CN116041908A - Modified epoxy resin with antifouling effect and preparation method thereof - Google Patents
Modified epoxy resin with antifouling effect and preparation method thereof Download PDFInfo
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- CN116041908A CN116041908A CN202310051154.2A CN202310051154A CN116041908A CN 116041908 A CN116041908 A CN 116041908A CN 202310051154 A CN202310051154 A CN 202310051154A CN 116041908 A CN116041908 A CN 116041908A
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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
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- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
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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
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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
- C09D5/16—Antifouling paints; Underwater paints
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Abstract
The invention discloses a modified epoxy resin with an antifouling effect and a preparation method thereof. The preparation method of the modified epoxy resin with the antifouling effect is characterized in that the antifouling composition is added into the epoxy resin, and the modified epoxy resin with the antifouling effect is obtained after uniform mixing. The antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method: extracting dried Chinese flowering crabapple leaf with ethanol under reflux to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves, namely the crabapple leaf extract. The modified epoxy resin has excellent antifouling performance to marine organisms; therefore, the coating prepared by taking the modified epoxy resin as a base material is used for ships or marine constructions; the marine antifouling agent can enable ships or marine buildings to show a certain antifouling capacity to marine organisms, so that the marine organisms are not easy to adsorb on the surface of the marine organisms.
Description
Technical Field
The invention relates to the technical field of modified epoxy resin, in particular to modified epoxy resin with an antifouling effect and a preparation method thereof.
Background
Epoxy resins are the generic name for a class of polymers containing more than two epoxy groups in the molecule; because of excellent physical and mechanical properties, electrical insulation properties and adhesion properties with various materials; therefore, the method is widely used for preparing coatings, composite materials, casting materials, adhesives and the like; it is widely used in various fields of national economy. The epoxy resin coating is prepared by taking epoxy resin as a base material, and is one of main synthetic resin coatings; such as architectural coatings, automotive coatings, marine coatings, machine coatings, and the like, are widely used.
However, the antifouling performance of the existing epoxy resin on marine organisms needs to be improved; when the coating prepared by using the epoxy resin as the base material is used for ship and ocean constructional engineering; due to the lack of antifouling property to marine organisms, marine organisms are easily adsorbed on the surface of ships or marine buildings. Therefore, the epoxy resin with antifouling performance to marine organisms has important application value.
Disclosure of Invention
In order to overcome at least one technical problem existing in the prior art, the invention firstly provides a preparation method of modified epoxy resin with an antifouling effect.
The technical scheme of the invention is as follows:
a preparation method of modified epoxy resin with an antifouling effect comprises the steps of adding an antifouling composition into the epoxy resin, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect.
Preferably, the anti-fouling composition is a begonia leaf extract;
the begonia leaf extract is prepared by the following method:
extracting dried Chinese flowering crabapple leaf with ethanol under reflux to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves, namely the crabapple leaf extract.
The inventor surprisingly found in the research that the modified epoxy resin obtained by adding the ethanol extract of the crabapple leaves into the epoxy resin has a certain antifouling performance on marine organisms.
Further preferably, the ethanol adopts an ethanol aqueous solution with the volume fraction of 70-95%.
Most preferably, the ethanol is an aqueous ethanol solution with a volume fraction of 95%.
Further preferably, the weight amount of the ethanol is 5-15 times of that of the dried crabapple leaves.
Most preferably, the ethanol is used in an amount of 10 times the weight of the dried crabapple leaves.
Further preferably, the ethanol extract of the crabapple leaf is further suspended by adding water to obtain a mixed solution; then adding an organic solvent for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract.
In further research, the inventor finds that the anti-fouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved by adding the begonia leaf extract obtained by extracting the begonia leaf ethanol extract with an organic solvent into the epoxy resin; the prepared modified epoxy resin has excellent antifouling performance to marine organisms.
Further preferably, the dosage ratio of the ethanol extract of the malus spectabilis leaves to the water and the organic solvent is 1 g:20-40 mL:20-40 mL.
Most preferably, the ethanol extract of the crabapple leaf and the water and the organic solvent are used in an amount ratio of 1g to 30mL.
Further preferably, the organic solvent consists of isooctane, trichloroethane and toluene.
The inventor discovers that the composition of the organic solvent in the extraction process plays a decisive factor for the prepared malus spectabilis leaf extract and for whether the prepared modified epoxy resin can be further and greatly improved on the antifouling performance of marine organisms.
The inventor researches in a large number of experiments show that the begonia leaf extract obtained by extracting with single isooctane, trichloroethane, toluene or other organic solvents or the begonia leaf extract obtained by extracting with the combination of other organic solvents can not greatly improve the antifouling performance of the prepared modified epoxy resin on marine organisms compared with the begonia leaf ethanol extract. Only the begonia leaf extract obtained by extraction with an organic solvent comprising isooctane, trichloroethane and toluene can further greatly improve the antifouling performance of the prepared modified epoxy resin on marine organisms compared with the begonia leaf ethanol extract.
Further preferably, the volume ratio of isooctane, trichloroethane and toluene is 5-8:1-3:1-2.
Most preferably, the volume ratio of isooctane, trichloroethane, and toluene is 7:2:1.
Preferably, the weight ratio of the epoxy resin to the anti-fouling composition is 100:3-10.
It is further preferred that the weight ratio of the epoxy resin to the anti-fouling composition is 100:4 to 6.
Most preferably, the weight ratio of epoxy resin to anti-fouling composition is 100:5.
Preferably, the anti-fouling composition consists of a begonia leaf extract, decyl glucopyranoside and cetyl trimethylammonium chloride.
The inventor further and surprisingly found in the research that the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved compared with the addition of the single crabapple leaf extract by adding the composition formed by mixing the crabapple leaf extract with decyl glucopyranoside and hexadecyl trimethyl ammonium chloride into the epoxy resin; the prepared modified epoxy resin has excellent antifouling performance to marine organisms.
However, the inventor also found that the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved compared with the addition of the single crabapple leaf extract by adding the composition formed by mixing the crabapple leaf extract with decyl glucopyranoside and hexadecyl trimethyl ammonium chloride into the epoxy resin; the antifouling property of the prepared modified epoxy resin to marine organisms cannot be further improved greatly by adding only the composition formed by mixing the begonia leaf extract with decyl glucopyranoside, or only the composition formed by mixing the begonia leaf extract with cetyltrimethylammonium chloride to the epoxy resin.
Further preferably, the weight ratio of the begonia leaf extract to decyl glucopyranoside to cetyl trimethylammonium chloride is 7-10:1-2:1-2.
Most preferably, the weight ratio of the begonia leaf extract to decyl glucopyranoside and cetyl trimethylammonium chloride is 8:1:1.
The invention also provides the modified epoxy resin with the antifouling effect, which is prepared by the preparation method.
The beneficial effects are that: the invention provides a brand new modified epoxy resin; according to the invention, the ethanol extract of the crabapple leaves is added into the epoxy resin, so that the obtained modified epoxy resin has a certain antifouling property on marine organisms. Particularly, the begonia leaf extract is obtained by adding the begonia leaf ethanol extract and extracting the begonia leaf ethanol extract by an organic solvent, so that the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved; the prepared modified epoxy resin has excellent antifouling performance to marine organisms. The modified epoxy resin has excellent antifouling performance to marine organisms; therefore, the coating prepared by taking the modified epoxy resin as a base material is used for ships or marine constructions; the marine antifouling agent can enable ships or marine buildings to show a certain antifouling capacity to marine organisms, so that the marine organisms are not easy to adsorb on the surface of the marine organisms.
Description of the preferred embodiments
The present invention is further explained below with reference to specific examples, which are not intended to limit the present invention in any way.
The following epoxy resin was used under the trademark E-51 of Baling petrochemical industry.
Example 1 preparation of modified epoxy resin having antifouling Effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method: adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves, namely the crabapple leaf extract.
Example 2 preparation of modified epoxy resin having antifouling Effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane, trichloroethane and toluene in a volume ratio of 7:2:1.
Example 3 preparation of modified epoxy resin with antifouling Effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the antifouling composition is 100:3;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding ethanol water solution with the volume fraction of 70% and 15 times of the weight of the dried Chinese flowering crabapple leaves into the mixture, heating the mixture to a boiling state, carrying out reflux extraction for 2 hours, and filtering the mixture after the extraction is finished to obtain an extracting solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g to 40mL;
the organic solvent consists of isooctane, trichloroethane and toluene in a volume ratio of 8:1:1.
Example 4 preparation of modified epoxy resin with antifouling Effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the antifouling composition is 100:10;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of 80% ethanol water solution by weight into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 1 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:20mL:20mL;
the organic solvent consists of isooctane, trichloroethane and toluene in a volume ratio of 5:3:2.
Example 5 preparation of modified epoxy resin having antifouling Effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is prepared by mixing a begonia leaf extract, decyl glucopyranoside and cetyl trimethyl ammonium chloride according to a weight ratio of 8:1:1;
the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane, trichloroethane and toluene in a volume ratio of 7:2:1.
Comparative example 1 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent is isooctane.
Comparative example 1 differs from example 2 in that in the preparation of the begonia leaf extract, only isooctane was used as the organic solvent for extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 2 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent is trichloroethane.
Comparative example 2 differs from example 2 in that during the preparation of the begonia leaf extract, only trichloroethane was used as the organic solvent for extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 3 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent is toluene.
Comparative example 3 differs from example 2 in that during the preparation of the begonia leaf extract, toluene alone was used as the organic solvent for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 4 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent is ethyl acetate.
Comparative example 4 differs from example 2 in that during the preparation of the begonia leaf extract, only ethyl acetate was used as the organic solvent for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 5 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent is n-butanol.
Comparative example 5 differs from example 2 in that in the preparation of the begonia leaf extract, only n-butanol was used as the organic solvent for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 6 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane and trichloroethane with a volume ratio of 7:3.
Comparative example 6 differs from example 2 in that during the preparation of the extract of the leaf of the malus spectabilis, only an organic solvent consisting of isooctane and trichloroethane is used for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 7 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane and toluene in a volume ratio of 7:3.
Comparative example 7 differs from example 2 in that in the preparation of the begonia leaf extract, only an organic solvent consisting of isooctane and toluene was used for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Preparation of modified epoxy resin having antifouling Effect of comparative example 8
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane, trichloroethane and ethyl acetate in a volume ratio of 7:2:1.
Comparative example 8 differs from example 2 in that during the preparation of the begonia leaf extract, an organic solvent consisting of isooctane, trichloroethane and ethyl acetate is used for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 9 preparation of modified epoxy resin having antifouling effect
Adding the antifouling composition and the epoxy resin into a dispersing mixer, and uniformly mixing to obtain the modified epoxy resin with the antifouling effect;
wherein the weight ratio of the epoxy resin to the anti-fouling composition is 100:5;
the antifouling composition is a begonia leaf extract; the begonia leaf extract is prepared by the following method:
(1) Adding 10 times of ethanol water solution with volume fraction of 95% into dried folium Mali Pumilae, heating to boiling state, reflux extracting for 2 hr, and filtering to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves;
(2) Adding water into the ethanol extract of the crabapple leaves for suspension to obtain a mixed solution; then adding an organic solvent into the mixed solution for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract;
wherein, the dosage ratio of the ethanol extract of the crabapple leaf to the water and the organic solvent is 1g:30mL:30mL;
the organic solvent consists of isooctane, n-butanol and toluene in a volume ratio of 7:2:1.
Comparative example 8 differs from example 2 in that during the preparation of the begonia leaf extract, an organic solvent consisting of isooctane, n-butanol and toluene is used for the extraction; in example 2, extraction was performed with an organic solvent consisting of isooctane, trichloroethane and toluene.
Comparative example 10 preparation of modified epoxy resin having antifouling effect
Comparative example 10 differs from example 5 in the composition of the anti-fouling composition; the remainder was the same as in example 5;
the antifouling composition is prepared by mixing a begonia leaf extract and decyl glucopyranoside according to a weight ratio of 8:2. A step of
The preparation method of the begonia leaf extract is the same as that of example 5.
Comparative example 11 preparation of modified epoxy resin having antifouling effect
Comparative example 11 differs from example 5 in that the composition of the anti-fouling composition is different; the remainder was the same as in example 5;
the antifouling composition is prepared by mixing a begonia leaf extract and cetyltrimethylammonium chloride according to a weight ratio of 8:2. A step of
The preparation method of the begonia leaf extract is the same as that of example 5.
Experimental example
50 parts by weight of modified epoxy resin with an antifouling effect, which is prepared in examples 1-5 and comparative examples 1-11, are respectively and uniformly mixed with 30 parts by weight of talcum powder filler, 2 parts by weight of silane coupling agent KH-560 and 40 parts by weight of epoxy resin curing agent 593 to prepare modified epoxy resin coatings, and the modified epoxy resin coatings are respectively sprayed on steel plates with the thickness of 2cm multiplied by 20cm, wherein the thickness of the sprayed coating is 1mm; solidifying for 24 hours at room temperature after the spraying is finished; the steel sheet to be tested is obtained. And meanwhile, preparing an epoxy resin coating by adopting unmodified E-51 epoxy resin according to the method, spraying the epoxy resin coating on the steel plate according to the method, and taking the steel plate as a control test steel plate.
Soaking all the test steel plates in the same sea water, taking out the steel plates after 6 months, and counting the number of organisms attached to each test steel plate; the test results are shown in Table 1.
TABLE 1 antifouling property test results of the modified epoxy resin of the invention on marine organisms
From the experimental data in table 1, it can be seen that the number of organisms attached to the test steel plate 1 is significantly smaller than that of the test steel plate 17. This illustrates: the ethanol extract of the crabapple leaves is added into the epoxy resin, and the obtained modified epoxy resin has certain antifouling performance on marine organisms.
As can be seen from the experimental data in table 1, the number of organisms attached to the test steel plates 2 to 4 was further significantly smaller than that of the test steel plate 1. This illustrates: compared with the ethanol extract of the crabapple leaves, the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved.
As can be seen from the experimental data in Table 1, the number of organisms attached to the test steel plates 6 to 14 is not significantly reduced compared with the test steel plate 1, and the reduction is far smaller than that of the test steel plates 2 to 4. This illustrates: the composition of the organic solvent in the extraction process plays a decisive factor for the prepared crabapple leaf extract and for whether the prepared modified epoxy resin can be further and greatly improved on the antifouling performance of marine organisms. The begonia leaf extract obtained by extraction with single isooctane, trichloroethane, toluene or other organic solvents, or the begonia leaf extract obtained by extraction with a combination of other organic solvents, can not greatly improve the antifouling property of the prepared modified epoxy resin to marine organisms compared with the begonia leaf ethanol extract. Only the begonia leaf extract obtained by extraction with an organic solvent comprising isooctane, trichloroethane and toluene can further greatly improve the antifouling performance of the prepared modified epoxy resin on marine organisms compared with the begonia leaf ethanol extract.
As can be seen from the experimental data in Table 1, the number of organisms attached to the test steel sheet 2 is significantly smaller than those of the test steel sheets 6 to 8. This illustrates: meanwhile, the begonia leaf extract obtained by extracting with an organic solvent consisting of isooctane, trichloroethane and toluene can synergistically improve the antifouling performance of the prepared modified epoxy resin on marine organisms.
As can be seen from the experimental data in table 1, the number of organisms attached to the test steel sheet 5 is further significantly smaller than those of the test steel sheets 2 to 4. This illustrates: the composition formed by mixing the begonia leaf extract with decyl glucopyranoside and cetyl trimethyl ammonium chloride is added into the epoxy resin, so that the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved compared with the case of adding the separate begonia leaf extract; the prepared modified epoxy resin has excellent antifouling performance to marine organisms.
As can be seen from the experimental data in Table 1, the number of organisms attached to the test steel plates 15 and 16 was not significantly reduced compared with the test steel plates 2 to 4, and the reduction was much smaller than that of the test steel plate 5. This illustrates: the composition formed by mixing the crabapple leaf extract with decyl glucopyranoside and cetyl trimethyl ammonium chloride is added into the epoxy resin, so that the antifouling performance of the prepared modified epoxy resin on marine organisms can be further greatly improved compared with the case of adding the single crabapple leaf extract; the antifouling property of the prepared modified epoxy resin to marine organisms cannot be further improved greatly by adding only the composition formed by mixing the begonia leaf extract with decyl glucopyranoside, or only the composition formed by mixing the begonia leaf extract with cetyltrimethylammonium chloride to the epoxy resin.
Claims (10)
1. A preparation method of modified epoxy resin with an antifouling effect is characterized in that an antifouling composition is added into the epoxy resin, and the modified epoxy resin with the antifouling effect is obtained after uniform mixing.
2. The method for preparing modified epoxy resin with antifouling effect according to claim 1, wherein the antifouling composition is a begonia leaf extract;
the begonia leaf extract is prepared by the following method:
extracting dried Chinese flowering crabapple leaf with ethanol under reflux to obtain extractive solution; concentrating and drying the extracting solution to obtain the ethanol extract of the crabapple leaves, namely the crabapple leaf extract.
3. The method for preparing modified epoxy resin with antifouling effect according to claim 2, wherein the ethanol is an aqueous ethanol solution with a volume fraction of 70-95%;
most preferably, the ethanol is an aqueous ethanol solution with a volume fraction of 95%.
4. The method for preparing modified epoxy resin with antifouling effect according to claim 2, wherein the weight amount of ethanol is 5-15 times of that of dried begonia leaves;
most preferably, the ethanol is used in an amount of 10 times the weight of the dried crabapple leaves.
5. The method for preparing modified epoxy resin with antifouling effect according to claim 2, wherein the ethanol extract of the crabapple leaf is further suspended in water to obtain a mixed solution; then adding an organic solvent for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the crabapple leaf extract.
6. The method for preparing modified epoxy resin with antifouling effect according to claim 5, wherein the dosage ratio of the ethanol extract of the crabapple leaf to water and the organic solvent is 1 g:20-40 mL:20-40 mL;
most preferably, the ethanol extract of the crabapple leaf and the water and the organic solvent are used in an amount ratio of 1g to 30mL.
7. The method for producing an antifouling modified epoxy resin according to claim 5, wherein said organic solvent comprises isooctane, trichloroethane and toluene.
8. The method for producing a modified epoxy resin having an antifouling effect according to claim 7, wherein the volume ratio of isooctane, trichloroethane and toluene is 5 to 8:1 to 3:1 to 2.
Most preferably, the volume ratio of isooctane, trichloroethane, and toluene is 7:2:1.
9. The method for producing a modified epoxy resin having an antifouling effect according to claim 1, wherein the weight ratio of the epoxy resin to the antifouling composition is 100:3 to 10;
further preferably, the weight ratio of the epoxy resin to the anti-fouling composition is from 100:4 to 6;
most preferably, the weight ratio of epoxy resin to anti-fouling composition is 100:5.
10. The modified epoxy resin with antifouling effect prepared by the preparation method of any one of claims 1 to 9.
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