CN115537095A - Luminous multi-section flexible bionic bait and preparation method thereof - Google Patents
Luminous multi-section flexible bionic bait and preparation method thereof Download PDFInfo
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- CN115537095A CN115537095A CN202210384503.8A CN202210384503A CN115537095A CN 115537095 A CN115537095 A CN 115537095A CN 202210384503 A CN202210384503 A CN 202210384503A CN 115537095 A CN115537095 A CN 115537095A
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- 239000011664 nicotinic acid Substances 0.000 title claims abstract description 65
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 230000007062 hydrolysis Effects 0.000 claims description 57
- 238000006460 hydrolysis reaction Methods 0.000 claims description 57
- 238000003756 stirring Methods 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 36
- 239000000839 emulsion Substances 0.000 claims description 32
- 229920005989 resin Polymers 0.000 claims description 29
- 239000011347 resin Substances 0.000 claims description 29
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 28
- 239000011248 coating agent Substances 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 28
- 238000010992 reflux Methods 0.000 claims description 23
- 239000008367 deionised water Substances 0.000 claims description 21
- 229910021641 deionized water Inorganic materials 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 20
- 239000007795 chemical reaction product Substances 0.000 claims description 18
- 239000003973 paint Substances 0.000 claims description 18
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 229920001909 styrene-acrylic polymer Polymers 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- ZFVMWEVVKGLCIJ-UHFFFAOYSA-N bisphenol AF Chemical compound C1=CC(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C=C1 ZFVMWEVVKGLCIJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000706 filtrate Substances 0.000 claims description 11
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 10
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 10
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000012074 organic phase Substances 0.000 claims description 10
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 10
- 229960001553 phloroglucinol Drugs 0.000 claims description 10
- DMAYBPBPEUFIHJ-UHFFFAOYSA-N 4-bromobut-1-ene Chemical compound BrCCC=C DMAYBPBPEUFIHJ-UHFFFAOYSA-N 0.000 claims description 9
- XKBGEWXEAPTVCK-UHFFFAOYSA-M methyltrioctylammonium chloride Chemical compound [Cl-].CCCCCCCC[N+](C)(CCCCCCCC)CCCCCCCC XKBGEWXEAPTVCK-UHFFFAOYSA-M 0.000 claims description 8
- IYDGMDWEHDFVQI-UHFFFAOYSA-N phosphoric acid;trioxotungsten Chemical compound O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.O=[W](=O)=O.OP(O)(O)=O IYDGMDWEHDFVQI-UHFFFAOYSA-N 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- 229960001701 chloroform Drugs 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 8
- 241000251468 Actinopterygii Species 0.000 description 7
- 125000003342 alkenyl group Chemical group 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000003828 vacuum filtration Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- 125000001246 bromo group Chemical group Br* 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 2
- 238000007792 addition Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010534 nucleophilic substitution reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01K—ANIMAL HUSBANDRY; CARE OF BIRDS, FISHES, INSECTS; FISHING; REARING OR BREEDING ANIMALS, NOT OTHERWISE PROVIDED FOR; NEW BREEDS OF ANIMALS
- A01K85/00—Artificial bait for fishing
- A01K85/01—Artificial bait for fishing with light emission, sound emission, scent dispersal or the like
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
- C08G59/027—Polycondensates containing more than one epoxy group per molecule obtained by epoxidation of unsaturated precursor, e.g. polymer or monomer
-
- 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
- C09D5/22—Luminous paints
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Environmental Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Marine Sciences & Fisheries (AREA)
- Animal Husbandry (AREA)
- Biodiversity & Conservation Biology (AREA)
- Paints Or Removers (AREA)
Abstract
The invention relates to the field of bionic bait, in particular to luminous multi-section flexible bionic bait and a preparation method thereof, which are used for solving the problem that fluorescence luminosity is reduced or even disappears when the existing luminous multi-section flexible bionic bait is immersed in water for a long time.
Description
Technical Field
The invention relates to the field of bionic bait, in particular to luminous multi-section flexible bionic bait and a preparation method thereof.
Background
The artificial bait sold in the market in the future has simple structure and low sensitivity, so the fishing efficiency is low. The patent with the application number of CN201220232815.9 discloses a luminous multi-section flexible swinging bionic bait, which mainly comprises the bionic bait and two three-fork fish hooks, wherein the bait body part of the bionic bait is of a multi-section skeleton structure, the head part of the bait is coated with red paint, the tail part of the bait is made of red soft plastic, the whole appearance of the bait is sprayed with fluorescent paint, so that the bait can attract a fish to bite the bionic bait, the fishing condition of the fishing person can be timely and accurately mastered by the fishing person, the efficiency of the bionic bait on a fishing rod is improved, if a fish bites the food of the artificial bait, the fishing person can flexibly shake up and down and left and right, when the fish bites the food of the artificial bait, the fishing float and the fishing rod of the floating float are required, and the like, the light emitted by the luminous multi-section flexible swinging bionic bait can be displayed by the fluorescent light, the sentiment of the fishing person can be improved, and the fishing person can be relieved from the fishing rod at night.
However, the existing fluorescent paint for the bionic bait has poor water resistance, and the coating is damaged after being immersed in water for a long time, so that the fluorescence luminosity of the luminous multi-section flexible bionic bait is reduced or even disappears, and the aim of attracting fishes to bite the bait is difficult to achieve.
How to improve the problem that the fluorescence luminosity is reduced or even disappears caused by long-time immersion of the existing luminous multi-section flexible bionic bait in water is the key of the invention, and therefore, a luminous multi-section flexible bionic bait and a preparation method thereof are urgently needed to solve the problems.
Disclosure of Invention
In order to overcome the technical problems, the invention aims to provide a luminous multi-section flexible bionic bait and a preparation method thereof, wherein the luminous multi-section flexible bionic bait comprises the following steps: the hydrolysis-resistant resin, the styrene-acrylic emulsion and the 4,4-diaminodiphenylmethane are stirred and mixed to obtain mixed emulsion, deionized water, the acrylate leveling agent, the silane coupling agent and the fluorescent powder are added into the mixed emulsion to be continuously stirred to obtain hydrolysis-resistant luminous paint, the hydrolysis-resistant luminous paint is sprayed on the bionic bait with a multi-section framework, and then the paint is solidified to form a coating, so that the luminous multi-section flexible bionic bait is obtained, and the problem that the fluorescence luminosity is reduced or even disappears due to the fact that the existing luminous multi-section flexible bionic bait is immersed in water for a long time is solved.
The purpose of the invention can be realized by the following technical scheme:
a luminous multi-section flexible bionic bait comprises a bionic bait and a hydrolysis-resistant luminous coating on the surface of the bionic bait;
the bionic bait is a bionic bait with a multi-section framework;
the hydrolysis-resistant luminescent coating is prepared by the following steps:
the method comprises the following steps: weighing 50-70 parts of hydrolysis-resistant resin, 30-40 parts of styrene-acrylic emulsion, 20-30 parts of deionized water, 5-15 parts of 4,4-diaminodiphenylmethane, 5-8 parts of acrylate leveling agent, 3-10 parts of silane coupling agent and 3.5-10.5 parts of fluorescent powder according to parts by weight for later use;
step two: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 70-90 ℃, stirring and mixing for 1-2h to obtain mixed emulsion;
step three: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2-3 hours to obtain hydrolysis-resistant luminous paint;
step four: and (3) spraying the hydrolysis-resistant luminescent coating and then curing to obtain the hydrolysis-resistant luminescent coating.
As a further scheme of the invention: the preparation method of the hydrolysis-resistant resin comprises the following steps:
a1: adding bisphenol AF, sodium hydroxide and acetone into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, heating to reflux reaction for 30-60min while stirring at the stirring rate of 200-300r/min, then dropwise adding deionized water while stirring, controlling the dropwise adding rate to be 3-5mL/min, continuing to stir and react for 30-40min after dropwise adding is finished, then dropwise adding 4-bromo-1-butene, controlling the dropwise adding rate to be 1-2 drops/s, keeping reflux reaction for 8-10h after dropwise adding is finished, cooling a reaction product to room temperature after reaction is finished, carrying out vacuum filtration, carrying out rotary evaporation on filtrate, dissolving in carbon tetrachloride, washing an organic phase with a sodium hydroxide solution for 2-3 times, then washing with distilled water for 2-3 times, and then carrying out rotary evaporation and drying to obtain an intermediate 1;
the reaction principle is as follows:
under the alkaline condition, bisphenol AF reacts with 4-bromo-1-butene, hydroxyl on the bisphenol AF and bromine atoms on the 4-bromo-1-butene generate nucleophilic substitution reaction, so that alkenyl is introduced, and the generated intermediate 1 contains alkenyl and hydroxyl and simultaneously contains a large amount of trifluoromethyl by controlling the dosage of the bisphenol AF and the bromine atoms on the 4-bromo-1-butene;
a2: adding phloroglucinol, phthalic anhydride and anhydrous ether into a three-neck flask provided with a stirrer, a thermometer and an air guide tube, introducing nitrogen for protection, stirring and reacting for 10-15h under the conditions that the temperature is 25-30 ℃ and the stirring speed is 300-500r/min, then adding the intermediate 1, continuously stirring and reacting for 20-30h, and after the reaction is finished, carrying out rotary evaporation on a reaction product to remove a solvent, thus obtaining an intermediate 2;
the reaction principle is as follows:
the preparation method comprises the following steps of reacting phloroglucinol with phthalic anhydride, carrying out esterification reaction on phenolic hydroxyl on the phloroglucinol with the phthalic anhydride to form a hyperbranched structure, introducing a large number of carboxyl groups, and then carrying out esterification reaction on the carboxyl groups and the phenolic hydroxyl on the intermediate 1 continuously to obtain an intermediate 2 containing a large number of C-F bonds and alkenyl groups;
a3: adding the intermediate 2, trichloromethane, phosphotungstic acid and methyl trioctyl ammonium chloride into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, dropwise adding hydrogen peroxide while stirring at the temperature of 30-32 ℃ and the stirring speed of 200-300r/min, controlling the dropwise adding speed to be 1-2 drops/s, carrying out reflux reaction for 8-10h after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, washing with distilled water for 2-3 times, drying an organic phase with anhydrous sodium sulfate, filtering, and carrying out rotary evaporation and drying on the filtrate to obtain the hydrolysis-resistant resin.
The reaction principle is as follows:
under the catalytic action of phosphotungstic acid and methyl trioctyl ammonium chloride, the intermediate 2 reacts with hydrogen peroxide, the hydrogen peroxide has strong oxidizing property, and the alkenyl on the intermediate 2 is oxidized to form an epoxy functional group, so that the hydrolysis-resistant resin is obtained.
As a further scheme of the invention: the dosage ratio of the bisphenol AF, the sodium hydroxide, the acetone, the deionized water and the 4-bromo-1-butene in the step A1 is 0.1mol:8.0g:120-150mL:20-30mL:0.11mol, and the mass fraction of the sodium hydroxide solution is 10-15%.
As a further scheme of the invention: the dosage ratio of the phloroglucinol, the phthalic anhydride, the anhydrous ether and the intermediate 1 in the step A2 is 0.1mol:0.3mol:100-150mL:0.33mol.
As a further scheme of the invention: the dosage ratio of the intermediate 2, the trichloromethane, the phosphotungstic acid, the methyl trioctyl ammonium chloride and the hydrogen peroxide in the step A3 is 0.1mol:80-100mL:1.0-1.2g:1.3-1.5g:0.2mol.
As a further scheme of the invention: a preparation method of luminous multi-section flexible bionic bait comprises the following steps:
s1: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 70-90 ℃, stirring and mixing for 1-2h to obtain mixed emulsion;
s2: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2-3 hours to obtain the hydrolysis-resistant luminous coating, wherein the silane coupling agent is one of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570;
s3: and spraying hydrolysis-resistant luminous paint on the bionic bait with the multi-section framework, and then curing to form a coating to obtain the luminous multi-section flexible bionic bait.
The invention has the beneficial effects that:
according to the light-emitting multi-section flexible bionic bait and the preparation method thereof, hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane are stirred and mixed to obtain mixed emulsion, deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder are added into the mixed emulsion to be continuously stirred to obtain hydrolysis-resistant light-emitting paint, the hydrolysis-resistant light-emitting paint is sprayed on the bionic bait with a multi-section framework, and then the paint is solidified to form a coating, so that the light-emitting multi-section flexible bionic bait is obtained; according to the preparation method, the bionic bait with the multi-section framework is used as the substrate, the bionic bait can be guaranteed to swing along with water flow, the fish luring property is improved, then the hydrolysis-resistant luminous paint is sprayed to form a coating and emit fluorescence, the fish luring property of the bionic bait is further improved, the fishing pleasure is increased, moreover, the coating formed by the hydrolysis-resistant luminous paint is good in water resistance, cannot bubble or peel off after being used for a long time, the continuous fluorescence emission can be guaranteed after the bionic bait is used, and the service life of the bionic bait is prolonged.
The hydrolysis-resistant resin is prepared in the process of preparing the hydrolysis-resistant luminous coating of the luminous multi-section flexible bionic bait, bisphenol AF and 4-bromo-1-butene are reacted to generate an intermediate 1 containing alkenyl and hydroxyl and containing a large amount of trifluoromethyl, phloroglucinol is reacted with phthalic anhydride to form a hyperbranched structure, a large amount of carboxyl is introduced, and then the carboxyl is continuously reacted with the intermediate 1 to obtain an intermediate 2 containing a large amount of C-F bonds and alkenyl, so that the intermediate 2 is reacted with hydrogen peroxide, the alkenyl on the intermediate 2 is oxidized to form an epoxy functional group, and the hydrolysis-resistant resin is obtained.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
this embodiment is a method for preparing a hydrolysis-resistant resin, comprising the steps of:
a1: adding 0.1mol of bisphenol AF, 8.0g of sodium hydroxide and 120mL of acetone into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser, heating to reflux reaction for 30min while stirring at a stirring speed of 200r/min, then dropwise adding 20mL of deionized water while stirring, controlling the dropwise adding speed to be 3mL/min, continuing to stir and react for 30min after dropwise adding is finished, then dropwise adding 0.11mol4-bromo-1-butene, controlling the dropwise adding speed to be 1 drop/s, keeping reflux reaction for 8h after dropwise adding is finished, cooling a reaction product to room temperature after reaction is finished, carrying out vacuum filtration, carrying out rotary evaporation on filtrate, dissolving the filtrate in carbon tetrachloride, washing an organic phase for 2 times by using a sodium hydroxide solution with the mass fraction of 10%, then washing for 2 times by using distilled water, and then carrying out rotary evaporation to dry to obtain an intermediate 1;
a2: adding 0.1mol of phloroglucinol, 0.3mol of phthalic anhydride and 100mL of anhydrous ether into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, stirring and reacting for 10 hours at the temperature of 25 ℃ and the stirring speed of 300r/min, then adding 0.33mol of the intermediate 1, continuously stirring and reacting for 20 hours, and after the reaction is finished, rotationally evaporating a reaction product to remove a solvent to obtain an intermediate 2;
a3: adding 0.1mol of the intermediate 2, 80mL of trichloromethane, 1.0g of phosphotungstic acid and 1.3g of methyl trioctyl ammonium chloride into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, dropwise adding 0.2mol of hydrogen peroxide while stirring at the temperature of 30 ℃ and the stirring rate of 200r/min, controlling the dropwise adding rate to be 1 drop/s, carrying out reflux reaction for 8 hours after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, washing the reaction product with distilled water for 2 times, drying an organic phase with anhydrous sodium sulfate, filtering, and carrying out rotary evaporation and drying on the filtrate to obtain the hydrolysis-resistant resin.
Example 2:
the embodiment is a method for preparing hydrolysis-resistant resin, which comprises the following steps:
a1: adding 0.1mol of bisphenol AF, 8.0g of sodium hydroxide and 135mL of acetone into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, heating to reflux reaction for 45min while stirring at a stirring speed of 250r/min, dropwise adding 25mL of deionized water while stirring, controlling the dropwise adding speed to be 4mL/min, continuing to stir and react for 35min after the dropwise adding is finished, dropwise adding 0.11mol4-bromo-1-butene, controlling the dropwise adding speed to be 2 drops/s, keeping reflux reaction for 9h after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out rotary evaporation on a filtrate, dissolving the filtrate in carbon tetrachloride, washing an organic phase for 3 times by using a sodium hydroxide solution with the mass fraction of 12%, then washing for 3 times by using distilled water, and carrying out rotary evaporation to dryness to obtain an intermediate 1;
a2: adding 0.1mol of phloroglucinol, 0.3mol of phthalic anhydride and 130mL of anhydrous ether into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, stirring and reacting for 12 hours at the temperature of 28 ℃ and the stirring speed of 400r/min, then adding 0.33mol of the intermediate 1, continuing stirring and reacting for 25 hours, and after the reaction is finished, rotationally evaporating a reaction product to remove a solvent to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 90mL of trichloromethane, 1.1g of phosphotungstic acid and 1.4g of methyl trioctyl ammonium chloride into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, dropwise adding 0.2mol of hydrogen peroxide while stirring at the temperature of 31 ℃ and the stirring rate of 250r/min, controlling the dropwise adding rate to be 2 drops/s, carrying out reflux reaction for 9 hours after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, washing the reaction product with distilled water for 3 times, drying an organic phase with anhydrous sodium sulfate, filtering, and carrying out rotary evaporation and drying on the filtrate to obtain the hydrolysis-resistant resin.
Example 3:
the embodiment is a method for preparing hydrolysis-resistant resin, which comprises the following steps:
a1: adding 0.1mol of bisphenol AF, 8.0g of sodium hydroxide and 150mL of acetone into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, heating to reflux reaction for 60min while stirring at the stirring speed of 300r/min, then dropwise adding 30mL of deionized water while stirring, controlling the dropwise adding speed to be 5mL/min, continuing to stir and react for 40min after the dropwise adding is finished, then dropwise adding 0.11mol 4-bromo-1-butene, controlling the dropwise adding speed to be 2 drops/s, keeping reflux reaction for 10h after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, carrying out vacuum filtration, carrying out rotary evaporation on filtrate, dissolving in carbon tetrachloride, washing an organic phase for 3 times by using a sodium hydroxide solution with the mass fraction of 15%, then washing for 3 times by using distilled water, and carrying out rotary evaporation and drying to obtain an intermediate 1;
a2: adding 0.1mol of phloroglucinol, 0.3mol of phthalic anhydride and 150mL of anhydrous ether into a three-neck flask provided with a stirrer, a thermometer and a gas guide tube, introducing nitrogen for protection, stirring and reacting for 15 hours at the temperature of 30 ℃ and the stirring speed of 500r/min, then adding 0.33mol of the intermediate 1, continuing stirring and reacting for 30 hours, and after the reaction is finished, rotationally evaporating a reaction product to remove a solvent to obtain an intermediate 2;
a3: adding 0.1mol of intermediate 2, 100mL of trichloromethane, 1.2g of phosphotungstic acid and 1.5g of methyl trioctyl ammonium chloride into a three-neck flask provided with a stirrer, a thermometer, a constant-pressure dropping funnel and a reflux condenser tube, dropwise adding 0.2mol of hydrogen peroxide while stirring at the temperature of 32 ℃ and the stirring rate of 300r/min, controlling the dropwise adding rate to be 2 drops/s, carrying out reflux reaction for 10 hours after the dropwise adding is finished, cooling a reaction product to room temperature after the reaction is finished, washing the reaction product with distilled water for 3 times, drying an organic phase with anhydrous sodium sulfate, filtering, and carrying out rotary evaporation and drying on a filtrate to obtain the hydrolysis-resistant resin.
Example 4:
the embodiment provides a preparation method of a luminous multi-section flexible bionic bait, which comprises the following steps:
b1: weighing 50 parts of hydrolysis-resistant resin, 30 parts of styrene-acrylic emulsion, 20 parts of deionized water, 5 parts of 4,4-diaminodiphenylmethane, 5 parts of acrylate leveling agent, 3 parts of silane coupling agent and 3.5 parts of fluorescent powder in the embodiment 1 in parts by weight for later use;
b2: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 70 ℃, stirring and mixing for 1h to obtain mixed emulsion;
b3: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2 hours to obtain the hydrolysis-resistant luminous coating, wherein the silane coupling agent is a silane coupling agent KH-550;
b4: and spraying hydrolysis-resistant luminous paint on the bionic bait with the multi-section framework, and then curing to form a coating to obtain the luminous multi-section flexible bionic bait.
Example 5:
the embodiment is a preparation method of a luminous multi-section flexible bionic bait, which comprises the following steps:
b1: weighing 60 parts of hydrolysis-resistant resin, 35 parts of styrene-acrylic emulsion, 25 parts of deionized water, 4,4-diaminodiphenylmethane 10 parts, 6 parts of acrylate leveling agent, 7 parts of silane coupling agent and 7 parts of fluorescent powder in the embodiment 2 in parts by weight for later use;
b2: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 80 ℃, stirring and mixing for 2 hours to obtain mixed emulsion;
b3: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2 hours to obtain the hydrolysis-resistant luminous coating, wherein the silane coupling agent is a silane coupling agent KH-560;
b4: and spraying hydrolysis-resistant luminous paint on the bionic bait with the multi-section framework, and then curing to form a coating to obtain the luminous multi-section flexible bionic bait.
Example 6:
the embodiment is a preparation method of a luminous multi-section flexible bionic bait, which comprises the following steps:
b1: weighing 70 parts of hydrolysis-resistant resin, 40 parts of styrene-acrylic emulsion, 30 parts of deionized water, 4,4-diaminodiphenylmethane 15 parts, 8 parts of acrylate leveling agent, 10 parts of silane coupling agent and 10.5 parts of fluorescent powder in the embodiment 3 in parts by weight for later use;
b2: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 90 ℃, stirring and mixing for 2 hours to obtain mixed emulsion;
b3: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 3 hours to obtain the hydrolysis-resistant luminous coating, wherein the silane coupling agent is a silane coupling agent KH-570;
b4: and (3) spraying hydrolysis-resistant luminous paint on the bionic bait with the multi-section framework, and then solidifying to form a coating to obtain the luminous multi-section flexible bionic bait.
Comparative example 1:
comparative example 1 differs from example 6 in that an epoxy resin EP-44 was used instead of the hydrolysis-resistant resin.
Comparative example 2:
comparative example 2 is a water-resistant coating of CN201410809306.1, which was sprayed on a multi-joint skeleton bionic bait, and cured to form a coating, to obtain the bionic bait.
The coating performances of the bionic bait of the examples 4-6 and the comparative examples 1-2 are detected, and the detection results are as follows:
| sample (I) | Surface hardness | Salt spray resistance of 10000h | Resistant 3% brine 600D | Water resistance 600D |
| Example 4 | 5H | No bubble and no peeling | No bubble and no peeling | No bubble and no peeling |
| Example 5 | 5H | No bubble and no peeling | No bubble and no peeling | No bubble and no peeling |
| Example 6 | 6H | No bubble and no peeling | No bubble and no peeling | No bubble and no peeling |
| Comparative example 1 | 4H | With bubbles and flaking | With bubbles and peeling | With bubbles and flaking |
| Comparative example 2 | 3H | With bubbles and flaking | With bubbles and flaking | With bubbles and without flaking |
Referring to the data in the table, according to the comparison between the example and the comparative example 1, it can be known that the water resistance of the hydrolysis-resistant luminescent coating can be greatly improved by using hydrolysis-resistant resin to replace epoxy resin EP-44, so that the bionic bait has a fluorescence effect for a long time, and the service life of the bionic bait is prolonged.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (6)
1. A luminous multi-section flexible bionic bait is characterized by comprising the bionic bait and a hydrolysis-resistant luminous coating on the surface of the bionic bait;
the bionic bait is a bionic bait with a multi-section framework;
the hydrolysis-resistant luminous coating is prepared by the following steps:
the method comprises the following steps: weighing 50-70 parts of hydrolysis-resistant resin, 30-40 parts of styrene-acrylic emulsion, 20-30 parts of deionized water, 5-15 parts of 4,4-diaminodiphenylmethane, 5-8 parts of acrylate leveling agent, 3-10 parts of silane coupling agent and 3.5-10.5 parts of fluorescent powder according to parts by weight for later use;
step two: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 70-90 ℃, stirring and mixing for 1-2h to obtain mixed emulsion;
step three: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2-3 hours to obtain hydrolysis-resistant luminous paint;
step four: and (3) spraying the hydrolysis-resistant luminous coating and then curing to obtain the hydrolysis-resistant luminous coating.
2. The light-emitting type multi-section flexible bionic bait according to claim 1, wherein the preparation method of the hydrolysis-resistant resin comprises the following steps:
a1: adding bisphenol AF, sodium hydroxide and acetone into a three-neck flask, heating to reflux reaction while stirring at a stirring speed, dropwise adding deionized water while stirring, continuously stirring for reaction after dropwise adding is finished, dropwise adding 4-bromo-1-butene, maintaining reflux reaction after dropwise adding is finished, cooling and filtering a reaction product after reaction is finished, rotatably evaporating filtrate, dissolving, washing an organic phase, and drying to obtain an intermediate 1;
a2: adding phloroglucinol, phthalic anhydride and anhydrous ether into a three-neck flask, stirring for reaction, then adding the intermediate 1, continuing stirring for reaction, and rotationally evaporating a reaction product after the reaction is finished to obtain an intermediate 2;
a3: adding the intermediate 2, trichloromethane, phosphotungstic acid and methyl trioctyl ammonium chloride into a three-neck flask, dropwise adding hydrogen peroxide while stirring, carrying out reflux reaction after dropwise adding, cooling and washing a reaction product after the reaction is finished, and drying an organic phase to obtain the hydrolysis-resistant resin.
3. The light-emitting type multi-section flexible bionic bait according to claim 2, wherein the dosage ratio of the bisphenol AF, the sodium hydroxide, the acetone, the deionized water and the 4-bromo-1-butene in the step A1 is 0.1mol:8.0g:120-150mL:20-30mL:0.11mol.
4. The light-emitting multi-section flexible bionic bait according to claim 2, wherein the phloroglucinol, phthalic anhydride, anhydrous ether and the intermediate 1 in the step A2 are used in an amount ratio of 0.1mol:0.3mol:100-150mL:0.33mol.
5. The light-emitting type multi-section flexible bionic bait according to claim 2, wherein the dosage ratio of the intermediate 2, the trichloromethane, the phosphotungstic acid, the methyl trioctyl ammonium chloride and the hydrogen peroxide in the step A3 is 0.1mol:80-100mL:1.0-1.2g:1.3-1.5g:0.2mol.
6. The preparation method of the light-emitting multi-section flexible bionic bait according to claim 1, characterized by comprising the following steps:
s1: heating hydrolysis-resistant resin, styrene-acrylic emulsion and 4,4-diaminodiphenylmethane to 70-90 ℃, stirring and mixing for 1-2h to obtain mixed emulsion;
s2: adding deionized water, an acrylate leveling agent, a silane coupling agent and fluorescent powder into the mixed emulsion, and continuously stirring for 2-3 hours to obtain the hydrolysis-resistant luminous coating, wherein the silane coupling agent is one of a silane coupling agent KH-550, a silane coupling agent KH-560 and a silane coupling agent KH-570;
s3: and spraying hydrolysis-resistant luminous paint on the bionic bait with the multi-section framework, and then curing to form a coating to obtain the luminous multi-section flexible bionic bait.
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