CN117625030A - Flame-retardant antibacterial wood paint coating and preparation method thereof - Google Patents
Flame-retardant antibacterial wood paint coating and preparation method thereof Download PDFInfo
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- CN117625030A CN117625030A CN202311694602.7A CN202311694602A CN117625030A CN 117625030 A CN117625030 A CN 117625030A CN 202311694602 A CN202311694602 A CN 202311694602A CN 117625030 A CN117625030 A CN 117625030A
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- 238000000034 method Methods 0.000 claims abstract description 13
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- Paints Or Removers (AREA)
Abstract
The invention discloses a flame-retardant antibacterial wood paint and a preparation method thereof, wherein the preparation method comprises the following steps: modified nano SiO 2 Dripping the mixture into a waterborne polyurethane prepolymer, adding triethylamine for neutralization reaction after the reaction, adding deionized water and ethylenediamine, and emulsifying to obtain the flame-retardant antibacterial wood lacquer coating; the modified nano SiO 2 The preparation method of (2) is as follows: nano SiO 2 After KH602 treatment, amino nano SiO is obtained 2 Aminating nano SiO 2 Dispersing in absolute ethanol to obtain dispersion, dropwise adding DOPO-OH solution into the dispersion under stirring, filtering, washing, and drying to obtain functional nanometer SiO 2 Work is performedEnergized nano SiO 2 Modified nano SiO is obtained by thiourea dioxide treatment 2 The method comprises the steps of carrying out a first treatment on the surface of the The obtained wood lacquer coating has excellent wear resistance, flexibility, hydrolysis resistance, bacteriostasis and flame retardance, and has stable effect and long duration.
Description
Technical Field
The invention relates to the field of wood paint, in particular to a flame-retardant antibacterial wood paint and a preparation method thereof.
Background
Under the large environment of the current green sustainable development, the adverse effects of the traditional solvent-based paint on the environment and the human health are widely paid attention, and the development and the utilization of healthy and environment-friendly water-based paint become research hot spots. The water-based wood coating takes water as a solvent, almost has no volatile organic matters and air pollutants, has wide application range, is safe and reliable in construction, and is favored by practitioners. Water-based paints, based on film-forming materials, can be broadly divided into three categories: the first type is water-based acrylic paint, which has good hardness and luster, but long drying time, poor water resistance and chemical resistance, and limits the application of the water-based acrylic paint; with the progress of technology, people continuously modify the water-based acrylic paint, and the development of the water-based acrylic paint is mature. The second type is aqueous epoxy coating, which has higher adhesion and chemical resistance, but poor storage stability and longer drying time. The cost of the aqueous acrylic coating and the aqueous epoxy coating is lower, and the aqueous acrylic coating and the aqueous epoxy coating have a larger specific gravity in the market. The third type is water-based polyurethane paint, the paint film has good flexibility, high and low temperature resistance, chemical resistance and the like, is a type with higher quality in the water-based paint, and is a water-based paint with larger potential.
The polyurethane has a unique molecular structure of a hard chain segment and a soft chain segment, and the formed paint film has good adhesive force, good flexibility, corrosion resistance and the like; the waterborne polyurethane is a novel polyurethane coating system taking water as a solvent or a dispersion medium, has the advantages of environmental protection, little or zero release of volatile organic compounds and accords with the sustainable development concept besides the advantages of the traditional solvent type polyurethane coating. The aqueous polyurethane is mainly formed by polyaddition reaction of polyisocyanate, polyether or polyol, a chain extender and a hydrophilic agent, and the obtained aqueous polyurethane has different properties due to various synthetic materials and processes, is widely applied to various fields such as paint, leather, adhesives and the like, and is a very potential aqueous paint.
The aqueous polyurethane coating has a plurality of excellent performances, but still has the bottleneck problems of poor water resistance, chemical resistance, abrasion resistance, hardness and the like, and large difference from the traditional solvent-based paint, and the aqueous polyurethane needs to be modified in order to solve the problems. The modification method is roughly divided into acrylic ester modification, epoxy resin modification, organic fluorine modification, organosilicon modification, nanomaterial modification and the like. The nano material has large specific surface area, excellent physical and mechanical properties, surface interface effect and photoelectric effect, can improve the mechanical properties of a paint film, endows the waterborne polyurethane with certain unique functions, and widens the application range of the waterborne polyurethane.
The Chinese patent document CN101575474B provides a water-based wood lacquer and a preparation method thereof, wherein the wood lacquer comprises water-based acrylic resin, a foam inhibitor, a defoaming agent, a film forming additive, nano silicon dioxide slurry, an antiseptic bactericide and water, and the water-based resin with rigid acrylic monomer is adopted to enhance the polishing performance of the water-based wood lacquer and achieve the comprehensive performance with excellent cost performance; the nano inorganic silica filler is added and uniformly dispersed in the system, so that the solid content and transparency of the product are improved, the product has the dual performance of the nano inorganic silica filler and the product, and the water-based wood lacquer with the dual performance of high solid content and high transparency is obtained.
The Chinese patent document CN1296448C provides a water-based wood lacquer which comprises A, B parts of components, wherein the specific components of the A part comprise 5.5-8.0% of film forming auxiliary agent, 0.3-0.5% of dispersing agent, 0.2-0.4% of wetting agent, 0.8-1.2% of cosolvent, 2.0-8.0% of pure water, 0.2-0.5% of flatting agent, 0.1-0.2% of thickening agent, 0.1-0.2% of surfactant, 0.2-0.5% of defoaming agent and 1.2-1.5% of mixture of nano silicon dioxide and nano titanium dioxide; the specific components of the part B are 75.0-85.0% of aqueous polyurethane emulsion and 4.0-5.0% of aqueous wax emulsion; the sum of the A part and the B part is 100%, and the water-based wood paint has the functions of sterilization, bacteriostasis and air purification, and has high hardness of paint film and good anti-blocking and anti-contamination properties.
The existing wood lacquer still has the defects of poor flame retardant property, bacteriostasis, pencil hardness and wear resistance, in order to widen the application range of the wood lacquer, researchers carry out a lot of modifications on the wood lacquer, but the existing common modification method is to blend nano materials into aqueous polyurethane emulsion through physical blending, the modification easily generates agglomeration of the nano materials, the performance of products is influenced, and the duration of the effect brought by modification is shorter.
Disclosure of Invention
In order to solve the defects existing in the prior art, the invention aims to provide the flame-retardant antibacterial wood lacquer coating and the preparation method thereof, and the obtained wood lacquer coating has excellent wear resistance, flexibility, hydrolysis resistance, antibacterial performance and flame retardance, and has stable effect and long duration.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a preparation method of a flame-retardant antibacterial wood paint comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 95-100 ℃ for 2-4 hours for later use; mixing PPG2000 and isophorone diisocyanate, reacting for 2-4 hours at 75-85 ℃, then adding dimethylolpropionic acid to react for 1-2 hours, cooling to 60-75 ℃, adding 1, 4-butanediol, trimethylolpropane and dibutyltin dilaurate, and reacting for 2-3 hours to obtain a waterborne polyurethane prepolymer;
(2) Modified nano SiO 2 Dispersing in acetone, carrying out ultrasonic treatment for 5-15 min, slowly dripping into a waterborne polyurethane prepolymer, reacting for 1-2 h, cooling to 30-40 ℃, adding triethylamine for neutralization for 0.5-1 h, then adding deionized water and ethylenediamine, emulsifying for 0.5-1 h at 1500-1800 r/min, and removing acetone by rotary evaporation after the reaction is finished, thus obtaining the flame-retardant antibacterial wood lacquer coating.
Preferably, in the step (1), the weight ratio of PPG2000, isophorone diisocyanate and dimethylolpropionic acid is 10: 11-15: 0.8 to 1.2; the weight ratio of 1, 4-butanediol, trimethylolpropane and dibutyltin dilaurate is 3-5: 1:0.02 to 0.04; the weight of the trimethylolpropane accounts for 1.5 to 3 percent of the total weight of the PPG2000 and the isophorone diisocyanate.
Preferably, in the step (2), the nano SiO is modified 2 The weight ratio of the polyurethane to the aqueous polyurethane prepolymer is 0.5-2: 100; the weight ratio of deionized water to ethylenediamine is 120-150: 1, a step of; modified nano SiO 2 The weight ratio of the catalyst to triethylamine is 1:0.4 to 0.9.
Preferably, the modified nano SiO 2 The preparation method of the (C) comprises the following steps:
a. nano SiO 2 Adding KH602 into deionized water, and performing ultrasonic treatmentStirring for reaction, filtering, washing and drying the product after the reaction is finished to obtain the amination nanometer SiO 2 ；
b. Aminated nano SiO 2 Dispersing in absolute ethanol to obtain dispersion, dropwise adding DOPO-OH solution into the dispersion under stirring, stirring for reaction, filtering, washing, and drying to obtain functional nanometer SiO 2 ；
c. Will functionalize nano SiO 2 Adding thiourea dioxide into deionized water, stirring for reaction, filtering, washing and drying the product after the reaction is finished to obtain modified nano SiO 2 。
Preferably, in step a, nano SiO 2 The weight volume of KH602 is 1g: 0.6-1.2 mL; ultrasonic treatment is carried out for 10-20 min, and stirring reaction is carried out for 8-16 h at the temperature of 40-60 ℃.
Preferably, in step b, the nano SiO is aminated 2 The weight-volume ratio of DOPO-OH solution is 10g: 50-80 mL; the weight fraction of DOPO-OH solution is 15-20wt%; the reaction condition is that stirring reaction is carried out for 16-20 h at 70-85 ℃.
Preferably, in step b, the DOPO-OH solution is prepared as follows: dissolving DOPO in absolute ethyl alcohol, adding 25-35 wt% hydrogen peroxide under stirring, stirring at 80-90 ℃ for reaction for 16-20 h, after the reaction is finished, removing a solvent by rotary evaporation, washing and drying to obtain DOPO-OH, and dissolving DOPO-OH in absolute ethyl alcohol to obtain DOPO-OH solution; the weight volume of DOPO and hydrogen peroxide is 20-30 g:120mL.
Preferably, in step c, the nano SiO is functionalized 2 The thiourea dioxide has a weight of 1:1.1 to 1.5; stirring reaction is carried out for 12-18 h at 70-90 ℃.
The invention also discloses a flame-retardant antibacterial wood paint prepared by the preparation method.
The invention also claims an application of the wood lacquer coating in wood flame retardance and bacteriostasis.
Compared with the prior art, the invention has the following beneficial effects:
1) The invention provides flame retardant and anti-flamingBacterial wood lacquer coating, KH602 is utilized to carry out nano SiO 2 Modifying to obtain aminated nano SiO 2 Then introducing flame retardant DOPO into nano SiO 2 The surface is obtained with functional nano SiO 2 And guanidizing modification is carried out on the nano SiO by thiourea dioxide to obtain modified nano SiO 2 Finally, modified nano SiO 2 The water-based polyurethane emulsion is obtained by adding the water-based polyurethane emulsion into a water-based polyurethane prepolymer, can endow the wood lacquer coating with long-acting and durable antibacterial and flame retardant properties, has no solvent volatilization in the construction process, and is very friendly to the environment and constructors.
2) The flame-retardant antibacterial wood lacquer coating provided by the invention uses KH602 to carry out nano SiO 2 The surface is modified, so that the hydroxyl content of the surface is effectively reduced, and the nano SiO is improved 2 The degree of the organization of the inorganic particles in the organic polymer is enhanced, and the nano SiO is reduced 2 Dispersing difficulty and agglomeration in polyurethane, and then bonding inorganic material nano SiO through chemical bond 2 Is introduced to polyurethane molecular chains, not only effectively solves the problem of compatibility between inorganic nano materials and polyurethane, improves the storage stability of wood lacquer coating, and meanwhile, the sites of a crosslinked network are effectively increased, and the compactness, the mechanical strength, the hydrolysis resistance and the wear resistance of the wood lacquer are obviously improved.
3) The flame-retardant antibacterial wood paint coating provided by the invention adopts H 2 O 2 Oxidizing DOPO to obtain DOPO-OH, and grafting DOPO phosphonate to amino nano SiO by acid-base neutralization reaction 2 Applying; on one hand, KH602 introduces long-chain alkyl, so that the toughness of polyurethane can be improved, and on the other hand, DOPO enhances the interaction between polyurethane molecular chains through hydrogen bond action and pi-pi action, so that the mechanical strength of the coating is improved.
4) According to the flame-retardant antibacterial wood lacquer coating provided by the invention, DOPO is introduced through the design reaction step, and thiourea dioxide and functionalized nano SiO are adopted 2 The reaction of (2) introduces the guanidine group, so that the guanidine group is effectively protected and prevented from being consumed by the reaction with DOPO-OH; the guanidino group may react with phosphorus by forming hydrogen bondsThe acid groups generate strong interaction ion pairs, and when contacting bacteria, the guanidine groups and the phosphate groups on the cell walls can induce double-tooth binding effect, so that the bacteria-inhibiting rate can be high even at low concentration.
5) The flame-retardant antibacterial wood lacquer coating provided by the invention is prepared into modified nano SiO 2 The N-P-Si composite flame retardant material can release phosphorus-containing free radicals to capture and quench active free radicals in combustion, and cut off combustible substance exchange; NH released after degradation of flame retardant material 3 The temperature of the surface of the wood can be reduced; nano SiO 2 When in combustion, a layer of Si-O-C bond protective layer is formed on the surface of the wood, so that the effect of shielding heat is achieved, and the excellent flame-retardant effect is achieved through cooperation of nitrogen, phosphorus and silicon.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the following examples. Of course, the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Unless otherwise specified, both chemical reagents and materials in the present invention are purchased through a market route or synthesized from raw materials purchased through a market route.
Nano SiO 2 Purchased from Beijing Jia An Heng technology Co., ltd., particle diameter of 15nm, specific surface area of 200m 2 /g。
The invention will be further illustrated by the following examples.
Example 1
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. 10g SiO of nanometer 2 Adding 12mL KH602 into 100mL deionized water, performing ultrasonic treatment for 20min, stirring at 60deg.C for 16h, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. 30g DOPO is dissolved in 100mL absolute ethanol, 120mL35wt% hydrogen peroxide is added under stirring, and the mixture is stirred at 90 ℃ for reaction for 20hAfter the completion, removing the solvent by rotary evaporation, washing with ethanol, drying to obtain DOPO-OH, and dissolving the DOPO-OH in absolute ethanol to obtain DOPO-OH solution; 10g of aminated nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 80mL 20wt% DOPO-OH solution into the dispersion under stirring, reacting at 85deg.C for 20 hr, filtering, washing with acetone, and drying to obtain functional nanometer SiO 2 ；
c. 10g of functionalized nano SiO 2 15g thiourea dioxide is added into 100mL deionized water, stirred and reacted for 18h at 90 ℃, and after the reaction is finished, the product is filtered, washed and dried to obtain the modified nano SiO 2 。
A preparation method of a flame-retardant antibacterial wood paint comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 100g of PPG2000 and 130g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 10g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 20g of 1, 4-butanediol, 4.6g of trimethylolpropane and 0.3g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of modified nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation after the reaction is finished to obtain the flame-retardant antibacterial wood lacquer coating.
Example 2
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. nano 1g SiO 2 Adding 0.6mL KH602 into 100mL deionized water, performing ultrasonic treatment for 20min, stirring at 40deg.C for reaction for 8 hr, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. 20g DOPO was dissolved in 100mL absolute ethanol and 120mL25wt% dioxygen was added with stirringStirring water at 80 ℃ for reaction for 16 hours, removing a solvent by rotary evaporation after the reaction is finished, washing with ethanol, drying to obtain DOPO-OH, and dissolving the DOPO-OH in absolute ethanol to obtain DOPO-OH solution; 10g of aminated nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 50mL 15wt% DOPO-OH solution into the dispersion under stirring, reacting at 70deg.C for 16h under stirring, filtering, washing with acetone, and drying to obtain functional nanometer SiO 2 ；
c. 10g of functionalized nano SiO 2 Adding 11g thiourea dioxide into 100mL deionized water, stirring at 70 ℃ for reaction for 12h, filtering, washing and drying the product after the reaction is finished to obtain modified nano SiO 2 。
A preparation method of a flame-retardant antibacterial wood paint comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of modified nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation after the reaction is finished to obtain the flame-retardant antibacterial wood lacquer coating.
Example 3
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. 10g SiO of nanometer 2 Adding 10mL KH602 into 100mL deionized water, performing ultrasonic treatment for 15min, stirring at 50deg.C for reaction for 10h, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. 25g DOPO was dissolved in 100mL absolute ethanolAdding 120mL30wt% hydrogen peroxide under stirring, stirring at 85 ℃ for reaction for 18 hours, removing a solvent by rotary evaporation after the reaction is finished, washing with ethanol, drying to obtain DOPO-OH, and dissolving the DOPO-OH in absolute ethanol to obtain DOPO-OH solution; 10g of aminated nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 60mL 16wt% DOPO-OH solution into the dispersion under stirring, stirring at 80deg.C for 18 hr, filtering, washing with acetone, and drying to obtain functional nanometer SiO 2 ；
c. 10g of functionalized nano SiO 2 Adding 13g thiourea dioxide into 100mL deionized water, stirring at 80 ℃ for reaction for 15h, filtering, washing and drying the product after the reaction is finished to obtain modified nano SiO 2 。
A preparation method of a flame-retardant antibacterial wood paint comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of modified nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation after the reaction is finished to obtain the flame-retardant antibacterial wood lacquer coating.
Example 4
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. 10g SiO of nanometer 2 10mL KH602 is added into 100mL deionized water, after ultrasonic treatment for 18min, stirring is carried out for reaction for 14h at 55 ℃, after the reaction is finished, the product is filtered, washed and dried, thus obtaining the amination nano SiO 2 ；
b. 28g of DOPO is dissolved in 100mL of absolute ethyl alcohol, 120mL of 30wt% hydrogen peroxide is added under stirring, stirring is carried out for 18h at 85 ℃, after the reaction is finished, the solvent is removed by rotary evaporation, ethanol is used for washing, drying is carried out to obtain DOPO-OH, and DOPO-OH is dissolved in the absolute ethyl alcohol to obtain DOPO-OH solution; 10g of aminated nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 70mL 18wt% DOPO-OH solution into the dispersion under stirring, reacting at 80deg.C for 18 hr, filtering the product after the reaction, washing with acetone, and drying to obtain functional nanometer SiO 2 ；
c. 10g of functionalized nano SiO 2 Adding 14g thiourea dioxide into 100mL deionized water, stirring at 85 ℃ for reaction for 16h, filtering, washing and drying the product after the reaction is finished to obtain modified nano SiO 2 。
A preparation method of a flame-retardant antibacterial wood paint comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of modified nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation after the reaction is finished to obtain the flame-retardant antibacterial wood lacquer coating.
Comparative example 1
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. dissolving 30g DOPO in 100mL absolute ethanol, adding 120mL35wt% hydrogen peroxide under stirring, stirring at 90 ℃ for reaction for 20h, removing solvent by rotary evaporation after the reaction, washing with ethanol, drying to obtain DOPO-OH, dissolving DOPO-OH in absolute ethanolObtaining DOPO-OH solution in ethanol; 10g of nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 80mL 20wt% DOPO-OH solution into the dispersion under stirring, reacting at 85deg.C for 20 hr, filtering, washing with acetone, and drying to obtain functional nanometer SiO 2 ；
b. 10g of functionalized nano SiO 2 Adding 15g thiourea dioxide into 100mL deionized water, stirring at 90 ℃ for reaction for 18h, filtering, washing and drying the product after the reaction is finished to obtain the guanylated nano SiO 2 ；
A preparation method of a wood lacquer coating comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of guanylated nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation to obtain the wood lacquer coating.
Comparative example 2
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. 10g SiO of nanometer 2 Adding 12mL KH602 into 100mL deionized water, performing ultrasonic treatment for 20min, stirring at 60deg.C for 16h, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. Dissolving 30g DOPO in 100mL absolute ethanol, adding 120mL35wt% hydrogen peroxide under stirring, stirring at 90 ℃ for reaction for 20h, removing solvent by rotary evaporation after the reaction, washing with ethanol, drying to obtain DOPO-OH, dissolving DOPO-OHDissolving in absolute ethyl alcohol to obtain DOPO-OH solution; 10g of aminated nano SiO 2 Dispersing in 100mL absolute ethanol to obtain dispersion, dropwise adding 80mL 20wt% DOPO-OH solution into the dispersion under stirring, reacting at 85deg.C for 20 hr, filtering, washing with acetone, and drying to obtain functional nanometer SiO 2 。
A preparation method of a wood lacquer coating comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of functionalized nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation to obtain the wood lacquer coating.
Comparative example 3
Modified nano SiO 2 The preparation method of (2) comprises the following steps:
a. 10g SiO of nanometer 2 Adding 12mL KH602 into 100mL deionized water, performing ultrasonic treatment for 20min, stirring at 60deg.C for 16h, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. 10g of aminated nano SiO 2 Adding 15g thiourea dioxide into 100mL deionized water, stirring at 90 ℃ for reaction for 18h, filtering, washing and drying the product after the reaction is finished to obtain the guanylated nano SiO 2 。
A preparation method of a wood lacquer coating comprises the following steps:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 100deg.C for 3 hr; 10g of PPG2000 and 13g of isophorone diisocyanate are mixed and reacted for 3 hours at 80 ℃, then 1g of dimethylolpropionic acid is added for reaction for 1.5 hours, the temperature is reduced to 70 ℃, 2g of 1, 4-butanediol, 0.46g of trimethylolpropane and 0.03g of dibutyltin dilaurate are added for reaction for 2.5 hours, and a waterborne polyurethane prepolymer is obtained;
(2) 2g of guanylated nano SiO 2 Dispersing in 20mL of acetone, carrying out ultrasonic treatment for 10min, slowly dripping into 100g of aqueous polyurethane prepolymer, reacting for 1.5h, cooling to 35 ℃, adding 1g of triethylamine for neutralization reaction for 1h, then adding 130g of deionized water and 1g of ethylenediamine, emulsifying for 1h at 1600r/min, and removing acetone by rotary evaporation to obtain the wood lacquer coating.
Taking a raw maple veneer, spraying a seal primer (purchased from Jia Bao Li chemical group Co., ltd.), drying, polishing, spraying a primer (purchased from Jia Bao Li chemical group Co., ltd.), drying, polishing, respectively spraying the wood lacquer coatings prepared in examples 1-4 and comparative examples 1-3 twice, and performing performance test after drying; pouring the wood lacquer coatings prepared in the examples 1-4 and the comparative examples 1-3 into a culture dish, and drying in an oven to obtain a pure lacquer film for performance test; the specific data are shown in Table 1.
Gloss determination reference GB/T4896.6-2013 furniture surface paint film physicochemical Property test part 6: gloss assay (gloss assay), adhesion assay reference GB/T4893.4-2013 furniture surface paint film physicochemical Property test part 4: adhesive force cross cutting measurement method, pencil hardness measurement reference GB/T6739-2006 "paint film hardness measured by color paint and varnish pencil method", water resistance and alkali resistance measurement reference GB/T4893.1-2021 "furniture surface paint film physicochemical Property test part 1: cold-resistant liquid determination method, flame-resistant time, flame propagation ratio, mass loss and carbonization volume determination reference GB12441-2018 facing fireproof paint, antibacterial performance reference QB/T2591 ≡2003 antibacterial plastics ≡antibacterial performance test method and antibacterial effect.
Table 1 wood lacquer coating performance parameters
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (10)
1. The preparation method of the flame-retardant antibacterial wood paint is characterized by comprising the following steps of:
(1) Vacuum drying PPG2000, 1, 4-butanediol and dimethylolpropionic acid at 95-100 ℃ for 2-4 hours for later use; mixing PPG2000 and isophorone diisocyanate, reacting for 2-4 hours at 75-85 ℃, then adding dimethylolpropionic acid to react for 1-2 hours, cooling to 60-75 ℃, adding 1, 4-butanediol, trimethylolpropane and dibutyltin dilaurate, and reacting for 2-3 hours to obtain a waterborne polyurethane prepolymer;
(2) Modified nano SiO 2 Dispersing in acetone, carrying out ultrasonic treatment for 5-15 min, slowly dripping into a waterborne polyurethane prepolymer, reacting for 1-2 h, cooling to 30-40 ℃, adding triethylamine for neutralization for 0.5-1 h, then adding deionized water and ethylenediamine, emulsifying for 0.5-1 h at 1500-1800 r/min, and removing acetone by rotary evaporation after the reaction is finished, thus obtaining the flame-retardant antibacterial wood lacquer coating.
2. The method according to claim 1, wherein in the step (1), the weight ratio of PPG2000, isophorone diisocyanate, and dimethylolpropionic acid is 10: 11-15: 0.8 to 1.2; the weight ratio of 1, 4-butanediol, trimethylolpropane and dibutyltin dilaurate is 3-5: 1:0.02 to 0.04; the weight of the trimethylolpropane accounts for 1.5 to 3 percent of the total weight of the PPG2000 and the isophorone diisocyanate.
3. The method according to claim 1, wherein in the step (2), the nano SiO is modified 2 The weight ratio of the polyurethane to the aqueous polyurethane prepolymer is 0.5-2: 100; the weight ratio of deionized water to ethylenediamine is 120-150: 1, a step of; modified nano SiO 2 The weight ratio of the catalyst to triethylamine is 1:0.4 to 0.9.
4. The method of claim 1, wherein the modified nano-SiO 2 The preparation method of the (C) comprises the following steps:
a. nano SiO 2 Adding KH602 into deionized water, performing ultrasonic treatment, stirring for reaction, filtering, washing, and drying to obtain amino nanometer SiO 2 ；
b. Aminated nano SiO 2 Dispersing in absolute ethanol to obtain dispersion, dropwise adding DOPO-OH solution into the dispersion under stirring, stirring for reaction, filtering, washing, and drying to obtain functional nanometer SiO 2 ；
c. Will functionalize nano SiO 2 Adding thiourea dioxide into deionized water, stirring for reaction, filtering, washing and drying the product after the reaction is finished to obtain modified nano SiO 2 。
5. The method according to claim 4, wherein in step a, nano SiO is used as a catalyst for the preparation of the nano SiO 2 The weight volume of KH602 is 1g: 0.6-1.2 mL; ultrasonic treatment is carried out for 10-20 min, and stirring reaction is carried out for 8-16 h at the temperature of 40-60 ℃.
6. The method according to claim 4, wherein in step b, the nano SiO is aminated 2 The weight-volume ratio of DOPO-OH solution is 10g: 50-80 mL; the weight fraction of DOPO-OH solution is 15-20wt%; the reaction condition is that stirring reaction is carried out for 16-20 h at 70-85 ℃.
7. The process of claim 4, wherein in step b, the DOPO-OH solution is prepared by: dissolving DOPO in absolute ethyl alcohol, adding 25-35 wt% hydrogen peroxide under stirring, stirring at 80-90 ℃ for reaction for 16-20 h, after the reaction is finished, removing a solvent by rotary evaporation, washing and drying to obtain DOPO-OH, and dissolving DOPO-OH in absolute ethyl alcohol to obtain DOPO-OH solution; the weight volume of DOPO and hydrogen peroxide is 20-30 g:120mL.
8. The method of claim 4, wherein in step c, the nano SiO is functionalized 2 The thiourea dioxide has a weight of 1:1.1 to 1.5; stirring reaction is carried out for 12-18 h at 70-90 ℃.
9. A flame retardant and bacteriostatic wood lacquer coating prepared by the preparation method according to any one of claims 1-8.
10. Use of the wood lacquer coating according to claim 9 in flame-retardant and bacteriostatic applications of woodware.
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| CN102399376A (en) * | 2010-09-09 | 2012-04-04 | 中国科学院化学研究所 | Silicon dioxide with organic functional molecules grafted on surface, preparation method thereof, and purpose thereof |
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| CN110590849A (en) * | 2019-10-08 | 2019-12-20 | 中国科学技术大学 | Phosphorus-nitrogen-containing DOPO derivative flame retardant and preparation method and application thereof |
| CN110903513A (en) * | 2019-12-03 | 2020-03-24 | 苏州诺博恩新材料科技有限公司 | Silicon dioxide core-shell antibacterial flame retardant and preparation method thereof |
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| CN102399376A (en) * | 2010-09-09 | 2012-04-04 | 中国科学院化学研究所 | Silicon dioxide with organic functional molecules grafted on surface, preparation method thereof, and purpose thereof |
| CN105968306A (en) * | 2016-05-25 | 2016-09-28 | 杭州吉华高分子材料股份有限公司 | Preparation method of nano-silicon-dioxide-modified water-based polyurethane |
| CN110590849A (en) * | 2019-10-08 | 2019-12-20 | 中国科学技术大学 | Phosphorus-nitrogen-containing DOPO derivative flame retardant and preparation method and application thereof |
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