CN116023818A - Core-shell structured barium sulfate composite material and preparation method and application thereof - Google Patents
Core-shell structured barium sulfate composite material and preparation method and application thereof Download PDFInfo
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- CN116023818A CN116023818A CN202211730679.0A CN202211730679A CN116023818A CN 116023818 A CN116023818 A CN 116023818A CN 202211730679 A CN202211730679 A CN 202211730679A CN 116023818 A CN116023818 A CN 116023818A
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Abstract
The invention belongs to the technical field of coatings, and discloses a barium sulfate composite material with a core-shell structure, and a preparation method and application thereof. The barium sulfate composite material with the core-shell structure sequentially comprises a nano barium sulfate layer, a silane layer and a carbon quantum dot layer from inside to outside. The barium sulfate composite material with the core-shell structure is prepared by a two-step method, firstly, nano barium sulfate with positive charges on the surface is prepared, then, carbon quantum dots are mixed with the nano barium sulfate with positive charges on the surface, and the nano barium sulfate with positive charges on the surface is assembled electrostatically. The paint has stable structure and good compatibility with basic paint formulas such as epoxy resin, acrylic resin and the like. The barium sulfate composite material with the core-shell structure is added into the coating, so that the UV radiation resistance of the coating can be effectively improved, the UV radiation resistance aging is prolonged, and the service life of the coating is prolonged; and the carbon quantum dots can be widely applied to the paint.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a barium sulfate composite material with a core-shell structure, and a preparation method and application thereof.
Background
The paint is a material widely used for coating the surface of an object to form a coating layer with good adhesion and certain strength. The paint can prolong the service life of the object, and make the object beautiful, etc. In the paint formulation, nano materials are an essential additive, and common additives comprise inorganic nano materials such as titanium dioxide, calcium carbonate, barium sulfate and the like. By adding the inorganic nano material, not only the firmness of the coating can be improved, but also the whiteness can be improved, and in addition, the effect of reducing the cost can be achieved.
The nano barium sulfate has similar refractive index with the base material (acrylic resin or epoxy resin, etc.) of the paint, has very high whiteness value and low cost, and is widely applied in paint formulas and has higher proportion. However, nano barium sulfate has a weak effect on improving the properties of the coating, such as UV radiation resistance, etc., when the coating is applied as a single additive only. Therefore, other anti-aging agents (such as UV absorbers) must be used in combination.
The existing commercial UV absorber can relieve ageing of UV radiation in sunlight on the paint, but has the problem of short timeliness, and is not matched with the service life of the paint which is longer than ten years.
Therefore, it is desirable to provide a coating containing nano barium sulfate that is highly effective and long-lasting against UV radiation, and that increases the useful life of the coating.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. Therefore, the invention provides a barium sulfate composite material with a core-shell structure, and a preparation method and application thereof. The barium sulfate composite material with the core-shell structure provided by the invention is added into the coating, so that the UV radiation resistance of the coating can be effectively improved, the UV radiation resistance aging can be prolonged, and the service life of the coating can be prolonged.
The first aspect of the invention provides a barium sulfate composite material with a core-shell structure.
Specifically, the barium sulfate composite material with the core-shell structure sequentially comprises a nano barium sulfate layer, a silane layer and a carbon quantum dot layer from inside to outside.
Preferably, the particle size of the nano barium sulfate is 20-700 nm; further preferably, the particle size of the nano barium sulfate is 50-400 nm.
The second aspect of the invention provides a preparation method of a barium sulfate composite material with a core-shell structure.
Specifically, the preparation method of the barium sulfate composite material with the core-shell structure comprises the following steps:
(1) Preparing nano barium sulfate with positive charges on the surface;
(2) Mixing the carbon quantum dots with the nano barium sulfate with positive charges on the surface prepared in the step (1), and carrying out electrostatic assembly in the stirring process to form the barium sulfate composite material with the core-shell structure.
Preferably, the nano barium sulfate with positive charges on the surface is obtained by carrying out surface modification on the nano barium sulfate by adopting silane with positive charges.
Preferably, the positively charged silane is an-NH-or-NH-containing silane 2 -a silane containing at least one methoxy or ethoxy group.
Further preferably, the positively charged silane is selected from at least one of 3-aminopropyl triethoxysilane, aminomethyl dimethyl ethoxysilane, 3-propylamine triethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, N- [3- (trimethoxysilyl) propyl ] ethylenediamine.
Preferably, the mass of the silane with positive charges is 0.1-5% of the mass of the nano barium sulfate; further preferably, the mass of the positively charged silane is 0.5% -3% of the mass of the nano barium sulfate.
More specifically, the preparation method of the barium sulfate composite material with the core-shell structure is selected from one of the modes (1) or (2):
(1) Dispersing nano barium sulfate and silane with positive charges in an alcohol solution, stirring for the first time, adding a carbon quantum dot solution, stirring for the second time, standing, separating solid from liquid to obtain a solid product, and drying the solid product to obtain the barium sulfate composite material with the core-shell structure; or (b)
(2) Mixing nano barium sulfate and silane with positive charges, adding carbon quantum dots, and stirring to obtain the barium sulfate composite material with the core-shell structure.
Preparing a barium sulfate composite material with a core-shell structure by a wet method, dispersing the nano barium sulfate and silane in an alcohol solution, and fully mixing to form a silane layer on the surface of the nano barium sulfate; and then adding a carbon quantum dot solution, continuing stirring, and carrying out electrostatic assembly on the negatively charged carbon quantum dots and the nano barium sulfate with the positively charged surface in the stirring process, wherein the carbon quantum dots are adsorbed on the surface of the nano barium sulfate to form a carbon quantum dot layer (a carbon quantum dot UV absorption layer), so as to form the barium sulfate composite material with the core-shell structure.
Preparing a barium sulfate composite material with a core-shell structure by a dry method, directly mixing the nano barium sulfate and the silane with positive charges, and fully contacting the nano barium sulfate with the silane by mechanical stirring to form a silane layer on the surface of the nano barium sulfate; and adding carbon quantum dots, continuing stirring, and carrying out electrostatic assembly on the carbon quantum dots with negative charges and the nano barium sulfate with positive charges on the surface in the stirring process, wherein the carbon quantum dots are adsorbed on the surface of the nano barium sulfate to form a carbon quantum dot layer (a carbon quantum dot UV absorption layer), so as to form the barium sulfate composite material with the core-shell structure.
The research shows that the core-shell structure barium sulfate composite material prepared by the wet method has more compact core-shell structure and strong stability, and can better improve the UV radiation resistance of the coating and the service life of the coating after being added into the coating.
Preferably, in the mode (1), the alcohol solution includes, but is not limited to, ethanol, methanol, and the like.
Preferably, in the mode (1) or (2), the carbon quantum dots are water-soluble carbon quantum dots. The carbon quantum dots are water-soluble carbon quantum dots with UV broad-spectrum absorption.
Preferably, in the mode (1), the concentration of the carbon quantum dot solution is 1 to 100mg/mL; further preferably, in the mode (1), the concentration of the carbon quantum dot solution is 5 to 50mg/mL; more preferably, in the above-mentioned mode (1), the concentration of the carbon quantum dot solution is 10 to 40mg/mL.
Preferably, in the mode (1), the mass ratio of the carbon quantum dots to the nano barium sulfate in the carbon quantum dot solution is (0.5-50): 1000; further preferably, in the above embodiment (1), the mass ratio of the carbon quantum dots to the nano barium sulfate in the carbon quantum dot solution is (1 to 30): 1000.
Preferably, in the above mode (1), the rotation speed of the primary stirring is 300 to 400r/min, and the time of the primary stirring is 10 to 100min.
Preferably, in the mode (1), the rotation speed of the secondary stirring is 450-600 r/min, and the time of the secondary stirring is 30-120 min.
Preferably, in the mode (1), the standing time is 12 to 48 hours; further preferably, in the above-mentioned mode (1), the time for the standing is 18 to 36 hours.
Preferably, in the mode (2), the mass ratio of the carbon quantum dots to the nano barium sulfate is (0.5-50): 1000; further preferably, in the above embodiment (2), the mass ratio of the carbon quantum dots to the nano barium sulfate is (1 to 30): 1000.
Preferably, in the mode (2), the stirring speed is 300-600 r/min, and the stirring time is 10-120 min.
The third aspect of the invention provides application of the barium sulfate composite material with the core-shell structure.
In particular to application of the barium sulfate composite material with the core-shell structure in paint.
In a third aspect, the invention provides a coating.
Specifically, the coating comprises the barium sulfate composite material with the core-shell structure.
Preferably, the coating is an oil-soluble coating.
Preferably, the coating further comprises an epoxy resin or/and an acrylic resin.
The research shows that the carbon quantum dot material has excellent UV absorption performance, including broad-spectrum UV absorption (200-400 nm), and the UV absorption has long-acting property. However, the carbon quantum dots are water-soluble materials and are incompatible with the oily paint which uses nano barium sulfate and epoxy resin as a base material. Aiming at the problem, the inventor successfully realizes the compounding of nano barium sulfate and carbon quantum dots by adopting a two-step method, and forms the barium sulfate composite material with a stable structure and a core-shell structure. The first step is to adopt N-containing silane with positive charges to carry out surface modification on the nano barium sulfate so that the surface of the nano barium sulfate is provided with positive charge groups; and in the second step, in the state of an aqueous solvent, compounding the positively charged nano barium sulfate with negatively charged carbon quantum dots by an electrostatic assembly method to obtain the composite material with the nano barium sulfate shell as the carbon quantum dots. The composite material not only keeps the intrinsic performance of the nano barium sulfate unchanged, but also has UV absorption performance. The barium sulfate composite material with the core-shell structure is used in the coating, so that the coating has high-efficiency and long-acting UV radiation resistance, and the service life of the coating can be prolonged; and the problem of incompatibility of the carbon quantum dots, nano barium sulfate and oily paint is solved, so that the carbon quantum dots can be widely used in paint, especially oily paint.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a barium sulfate composite material with a core-shell structure, which consists of inner core nanometer barium sulfate and outer shell carbon quantum dots. The composite material is prepared by a two-step method, firstly, nano barium sulfate with positive charges on the surface is prepared, then, carbon quantum dots are mixed with the nano barium sulfate with positive charges on the surface, and the nano barium sulfate with positive charges on the surface is assembled electrostatically. The composite material has stable structure and good compatibility with basic paint formulas such as epoxy resin, acrylic resin and the like. The barium sulfate composite material with the core-shell structure is added into the coating, so that the UV radiation resistance of the coating can be effectively improved, the UV radiation resistance aging is prolonged, and the service life of the coating is prolonged; and the carbon quantum dots can be widely applied to the paint.
Detailed Description
In order to make the technical solutions of the present invention more apparent to those skilled in the art, the following examples will be presented. It should be noted that the following examples do not limit the scope of the invention.
The particle size of the nano barium sulfate used in the following examples and base coating materials was 50 to 400nm. The starting materials, reagents or apparatus used, unless otherwise indicated, are those which are commercially available in conventional manner or may be obtained by methods known in the art.
Example 1
1000g of nano barium sulfate is weighed, 10g of 3-aminopropyl triethoxysilane is weighed and dispersed into 30mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 10mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 2
1000g of nano barium sulfate is weighed, 10g of aminomethyl dimethyl ethoxy silane is weighed and dispersed into 30mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 15mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 3
1000g of nano barium sulfate is weighed, 10g of bis [3- (triethoxysilyl) propyl ] amine is weighed and dispersed into 30mL of ethanol solvent, the nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 20mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 4
1000g of nano barium sulfate is weighed, 10g N- [3- (trimethoxy silicon based) propyl ] ethylenediamine is weighed and dispersed into 30mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 25mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 5
1000g of nano barium sulfate is weighed, 5g of 3-aminopropyl triethoxysilane is weighed and dispersed into 20mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 30mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 6
1000g of nano barium sulfate is weighed, 20g of 3-aminopropyl triethoxysilane is weighed and dispersed into 80mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 30min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 35mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 7
1000g of nano barium sulfate is weighed, 10g of 3-aminopropyl triethoxysilane is weighed and dispersed into 50mL of ethanol solvent, nano barium sulfate is added and mixed, and the mixture is placed into a high-speed stirrer to be stirred for 40min at 350 r/min; then adding 1mL of water-soluble carbon quantum dot with the mass concentration of 40mg/mL, continuously stirring for 60min at 500 rpm, standing for 24h, and performing suction filtration and drying treatment to obtain the core-shell structure nano barium sulfate composite material with the UV absorption function.
Example 8
Weighing 1000g of nano barium sulfate and 10g of 3-aminopropyl triethoxysilane, and mixing; weighing 40mg of solid carbon quantum dots, directly adding the solid carbon quantum dots into the mixture, then placing the mixture into a high-speed stirrer, stirring the mixture at a high speed for 30min at 500 rpm, taking out the mixture, and drying the mixture to obtain the core-shell nano barium sulfate composite material with the UV absorption function.
Example 9
Weighing 1000g of nano barium sulfate and 10g of 3-aminopropyl triethoxysilane, and mixing; weighing 60mg of solid carbon quantum dots, directly adding the solid carbon quantum dots into the mixture, then placing the mixture into a high-speed stirrer, stirring the mixture at a high speed for 30min at 500 rpm, taking out the mixture, and drying the mixture to obtain the core-shell nano barium sulfate composite material with the UV absorption function.
Product effect test
The core-shell structure nano barium sulfate composite materials prepared in examples 1 to 9 are added into the coating, and the addition amount is 20%. The specific formula is as follows: epoxy resin, dimethylbenzene, n-butyl alcohol, dispersing agent, defoaming agent, leveling agent and nano barium sulfate composite material with core-shell structure, which is prepared in the embodiment 1-9 of the invention.
The preparation method comprises the following steps: according to the mass percentage, 10 percent of dimethylbenzene, 8 percent of n-butyl alcohol, 0.4 percent of dispersing agent, 0.3 percent of defoaming agent, 0.2 percent of leveling agent, 61.1 percent of epoxy resin and 20 percent of core-shell nano barium sulfate composite material in the examples 1 to 9 of the invention are respectively weighed. The raw materials are placed in a high molecular reaction vessel and fully stirred for more than 3 hours, so as to obtain the coating emulsion corresponding to the coatings 1-9.
The anti-aging performance test is carried out on the coatings 1 to 9 and the base coating (10 percent of dimethylbenzene, 8 percent of n-butyl alcohol, 0.4 percent of dispersing agent, 0.3 percent of defoaming agent, 0.2 percent of flatting agent, 61.1 percent of epoxy resin and 20 percent of pure nano barium sulfate), and the specific test process is as follows:
(1) 0.5g of the paint and the base paint of examples 1 to 9 were respectively dropped onto a 20mm X60 mm glass plate, and then 0.5g of the paint was uniformly coated on the glass plate by means of blade coating. And standing for 24 hours until the paint is completely solidified, and obtaining a paint sample.
(2) The above-described fully cured paint samples were then,is placed in an ultraviolet aging oven (ultraviolet wavelength: 340nm, power: 0.51W (m) 2 Nm), an accelerated aging test was performed. The test results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the paint prepared by adding the nano barium sulfate composite material with the core-shell structure provided by the embodiment of the invention has the service life obviously longer than that of the paint with the basic formula. And when the same amount of carbon quantum dots (or more carbon quantum dots) are added, the aging resistance of the paint prepared by adding the nano barium sulfate composite material with the core-shell structure prepared by adopting a wet method is better than that of the paint prepared by adding the nano barium sulfate composite material with the core-shell structure prepared by adopting a dry method.
Claims (10)
1. The barium sulfate composite material with the core-shell structure is characterized by sequentially comprising nano barium sulfate, a silane layer and a carbon quantum dot layer from inside to outside.
2. The method according to claim 1, wherein the particle size of the nano barium sulfate is 20-700 nm.
3. The method for preparing the barium sulfate composite material with the core-shell structure according to claim 1 or 2, which is characterized by comprising the following steps:
(1) Preparing nano barium sulfate with positive charges on the surface;
(2) Mixing the carbon quantum dots with the nano barium sulfate with positive charges on the surface prepared in the step (1), and carrying out electrostatic assembly in the stirring process to form the barium sulfate composite material with the core-shell structure.
4. The method according to claim 3, wherein the nano barium sulfate with positive charges on the surface is obtained by surface modification of nano barium sulfate with silane with positive charges.
5. The process of claim 4, wherein the positively charged silane is an-NH-or-NH-containing silane 2 -a silane containing at least one methoxy or ethoxy group.
6. The method according to claim 5, wherein the positively charged silane is at least one selected from the group consisting of 3-aminopropyl triethoxysilane, aminomethyl dimethyl ethoxysilane, 3-propylamine triethoxysilane, bis [3- (triethoxysilyl) propyl ] amine, and N- [3- (trimethoxysilyl) propyl ] ethylenediamine.
7. The method according to any one of claims 4 to 6, wherein the mass of the positively charged silane is 0.1% to 5% of the mass of the nano barium sulfate; preferably, the mass of the positively charged silane is 0.5% -3% of the mass of the nano barium sulfate.
8. The production method according to any one of claims 3 to 6, wherein the production method is selected from one of modes (1) or (2):
(1) Dispersing nano barium sulfate and silane with positive charges in an alcohol solution, stirring for the first time, adding a carbon quantum dot solution, stirring for the second time, standing, separating solid from liquid to obtain a solid product, and drying the solid product to obtain the barium sulfate composite material with the core-shell structure; or (b)
(2) Mixing nano barium sulfate and silane with positive charges, adding carbon quantum dots, and stirring to obtain the barium sulfate composite material with the core-shell structure.
9. Use of the core-shell structured barium sulfate composite material of claim 1 or 2 in a coating.
10. A coating comprising the core-shell barium sulfate composite material of claim 1 or 2; preferably, the coating is an oil-soluble coating.
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