CN112300602A - Modification method of inorganic filler - Google Patents

Modification method of inorganic filler Download PDF

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Publication number
CN112300602A
CN112300602A CN202011186934.0A CN202011186934A CN112300602A CN 112300602 A CN112300602 A CN 112300602A CN 202011186934 A CN202011186934 A CN 202011186934A CN 112300602 A CN112300602 A CN 112300602A
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inorganic filler
mill
powder
modifying
modification
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王益庆
王帅
沈家锋
李晓林
张立群
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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    • C09C1/30—Silicic acid
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    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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Abstract

The invention provides a method for modifying inorganic filler, which comprises the steps of crushing the inorganic filler to a certain mesh number by a mechanical crusher, carrying out superfine grinding by a jet mill to obtain superfine powder, carrying out high-temperature treatment on the superfine powder, and introducing the superfine powder into a powder modifying machine to add an activating agent and a coupling agent for surface modification to obtain the modified inorganic filler. The inorganic filler obtained by the method has superfine and uniform particle size distribution, good surface modification effect, high maturity of process equipment and easy industrialization, and can be used as a reinforcing filler for silicon rubber products.

Description

Modification method of inorganic filler
Technical Field
The invention relates to the technical field of fine chemical engineering application, in particular to a modification method of an inorganic filler, which is mainly applied to reinforcement of a silicon rubber product.
Background
The silicon rubber is widely applied to the fields of industry and agriculture, medical industry, aerospace and the like due to the excellent performance of the silicon rubber. The silicon rubber has special basic structural units, a main chain is formed by silicon oxygen chain links, and a side chain is connected with organic groups such as methyl, ethyl, vinyl, phenyl and the like through silicon atoms, so that the silicon rubber has the functions of inorganic substances and the characteristics of organic substances such as electrical insulation, aging resistance, high and low temperature resistance, solvent resistance and the like. But the raw silicon rubber has poor mechanical property and low thermal conductivity. Therefore, it is necessary to add an inorganic filler capable of improving the physicochemical properties thereof to satisfy various requirements. For example, the carbon black is filled into the silicon rubber to prepare a conductive material with the similar high conductive level; the white carbon black, the calcium carbonate and the silicon micropowder can be used as a reinforcing agent of the silicone rubber, so that the mechanical property of the silicone rubber is greatly improved; ceramic materials such as alumina, boron nitride, silicon carbide, zinc oxide, and carbon fibers, graphite, graphene, carbon nanotubes, etc. introduced into polymer composite materials can improve the thermal conductivity of polymer matrix composite materials, and have been widely used as thermal conductive fillers.
However, the physical form and chemical structure of inorganic fillers are significantly different from those of silicone rubber, and the fillers are often subjected to surface modification to improve the compatibility with silicone rubber. For example, patent CN109354876A mixes a coupling agent whose main chain contains aromatic ring and heterocycle with an organic solvent and water according to a certain proportion, hydrolyzes to prepare a modifier emulsion, adds the modifier emulsion into a suspension of white carbon black, then filters, dries, and pulverizes to obtain modified white carbon black having good compatibility with silicone rubber, and the mechanical properties of silicone rubber are significantly improved.
Patent CN108752981A discloses a modified calcium carbonate and its application in preparing silicone rubber, which is prepared by first surface-treating calcium carbonate with pentaerythritol palmitate and sodium polysilsesquioxane sulfosuccinate, and then performing secondary surface modification with poly aminopropyl methyl silsesquioxane and rapeseed oil fatty acid alkanolamide borate. The mechanical property of the modified calcium carbonate filled silicone rubber is obviously improved. However, the wet modification is complicated in operation, difficult to control the modification degree, and difficult to industrialize.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention provides a method for modifying inorganic filler, which comprises the steps of grinding the inorganic filler to a certain mesh number by a mechanical mill, carrying out superfine grinding by a jet mill to obtain superfine powder, carrying out high-temperature treatment on the superfine powder, introducing the superfine powder into a powder modifying machine, adding an activating agent and a coupling agent, and carrying out surface modification to obtain the modified inorganic filler. The inorganic filler obtained by the method has superfine and uniform particle size distribution, good surface modification effect, high maturity of process equipment and easy industrialization, and can be used as a reinforcing filler for silicon rubber products.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
1. a method for modifying an inorganic filler, comprising the steps of:
(a) the inorganic filler is crushed by a mechanical mill and is sieved by a powder classifier to obtain 800 meshes of 100-;
(b) then the inorganic filler in the step (a) is introduced into a jet mill, the ultrafine grinding is carried out by controlling the grinding conditions, and the obtained product is sieved by a powder classifier to obtain 800-6000-mesh powder with the bulk density of 30-120kg/m3The superfine powder of (1);
(c) performing high-temperature treatment on the ultrafine powder at the temperature of 200-600 ℃ for 0.1-3h, wherein the ignition loss is less than or equal to 2%;
(d) introducing into a powder modifying machine, adding an activating agent and an organosilane modifying agent for surface modification,
obtaining modified inorganic filler with the activation degree of more than or equal to 95 percent;
preferably, the amount of activator added is 0.1 to 10% by mass of the inorganic filler,
preferably, the organosilane modifier is added in an amount of 0.1-30% by mass of the inorganic filler, preferably in an amount of 0.1-30%, more preferably in an amount of 0.1-15%, more preferably in an amount of 1-20%, more preferably in an amount of 5-25%;
2. further, the inorganic filler is one or a combination of more of calcium carbonate, silica micropowder, aluminum dioxide, kaolin, barium sulfate, magnesium silicate and the like;
3. further, in the step (a), the mechanical mill is a dry ball mill, a tooth mill, a hammer mill, a knife mill, a turbine mill, a grinding mill or a milling mill;
preferably, the mechanical mill is a hammer mill, a knife mill or a grinding mill;
4. further, the jet mill in the step (b) is a flat jet mill, a fluidized bed opposite-spraying jet mill, a circulating pipe type jet mill, an opposite-spraying jet mill or a target jet mill;
5. further, in the step (c), the high-temperature treatment device is a dynamic calcining furnace, a rotary kiln and the like, the high-temperature treatment temperature is 200-;
preferably, the temperature of the treatment is 300-600 ℃, and the more preferred temperature is 400-550 ℃;
preferably, the high-temperature treatment time is 1-2 h;
6. further, in the step (d), the active agent is stearic acid, sodium stearate, zinc stearate, or the like.
7. Further, in step (d), the organosilane modifier: aminosilane coupling agent, silazane, aluminate coupling agent, silane coupling agent, titanate coupling agent, and the like.
8. Further, in the step (d), the powder modifying machine is a high-speed mixer, a double-cone mixer, a continuous powder modifying machine, a honeycomb mill, a disc nest mill and the like, the modifying temperature is 60-200 ℃, and the modifying time is 0.1-2 h.
This application differs from other modifications in that: the pulverization of the inorganic filler can easily realize ultrafine pulverization by pulverization and classification such as ball milling, mechanical pulverization, jet milling, etc., which are readily available techniques. However, inorganic fillers are used in silicone rubbers, and the inorganic fillers are difficult to disperse during kneading because of the low viscosity of the silicone rubber, and the ultrafine inorganic fillers are greatly affected by the state of accumulation among the inorganic filler particles, the size of aggregates, the surface hydroxyl content, and the like, depending on the dispersion, although the particle size is reduced.
Therefore, the particle size of the product is not controlled, the stacking state and the moisture content of the inorganic filler are controlled, and the particle size of 800-6000-order materials with the stacking density of 30-120kg/m are obtained by controlling the mechanical crushing power (not less than 70 percent of rated power), the crushing speed, the classification pressure of airflow crushing, the air inlet quantity and the feeding quantity3The low bulk density of the superfine inorganic filler is the key point, and different inorganic fillers can obtain 30-120kg/m by different control processes due to different structures3The ultrafine powder of (1) such as ground calcium carbonate is obtained by controlling the conditions to be relatively severe in order to obtain an ultrafine powder having a small bulk density, and thus the range of the bulk density is obtained by controlling the pulverizing equipment during the pulverizing process to a smaller rangeAre important process parameters provided by the application.
After the high-temperature treatment of the sample, the hydroxyl and free water between particles are treated, the structure between aggregates is destroyed, and the stacking state of the inorganic filler is crushed and treated at high temperature to obtain the structure with lower stacking density (30-100 kg/m)3)。
And then the inorganic filler with lower bulk density is organically modified, and the dispersion of the inorganic filler in the silicone rubber is improved again by utilizing the principle of similarity and intermiscibility, so that the effect of reinforcing is greatly improved. And modification equipment such as a high-speed mixer, a honeycomb mill and a disc nest mill used for modification can ensure that the inorganic filler is fully contacted with the modifier in the dry modification process, so that the modification effect is improved. In particular to a honeycomb mill and a disc nest mill type modifying machine, because a large number of hollow disc structures exist in a grinding cavity, a plurality of nest type rotational flows are formed between the discs and a special lining plate, and the air flow impact force between the disc structures and the special lining plate can fully break up solid powder. The contact between the inorganic filler and the modifier can be controlled by controlling the wind speed, the feeding amount and the like, and meanwhile, the system can be heated, so that the modifier is fully contacted with the inorganic filler, the coating modification is better completed, the coating rate is greatly improved, and the modified inorganic filler with high activation degree is obtained.
Therefore, on the basis of modification by crushing with a traditional crusher, the method mainly optimizes the bulk density, hydroxyl content and moisture content of the inorganic filler and the activation degree of a modified product, and obtains the inorganic filler dry modification process with high efficiency, low cost and excellent modification effect.
Compared with the prior art, the invention has the beneficial effects that:
(1) the dry modification method of the inorganic filler provided by the invention is convenient, simple and easy to operate, can refine inorganic filler particles to 2000-4000 meshes, and has small bulk density.
(2) The modification method of the inorganic filler provided by the invention has the advantages of high equipment maturity, easy industrialization, high product activation degree and suitability for the production fields of silicon rubber products and the like.
(3) The modification method of the inorganic filler provided by the invention has the advantages of small particles, uniform particle size distribution, stable quality, small porosity, high yield, good surface modification effect and the like.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following detailed description, but those skilled in the art will understand that the following described examples are some, not all, of the examples of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present 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. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
100kg of 400-mesh silicon micropowder is crushed to 800 meshes by a knife type crusher and then is subjected to superfine grinding to 3000 meshes by a jet mill, and the bulk density is 30kg/m3And performing high-temperature treatment at 400 ℃ for 1h in a dynamic calcining furnace, controlling the ignition loss to be less than or equal to 2%, introducing the superfine powder into a honeycomb mill for modification, adding 0.1kg of sodium stearate and 1kg of polydimethylsiloxane for surface modification at the modification temperature of 200 ℃ for 1h to obtain modified silicon micropowder, wherein the activation degree of the modified superfine silicon micropowder is more than or equal to 95%.
Example 2
Pulverizing 100kg of 20 mesh kaolin into 100 mesh by hammer mill, and micronizing into 8000 mesh by flat jet mill with bulk density of 120kg/m3And performing high-temperature treatment at 600 ℃ for 0.1h in a dynamic calcining furnace, controlling the ignition loss to be less than or equal to 1%, introducing the ultrafine powder into a high-speed mixer for modification, adding 1kg of stearic acid and 5kg of KH550 for surface modification at the modification temperature of 60 ℃ for 0.1h to obtain modified ultrafine kaolin, wherein the activation degree of the obtained modified ultrafine kaolin is more than or equal to 99%.
Example 3
100kg of light calcium carbonate with 100 meshes is ground into 500 meshes by a grinding type grinder, and then is subjected to superfine grinding to 6000 meshes by a jet mill through a flat fluidized bed, and the bulk density is 30kg/m3And carrying out high-temperature treatment at 200 ℃ for 3h in a rotary kiln, controlling the ignition loss to be less than or equal to 1%, introducing the ultrafine powder into a continuous powder modifying machine for modification, adding 1kg of stearic acid and 0.1kg of Si-69 for surface modification at the modification temperature of 90 ℃ for 0.5h to obtain modified ultrafine calcium carbonate, wherein the activation degree of the modified ultrafine calcium carbonate is greater than or equal to 96%.
Example 4
100kg of 80-mesh barium sulfate is ground to 400 meshes by a dry ball mill and then is subjected to ultrafine grinding to 4000 meshes by a circulating tube type air flow mill, and the bulk density is 80kg/m3And performing high-temperature treatment at 600 ℃ for 2 hours in a dynamic calcining furnace, controlling the ignition loss to be less than or equal to 1%, introducing the ultrafine powder into a disc nest mill for modification, adding 1kg of zinc stearate and 7kg of KH570 for surface modification, wherein the modification temperature is 170 ℃, and the modification time is 0.1 hour, so as to obtain modified ultrafine barium sulfate, and the activation degree of the obtained modified ultrafine barium sulfate is more than or equal to 95%.
Example 5
100kg of magnesium silicate of 100 meshes is ground into 300 meshes by a dry ball mill and then is subjected to superfine grinding to 3000 meshes by a circulating pipe type air flow mill, and the bulk density is 100kg/m3And carrying out high-temperature treatment at 600 ℃ for 0.8h in a dynamic calcining furnace, controlling the ignition loss to be less than or equal to 1%, introducing the superfine powder into a honeycomb mill for modification, adding 1kg of stearic acid and 4kg of aminosilane coupling agent for surface modification, wherein the modification temperature is 120 ℃, and the modification time is 2h to obtain modified superfine magnesium silicate, wherein the activation degree of the obtained modified superfine magnesium silicate is more than or equal to 95%.
Example 6
100kg of 325-mesh aluminum dioxide is crushed to 600 meshes by a knife type crusher, and then the ultrafine crushing is carried out to 2000 meshes by a jet mill, the bulk density is 40kg/m3To obtain superfine powder, and treating at 450 deg.C for 1.5 hr in a dynamic calcining furnace to control the firingReducing by less than or equal to 2 percent, introducing the superfine powder into a honeycomb mill for modification, adding 2kg of stearic acid and 7.5kg of aminosilane for surface modification at the modification temperature of 180 ℃ for 1 hour to obtain modified superfine aluminum dioxide, wherein the activation degree of the modified superfine aluminum dioxide is more than or equal to 98 percent.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are merely illustrative of the technical solution of the present invention and are not restrictive; those of ordinary skill in the art will understand that: modifications may be made to the above-described embodiments, or equivalents may be substituted for some or all of the features thereof without departing from the spirit and scope of the present invention; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; it is therefore intended to cover in the appended claims all such alternatives and modifications that are within the scope of the invention.

Claims (8)

1. A method for modifying an inorganic filler, comprising the steps of:
(a) the inorganic filler is crushed by a mechanical mill and is sieved by a powder classifier to obtain 800 meshes of 100-;
(b) then the inorganic filler in the step (a) is introduced into a jet mill, the ultrafine grinding is carried out under the controlled grinding condition, and the mixture is sieved by a powder classifier to obtain 800-6000-mesh powder with the bulk density of 30-120kg/m3The superfine powder of (1);
(c) performing high-temperature treatment on the ultrafine powder at the temperature of 200-600 ℃ for 0.1-3h, wherein the ignition loss is less than or equal to 2%;
(d) introducing into a powder modifying machine, adding an activating agent and an organosilane modifying agent for surface modification to obtain a modified inorganic filler, wherein the activation degree is more than or equal to 95%; the modification temperature is 60-200 ℃, and the modification time is 0.1-2 h;
the addition amount of the activating agent is 0.1-10% of the mass of the inorganic filler,
the addition amount of the organosilane modifier is 0.1-30% of the mass of the inorganic filler.
2. The method for modifying an inorganic filler according to claim 1, wherein the inorganic filler is one or a combination of calcium carbonate, silica powder, aluminum dioxide, kaolin, barium sulfate and magnesium silicate.
3. The method for modifying an inorganic filler according to claim 1, wherein in the step (a), the mechanical mill is a dry ball mill, a tooth mill, a hammer mill, a knife mill, a turbine mill, a grinding mill or a milling mill.
4. The method of claim 1, wherein the jet mill in step (b) is a flat jet mill, a fluidized bed counter-jet mill, a circulating tube jet mill, a counter-jet mill, or a target jet mill.
5. The method for modifying an inorganic filler according to claim 1, wherein the temperature of the treatment in step (c) is 300-600 ℃ and the treatment time is 1-2 h.
6. The method of claim 1, wherein in step (d), the active agent is stearic acid, sodium stearate, or zinc stearate.
7. A process for modifying an inorganic filler according to claim 1, wherein in step (d), the organosilane modifier: aminosilane coupling agent, silazane, aluminate coupling agent, silane coupling agent or titanate coupling agent, etc.
8. The method of claim 1, wherein in step (d), the powder modifier is a high-speed mixer, a double-cone mixer, a continuous powder modifier, a honeycomb mill or a disc-nest mill.
CN202011186934.0A 2020-10-29 2020-10-29 Modification method of inorganic filler Pending CN112300602A (en)

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CN113549342A (en) * 2021-09-02 2021-10-26 和也健康科技有限公司 Method for modifying surface of stone needle powder
CN113636846A (en) * 2021-10-14 2021-11-12 季华实验室 Ceramic powder modifying method
CN114800763A (en) * 2022-05-23 2022-07-29 广西科学院 Preparation method of high-strength shaving board
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CN115066469A (en) * 2021-05-07 2022-09-16 德州学院 Method for preparing composite pigment and filler for coating by using gasified slag
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113004718A (en) * 2021-03-15 2021-06-22 刘绍辉 Superfine active silicon micro powder applied to electronic industry and preparation method thereof
CN115023301A (en) * 2021-04-29 2022-09-06 德州学院 Method for comprehensively utilizing oil sand tailings
CN115066469A (en) * 2021-05-07 2022-09-16 德州学院 Method for preparing composite pigment and filler for coating by using gasified slag
CN113549342A (en) * 2021-09-02 2021-10-26 和也健康科技有限公司 Method for modifying surface of stone needle powder
CN113636846A (en) * 2021-10-14 2021-11-12 季华实验室 Ceramic powder modifying method
CN113636846B (en) * 2021-10-14 2022-02-22 季华实验室 Ceramic powder modifying method
CN114800763A (en) * 2022-05-23 2022-07-29 广西科学院 Preparation method of high-strength shaving board
CN115739347A (en) * 2022-08-19 2023-03-07 王伟博 Preparation method and application of nano calcium carbonate for food additive
CN115521639A (en) * 2022-09-16 2022-12-27 绩溪县黄山石英有限公司 Superfine silica powder for latex paint
CN115778830A (en) * 2022-11-29 2023-03-14 安徽格锐新材料科技有限公司 Cosmetic-grade superfine synthetic mica powder and preparation method thereof

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Application publication date: 20210202