CN107857901A - A kind of metakaolin gum filler and preparation method thereof - Google Patents

A kind of metakaolin gum filler and preparation method thereof Download PDF

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Publication number
CN107857901A
CN107857901A CN201711022164.4A CN201711022164A CN107857901A CN 107857901 A CN107857901 A CN 107857901A CN 201711022164 A CN201711022164 A CN 201711022164A CN 107857901 A CN107857901 A CN 107857901A
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kaolin
metakaolin
parts
filter cake
particle
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邵建聪
梅明军
柯汉明
李坤
王志国
许天翼
莫少建
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Gaoling Sci & Tech Co Ltd Maoming
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Gaoling Sci & Tech Co Ltd Maoming
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/04Carbon
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/34Silicon-containing compounds
    • C08K3/346Clay
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/02Ingredients treated with inorganic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/04Ingredients treated with organic substances
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/017Additives being an antistatic agent

Abstract

The invention belongs to gum filler technical field, and in particular to a kind of metakaolin gum filler and preparation method thereof.The metakaolin gum filler includes each component of following parts by weight:50~75 parts of metakaolin, 25~35 parts of carboxylated graphene oxide, 5~15 parts of low-alkalinity sulphoaluminate cement, 5~15 parts of flyash, 5~15 parts of plasticizer.Its preparation method is:50~75 parts of kaolin, 25~35 parts of carboxylated graphene oxide, 5~15 parts of low-alkalinity sulphoaluminate cement, 5~15 parts of flyash and 5~15 parts of plasticizer are mixed successively, obtain metakaolin gum filler.Metakaolin gum filler material property provided by the present invention is controllable, and technique ginseng easily realizes that technological process is simple, and cost is low, has excellent elastic, anti-flexibility, elongation rate of tensile failure, antistatic behaviour and scratch-resistant performance suitable for industrialization large-scale production.

Description

A kind of metakaolin gum filler and preparation method thereof
Technical field
The invention belongs to gum filler technical field, and in particular to a kind of metakaolin gum filler and preparation method thereof.
Background technology
Rubber industry serves supporting effect to Chinese national economy, especially with China's Mechanization Level raising with And new diseases, rubber industry constantly interpenetrate with association area, application and the field of rubber, product have been opened up It is widely used in metallurgy, Aeronautics and Astronautics, harbour, automobile, weaving, light industry, engineering machinery, mine, oil, building, ocean, agriculture The fields such as industry.The maximum filler of rubber usage amount is carbon black and white carbon at present.But both material prices are expensive, prepare energy Consumption is high and crocking resistance is inadequate, can not meet the requirement of the low-carbon environment-friendly of China's strategy of sustainable development completely.
For kaolin due to its rich reserves, cost is cheap, is easy to exploit, and with its excellent mechanical property in field of stuffing In application it is more and more noticeable.But in the filler as rubber, because common kaolin is inorganic rigid grain in itself Son, size is larger, too much addition often lead to material mechanical strength decline, it is brittle the shortcomings of, have a strong impact on rubber material The mechanical property of material.
As Preparation Technique of Powders promotes to nanoscale, the chemical composition of nano kaoline raw material relatively kaolinite Theoretical value, category environmental suitability, nontoxicity and content of beary metal meet the material of environmental requirement, and because its is special Small-size effect, while the mechanical property of rubber is strengthened, the air-tightness of elastomeric material can be improved, it is defeated so as to reduce conveyer belt The frictional force of fortune process, reduces abrasion, and nano kaoline has obtained people and widely paid close attention to.But nano kaoline gathers with organic The interfacial property of compound is different, poor compatibility, it is difficult to it is dispersed, solve agglomeration traits of the nano kaoline in rubber just into For the key of its application.As Application No. 201010289872.6 patent using activator cetyl trimethylammonium bromide and Stearic acid modified kaolin is as gum filler, for achieving preferable mechanical property during tyres for passenger cars.But this side Method antistatic effect deficiency, its crocking resistance are not embodied;Application No. 200510018202.X patent is directly adopted Use AlCl3·3H20 and stearic acid Coaseries kaolin is activated for preparing butyl rubber bottle stopper reinforced filling as activating agent, this Kind method prepares simple, it is possible to increase the physical and mechanical properties of bottle stopper, but it is difficult to conveyer belt, cable covering, rubber roll, iron The large-scale Rubber Industry such as sleeper pad, sebific duct, rubber blanket field.
The content of the invention
To solve the deficiencies in the prior art, the invention provides a kind of metakaolin gum filler and preparation method thereof.This The there is provided metakaolin gum filler material property of invention is controllable, and technique ginseng easily realizes that technological process is simple, and cost is low, There is excellent elastic, anti-flexibility, elongation rate of tensile failure, antistatic behaviour and rub suitable for industrialization large-scale production Energy.
Technical scheme provided by the present invention is as follows:
A kind of metakaolin gum filler, include each component of following parts by weight:50~75 parts of metakaolin, carboxylated 25~35 parts of graphene oxide, 5~15 parts of low-alkalinity sulphoaluminate cement, 5~15 parts of flyash, 5~15 parts of plasticizer.
Specifically, the preparation method of the carboxylated graphene oxide comprises the following steps:
1) the ether hydroxylating of graphene oxide, is obtained into hydroxylating oxidation stone at backflow in graphene oxide water solution Black alkene;
2) by the hydroxycarboxyl group of hydroxylating graphene oxide, carboxylated graphene oxide is obtained.
The carboxylated graphene oxide that above-mentioned technical proposal is provided can increase elongation rate of tensile failure, antistatic behaviour and abrasion-resistant Performance.
Specifically, the metakaolin is prepared by following steps:
1) the kaolin filter cake that solid content is 65~70% is prepared, particle diameter is below two microns in the kaolin filter cake The content of kaolin particle accounts for more than the 85wt% of kaolin particle in the kaolin filter cake;
2) the kaolin filter cake that step 1) obtains is flashed under the conditions of -200pa~-100pa tiny structures, dried, obtained Kaolin dry powder of the moisture content below 2.5%;
3) kaolin dry powder that step 2) obtains is calcined, calcining heat is 750~850 DEG C, calcination time 1.0 ~2.0 hours, obtain thermal activation kaolin;
4) the thermal activation kaolin obtained by step 3) is subjected to depolymerization, that is, eliminates and sintered caused by high-temperature calcination The caking of reunion, obtains metakaolin.
Specifically, in step 1), the preparation method of described kaolin filter cake is:By the height that solid content is 10~15% Ridge soil ore pulp is classified and settled, and accounts for the content of kaolin particle of the particle diameter below two microns in the kaolin ore slurry More than the 85wt% of kaolin particle in the kaolin ore slurry, then it is 20~25% that kaolin ore slurry is concentrated into solid content, By the kaolin ore slurry press filtration after concentration, the kaolin filter cake that the solid content is 65~70% is obtained.
Specifically, in step 3), the calcining heat is 750~820 DEG C, and calcination time is 75min~100min.
Preferably, the metakaolin is prepared by following steps:
1) the kaolin filter cake that solid content is 68~70% is prepared, particle diameter is below two microns in the kaolin filter cake The content of kaolin particle accounts for 90~95 wt% of kaolin particle in the kaolin filter cake;
2) the kaolin filter cake that step 1) obtains is flashed under the conditions of -200pa~-100pa tiny structures, dried, obtained Kaolin dry powder of the moisture content below 2.0%;
3) combustion medium calcining step 2 is used as using natural gas or liquefied petroleum gas) obtained by kaolin dry powder, calcining temperature Spend for 750~850 DEG C, calcination time is 1.5~2 hours, obtains thermal activation kaolin;
4) the thermal activation kaolin for obtaining step 3) carries out depolymerization, and borate coupling is added in depolymehzation process Agent, caused agglomeration when eliminating high-temperature calcination lump and increase kaolin powder surface-active, obtain metakaolin, its In, the percentage by weight of the dosage of the boric acid ester coupler and the hot metakaolin is 1.5~2.5%.
Preferably, the preparation method of the kaolin filter cake in the step 1) is:It is 10~15% by solid content Kaolin ore slurry is classified and settled, and makes the content of kaolin particle of the particle diameter below two microns in the kaolin ore slurry More than the 85wt% of kaolin particle in the kaolin ore slurry is accounted for, then institute is adjusted by 98% concentrated sulfuric acid of weight/mass percentage composition The pH to 2.0~3.0 of kaolin ore slurry is stated, adds 5~8wt of the kaolin ore slurry solid content ‰ sodium dithionite stirring Bleaching, control whiteness is more than 85%, then it is 20~25% that kaolin ore slurry is concentrated into solid content, by the kaolinite after concentration Native ore pulp press filtration, the filter cake that solid content is 55~60% is obtained, by the filter cake, the hexa metaphosphoric acid of the 4~5wt of filter cake ‰ Sodium, the sodium polyacrylate solution that weight/mass percentage composition is 10% mix, wherein Sodium Polyacrylate in the sodium polyacrylate solution Be 2~3 ‰ with the percentage by weight of the filter cake, and using sodium hydroxide solution regulation pH that weight/mass percentage composition is 40% to Stir slurrying after 6.0, by grinding, delaminate after slurrying, make in the ore pulp after the filter cake slurrying particle diameter below two microns The content of kaolin particle accounts for 90~95wt% of kaolin particle in the ore pulp after the filter cake slurrying, then will pass through grinding, The ore pulp press filtration delaminated to solid content is 64~67%, obtains kaolin filter cake.
Have a choosing, the calcining heat in the step 3) is 780~820 DEG C, calcination time be 80min~ 100min。
Preferably, the dosage of the boric acid ester coupler added in depolymehzation process in the step 4) and the heat are higher The percentage by weight of ridge soil is 2.0%.
Present invention also offers the preparation method of metakaolin gum filler provided by the present invention, comprise the following steps: By 50~75 parts of kaolin, 25~35 parts of carboxylated graphene oxide, 5~15 parts of low-alkalinity sulphoaluminate cement, 5~ 15 parts of flyash and 5~15 parts of plasticizer mix successively, obtain metakaolin gum filler.
The beneficial effects of the present invention are:
Material property of the present invention is controllable, and technological parameter is easily realized, technological process is simple, and cost is low, big suitable for industrializing Large-scale production, metakaolin gum filler have highly conductive, rub resistance characteristic, are made of such a metakaolin gum filler Rubber there is excellent elastic, anti-flexibility, elongation rate of tensile failure, antistatic behaviour and scratch-resistant performance, have very high Practical value.
Embodiment
The principles and features of the present invention are described below, and the given examples are served only to explain the present invention, is not intended to limit Determine the scope of the present invention.
Embodiment 1
1) kaolin ore slurry that solid content is 15% is classified and settled, make in the kaolin ore slurry particle diameter two The content of kaolin particle below micron accounts for more than the 85wt% of kaolin particle in the kaolin ore slurry, then with quality hundred Divide the concentrated sulfuric acid that content is 98% to adjust the pH to 2.0 of the kaolin ore slurry, add the kaolin ore slurry solid content 8wt ‰ sodium dithionite stirring bleaching, control whiteness is more than 85%, then kaolin ore slurry is concentrated into solid content and is 20%, by the kaolin ore slurry press filtration after concentration, the filter cake that solid content is 60% is obtained, by the filter cake, the filter cake 4wt ‰ Calgon, weight/mass percentage composition be 10% sodium polyacrylate solution mix, wherein in the sodium polyacrylate solution The percentage by weight of Sodium Polyacrylate and the filter cake is 3 ‰, and is adjusted by 40% sodium hydroxide solution of weight/mass percentage composition Slurrying is stirred after section pH to 6.0, by grinding, delaminate after slurrying, makes in the ore pulp after the filter cake slurrying particle diameter at two microns The content of following kaolin particle accounts for the 90wt% of kaolin particle in the ore pulp after the filter cake slurrying, then will pass through and grind The ore pulp press filtration grind, delaminated to solid content is 67%, obtains kaolin filter cake;
2) the kaolin filter cake for obtaining step 1) is flashed under the conditions of -200pa tiny structures, dried, and is obtained moisture content and is existed Less than 2.0% kaolin dry powder;
3) combustion medium calcining step 2 is used as using natural gas or liquefied petroleum gas) obtained by kaolin dry powder, calcining temperature Spend for 820 DEG C, calcination time 80min, obtain thermal activation kaolin;
4) the thermal activation kaolin for obtaining step 3) carries out depolymerization, and borate coupling is added in depolymehzation process The percentage by weight of agent, the dosage of boric acid ester coupler and the hot metakaolin is 2.0%, eliminates generation during high-temperature calcination Agglomeration lump and increase kaolin powder surface-active, obtain metakaolin, wherein, the use of the boric acid ester coupler The percentage by weight of amount and the hot metakaolin is 2.5%;
5) graphene oxide is prepared, after washing three times with watery hydrochloric acid and deionized water, is made into 2mg/mL solution;
6) pH to 8.0 is adjusted using sodium hydroxide solution, is heated to 70 DEG C, flow back 4h, is cooled to room temperature;
7) acid permanganate soln is added, 4h is reacted at room temperature, adds acetone, is centrifuged, freezes, obtains carboxylated graphite oxide Alkene;
8) by 50 parts of kaolin, 35 parts of carboxylated graphene oxide, 5 parts of low-alkalinity sulphoaluminate cement, 15 parts Flyash and 5 parts of plasticizer mix successively, obtain metakaolin gum filler 1.
150g metakaolins gum filler 1 is uniformly mixed with 1000g rubber-baseds with raw material, 70g auxiliary agents etc., then will Material preheats 15 minutes at 160 degree, then by mixture in 150 degree of mixings, mixing time 15 minutes, then by tabletting work Skill, elastomeric material 1 is made.
The composite tensile strength is more than 30MPa to elastomeric material 1 after tested, and elongation rate of tensile failure is more than 500%, aging Post-tensioning intensity and elongation rate of tensile failure rate of change:- 15~+15%, abrasion loss is less than 80mm3, and impact property reaches 12kJ/m2, Tensile strength reaches 28MPa, the Ω c of surface resistivity ρ s < 100 Ω cm, volume resistance ρ v < 95.
Embodiment 2
1) kaolin ore slurry that solid content is 10% is classified and settled, make in the kaolin ore slurry particle diameter two The content of kaolin particle below micron accounts for more than the 85wt% of kaolin particle in the kaolin ore slurry, then with quality hundred Divide the concentrated sulfuric acid that content is 98% to adjust the pH to 3.0 of the kaolin ore slurry, add the kaolin ore slurry solid content 5wt ‰ sodium dithionite stirring bleaching, control whiteness is more than 85%, then kaolin ore slurry is concentrated into solid content and is 25%, by the kaolin ore slurry press filtration after concentration, the filter cake that solid content is 55% is obtained, by the filter cake, the filter cake 5wt ‰ Calgon, weight/mass percentage composition be 10% sodium polyacrylate solution mix, wherein in the sodium polyacrylate solution The percentage by weight of Sodium Polyacrylate and the filter cake is 2 ‰, and is adjusted by 40% sodium hydroxide solution of weight/mass percentage composition Slurrying is stirred after section pH to 6.0, by grinding, delaminate after slurrying, makes in the ore pulp after the filter cake slurrying particle diameter at two microns The content of following kaolin particle accounts for the 95wt% of kaolin particle in the ore pulp after the filter cake slurrying, then will pass through and grind The ore pulp press filtration grind, delaminated to solid content is 64%, obtains kaolin filter cake;
2) the kaolin filter cake for obtaining step 1) is flashed under the conditions of -100pa tiny structures, dried, and is obtained moisture content and is existed Less than 2.0% kaolin dry powder;
3) combustion medium calcining step 2 is used as using natural gas or liquefied petroleum gas) obtained by kaolin dry powder, calcining temperature Spend for 780 DEG C, calcination time 100min, obtain thermal activation kaolin;
4) the thermal activation kaolin for obtaining step 3) carries out depolymerization, and borate coupling is added in depolymehzation process The percentage by weight of agent, the dosage of boric acid ester coupler and the hot metakaolin is 2.0%, eliminates generation during high-temperature calcination Agglomeration lump and increase kaolin powder surface-active, obtain metakaolin, wherein, the use of the boric acid ester coupler The percentage by weight of amount and the hot metakaolin is 1.5%;
5) graphene oxide is prepared, after washing three times with watery hydrochloric acid and deionized water, is made into 2mg/mL solution;
6) pH to 8.0 is adjusted using sodium hydroxide solution, is heated to 70 DEG C, flow back 4h, is cooled to room temperature;
7) acid permanganate soln is added, 4h is reacted at room temperature, adds acetone, is centrifuged, freezes, obtains carboxylated graphite oxide Alkene;
8) by 75 parts of kaolin, 25 parts of carboxylated graphene oxide, 15 parts of low-alkalinity sulphoaluminate cement, 5 parts Flyash and 15 parts of plasticizer mix successively, obtain metakaolin gum filler 2.
150g metakaolins gum filler 2 is uniformly mixed with 1000g rubber-baseds with raw material, 70g auxiliary agents etc., then will Material preheats 15 minutes at 160 degree, then by mixture in 150 degree of mixings, mixing time 15 minutes, then by tabletting work Skill, elastomeric material 1 is made.
The composite tensile strength is more than 28MPa to elastomeric material 1 after tested, and elongation rate of tensile failure is more than 500%, aging Post-tensioning intensity and elongation rate of tensile failure rate of change:- 10~+15%, abrasion loss is less than 85mm3, and impact property reaches 10.5kJ/ M2, tensile strength reach 26MPa, the Ω c of surface resistivity ρ s < 95 Ω cm, volume resistance ρ v < 98.
Embodiment 3
1) kaolin ore slurry that solid content is 102% is classified and settled, particle diameter in the kaolin ore slurry is existed The content of less than two microns of kaolin particle accounts for more than the 85wt% of kaolin particle in the kaolin ore slurry, then with quality Percentage composition is that 98% concentrated sulfuric acid adjusts the pH to 2.5 of the kaolin ore slurry, adds the kaolin ore slurry solid content 6wt ‰ sodium dithionite stirring bleaching, control whiteness is more than 85%, then kaolin ore slurry is concentrated into solid content and is 22%, by the kaolin ore slurry press filtration after concentration, the filter cake that solid content is 58% is obtained, by the filter cake, the filter cake 4wt ‰ Calgon, weight/mass percentage composition be 10% sodium polyacrylate solution mix, wherein in the sodium polyacrylate solution The percentage by weight of Sodium Polyacrylate and the filter cake is 2.5 ‰, and using weight/mass percentage composition as 40% sodium hydroxide solution Slurrying is stirred after regulation pH to 6.0, by grinding, delaminating after slurrying, makes particle diameter in the ore pulp after the filter cake slurrying micro- two The content of kaolin particle below rice accounts for the 92wt% of kaolin particle in the ore pulp after the filter cake slurrying, then will pass through and grind The ore pulp press filtration grind, delaminated to solid content is 65%, obtains kaolin filter cake;
2) the kaolin filter cake for obtaining step 1) is flashed under the conditions of -150pa tiny structures, dried, and is obtained moisture content and is existed Less than 2.0% kaolin dry powder;
3) combustion medium calcining step 2 is used as using natural gas or liquefied petroleum gas) obtained by kaolin dry powder, calcining temperature Spend for 800 DEG C, calcination time 90min, obtain thermal activation kaolin;
4) the thermal activation kaolin for obtaining step 3) carries out depolymerization, and borate coupling is added in depolymehzation process The percentage by weight of agent, the dosage of boric acid ester coupler and the hot metakaolin is 2.0%, eliminates generation during high-temperature calcination Agglomeration lump and increase kaolin powder surface-active, obtain metakaolin, wherein, the use of the boric acid ester coupler The percentage by weight of amount and the hot metakaolin is 2%;
5) graphene oxide is prepared, after washing three times with watery hydrochloric acid and deionized water, is made into 2mg/mL solution;
6) pH to 8.0 is adjusted using sodium hydroxide solution, is heated to 70 DEG C, flow back 4h, is cooled to room temperature;
7) acid permanganate soln is added, 4h is reacted at room temperature, adds acetone, is centrifuged, freezes, obtains carboxylated graphite oxide Alkene;
8) by 65 parts of kaolin, 30 parts of carboxylated graphene oxide, 10 parts of low-alkalinity sulphoaluminate cement, 10 parts Flyash and 10 parts of plasticizer mix successively, obtain metakaolin gum filler 3.
150g metakaolins gum filler 3 is uniformly mixed with 1000g rubber-baseds with raw material, 70g auxiliary agents etc., then will Material preheats 15 minutes at 160 degree, then by mixture in 150 degree of mixings, mixing time 15 minutes, then by tabletting work Skill, elastomeric material 1 is made.
The composite tensile strength is more than 32MPa to elastomeric material 1 after tested, and elongation rate of tensile failure is more than 480%, aging Post-tensioning intensity and elongation rate of tensile failure rate of change:- 15~+20%, abrasion loss is less than 90mm3, and impact property reaches 12kJ/m2, Tensile strength reaches 30MPa, the Ω c of surface resistivity ρ s < 100 Ω cm, volume resistance ρ v < 100.
The better embodiment of the present invention is the foregoing is only, is not intended to limit the invention, all spirit in the present invention Within principle, any modification, equivalent substitution and improvements made etc., it should be included in the scope of the protection.

Claims (10)

1. a kind of metakaolin gum filler, it is characterised in that include each component of following parts by weight:Metakaolin 50~75 Part, 25~35 parts of carboxylated graphene oxide, 5~15 parts of low-alkalinity sulphoaluminate cement, 5~15 parts of flyash, plasticizer 5~ 15 parts.
2. metakaolin gum filler according to claim 1, it is characterised in that the system of the carboxylated graphene oxide Preparation Method comprises the following steps:
1) the ether hydroxylating of graphene oxide, is obtained into hydroxylating graphene oxide at backflow in graphene oxide water solution;
2) by the hydroxycarboxyl group of hydroxylating graphene oxide, carboxylated graphene oxide is obtained.
3. metakaolin gum filler according to claim 1, it is characterised in that:The metakaolin is by following steps system It is standby to obtain:
1) solid content is prepared as 65~70% kaolin filter cake, kaolinite of the particle diameter below two microns in the kaolin filter cake The content of soil particle accounts for more than the 85wt% of kaolin particle in the kaolin filter cake;
2) the kaolin filter cake that step 1) obtains is flashed under the conditions of -200pa~-100pa tiny structures, dried, obtained aqueous Kaolin dry powder of the rate below 2.5%;
3) kaolin dry powder that step 2) obtains is calcined, calcining heat be 750~850 DEG C, calcination time be 1.0~ 2.0 hours, obtain thermal activation kaolin;
4) the thermal activation kaolin obtained by step 3) is subjected to depolymerization, eliminates agglomeration caused by high-temperature calcination Caking, obtains metakaolin.
4. metakaolin gum filler according to claim 3, it is characterised in that in step 1), the filter of described kaolin The preparation method of cake is:The kaolin ore slurry that solid content is 10~15% is classified and settled, makes the kaolin ore slurry The content of kaolin particle of the middle particle diameter below two microns accounts for more than the 85wt% of kaolin particle in the kaolin ore slurry, It is 20~25% that kaolin ore slurry is concentrated into solid content again, by the kaolin ore slurry press filtration after concentration, obtains the solid content For 65~70% kaolin filter cake.
5. metakaolin gum filler according to claim 3, it is characterised in that:In step 3), the calcining heat is 750~820 DEG C, calcination time is 75min~100min.
6. metakaolin gum filler according to claim 1, it is characterised in that the metakaolin is by following steps system It is standby to obtain:
1) solid content is prepared as 68~70% kaolin filter cake, kaolinite of the particle diameter below two microns in the kaolin filter cake The content of soil particle accounts for 90~95wt% of kaolin particle in the kaolin filter cake;
2) the kaolin filter cake that step 1) obtains is flashed under the conditions of -200pa~-100pa tiny structures, dried, obtained aqueous Kaolin dry powder of the rate below 2.0%;
3) combustion medium calcining step 2 is used as using natural gas or liquefied petroleum gas) obtained by kaolin dry powder, calcining heat is 750~850 DEG C, calcination time is 1.5~2 hours, obtains thermal activation kaolin;
4) the thermal activation kaolin for obtaining step 3) carries out depolymerization, and boric acid ester coupler is added in depolymehzation process, is disappeared Caused agglomeration during except high-temperature calcination lumps and increases kaolin powder surface-active, obtains metakaolin, wherein, institute It is 1.5~2.5% that the dosage of boric acid ester coupler, which is stated, with the percentage by weight of the hot metakaolin.
7. metakaolin gum filler according to claim 6, it is characterised in that the kaolin in the step 1) The preparation method of filter cake is:The kaolin ore slurry that solid content is 10~15% is classified and settled, makes the kaolin ore In slurry the content of kaolin particle of the particle diameter below two microns account for the 85wt% of kaolin particle in the kaolin ore slurry with On, then the pH to 2.0~3.0 using weight/mass percentage composition as 98% concentrated sulfuric acid regulation kaolin ore slurry, add the height Ridge 5~8wt of soil ore pulp solid content ‰ sodium dithionite stirring bleaching, control whiteness is more than 85%, then by kaolin ore It is 20~25% that slurry, which is concentrated into solid content, by the kaolin ore slurry press filtration after concentration, obtains the filter cake that solid content is 55~60%, The filter cake, the calgon of the 4~5wt of filter cake ‰, the sodium polyacrylate solution that weight/mass percentage composition is 10% are mixed Close, wherein the percentage by weight of Sodium Polyacrylate and the filter cake is 2~3 ‰ in the sodium polyacrylate solution, and with quality The sodium hydroxide solution that percentage composition is 40% stirs slurrying after adjusting pH to 6.0, by grinding, delaminating after slurrying, makes described The content of kaolin particle of the particle diameter below two microns is accounted in the ore pulp after the filter cake slurrying in ore pulp after filter cake slurrying 90~95wt% of kaolin particle, then will be 64~67% by grinding, the ore pulp press filtration delaminated to solid content, obtain kaolinite Native filter cake.
8. metakaolin gum filler according to claim 6, it is characterised in that:The calcining temperature in the step 3) Spend for 780~820 DEG C, calcination time is 80min~100min.
9. according to any described metakaolin gum filler of claim 6 to 8, it is characterised in that:In the step 4) The percentage by weight of the dosage of the boric acid ester coupler added in depolymehzation process and the hot metakaolin is 2.0%.
A kind of 10. preparation method of metakaolin gum filler according to any one of claims 1 to 9, it is characterised in that bag Include following steps:In parts by weight, by 50~75 parts of kaolin, 25~35 parts of carboxylated graphene oxide, 5~15 parts Low-alkalinity sulphoaluminate cement, 5~15 parts of flyash and 5~15 parts of plasticizer mix successively, obtain metakaolin rubber Filler.
CN201711022164.4A 2017-10-26 2017-10-26 A kind of metakaolin gum filler and preparation method thereof Pending CN107857901A (en)

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CN112940188B (en) * 2021-02-25 2022-04-29 深圳市台钜电工有限公司 Anti-bending rubber material for data line and preparation method thereof
CN113861726A (en) * 2021-09-29 2021-12-31 广东宝丰陶瓷科技发展股份有限公司 Preparation method for low-grade kaolin composite efficient activation modification

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Application publication date: 20180330