生物科技有限公司 Coating method of low-fluorine fluorophlogopite
CN112522986A (en) * 2020-11-27 2021-03-19 山东鲁阳节能材料股份有限公司 Adsorption type inorganic combined fiber paper and preparation method thereof
CN114808508A (en) * 2022-03-21 2022-07-29 华南理工大学 Insulating paste and preparation method thereof
CN114808508B (en) * 2022-03-21 2022-12-16 华南理工大学 Insulating paste and preparation method thereof

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Application publication date: 20190118