CN110872464B - Hydrophilic self-cleaning nano aluminum hydroxide, preparation method thereof and acrylic acid composition - Google Patents
Hydrophilic self-cleaning nano aluminum hydroxide, preparation method thereof and acrylic acid composition Download PDFInfo
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- CN110872464B CN110872464B CN201811023620.1A CN201811023620A CN110872464B CN 110872464 B CN110872464 B CN 110872464B CN 201811023620 A CN201811023620 A CN 201811023620A CN 110872464 B CN110872464 B CN 110872464B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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Abstract
The invention discloses hydrophilic self-cleaning nano aluminum hydroxide, which has a particle size range of 10-40nm and is prepared by hydrolysis reaction of an organic solvent, a surfactant, an aluminum salt and an inorganic salt, wherein the molar ratio of the organic solvent to the surfactant to the aluminum salt to the inorganic salt is as follows: (20-80) to (0.4-1) to 1: 3, wherein the organic solvent is absolute ethyl alcohol, propyl alcohol, isopropyl alcohol and n-butyl alcohol; the surfactant is sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexadecyl sulfonate and sodium hexadecyl benzene sulfonate; the inorganic salt is sodium bicarbonate or sodium carbonate. The invention also discloses a preparation method of the hydrophilic self-cleaning nano aluminum hydroxide and an acrylic acid composition containing the hydrophilic self-cleaning nano aluminum hydroxide.
Description
Technical Field
The invention relates to hydrophilic self-cleaning nano aluminum hydroxide, and further relates to a preparation method of the hydrophilic self-cleaning nano aluminum hydroxide and an acrylic acid composition containing the hydrophilic self-cleaning nano aluminum hydroxide.
Background
Aluminum hydroxide, commonly used as an inorganic flame retardant additive, is not only flame retardant, but also smoke-proof, and does not produce dripping and toxic gases, thus achieving wider application, being a flame retardant with the largest and most widely used amount, and increasing the usage amount year by year, and being commonly used in the industries of thermosetting plastics, thermoplastic plastics, synthetic rubber, coatings, building materials and the like. Aluminum hydroxide is also an important antacid and has the functions of resisting acid, stopping bleeding locally, protecting ulcer surfaces and the like.
Chinese patent CN101970356A discloses a preparation method of modified aluminum hydroxide mixed powder, which is mainly used as a filler of rubber and plastics; chinese patent CN102010620A discloses a method for preparing nano aluminum hydroxide dispersion, which is mainly used as an ink absorbing material; chinese patent CN104944457A discloses a preparation method of surface modified aluminum hydroxide, which is mainly used as a flame retardant in the electronic industry.
Disclosure of Invention
In view of the above-mentioned shortcomings in the prior art, according to the embodiments of the present invention, it is desirable to provide a hydrophilic self-cleaning nano aluminum hydroxide, which is intended to provide hydrophilic self-cleaning effect and anti-glare function to the aluminum hydroxide nano particles; in addition, a preparation method of the acrylic acid composition containing the hydrophilic self-cleaning nano aluminum hydroxide and the acrylic acid composition containing the hydrophilic self-cleaning nano aluminum hydroxide are also provided.
According to the embodiment, the hydrophilic self-cleaning nano aluminum hydroxide provided by the invention has the particle size ranging from 10 nm to 40nm and is prepared by hydrolysis reaction of an organic solvent, a surfactant, an aluminum salt and an inorganic salt, wherein the molar ratio of the organic solvent to the surfactant to the aluminum salt to the inorganic salt is as follows: (20-80) to (0.4-1) to 1: 3, wherein the organic solvent is absolute ethyl alcohol, propyl alcohol, isopropyl alcohol and n-butyl alcohol; the surfactant is sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexadecyl sulfonate and sodium hexadecyl benzene sulfonate; the inorganic salt is sodium bicarbonate or sodium carbonate.
According to one embodiment, in the hydrophilic self-cleaning nano aluminum hydroxide, the aluminum salt is aluminum sulfate and aluminum ammonium sulfate.
According to the embodiment, the preparation method of the hydrophilic self-cleaning nano aluminum hydroxide provided by the invention comprises the following steps:
(1) uniformly mixing an aluminum salt solution, an organic solvent and a surfactant, and stirring in a water bath at the temperature of 60-80 ℃, wherein the stirring speed is 150 revolutions per minute;
(2) dropwise adding an inorganic salt solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2ml/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and carrying out aging crystallization reaction for 8-24 hours at the temperature of 60-120 ℃;
(3) filtering the product obtained in the step (2), washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 80-120 ℃ for 8-24 hours to prepare aluminum hydroxide;
(4) mixing the aluminum hydroxide obtained in the step (3) with petroleum ether, uniformly stirring, slowly adding a modifier, and stirring at the speed of 500 revolutions per minute for 30 minutes, wherein the aluminum hydroxide, the petroleum ether and the modifier are 20-30wt%, 65-79wt% and 1-5 wt%; drying at 80-120 deg.c and grinding to obtain hydrophilic self-cleaning nano aluminum hydroxide of 10-40nm size.
According to one embodiment of the invention, in the preparation method of the hydrophilic self-cleaning nano aluminum hydroxide, in the step (4), the boiling range of petroleum ether is 30-60 ℃, 60-90 ℃ and 90-120 ℃.
According to an embodiment, in the preparation method of the hydrophilic self-cleaning nano aluminum hydroxide, in the step (4), the modifier is a polyethylene glycol polymer with a molecular weight of 200-1000.
According to an embodiment, in the preparation method of the hydrophilic self-cleaning nano aluminum hydroxide, the polyethylene glycol polymer with the molecular weight of 200-1000 is polyethylene glycol dicarboxylic acid, methoxy polyethylene glycol or carboxymethylated methoxy polyethylene glycol.
According to the embodiment, the acrylic acid composition provided by the invention comprises the following substances in percentage by mass:
10-20 wt% of hydrophilic self-cleaning aluminum hydroxide;
30-40 wt% of organic solvent or water;
40-60 wt% of acrylic resin;
the organic solvent is ethyl acetate, butyl acetate and xylene; the acrylic resin is UV-curable water-based acrylic resin or UV-curable oily acrylic resin.
Compared with the prior art, the invention modifies the polyethylene glycol polymer with hydroxyl or carboxyl groups on the surface of the nano aluminum hydroxide through hydrothermal chemical reaction, thereby enabling the aluminum hydroxide to have the hydrophilic self-cleaning function. The subsequent examples and experimental examples prove that the acrylic acid composition containing the hydrophilic self-cleaning nano aluminum hydroxide is added into the UV glue, and the contact angle is less than 5 degrees after construction; after contacting with water, the water diffuses on the surface of the substrate to form an even water film, so that the substrate surface can be completely soaked, stains can be isolated, the stains can be taken away under the action of the gravity of the water, and the self-cleaning effect is achieved. Because the aluminum hydroxide nano particles can diffusely reflect light, and are added into the UV glue, the dried aluminum hydroxide nano particles have good anti-dazzle effect; in addition, the invention also has the characteristics of simple preparation method, low cost, easy industrialization and the like.
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FIG. 1 is a schematic diagram of the hydrophilic self-cleaning effect of the UV glue after drying in the experimental example.
Detailed Description
The invention is further illustrated with reference to the following figures and specific examples. These examples are to be construed as merely illustrative and not limitative of the remainder of the disclosure in any way whatsoever. After reading the description of the invention, one skilled in the art can make various changes and modifications to the invention, and such equivalent changes and modifications also fall into the scope of the invention defined by the claims.
The starting materials used in the following examples of the present invention are all commercially available products unless otherwise specified.
Example 1
(1) Adding 20ml of ethanol and 1.5g of sodium dodecyl benzene sulfonate into 250ml of 0.03mol/l aluminum sulfate solution, and stirring in a water bath at the temperature of 60 ℃ at the stirring speed of 150 revolutions per minute;
(2) and (2) dropwise adding a 10% sodium carbonate solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2ml/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and performing aging crystallization reaction for 20 hours at the temperature of 80 ℃.
(3) And (3) filtering the product obtained in the step (2), washing the product by deionized water and absolute ethyl alcohol, and drying the product for 20 hours at the temperature of 80 ℃ to prepare the aluminum hydroxide.
(4) 20g of the aluminum hydroxide prepared in step (3) and 78g of petroleum ether (boiling range 30-60 ℃) were mixed and stirred uniformly. Then 2g of the modifier methoxypolyethylene glycol was slowly added and stirred at 500 rpm for 30 minutes. Drying at 80 deg.C for 6 hr, and grinding to obtain hydrophilic self-cleaning nano aluminium hydroxide with particle size of 10-40 nm.
20g of the hydrophilic self-cleaning nano aluminum hydroxide prepared in example 1 and 40 g of xylene are mixed and stirred uniformly, and then 40 g of UV curing solvent type acrylic resin is added and stirred uniformly to prepare a composition.
Example 2
(1) Adding 20ml of propanol and 1.5g of sodium dodecyl sulfate into 250ml of 0.04mol/l aluminum ammonium sulfate solution, and stirring in a water bath at 70 ℃ at the stirring speed of 150 revolutions per minute;
(2) and (2) dropwise adding a 12% sodium bicarbonate solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2ml/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and performing aging crystallization reaction for 18 hours at the temperature of 100 ℃.
(3) And (3) filtering the product obtained in the step (2), washing the product by deionized water and absolute ethyl alcohol, and drying the product for 18 hours at the temperature of 100 ℃ to prepare the aluminum hydroxide.
(4) 25g of aluminum hydroxide prepared by the method of step (3) and 72g of petroleum ether (boiling range 60-90 ℃) were mixed and stirred uniformly. Then 3g of the modifier polyethylene glycol dicarboxylic acid was slowly added and stirred at 500 rpm for 30 minutes. Drying for 8 hours at 100 ℃, and grinding to obtain the hydrophilic self-cleaning modified nano aluminum hydroxide with the particle size range of 10-40 nm.
20g of the hydrophilic self-cleaning nano aluminum hydroxide prepared in the example 2 and 30g of ethyl acetate are mixed and stirred uniformly, and then 50 g of UV curing oily acrylic resin is added and stirred uniformly to prepare the composition.
Example 3
(1) Adding 20ml of isopropanol and 1.5g of sodium hexadecylsulfonate into 250ml of 0.05mol/l aluminum sulfate solution, and stirring in a water bath at the temperature of 80 ℃ at the stirring speed of 150 revolutions per minute;
(2) and (2) dropwise adding a 14% sodium bicarbonate solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2ml/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and performing aging crystallization reaction for 16 hours at the temperature of 110 ℃.
(3) And (3) filtering the product obtained in the step (2), washing the product by deionized water and absolute ethyl alcohol, and drying the product for 16 hours at the temperature of 110 ℃ to prepare the aluminum hydroxide.
(4) 30g of the aluminum hydroxide prepared in step (3) and 66g of petroleum ether (boiling range 60-90 ℃) were mixed and stirred uniformly. Then 4g of the modifier polyethylene glycol dicarboxylic acid was slowly added and stirred at 500 rpm for 30 minutes. Then vacuum drying for 8 hours at 110 ℃ and grinding to prepare the hydrophilic self-cleaning modified nano aluminum hydroxide with the particle size range of 10-40 nm.
20g of the hydrophilic self-cleaning nano aluminum hydroxide prepared in the example 2 and 30g of butyl acetate are mixed and stirred uniformly, and then 50 g of UV curing oily acrylic resin is added and stirred uniformly to prepare the composition.
Example 4
(1) Adding 20ml of n-butyl alcohol and 1.5g of sodium hexadecylbenzene sulfonate into 250ml of 0.04mol/l aluminum ammonium sulfate solution, and stirring in a water bath at 65 ℃ at the stirring speed of 150 revolutions per minute;
(2) and (2) dropwise adding 11% sodium bicarbonate solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2ml/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and carrying out aging crystallization reaction for 12 hours at the temperature of 80 ℃.
(3) And (3) filtering the product obtained in the step (2), washing the product by deionized water and absolute ethyl alcohol, and drying the product at the temperature of 80 ℃ for 12 hours to prepare the aluminum hydroxide.
(4) 22g of aluminum hydroxide prepared by the method of step (3) and 75g of petroleum ether (boiling range 60-90 ℃) were mixed and stirred uniformly. Then 3g of the modifier polyethylene glycol dicarboxylic acid was slowly added and stirred at 500 rpm for 30 minutes. And then dried for 9 hours at 100 ℃ and ground to prepare the hydrophilic self-cleaning modified nano aluminum hydroxide with the particle size range of 10-40 nm.
20g of the hydrophilic self-cleaning nano aluminum hydroxide prepared in example 4 and 30g of butyl acetate were mixed and stirred uniformly, and then 50 g of UV-curable oily acrylic resin was added and stirred uniformly to prepare a composition.
Test examples
As shown in FIG. 1, the hydrophilic self-cleaning aluminum hydroxide-containing acrylic compositions prepared in examples 1 to 4 were added to a commercially available TYU-6100PC surface hardening UV glue in an amount of 8% (example 1), 7% (example 4), 6% (example 2) and 6% (example 3), respectively, and the UV glue was applied to the surface of the PC sample (curing conditions: 365-2Curing time of 6 seconds), and after the sample is completely dried, testing the contact angle of the surface,Hardness and antiglare properties.
As can be seen from Table 1, examples 1 to 4 all had contact angles of less than 5 ℃ and had excellent hydrophilic properties and antiglare properties. Examples 2 and 3, which use polyethylene glycol dicarboxylic acid having a strong carboxyl hydrophilic group, have a smaller contact angle and thus have more excellent hydrophilic properties. UGR measured according to national standard GB50034-2004 is less than 13, and the anti-dazzle effect is good.
TABLE 1 Performance testing of examples 1-4
| Contact angle | Anti-dazzle (UGR) | Hardness of | |
| Example 1 | 4.6° | 12 | 2H |
| Example 2 | 3.2° | 11 | 2H |
| Example 3 | 3.4° | 10 | 2H |
| Example 4 | 4.8° | 12 | 2H |
Claims (2)
1. The preparation method of the hydrophilic self-cleaning nano aluminum hydroxide has the particle size range of 10-40nm and is prepared by hydrolysis reaction of an organic solvent, a surfactant, an aluminum salt and an inorganic salt, wherein the molar ratio of the organic solvent to the surfactant to the aluminum salt to the inorganic salt is as follows: (20-80): (0.4-1): 1: 3, the organic solvent is absolute ethyl alcohol, propanol, isopropanol and n-butanol, the surfactant is sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, sodium hexadecyl sulfonate and sodium hexadecyl benzene sulfonate, the inorganic salt is sodium bicarbonate or sodium carbonate, and the aluminum salt is aluminum sulfate and ammonium aluminum sulfate, and the method is characterized by comprising the following steps:
(1) uniformly mixing an aluminum salt solution, an organic solvent and a surfactant, and stirring in a water bath at the temperature of 60-80 ℃, wherein the stirring speed is 150 revolutions per minute;
(2) dropwise adding an inorganic salt solution into the mixed solution obtained in the step (1), wherein the dropwise adding speed is 2mL/min, detecting the pH value by using an acidimeter in the reaction process, stopping the reaction when the pH value is more than 4, placing the mixture into an autoclave with a polytetrafluoroethylene lining, and carrying out aging crystallization reaction for 8-24 hours at the temperature of 60-120 ℃;
(3) filtering the product obtained in the step (2), washing with deionized water and absolute ethyl alcohol, and drying at the temperature of 80-120 ℃ for 8-24 hours to prepare aluminum hydroxide;
(4) mixing the aluminum hydroxide and the petroleum ether obtained in the step (3), uniformly stirring, slowly adding the modifier, and stirring at the speed of 500 revolutions per minute for 30 minutes, wherein the weight ratio of the aluminum hydroxide to the petroleum ether to the modifier is 20-30 percent, 65-79 percent and 1-5 percent; drying at 80-120 ℃ and grinding to prepare the hydrophilic self-cleaning nano aluminum hydroxide with the particle size range of 10-40nm, wherein:
in the step (4), the modifier is polyethylene glycol polymer with molecular weight between 200-1000, and the polyethylene glycol polymer with molecular weight between 200-1000 is polyethylene glycol dicarboxylic acid, methoxy polyethylene glycol or carboxymethylated methoxy polyethylene glycol.
2. The preparation method of the hydrophilic self-cleaning nano aluminum hydroxide according to claim 1, wherein in the step (4), the boiling range of petroleum ether is 30-60 ℃, 60-90 ℃ or 90-120 ℃.
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