CN106854434A - A kind of energy-accumulating luminous paint - Google Patents
A kind of energy-accumulating luminous paint Download PDFInfo
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- CN106854434A CN106854434A CN201611121290.0A CN201611121290A CN106854434A CN 106854434 A CN106854434 A CN 106854434A CN 201611121290 A CN201611121290 A CN 201611121290A CN 106854434 A CN106854434 A CN 106854434A
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- 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
- C09D179/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09D161/00 - C09D177/00
- C09D179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1535—Five-membered rings
- C08K5/1539—Cyclic anhydrides
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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
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
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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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- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
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- 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
- C09D5/22—Luminous paints
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a kind of energy-accumulating luminous paint, by weight, including following components：The concave convex rod of 3~14 weight portions, the strontium aluminate of 3~15 weight portions, the nano titanium oxide of 3~12 weight portions, the boccaro of 3~11 weight portions, the precipitated calcium carbonate of 5~10 weight portions, the KH 560 of 1~5 weight portion, the KH 550 of 1~5 weight portion, the epoxy-capped polyetheramine of 5~10 weight portions, the beta cyclodextrin modified amido end-blocking sulfonate polybenzimidazole of 8~10 weight portions, the 1 of 4~6 weight portions, 4, 5, 8 naphthalenetetracarbacidic acidic acid anhydrides, the sulfonic acid of 8 naphthylamines 1 of 1~4 weight portion, the 1 of 3~5 weight portions, 5 naphthalenedisulfonic acids, the dodecanedioic acid of 5~10 weight portions, the deionized water of the dimethyl sulfoxide (DMSO) of 20~50 weight portions and 50~100 weight portions.
Description
Technical field
The invention belongs to technical field of coatings, more particularly it relates to a kind of energy-accumulating luminous paint.
Background technology
Energy-accumulating luminous paint is a kind of new type functional coating, good indicating effect can be presented in the dark and beautification is imitated
Really, in emergent label, gap marker, power switch, enamel place name plates, way mark, toy, handicraft, clock and watch, instrument
The aspects such as disk, textile, fire-fighting equipment, military affairs, facility of camping all have been widely used.Existing energy-accumulating luminous paint is existed
Following shortcoming：
(1) weatherability of product, water resistance can not typically reach requirement；
(2) when there is fire, the film forming matter of these fireproof coatings can not bear drastically elevated temperature and quickly by
Burn, and fire-proof can not be played a part of；
(3) poor performance such as anti-corrosion, acid and alkali-resistance.
Hence it is highly desirable to pass through the improvement of formula, obtain that weatherability is strong, fire resistance is good and with anti-corrosion, Yi Jinai
The energy-accumulating luminous paint of soda acid ability.
The content of the invention
In order to solve the above problems, one aspect of the present invention provides a kind of energy-accumulating luminous paint, by weight, including
Following components：
The concave convex rod of 3~14 weight portions, the strontium aluminate of 3~15 weight portions, the nano titanium oxide of 3~12 weight portions, 3~
The boccaro of 11 weight portions, the precipitated calcium carbonate of 5~10 weight portions, the KH-560 of 1~5 weight portion, the KH-550 of 1~5 weight portion,
The epoxy-capped polyetheramine of 5~10 weight portions, beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole, 4 of 8~10 weight portions
The 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of~6 weight portions, the 8- naphthylamines -1- sulfonic acid of 1~4 weight portion, the 1,5- naphthalenes two of 3~5 weight portions
Sulfonic acid, the dodecanedioic acid of 5~10 weight portions, the dimethyl sulfoxide (DMSO) of 20~50 weight portions and 50~100 weight portions go from
Sub- water；
Preferably, described energy-accumulating luminous paint, by weight, including following components：
The concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, the purple of 9 weight portions
Sand, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped polyethers of 8 weight portions
Amine, the beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole of 9 weight portions, 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride, 3 of 5 weight portions
8- naphthylamines -1- sulfonic acid, the 1,5- naphthalenedisulfonic acids of 4 weight portions, the dodecanedioic acid of 8 weight portions, the two of 30 weight portions of weight portion
The deionized water of methyl sulfoxide and 70 weight portions.
In one embodiment, the epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine.
In one embodiment, the beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared by following methods
Form：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Compared with prior art, beneficial effects of the present invention are：
1st, epoxy-capped polyetheramine contains great amount of hydroxy group, can greatly improve the cohesive force of coating and base material, improves coating
Ageing-resistant ability, additionally, it can also react with amino, improve crosslink density and solidification rate, a large amount of rigidity on this outside chain
The introducing of phenyl ring, can improve the distance of strand, improve flame retardant effect.
2nd, polybenzimidazoles has excellent weatherability, ageing-resistant ability and fire resistance, is pasted by sulfonation and β-ring
Essence is modified can both to have greatly improved its compatibility with system, and the crosslink density of system can be greatly improved again, improve cohesion
And intensity, so as to provide Advantageous Effects of the invention.
3rd, Isosorbide-5-Nitrae, 5,8- naphthalenetetracarbacidic acidic acid anhydrides can react with amino, greatly improve the crosslinking rate of system, when shortening solidification
Between, so as to provide Advantageous Effects of the invention.
4th, the addition of 8- naphthylamines -1- sulfonic acid and 1,5- naphthalenedisulfonic acid can further improve the rigidity of system, and simultaneously with
There is ionomer in imidazole group, improve the crosslink density of system, cohesion and intensity further be improved, so that there is provided this hair
Bright Advantageous Effects.
Specific embodiment
Raw material:
All tetramines, diacid are purchased from CTI, SigmaAldrich, AlfaAesar or SCRC, and directly use, without
It is further purified.Epoxy silane coupling agent KH-560 and amino silicane coupling agent KH-550 has purchased from Chinese medicines group chemical reagent
Limit company.Concave convex rod (mesh of particle diameter 800), strontium aluminate (5 microns of particle diameter), nano titanium oxide (particle diameter 100nm), boccaro (particle diameter
500 mesh) and precipitated calcium carbonate (mesh of particle diameter 500) be purchased from Chemical Reagent Co., Ltd., Sinopharm Group, other raw materials are purchased from me
Fourth reagent Co., Ltd.
Embodiment 1
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, 9 weight portions beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions,
8- naphthylamines -1- sulfonic acid, the 1,5- naphthalenedisulfonic acids of 4 weight portions, the dodecanedioic acid of 8 weight portions, the two of 30 weight portions of 3 weight portions
The deionized water of methyl sulfoxide and 70 weight portions is added in agravic blender, opens fly cutter, to avoid the occurrence of bonding, is prevented
Stirring is uneven, and mixing time is 10 minutes, discharging.
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine；
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 2
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, the amino-terminated sulfonate polybenzimidazole of 9 weight portions, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions, the 8- of 3 weight portions
Naphthylamines -1- sulfonic acid, the 1,5- naphthalenedisulfonic acids of 4 weight portions, the dodecanedioic acid of 8 weight portions, 30 weight portions dimethyl sulfoxide (DMSO) with
And 70 weight portion deionized water add agravic blender in, open fly cutter, to avoid the occurrence of bonding, prevent stirring inequality,
Mixing time is 10 minutes, discharging.
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine；
The amino-terminated sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained.
Embodiment 3
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the beta-schardinger dextrin of 9 weight portions change
The amino-terminated sulfonate polybenzimidazole of property, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions, 8- naphthylamines -1- sulfonic acid, 4 of 3 weight portions
The 1,5- naphthalenedisulfonic acids of weight portion, the dodecanedioic acid of 8 weight portions, the dimethyl sulfoxide (DMSO) of 30 weight portions and 70 weight portions go
Ionized water is added in agravic blender, opens fly cutter, to avoid the occurrence of bonding, prevents stirring uneven, and mixing time is 10 points
Clock, discharging.
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 4
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions, the 8- naphthylamines -1- sulfonic acid of 3 weight portions, the sulphur of 1,5- naphthalenes two of 4 weight portions
The deionized water of acid, the dodecanedioic acid of 8 weight portions, the dimethyl sulfoxide (DMSO) of 30 weight portions and 70 weight portions adds agravic stirring
Mix in machine, open fly cutter, to avoid the occurrence of bonding, prevent stirring uneven, mixing time is 10 minutes, discharging.
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine.
Embodiment 5
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, 9 weight portions beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions,
The deionized water of the dodecanedioic acid of 8 weight portions, the dimethyl sulfoxide (DMSO) of 30 weight portions and 70 weight portions adds agravic stirring
In machine, fly cutter is opened, to avoid the occurrence of bonding, prevent stirring uneven, mixing time is 10 minutes, discharging；
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine；
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 6
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, the beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole of 9 weight portions, the 8- naphthylamines -1- sulfonic acid of 3 weight portions, 4 weight
Part 1,5- naphthalenedisulfonic acids, the dodecanedioic acid of 8 weight portions, the deionization of the dimethyl sulfoxide (DMSO) of 30 weight portions and 70 weight portions
Water is added in agravic blender, opens fly cutter, to avoid the occurrence of bonding, prevents stirring uneven, and mixing time is 10 minutes, is gone out
Material.
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine；
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Embodiment 7
By the concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, 9 weight portions
Boccaro, the precipitated calcium carbonate of 8 weight portions, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, the epoxy-capped of 8 weight portions gather
Ether amines, the beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole of 9 weight portions, the dodecanedioic acid of 8 weight portions, 30 weight portions
Dimethyl sulfoxide (DMSO) and 70 weight portions deionized water add agravic blender in, open fly cutter, to avoid the occurrence of bonding,
Prevent stirring uneven, mixing time is 10 minutes, discharging.
The epoxy-capped polyetheramine is prepared from by following methods：
In the dry three-necked bottles of 1000mL, the benzylamine and 500 of 100 grams epoxy resin E51,0.24mol is sequentially added
Gram dimethyl sulfoxide (DMSO), leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to
Room temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, take out
Filter and collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine；
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polies containing 86wt% phosphorus pentoxides
In phosphoric acid, then the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are added to
In reaction solution, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, mistake
Product is filtered and collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxy chloropropionate are sequentially added
Alkane, 13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen
Protect and 80 DEG C reaction 2 hours after, be down to room temperature, in precipitating to chloroform, filter and collect product, at 60 DEG C be vacuum dried
20 hours, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
Test condition
Energy-accumulating luminous paint obtained by embodiment 1-7 is coated on road, and test performance.
Antifriction performance：By standard GB/T1768-79 (89, method of testing is to use alcohol wear-resistant tester, plus 500g weight
Counterweight, the alcohol of 99.7% concentration is infiltrated with white cotton, is rubbed back and forth, and recording ink starts number of times during destruction.
Other performance, according to GA98-2005 standard testings, specially：
1st, surface drying time answers≤24h
2nd, adhesion strength >=0.1Mpa
3rd, water resistance：After 720h, coating does not ftracture, aliquation, come off
4th, acid resistance：After 360h, coating does not ftracture, aliquation, come off
5th, alkali resistance：After 360h, coating does not ftracture, aliquation, come off
6th, freeze-thawing resistant circulation experiment (secondary)：After 15 times, coating does not ftracture, aliquation, come off
7th, fire resistance：Coating layer thickness is 20mm, and fire endurance is not less than 2h
Test result is shown in Table 1.
Table 1
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 |
| Drying time, surface drying/h | 1.8 | 6.9 | 9.5 | 11.8 | 4.5 | 3.8 | 53 |
| Adhesion strength/Mpa | 0.53 | 0.15 | 0.08 | 0.08 | 0.39 | 0.37 | 0.26 |
| Water resistance/h | ＞ 1000 | ＜ 100 | ＜ 380 | ＜ 200 | ＞ 1000 | ＞ 1000 | ＞ 1000 |
| Acid resistance/h | ＞ 1000 | ＜ 100 | ＜ 360 | ＞ 1000 | ＞ 1000 | ＞ 1000 | ＞ 1000 |
| Alkali resistance/h | ＞ 800 | ＜ 100 | ＜ 360 | ＞ 800 | ＞ 800 | ＞ 800 | ＞ 800 |
| Freeze-thawing resistant circulation/number of times | ＞ 40 | ＜ 15 | ＜ 15 | ＜ 15 | ＞ 40 | ＞ 40 | ＞ 40 |
| Fire endurance/h | 4.9 | 0.8 | 0.9 | 0.9 | 3.2 | 4.5 | 2.2 |
| Rub resistance number of times | 1324 | 219 | 190 | 112 | 1209 | 1112 | 987 |
Data above can be seen that and not use epoxy-capped polyetheramine, beta-schardinger dextrin modified amido end-blocking sulfonated polyphenyl
And imidazoles, Isosorbide-5-Nitrae, the coating of 5,8- naphthalenetetracarbacidic acidic acid anhydrides, 8- naphthylamines -1- sulfonic acid and 1,5- naphthalenedisulfonic acid compares, painting of the invention
Material has obvious better performance, is thus provided that Advantageous Effects of the invention.
Claims (4)
1. a kind of energy-accumulating luminous paint, it is characterised in that by weight, including following components：
The concave convex rod of 3~14 weight portions, the strontium aluminate of 3~15 weight portions, the nano titanium oxide of 3~12 weight portions, 3~11 weights
Measure the boccaro of part, the precipitated calcium carbonate of 5~10 weight portions, the KH-560 of 1~5 weight portion, the KH-550 of 1~5 weight portion, 5~
The epoxy-capped polyetheramine of 10 weight portions, beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole, 4~6 of 8~10 weight portions
The 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of weight portion, the 8- naphthylamines -1- sulfonic acid of 1~4 weight portion, the sulphur of 1,5- naphthalenes two of 3~5 weight portions
The deionization of acid, the dodecanedioic acid of 5~10 weight portions, the dimethyl sulfoxide (DMSO) of 20~50 weight portions and 50~100 weight portions
Water.
2. energy-accumulating luminous paint according to claim 1, it is characterised in that by weight, including following components：
The concave convex rod of 14 weight portions, the strontium aluminate of 11 weight portions, the nano titanium oxide of 12 weight portions, the boccaro of 9 weight portions, 8
The precipitated calcium carbonate of weight portion, the KH-560 of 3 weight portions, the KH-550 of 5 weight portions, epoxy-capped polyetheramine, 9 of 8 weight portions
The beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole of weight portion, the 1,4,5,8 naphthalenetetracarboxylic acid acid anhydride of 5 weight portions, 3 weight
8- naphthylamines -1- the sulfonic acid, the 1,5- naphthalenedisulfonic acids of 4 weight portions, the dodecanedioic acid of 8 weight portions, the dimethyl of 30 weight portions of part
The deionized water of sulfoxide and 70 weight portions.
3. energy-accumulating luminous paint according to claim 1, it is characterised in that the epoxy-capped polyetheramine is by following methods
It is prepared from：
In the dry three-necked bottles of 1000mL, sequentially add 100 grams epoxy resin E51,0.24mol benzylamine and 500 gram two
Methyl sulfoxide, leads to nitrogen protection and magnetic agitation；After 1h is stirred at room temperature, heat up 80 DEG C of reaction 4h, after reaction terminates, is down to room
Temperature, and pour into rapidly in 150mL deionized waters, obtain a large amount of solids of sedimentation；With after the deionized water cyclic washing product, suction filtration
And collected polymer, in vacuum drying oven, 60 DEG C of dryings 20 hours obtain epoxy-capped polyetheramine.
4. energy-accumulating luminous paint according to claim 1, it is characterised in that the beta-schardinger dextrin modified amido blocks sulfonation
Polybenzimidazoles is prepared from by following methods：
By the 3 of 0.11 mole, 3 '-diaminobenzidine is first dissolved in 1000 grams of polyphosphoric acids containing 86wt% phosphorus pentoxides
In, the 5- sulfonic group M-phthalic acids of 0.02 mole of 5- amino isophthalic acids and 0.08 mole are then added to reaction
In liquid, nitrogen protection and 210 DEG C reaction 15 hours after, be down to room temperature, in precipitating to water, then with ammoniacal liquor neutralize, filtering simultaneously
Product is collected, in being vacuum dried 10 hours at 120 DEG C, amino-terminated sulfonate polybenzimidazole is obtained；
In 500 milliliters of three-necked bottles, sequentially add 0.2 gram of beta-schardinger dextrin, 0.05 gram of NaOH, 0.05 gram of epoxychloropropane,
13 grams of amino-terminated sulfonate polybenzimidazoles obtained above, 100 ml methanols and 200 milliliters of dimethyl sulfoxide (DMSO)s, nitrogen are protected
Protect and after 80 DEG C of reactions 2 hours, be down to room temperature, in precipitating to chloroform, product is filtered and collect, in being vacuum dried 20 at 60 DEG C
Hour, obtain beta-schardinger dextrin modified amido end-blocking sulfonate polybenzimidazole.
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| CN108796656A (en) * | 2018-07-06 | 2018-11-13 | 上海曙雀贸易有限公司 | A kind of high-performance of dopen Nano yttrium oxide is anti-fake, can trace to the source yarn |
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