CN111748219B - Surface modification method of conductive material and application of conductive material in polyacrylate coating - Google Patents
Surface modification method of conductive material and application of conductive material in polyacrylate coating Download PDFInfo
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- C09D155/00—Coating compositions based on homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C09D123/00 - C09D153/00
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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Abstract
The invention relates to an organic surface modification method of inorganic composite powder, in particular to a surface modification method of a conductive material and application thereof in polyacrylate coating. The modified inorganic conductive material is added into the polyacrylate coating, and the acidic groups on the surface of the modified conductive powder can be combined with the molecular chain of the polyacrylate film-forming resin by chemical bonds, so that the cross-linking degree among the molecular chains of the polyacrylate is improved, and the dispersion stability of the coating and the conductive and mechanical properties of the coating are improved integrally.
Description
Technical Field
The invention relates to a novel organic surface modification method of inorganic composite powder, in particular to an organic surface modification method of inorganic conductive powder and a preparation method of conductive paint thereof.
Background
The conductive coating can be used for surface coating of products such as plastics, rubber, synthetic fibers, glass and the like, and is widely applied to industries such as automobiles, household appliances, electronic instruments, packaging, building materials and the like. The conductive paint used at present is usually prepared by adding inorganic conductive material into insulating polymer (film-forming resin) to make the coating layer have conductive property after curing and film-forming. The key technical problem is that the interface bonding capability between the inorganic conductive material and the film-forming resin greatly affects the stability, dispersibility, conductivity, mechanical properties and the like of the coating (layer). At present, the effective approach is to add the organic modifier with reactive groups into the coating after the surface of the inorganic conductive material is functionally modified. The water-based polyacrylate emulsion is a film-forming resin commonly used in conductive coatings due to the advantages of convenient construction, environmental protection and the like. In the previous research work, inorganic conductive materials (Chinese patent, preparation method and CN201710578196.6, CN201710578228.2 or CN201710594663.4) are added into aqueous polyacrylate emulsion (Chinese patent, application No. 201810875363.8 and application No. 201910336421.4), and the prepared conductive coating has the problems of short storage period, layering and the like, and the coating after being cured into a film has poor conductive performance and mechanical property and the like. The key is how to carry out organic surface modification on the inorganic conductive material and improve the chemical bond acting force between the inorganic conductive material and the molecular chain of the water-based polyacrylate. In addition, how to realize the conversion from the aqueous polyacrylate emulsion to the cured hydrophobic coating in the coating process is another key technical problem to be solved by the conductive coating.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides an organic surface modification method of inorganic conductive powder and a preparation method of the inorganic conductive powder in an acrylate conductive coating, and aims to improve the interface bonding performance between an inorganic conductive material and a polyacrylate molecular chain and the crosslinking degree between the polyacrylate molecular chains and simultaneously realize the conversion of a water-based polyacrylate emulsion to a cured hydrophobic coating.
In order to solve the technical problems, the invention adopts the technical scheme that:
1. spraying chlorosilane into the conductive powder while stirring at room temperature, wherein the mass ratio of the chlorosilane to the conductive powder is 0.03-0.1: 1; after spraying, quickly and continuously introducing ammonia gas into the chlorosilane-sprayed modified conductive powder for continuous adsorption reaction for 20-40 minutes, wherein the flow of the ammonia gas is controlled to be 0.03-0.1 cubic meter per second, so as to prepare amino functionalized modified conductive powder;
the conductive powder in the step 1 is an attapulgite/conductive polymer composite material (preferably an attapulgite/polyaniline composite material), the preparation method is the same as that of the Chinese patent invention CN201710578196.6, the attapulgite-mica-based conductive composite material, the preparation method is the same as that of the Chinese patent invention CN201710578228.2 or the three-dimensional attapulgite-mica-based conductive composite material, and the preparation method is the same as that of the Chinese patent invention CN 201710594663.4;
the chlorosilane in the step 1 is one of methyltrichlorosilane (molecular weight of 149.45) or 3-chloropropyltrichlorosilane (molecular weight of 211.98).
2. Dispersing the amino functionalized modified conductive powder prepared in the step 1 into deionized water, wherein the mass ratio of the amino functionalized modified conductive powder to the deionized water is 0.05-0.2: 1, adding amino trimethylene phosphonic acid into the system while stirring, wherein the mass ratio of the amino trimethylene phosphonic acid to the modified conductive powder is 0.02-0.1: 1, continuing stirring for reaction for 30-60 minutes, filtering, washing, drying at 60-80 ℃, and crushing to obtain organic acid modified conductive powder;
3. adding the organic modified conductive powder obtained in the step 2, the film-forming resin emulsion, the dispersing agent, the flatting agent and the defoaming agent into a kettle, wherein: the polyacrylate conductive coating is prepared by uniformly stirring and dispersing 30-50 parts by weight of film-forming resin emulsion, 3-10 parts by weight of organic modified conductive powder, 0.5-1.5 parts by weight of dispersing agent, 0.1-0.3 part by weight of defoaming agent and 0.2-0.6 part by weight of flatting agent.
The film-forming resin in the step 3 is water-based polyacrylate emulsion, and specifically is one of Chinese invention patent (application number: 201810875363.8) or Chinese invention patent (application number: 201910336421.4).
The dispersant in the step 3 is one of BYK-163, BYK-180, BYK-P104 and BYK-P105; the defoaming agent is one of BYK-141, BYK-053, BYK-070 and BYK-066N; the leveling agent is one of BYK-333, BYK-348, BYK-346 and BYK-358N.
The invention has the beneficial effects that:
1. compared with the inorganic conductive powder directly modified by amino silane coupling agent (such as aminopropyl triethoxysilane), the invention firstly adopts chlorosilane to modify the inorganic conductive powder and then adopts a gas phase method for modification, namely, ammonia is introduced to aminate the inorganic conductive powder, and the advantages are that: the reaction activity of the chlorosilane is obviously stronger than that of a silane coupling agent, so that the content of the chlorosilane modifying agent grafted on the surface of the inorganic conductive powder is higher than that of the silane coupling agent, and the improvement of the organic surface modification effect of the inorganic conductive powder is facilitated; secondly, the introduced ammonia reacts with Cl groups which are not completely reacted in the chlorosilane on the surface of the conductive powder to generate Si-N bonds, namely, amino groups are grafted on the surface of the conductive powder, thereby realizing the amino functionalization on the surface of the inorganic conductive powder material.
2. The invention adopts organic acid-amino trimethylene phosphonic acid to further modify aminated inorganic conductive powder, and the amino trimethylene phosphonic acid can react with amino groups on the surface of the inorganic conductive powder and is combined in a chemical bond form; thereby preparing the organic phosphonic acid modified inorganic conductive powder material. The modified inorganic conductive material is added into the polyacrylate coating, and the acid groups on the surface of the modified conductive powder can be combined with hydrophilic groups (such as hydroxyl) in the organic molecular chain of polyacrylate (film-forming resin) by chemical bonds, so that the interface combination performance between the conductive powder and the film-forming resin is improved, and the dispersion stability of the coating is improved on the whole; on the other hand, the cross-linking effect is achieved, the cross-linking degree between polyacrylate molecular chains is improved, and the number of hydrophilic groups in polyacrylate molecular chains is reduced to a certain extent, so that the conductivity, mechanical property and water resistance of the coating are effectively improved.
Drawings
FIG. 1 shows Thermogravimetric (TG) curves of amino-functionalized modified conductive powders of example 4 and comparative example 1. As can be seen from FIG. 1, under the condition that other modification processes are not changed, compared with the modification of the traditional aminosilane coupling agent, the weight loss rate of the modified conductive powder by the chlorosilane-ammonia gas phase method is higher, which shows that the organic modification method adopted by the invention has better modification effect on the conductive powder.
FIG. 2 is a photograph of an actual coating for measuring surface resistance in example 4.
Detailed Description
Example 1
1. Spraying 0.3 kg of methyltrichlorosilane into 10.0 kg of attapulgite/polyaniline composite conductive powder (the preparation method is CN201710578196.6 example 4) while stirring at room temperature; after spraying, quickly and continuously introducing ammonia gas into the silane modified conductive powder for adsorption reaction for 20 minutes, wherein the flow of the ammonia gas is controlled to be 0.03 cubic meter per second, and thus, the amino functional modified conductive powder is prepared;
2. dispersing 10 kg of amino functionalized modified conductive powder into 200 kg of deionized water, adding 0.2 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reaction for 30 minutes, filtering, washing, drying at 60 ℃, and crushing to obtain organic acid modified conductive powder;
3. 30 parts of polyacrylate emulsion (the preparation method is CN201810875363.8 example 1: polyglycolide modified polyacrylate emulsion), 3 parts of organic modified conductive powder, 0.5 part of BYK-163 dispersing agent, 0.1 part of BYK-141 defoaming agent and 0.2 part of BYK-333 leveling agent are added into a kettle and stirred and dispersed uniformly to prepare the polyacrylate conductive coating.
Example 2
1. Spraying 1.0 kg of 3-chloropropyltrichlorosilane into 10.0 kg of three-dimensional attapulgite-mica-based conductive composite conductive powder (the preparation method is the embodiment 1 of the Chinese invention patent CN201710594663.4) while stirring at room temperature; after spraying, quickly and continuously introducing ammonia gas into the silane modified conductive powder for adsorption reaction for 35 minutes, wherein the flow of the ammonia gas is controlled to be 0.065 cubic meter per second, and thus, the amino functionalized modified conductive powder is prepared;
2. dispersing 10 kg of amino functionalized modified conductive powder into 50 kg of deionized water, adding 1.0 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reaction for 60 minutes, filtering, washing, drying at 80 ℃, and crushing to obtain organic acid modified conductive powder;
3. 50 parts of polyacrylate emulsion (the preparation method is that the preparation method is Chinese invention patent application No. 201910336421.4 embodiment 1: organic silicon/epoxy resin synergistic modified acrylate composite emulsion), 10 parts of organic modified conductive powder, 1.5 parts of BYK-180 dispersant, 0.3 part of BYK-053 defoamer and 0.6 part of BYK-flatting agent are added into a kettle to be stirred and dispersed uniformly, thus obtaining the polyacrylate conductive coating.
Example 3
1. Spraying 0.65 kg of methyltrichlorosilane into 10.0 kg of attapulgite-mica/polyaniline conductive composite material conductive powder (the preparation method is CN201710578228.2 example 1 of the invention patent in China) while stirring at room temperature; after spraying, quickly and continuously introducing ammonia gas into the silane modified conductive powder for adsorption reaction for 30 minutes, wherein the flow of the ammonia gas is controlled to be 0.1 cubic meter per second, and thus, the amino functionalized modified conductive powder is prepared;
2. dispersing 10 kg of amino functionalized modified conductive powder into 100 kg of deionized water, adding 0.6 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reaction for 45 minutes, filtering, washing, drying at 70 ℃, and crushing to obtain organic acid modified conductive powder;
3. 40 parts of polyacrylate emulsion (the preparation method is that polyglycolide modified polyacrylate emulsion in the embodiment 1 of the Chinese invention patent application No. 201810875363.8), 6.5 parts of organic modified conductive powder, 1.0 part of BYK-P104 dispersant, 0.2 part of BYK-070 defoaming agent and 0.4 part of BYK-346 leveling agent are added into a kettle to be stirred and dispersed uniformly, thus obtaining the polyacrylate conductive coating.
Example 4
1. Spraying 0.5 kg of 3-chloropropyltrichlorosilane into 10.0 kg of three-dimensional attapulgite-mica-based conductive composite conductive powder (the preparation method is the same as that in embodiment 1 of Chinese patent CN201710594663.4) while stirring at room temperature; after spraying, quickly and continuously introducing ammonia gas into the silane modified conductive powder for adsorption reaction for 40 minutes, wherein the flow of the ammonia gas is controlled to be 0.08 cubic meter per second, and thus, the amino functionalized modified conductive powder is prepared;
2. dispersing 10 kg of amino functionalized modified conductive powder into 125 kg of deionized water, adding 0.5 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reaction for 50 minutes, filtering, washing, drying at 75 ℃, and crushing to obtain organic acid modified conductive powder;
3. 45 parts of polyacrylate emulsion (the preparation method is that the organic silicon/epoxy resin synergistic modified acrylate composite emulsion in the embodiment 1 of the Chinese invention patent application number: 201910336421.4) and 8 parts of organic modified conductive powder are taken, 1.3 parts of BYK-P105 dispersant, 0.3 part of BYK-066N defoamer and 0.3 part of BYK-358N flatting agent are added into a kettle to be stirred and dispersed uniformly, and then the polyacrylate conductive coating is prepared.
Comparative example 1
In comparative example 1, the procedure of modifying conductive powder with 3-chloropropyltrichlorosilane and ammonia gas used in step 1 in example 4 was changed to a procedure of modifying conductive powder with aminosilane coupling agent (aminopropyltriethoxysilane), and other process conditions were not changed, and the specific operation steps were as follows:
1. spraying 0.5 kg aminopropyltriethoxysilane into 10.0 kg conductive powder (the preparation method is the same as the Chinese invention patent CN201710594663.4) while stirring at room temperature, and continuously stirring for reaction for 40 minutes after spraying, wherein the flow rate of ammonia gas is controlled to be 0.08 cubic meter/second, so as to obtain amino functionalized modified conductive powder;
2. dispersing 10 kg of amino functionalized modified conductive powder into 125 kg of deionized water, adding 0.5 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reaction for 50 minutes, filtering, washing, drying at 75 ℃, and crushing to obtain organic acid modified conductive powder;
3. 45 parts of polyacrylate emulsion (the preparation method is the same as the preparation method of the Chinese invention patent application number CN201910336421.4), 8 parts of organic acid modified conductive powder, 1.3 parts of BYK-P105 dispersing agent, 0.3 part of BYK-066N defoaming agent and 0.3 part of BYK-358N flatting agent are added into a kettle to be stirred and dispersed uniformly, and then the acrylate conductive coating is prepared.
Comparative example 2
In comparative example 2, the steps 1 and 2 in example 4 are removed, other process conditions are not changed, and the specific operation steps are as follows:
adding 45 parts of polyacrylate emulsion (the preparation method is the same as CN201910336421.4), 8 parts of conductive powder (the preparation method is the same as CN201710594663.4), 1.3 parts of BYK-P105 dispersing agent, 0.3 part of BYK-066N defoaming agent and 0.3 part of BYK-358N flatting agent into a kettle, and uniformly stirring and dispersing to obtain the polyacrylate conductive coating.
Comparative example 3
In comparative example 3, the step 1 in example 4 was removed, and other process conditions were not changed, and the specific operation steps were as follows:
1. dispersing 10 kg of conductive powder into 125 kg of deionized water, adding 0.5 kg of amino trimethylene phosphonic acid into the system while stirring, continuously stirring for reacting for 50 minutes, filtering, washing, drying at 75 ℃, and crushing to obtain organic acid modified conductive powder;
2. 45 parts of polyacrylate emulsion (the preparation method is the same as the preparation method of the Chinese invention patent application number: 201910336421.4), 8 parts of organic acid modified conductive powder, 1.3 parts of BYK-P105 dispersing agent, 0.3 part of BYK-066N defoaming agent and 0.3 part of BYK-358N flatting agent are added into a kettle to be stirred and dispersed uniformly, and then the polyacrylate conductive coating is prepared.
Comparative example 4
In comparative example 4, the step 2 in example 4 was removed, and other process conditions were not changed, and the specific operation steps were as follows:
1. spraying 0.5 kg of 3-chloropropyltrichlorosilane into 10.0 kg of conductive powder (the preparation method is the same as the Chinese patent CN201710594663.4) while stirring at room temperature; after spraying, quickly and continuously introducing ammonia gas into the silane modified conductive powder for adsorption reaction for 40 minutes, wherein the flow of the ammonia gas is controlled to be 0.08 cubic meter per second, and thus, the amino functionalized modified conductive powder is prepared;
2. 45 parts of polyacrylate emulsion (the preparation method is the same as that of Chinese invention patent CN201910336421.4), 8 parts of amino functional modified conductive powder, 1.3 parts of BYK-P105 dispersing agent, 0.3 part of BYK-066N defoaming agent and 0.3 part of BYK-358N flatting agent are added into a kettle to be stirred and dispersed uniformly, and then the polyacrylate conductive coating is prepared.
Evaluation of Performance
The coatings prepared in examples 1 to 4 and comparative examples 1 to 4 were uniformly applied to ABS plastic panels and polished tinplate using a wire bar coater (80 mesh), the coating thickness was controlled at 50 μm, and dried (cured) at 80 ℃ for 30 minutes to obtain conductive composite coatings, and the related performance tests were carried out, with the test results as in table 1.
And (3) surface resistance testing: and measuring the surface resistance values of different positions of the ABS plastic plate coating by using a Model-800 surface resistance tester, and measuring three times to obtain an average value.
Mechanical property testing was performed on tinplate coatings. And (3) impact strength test: the weight is 1kg, expressed as the maximum height which does not cause damage to the coating on the tinplate, in kg cm, according to the measurement standard GB/T1732-1993 'paint film impact resistance measurement method'. And (3) testing the adhesive force: the adhesion of the coating was determined using GB/T9286-1998. And (3) hardness testing: measured according to GB/T6739-2006.
Water contact angle test: the water contact angle of the coating surface was determined using a DSA25 model optical water contact angle analyzer (KRUSS, Germany). And (3) placing the ABS plastic plate coating under an optical water contact angle analyzer to perform a water contact angle test, performing a parallel test for three times, and taking an average value.
TABLE 1
Claims (8)
1. A surface modification method of a conductive material is characterized by comprising the following modification steps:
(1) spraying chlorosilane into the conductive powder while stirring at room temperature, continuously introducing ammonia gas into the chlorosilane-sprayed modified conductive powder after spraying to continue adsorption reaction, and obtaining amino functionalized modified conductive powder after the reaction is finished;
(2) dispersing the amino functionalized modified conductive powder into deionized water, adding aminotrimethylene phosphonic acid into the system while stirring, continuously stirring for reaction, filtering, washing, drying and crushing after the reaction to obtain the modified conductive powder.
2. The method for modifying the surface of a conductive material according to claim 1, wherein the chlorosilane is one of methyltrichlorosilane and 3-chloropropyltrichlorosilane.
3. The surface modification method of the conductive material according to claim 1, wherein the conductive powder is an attapulgite-mica-based conductive composite material or an attapulgite/conductive polymer composite material.
4. The method for modifying the surface of a conductive material according to claim 1, wherein the mass ratio of the chlorosilane to the conductive powder in the step (1) is 0.03-0.1: 1.
5. The method for modifying the surface of a conductive material according to claim 1, wherein ammonia gas is introduced for adsorption reaction for 20 to 40 minutes.
6. The method for modifying the surface of a conductive material according to claim 1, wherein the mass ratio of the aminotrimethylene phosphonic acid to the modified conductive powder in the step (2) is 0.02 to 0.1:1, and the reaction is carried out with stirring for 30 to 60 minutes.
7. Use of a conductive material modified by the method according to any one of claims 1 to 6 in a polyacrylate emulsion.
8. The application of the conductive material in polyacrylate emulsion according to claim 7, wherein the polyacrylate conductive coating is obtained by uniformly stirring and dispersing 30-50 parts of water-based polyacrylate emulsion, 3-10 parts of modified conductive powder, 0.5-1.5 parts of dispersing agent, 0.1-0.3 part of defoaming agent and 0.2-0.6 part of leveling agent.
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