CN109517523A - A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent - Google Patents
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent Download PDFInfo
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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
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- C08F218/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
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- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
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- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
- C08G81/02—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers at least one of the polymers being obtained by reactions involving only carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses a kind of preparation methods of light resistance core-shell type aqueous acrylic resin coating and finishing agent, using the raw material that following weight proportion is added into 500ml three-necked flask: water, emulsifier, methacrylic acid, it is warming up to 40 ~ 50 DEG C, stir 30min, A monomer is added, emulsifies 30 ~ 40min；It is warming up to 70 DEG C and starts logical recirculation water, 2h is kept the temperature after being warming up to 80 DEG C, 0.2 ~ 0.4g(of initiator 6g water is added dropwise and dissolves), time for adding continues 30 ~ 70min, reacts 2h after dripping, and obtains stratum nucleare lotion；B monomer and the initiator (being dissolved with 6g water) of 0.2 ~ 0.5g is added dropwise simultaneously into gained stratum nucleare lotion, time for adding continues 40min, 85 ~ 95 DEG C, which are kept the temperature, after dripping is stirred to react 1 ~ 2h, 0.4 g of emulsifier, 0.1 ~ 0.3g of crosslinking agent and Xanthophyll cycle fixative reaction time 40min are added at such a temperature, add ammonium hydroxide tune pH value to 7 ~ 8, the core-shell type aqueous acrylic resin coating of light resistance and finishing agent, gained coating and finishing agent have stronger light resistance.
Description
Technical field
The invention belongs to water soluble acrylic acid esters resin paint fields, and in particular to a kind of core-shell type aqueous propylene of light resistance
The preparation method of esters of gallic acid cold coating and finishing agent.
Background technique
The kind of Chinese acrylic resin comparatively perfect, but with it is external it is advanced go together compared with, production scale, technique
There is also certain gaps for the product that control and part property require.
The building coating of China ratio shared in acrylic coating is 24%, is in the medium development level in the world.At present
The annual output of China is at 500,000 tons or so, and wherein interior wall accounts for 60%, and exterior wall accounts for 25%, other account for 15%.
Although China's coating used at present, still based on low and middle-grade, the kind of Chinese acrylic coating is more complete, with
Developed country compares, gap and the kind for not lying in coating, but raw material, production equipment, production technology and production-scale
Gap.Wherein production scale is larger, the higher enterprise of technology starting point, and the product technology content of production is high, high-quality.
Acrylic resin paint has excellent color, protects color and heat-resisting, the performances such as chemicals-resistant, belongs to good.Extensively
For automobile, aviation, medical instrument, instrument and meter, wood furniture etc..
201810556380.5 being related to carbon nanotube and the modified light resistance water soluble acrylic acid esters resin coating of graphene
Preparation method, water, emulsifier, acrylic acid and aqueous gelatin solution are added into reaction system, reaction temperature is risen to 40 DEG C,
It is stirred to react 70min, A monomer, 40 ~ 90min of emulsification times is added；When temperature is raised to 70 DEG C of logical recirculation waters, to 80 DEG C of temperature
When start be added dropwise 0.3 ~ 0.6 part of ammonium persulfate weight, time for adding 1h, 1 ~ 3h of insulation reaction obtain stratum nucleare lotion；Wherein over cure
Sour ammonium is dissolved with 6 parts of water；B monomer, the aqueous gelatin solution weight 5 ~ 6 of mass concentration 3~5% is added dropwise simultaneously into stratum nucleare lotion
Part, 0.3 ~ 0.7 part of ammonium persulfate weight, time for adding 1 ~ 2h, 85 ~ 95 DEG C of 1.5 ~ 2h of insulation reaction time, then crosslinking agent is added dropwise
0.5 ~ 1.0 part of weight and photostabilized material, 1 ~ 2h of insulation reaction time, reduce the temperature to 50 DEG C；Gained acrylic resin
Light resistance is good, and the emulsification dosage used is few, and it is succinct convenient to be added.
Summary of the invention
The invention discloses a kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent,
Selection light inhibitor obtains double bond to acrylic monomers and protects, it is prevented to be oxidized, wherein trimethyl orthoformate, substance A and
Substance B promotes light inhibitor to obtain inhibiting effect, and substance B is grafted in acrylic resin, and resin is inhibited to obtain xanthochromia, selects light
Inhibit fixative that light inhibitor to be fixed in acrylic resin, keeps color inhibition persistence.
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, substance A 0.03125g and substance B 0.0027g, are placed in 50mL's
In closed container, the distilled water of 15g is added, is stirred to react 40 ~ 80min, adjusts pH to 5, it is stirred to react 12 at 75 ~ 90 DEG C ~
22h, is cooled to natural cooling at 40 DEG C, and suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) it is added the raw material of following weight proportion into 500ml three-necked flask: 40 ~ 60 g of water, emulsifier 0.6 ~
1.5g, 0.6 ~ 1.0 g of methacrylic acid, are warming up to 40 ~ 50 DEG C, stir 30min, are added A monomer, and emulsification 30 ~
40min ；It is warming up to 70 DEG C and starts logical recirculation water, 2h is kept the temperature after being warming up to 80 DEG C, it is water-soluble with 6g that 0.2 ~ 0.4g(of initiator is added dropwise
Solution), time for adding continues 30 ~ 70min, reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomer is by 0.3 ~ 2.0g of hydroxy-ethyl acrylate, 3 ~ 4 g of butyl acrylate, methyl methacrylate 2 ~ 4
G, 1.0 ~ 2.0 g of ethyl acrylate and 0.8 ~ 1.2g of acrylamide are mixed；
(3) B monomer and the initiator (being dissolved with 6g water) of 0.2 ~ 0.5g is added dropwise simultaneously into stratum nucleare lotion obtained by step (2),
Time for adding continues 40min, keeps the temperature 85 ~ 95 DEG C after dripping and is stirred to react 1 ~ 2h, and emulsifier 0.4 is added at such a temperature
G, 0.1 ~ 0.3g of crosslinking agent and Xanthophyll cycle 0.2 ~ 0.4g of fixative, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, obtain
The core-shell type aqueous acrylic resin coating of light resistance and finishing agent；
The B monomer is by 1 ~ 3g of butyl acrylate, 1 ~ 4 g of methyl acrylate, 2.5 ~ 4.5g of ethyl acrylate, propylene
Sour 1.0 ~ 1.5 g of hydroxyl ethyl ester mixing composition.
Substance A is 2- methoxyl group -4- methylphenol, 2,6- syringol, 3,3- dimethacrylate, chloroacetic acid
Any one；Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, sulfuric acid
Aluminium 1.4g is stirred to react 1 ~ 3h at 40 ~ 50 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；Cause
Agent is potassium peroxydisulfate, ammonium persulfate, azo dicyclohexyl formonitrile HCN (abbreviation AIP, VA-061 initiator), azo dicyano valeric acid
Any one in (abbreviation ACVA, V-501)；The crosslinking agent is N,N methylene bis acrylamide, divinylbenzene, two
Any one of second triamine, vinyltriethoxysilane；The Xanthophyll cycle fixative is by diethyl malonate 1-5g, methyl-prop
Diethyl adipate 1-2g and acetaldehyde 1.6 ~ 2.4 are added in ethyl alcohol 15g, sodium ethoxide 1.6g, and 2h is stirred to react at 70 DEG C, distillation
Solvent is removed, Xanthophyll cycle fixative is obtained.
Present invention has an advantage that
(1) selection light inhibitor obtains double bond to acrylic monomers and protects, it is prevented to be oxidized, wherein trimethyl orthoformate,
Substance A and substance B promote light inhibitor to obtain inhibiting effect, and substance B is grafted in acrylic resin, inhibit resin xanthochromia,
Light inhibitor is fixed in acrylic resin for selection Xanthophyll cycle fixative, keeps color inhibition persistence.
(2) present invention, which is prepared into light inhibitor, has preparation time short, high-efficient to obtain advantage.
Specific embodiment
Embodiment 1
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, 2- methoxyl group -4- methylphenol 0.03125g and substance
B0.0027g is placed in the closed container of 50mL, adds the distilled water of 15g, is stirred to react 40min, adjusts pH to 5, and 75 DEG C
Under be stirred to react 12h, be cooled to natural cooling at 40 DEG C, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) raw material of following weight proportion: water 40g, emulsifier 0.6g, methyl-prop is added into 500ml three-necked flask
0.6 g of olefin(e) acid is warming up to 40 DEG C, stirs 30min, and A monomer is added, and emulsifies 30min；70 DEG C are warming up to start to lead to
Recirculation water keeps the temperature 2h after being warming up to 80 DEG C, potassium peroxydisulfate 0.2g(6g water is added dropwise and dissolves), time for adding continues 30min, is added dropwise
2h is reacted after complete, obtains stratum nucleare lotion；
The A monomer is by hydroxy-ethyl acrylate 0.3g, butyl acrylate 3g, methyl methacrylate 2g, acrylic acid
Ethyl ester 1.0g and acrylamide 0.8g are mixed；
(3) B monomer and the potassium peroxydisulfate (being dissolved with 6g water) of 0.2g, drop is added dropwise simultaneously into stratum nucleare lotion obtained by step (2)
Continue 40min between added-time, keep the temperature 85 DEG C after dripping and be stirred to react 1h, emulsifier 0.4 g, N, N- are added at such a temperature
Methylene-bisacrylamide 0.1g and Xanthophyll cycle fixative 0.2g, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, obtain
The core-shell type aqueous acrylic resin coating of light resistance and finishing agent；
The B monomer is by butyl acrylate 1g, methyl acrylate 1g, ethyl acrylate 2.5g, hydroxy-ethyl acrylate
1.0g mixing composition.
Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate
1.4g is stirred to react 1h at 40 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；
Diethyl malonate 1g, methyl-malonic ester 1g and acetaldehyde 1.6g are added to ethyl alcohol by the Xanthophyll cycle fixative
In 15g, sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.(emulsifier and initiation
Using identical in the every step of agent)
Embodiment 2
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, 2,6- syringol 0.03125g and substance
B0.0027g is placed in the closed container of 50mL, adds the distilled water of 15g, is stirred to react 80min, adjusts pH to 5, and 90 DEG C
Under be stirred to react 22h, be cooled to natural cooling at 40 DEG C, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) raw material of following weight proportion: 60 g of water, emulsifier 1.5g, methyl-prop is added into 500ml three-necked flask
1.0 g of olefin(e) acid is warming up to 50 DEG C, stirs 30min, and A monomer is added, and emulsifies 40min；70 DEG C are warming up to start to lead to back
Flowing water keeps the temperature 2h after being warming up to 80 DEG C, ammonium persulfate initiator 0.4g(6g water is added dropwise and dissolves), time for adding continues 70min,
2h is reacted after dripping, and obtains stratum nucleare lotion；
The A monomer is by hydroxy-ethyl acrylate 2.0g, 4 g of butyl acrylate, 4 g of methyl methacrylate, acrylic acid
Ethyl ester 2.0 g and acrylamide 1.2g are mixed；
(3) B monomer is added dropwise simultaneously into stratum nucleare lotion obtained by step (2) and the ammonium persulfate initiator of 0.5g is (water-soluble with 6g
Solution), time for adding continues 40min, after dripping keep the temperature 95 DEG C be stirred to react 2h, at such a temperature addition 0.4 g of emulsifier,
Divinylbenzene 0.3g and Xanthophyll cycle fixative 0.4g, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, obtain light resistance
Core-shell type aqueous acrylic resin coating and finishing agent；
The B monomer is by butyl acrylate 3g, 4 g of methyl acrylate, ethyl acrylate 4.5g, hydroxy-ethyl acrylate
1.5 g mixing composition.
Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate
1.4g is stirred to react 3h at 50 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；
Diethyl malonate 5g, methyl-malonic ester 2g and acetaldehyde 2.4g are added to ethyl alcohol by the Xanthophyll cycle fixative
In 15g, sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.
Embodiment 3
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, 3,3- dimethacrylate 0.03125g and substance
B0.0027g is placed in the closed container of 50mL, adds the distilled water of 15g, is stirred to react 60min, adjusts pH to 5, and 80 DEG C
Under be stirred to react 17h, be cooled to natural cooling at 40 DEG C, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) raw material of following weight proportion: 50 g of water, emulsifier 1.0g, methyl-prop is added into 500ml three-necked flask
0.8 g of olefin(e) acid is warming up to 45 DEG C, stirs 30min, and A monomer is added, and emulsifies 35min；70 DEG C are warming up to start to lead to
Recirculation water keeps the temperature 2h after being warming up to 80 DEG C, azo dicyclohexyl formonitrile HCN (abbreviation AIP, VA-061 initiator) 0.3g(is added dropwise and uses
The dissolution of 6g water), time for adding continues 50min, reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomer is by hydroxy-ethyl acrylate 1.15g, butyl acrylate 3.5g, 3 g of methyl methacrylate, propylene
Acetoacetic ester 1.5 g and acrylamide 1.0g are mixed；
(3) B monomer and the initiator (being dissolved with 6g water) of 0.35g, drop is added dropwise simultaneously into stratum nucleare lotion obtained by step (2)
Continue 40min between added-time, keep the temperature 90 DEG C after dripping and be stirred to react 1.5h, 0.4 g of emulsifier, diethyl are added at such a temperature
Triamine 0.2g and Xanthophyll cycle fixative 0.3g, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, it is hud typed to obtain light resistance
Water soluble acrylic acid esters resin coating and finishing agent；
The B monomer is by butyl acrylate 2g, 2.5 g of methyl acrylate, ethyl acrylate 3.5g, acrylic acid hydroxyl second
Ester 1.25g mixing composition.
Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate
1.4g is stirred to react 2h at 45 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；
Diethyl malonate 3g, methyl-malonic ester 1.5g and acetaldehyde 2.0g are added to ethyl alcohol by the Xanthophyll cycle fixative
In 15g, sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.
Embodiment 4
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, chloroacetic acid 0.03125g and substance B 0.0027g, are placed in
In the closed container of 50mL, the distilled water of 15g is added, is stirred to react 50min, pH to 5 is adjusted, is stirred to react 16h at 80 DEG C,
It is cooled to natural cooling at 40 DEG C, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) raw material of following weight proportion: water 55g, emulsifier 0.9g, methyl-prop is added into 500ml three-necked flask
Olefin(e) acid 0.7g is warming up to 40 DEG C, stirs 30min, and A monomer is added, and emulsifies 30min；70 DEG C are warming up to start to lead to
Recirculation water keeps the temperature 2h after being warming up to 80 DEG C, azo dicyano valeric acid (abbreviation ACVA, V-501) 0.2g(6g water is added dropwise and dissolves),
Time for adding continues 30min, reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomer is by hydroxy-ethyl acrylate 1.0g, butyl acrylate 3.5g, methyl methacrylate 2g, propylene
Acetoacetic ester 1.0 g and acrylamide 1.2g are mixed；
(3) be added dropwise simultaneously into stratum nucleare lotion obtained by step (2) B monomer and 0.5g azo dicyano valeric acid (abbreviation ACVA,
V-501) (with 6g water dissolve), time for adding continues 40min, after dripping heat preservation 95 DEG C be stirred to react 1h, at such a temperature plus
Enter 0.4 g of emulsifier, vinyltriethoxysilane 0.1g and Xanthophyll cycle fixative 0.4g, reaction time 40min add ammonium hydroxide
It adjusts pH value to 7 ~ 8, obtains the core-shell type aqueous acrylic resin coating of light resistance and finishing agent；
The B monomer is by butyl acrylate 3g, 1 g of methyl acrylate, ethyl acrylate 2.5g, hydroxy-ethyl acrylate
1.5 g mixing composition.
Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate
1.4g is stirred to react 2h at 45 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；
The Xanthophyll cycle fixative by diethyl malonate 2g, methyl-malonic ester 2g and acetaldehyde 2g be added to ethyl alcohol 15g,
In sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.
Embodiment 5
A kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
(1) preparation of light inhibitor: phenyl-phosphonic acid, the 0.0428g of the 2,2'- bipyridyl and 0.043g that weigh 0.0337g are anhydrous
Copper sulphate, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, 2- methoxyl group -4- methylphenol 0.03125g and substance
B0.0027g is placed in the closed container of 50mL, adds the distilled water of 15g, is stirred to react 70min, adjusts pH to 5, and 90 DEG C
Under be stirred to react 13h, be cooled to natural cooling at 40 DEG C, suction filtration obtains bulk crystals, obtains the light inhibitor.
(2) raw material of following weight proportion: 60 g of water, emulsifier 1.5g, methyl-prop is added into 500ml three-necked flask
0.6 g of olefin(e) acid is warming up to 40 DEG C, stirs 30min, and A monomer is added, and emulsifies 40min；70 DEG C are warming up to start to lead to
Recirculation water keeps the temperature 2h after being warming up to 80 DEG C, potassium peroxydisulfate initiator 0.4g(6g water is added dropwise and dissolves), time for adding is lasting
30min reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomer is by hydroxy-ethyl acrylate 2.0g, 3.5 g of butyl acrylate, 2 g of methyl methacrylate, third
Olefin(e) acid ethyl ester 1.0 g and acrylamide 0.8g are mixed；
(3) B monomer is added dropwise simultaneously into stratum nucleare lotion obtained by step (2) and the potassium peroxydisulfate initiator of 0.5g is (water-soluble with 6g
Solution), time for adding continues 40min, after dripping keep the temperature 95 DEG C be stirred to react 1h, at such a temperature addition 0.4 g of emulsifier,
N, N- methylene-bisacrylamide 0.1g and Xanthophyll cycle fixative 0.2g, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~
8, obtain the core-shell type aqueous acrylic resin coating of light resistance and finishing agent；
The B monomer is by butyl acrylate 3g, 1 g of methyl acrylate, ethyl acrylate 2.5g, hydroxy-ethyl acrylate
1.5 g mixing composition.
Substance B the preparation method comprises the following steps: by ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate
1.4g is stirred to react 2h at 45 DEG C, adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B；
Emulsifier is the mixture that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1；
Diethyl malonate 3g, methyl-malonic ester 1g and acetaldehyde 1.6g are added to ethyl alcohol by the Xanthophyll cycle fixative
In 15g, sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.
For quantitative description acrylic resin resistance to light of coating energy, detected using spectrophotometer, with
To inverse difference △ E, to describe the light resistance of acrylic resin.△ E represents color change degree, and △ E is bigger, face
Color change is more obvious.In general, △ E value is 0~1.5 category slight change；△ E value is that 1.5~3.0 categories can feel variation；
△ E value be 3.0~6.0 belong to significant changes (referring to Wang Fang, Dang Gaochao, Wang Liqin, several organic historical relic's protection polymer coatings
Light degradation [J] Northwest University journal, 2005,35 (5): 56~58), the present invention put using based on the △ E of 600min as
Judgment basis.
Manufactured acrylic resin film is placed on ultraviolet light and aging experimental box (illumination wavelength be 350 nm, 50 DEG C)
In, the abundant xanthochromia of 48 h of illumination under conditions of specimen surface is parallel with fluorescent tube bottom surface, distance is 250 mm obtains light
According to the acrylic resin film after xanthochromia.Using ultraviolet-visible-near infrared spectrometer, the transmission of acrylic resin film is measured
Rate, wavelength scanning range are 200~800 nm, and the present invention selects 400nm measurement (Ren Longfang).
1 test data of table
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 16.05 | 18.51 | 18.98 | 17.34 | 16.24 | 26.28 |
| △E/600min | 0.5 | 0.5 | 0.6 | 0.5 | 0.4 | 0.7 |
| Xanthochromia grade | 0.5 | 0.5 | 1.0 | 0.5 | 1.0 | 1.5 |
The patent of invention example 1 of comparative sample using background of invention is compared as benchmark, as it can be seen from table 1 this hair
It is bright that there is apparent light resistance compared to comparison patent of invention.
2 test data of table (not plus light inhibitor)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 35.08 | 45.32 | 48.32 | 43.23 | 45.76 | 26.28 |
| △E/600min | 2.2 | 2.6 | 2.8 | 2.6 | 2.8 | 0.7 |
| Xanthochromia grade | 3.0 | 3.5 | 3.5 | 3.5 | 3.0 | 1.5 |
From table 2 it can be seen that not adding the present invention of light inhibitor that there is poor light resistance.
3 test data of table (not plus substance A)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| △E/600min | 1.6 | 1.8 | 1.8 | 2.1 | 1.9 | 0.7 |
| Xanthochromia grade | 1.5 | 2.0 | 2.0 | 2.5 | 2.0 | 1.5 |
From table 3 it can be seen that not adding the present invention of substance A that there is poor light resistance.
4 test data of table (not plus substance B)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| △E/600min | 1.7 | 1.9 | 1.4 | 1.9 | 1.6 | 0.7 |
| Xanthochromia grade | 1.5 | 2.0 | 1.5 | 2.0 | 1.5 | 1.5 |
From table 4, it can be seen that not adding the present invention of substance B that there is poor light resistance.
5 test data of table (not plus Xanthophyll cycle fixative)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative sample | |
| Light transmittance/% | 27.35 | 31.12 | 30.45 | 31.78 | 33.58 | 26.28 |
As can be seen from Table 5, not plus the light transmittance of Xanthophyll cycle fixative improve.
Claims (7)
1. a kind of preparation method of light resistance core-shell type aqueous acrylic resin coating and finishing agent, it is characterised in that:
The preparation of light inhibitor: the anhydrous sulphur of phenyl-phosphonic acid, 0.0428g of the 2,2'- bipyridyl and 0.043g of 0.0337g is weighed
Sour copper, 0.3542g sodium molybdate, trimethyl orthoformate 0.24g, substance A 0.03125g and substance B 0.0027g, are placed in the close of 50mL
It closes in container, adds the distilled water of 15g, be stirred to react 40 ~ 80min, adjust pH to 5, it is stirred to react 12 at 75 ~ 90 DEG C ~
22h, is cooled to natural cooling at 40 DEG C, and suction filtration obtains bulk crystals, obtains the light inhibitor；
(2) raw material of following weight proportion: 40 ~ 60 g of water, 0.6 ~ 1.5g of emulsifier, first is added into 500ml three-necked flask
0.6 ~ 1.0 g of base acrylic acid is warming up to 40 ~ 50 DEG C, stirs 30min, and A monomer is added, and emulsifies 30 ~ 40min；It rises
Temperature starts logical recirculation water to 70 DEG C, and 2h is kept the temperature after being warming up to 80 DEG C, and 0.2 ~ 0.4g(of initiator 6g water is added dropwise and dissolves), it is added dropwise
Time continues 30 ~ 70min, reacts 2h after dripping, and obtains stratum nucleare lotion；
The A monomer is by 0.3 ~ 2.0g of hydroxy-ethyl acrylate, 3 ~ 4 g of butyl acrylate, methyl methacrylate 2 ~ 4
G, 1.0 ~ 2.0 g of ethyl acrylate and 0.8 ~ 1.2g of acrylamide are mixed；
(3) B monomer and the initiator (being dissolved with 6g water) of 0.2 ~ 0.5g is added dropwise simultaneously into stratum nucleare lotion obtained by step (2),
Time for adding continues 40min, keeps the temperature 85 ~ 95 DEG C after dripping and is stirred to react 1 ~ 2h, and emulsifier 0.4 is added at such a temperature
G, 0.1 ~ 0.3g of crosslinking agent and Xanthophyll cycle 0.2 ~ 0.4g of fixative, reaction time 40min, add ammonium hydroxide tune pH value to 7 ~ 8, obtain
The core-shell type aqueous acrylic resin coating of light resistance and finishing agent；
The B monomer is by 1 ~ 3g of butyl acrylate, 1 ~ 4 g of methyl acrylate, 2.5 ~ 4.5g of ethyl acrylate, propylene
Sour 1.0 ~ 1.5 g of hydroxyl ethyl ester mixing composition.
2. the preparation of a kind of light resistance core-shell type aqueous acrylic resin coating and finishing agent as described in claim 1
Method, which is characterized in that substance A be 2- methoxyl group -4- methylphenol, 2,6- syringol, 3,3- dimethacrylate,
Any one of chloroacetic acid.
3. a kind of preparation method of light-resistant waterborne polyurethane coating as described in claim 1, substance B the preparation method comprises the following steps:
Ethylene-ethyl acetate 11.5g, methacrylaldehyde 4.2g, acrylamide 3.4g, aluminum sulfate 1.4g are stirred to react 1 at 40 ~ 50 DEG C ~
3h adds 10g water and adjusts pH to 4, the reaction was continued 30min, obtains substance B.
4. the system of a kind of light resistance core-shell type aqueous acrylic resin coating and finishing agent as described in claim 1
Preparation Method, which is characterized in that emulsifier is that neopelex is mixed with fatty alcohol polyoxyethylene ether by weight 2:1
Mixture.
5. a kind of preparation method of the hud typed acrylic resin coating of light resistance as described in claim 1, feature
It is, initiator is potassium peroxydisulfate, ammonium persulfate, azo dicyclohexyl formonitrile HCN (abbreviation AIP, VA-061 initiator), azo
Any one in dicyano valeric acid (abbreviation ACVA, V-501).
6. a kind of preparation side of light resistance core-shell type aqueous acrylic resin coating and finishing agent as described in claim 1
Method, the crosslinking agent are N, N- methylene-bisacrylamide, divinylbenzene, Diethylenetriamine, vinyltriethoxysilane
Any one.
7. a kind of preparation side of light resistance core-shell type aqueous acrylic resin coating and finishing agent as described in claim 1
Diethyl malonate 1-5g, methyl-malonic ester 1-2g and acetaldehyde 1.6 ~ 2.4 are added to by method, the Xanthophyll cycle fixative
In ethyl alcohol 15g, sodium ethoxide 1.6g, it is stirred to react 2h at 70 DEG C, solvent is distilled off, obtains Xanthophyll cycle fixative.
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|---|---|---|---|---|
| CN102875723A (en) * | 2012-10-26 | 2013-01-16 | 烟台大学 | Preparation method of flame-retardant core-shell-type acrylic resin |
| CN104017456A (en) * | 2014-06-15 | 2014-09-03 | 段宝荣 | Method for preparing light resistant and antiflaming aqueous acrylate resin coating |
| CN106995578A (en) * | 2016-01-26 | 2017-08-01 | 合肥杰事杰新材料股份有限公司 | Color inhibition low-transmittance acrylonitrile-butadiene-styrene (ABS)/Polycarbonate alloy material and preparation method thereof |
| CN108329785A (en) * | 2015-09-16 | 2018-07-27 | 段宝荣 | A kind of light resistance water paint and adhesive preparation method |
| CN108912929A (en) * | 2018-06-26 | 2018-11-30 | 段小宁 | Fire-retardant, the aqueous nucleocapsid acrylic resin coating of antibiotic property and paint preparation method |
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2018
- 2018-12-02 CN CN201811461312.7A patent/CN109517523A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102875723A (en) * | 2012-10-26 | 2013-01-16 | 烟台大学 | Preparation method of flame-retardant core-shell-type acrylic resin |
| CN104017456A (en) * | 2014-06-15 | 2014-09-03 | 段宝荣 | Method for preparing light resistant and antiflaming aqueous acrylate resin coating |
| CN108329785A (en) * | 2015-09-16 | 2018-07-27 | 段宝荣 | A kind of light resistance water paint and adhesive preparation method |
| CN106995578A (en) * | 2016-01-26 | 2017-08-01 | 合肥杰事杰新材料股份有限公司 | Color inhibition low-transmittance acrylonitrile-butadiene-styrene (ABS)/Polycarbonate alloy material and preparation method thereof |
| CN108912929A (en) * | 2018-06-26 | 2018-11-30 | 段小宁 | Fire-retardant, the aqueous nucleocapsid acrylic resin coating of antibiotic property and paint preparation method |
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