CN109439124A - Woodcare paint aqueous dumb light self-crosslinking acrylic lotion and its synthetic method - Google Patents
Woodcare paint aqueous dumb light self-crosslinking acrylic lotion and its synthetic method Download PDFInfo
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- CN109439124A CN109439124A CN201811170985.7A CN201811170985A CN109439124A CN 109439124 A CN109439124 A CN 109439124A CN 201811170985 A CN201811170985 A CN 201811170985A CN 109439124 A CN109439124 A CN 109439124A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D143/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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Abstract
The invention discloses a kind of woodcare paint aqueous dumb light self-crosslinking acrylic lotions and its synthetic method, raw material includes monomer, functional monomer, solvent, neutralizer, buffer, initiator, emulsifier and delustering agent, by weight: wherein monomer includes 3-12 parts of methacrylic acid, 120-300 parts of methyl methacrylate, 2-20 parts of butyl acrylate, 10-50 parts of styrene and 40-120 parts of Isooctyl acrylate monomer；Functional monomer is Diacetone Acrylamide 4-14 parts, 3-10 parts of adipic dihydrazide and 1-10 parts of vinyltrimethoxysilane；Solvent is deionized water 500-800 parts；Neutralizer is ammonium hydroxide 2-10 parts；Buffer is sodium bicarbonate 0.2-1 parts；Initiator is ammonium persulfate 0.5-3 parts, 0.1-2 parts of tert-butyl hydroperoxide and 0.1-2 parts of ascorbic acid；Emulsifier is lauryl sodium sulfate 0.5-8 parts；Delustering agent is fumed silica 5-35 parts.The invention product has excellent transparency, excellent water resistance, excellent alcohol resistance, the characteristic of dumb light, can arrange in pairs or groups and manufacture any gloss aqueous woodware paint.
Description
Technical field
The present invention relates to furniture decorations, finishing, more particularly, to a kind of aqueous dumb light self-crosslinking acrylic cream of woodcare paint
Liquid and its synthetic method are widely used in wood furniture finishing coat coating.
Background technique
As environmental consciousness is increasingly enhanced, demand of the water paint in Chinese market is increasing, deeply build,
Multiple industries such as furniture, automobile.Since water paint is that have for opposite oil paint with water as solvent or decentralized medium
There is the features such as nontoxic, tasteless, nonflammable.
It is many countries of representative to the limit of solvent based coating using developed country to protect environment for the survival of mankind
System is increasingly stringenter, so that coating be promoted not cause damages to ecological environment, is not had a negative impact to human health " green
Color coating " or " Environmentally friendly coatings " direction are developed.The U.S., Europe, Japan and other countries all put into effect environmental regulation, it is specified that
Stringent VOC emission standard, most representational is German Clean Air Act, 66 regulations, Germany's AT-Luft method in the U.S.
Rule, european union directive, etc. worldwide environmental protection index, greatly promotion exported product " water " generation " oily process.
As Furniture manufacturing big country and big export country, the development of Chinoiserie coating industry is largely by domestic and international political affairs
The influence of plan regulation.Most tight environmental law appearance, the collection of the coating consumption tax, make traditional paint industry face severe choose in history
War.Market is more vigorous for the demand of water-borne wood coating, and water-borne wood coating becomes recent studies on hot spot.Especially for one
A little wood furniture varnish dumb light painting effects, customer requirement transparency are high.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of aqueous dumb light self-crosslinking acrylic lotion of woodcare paint and
Its synthetic method, solves existing following problems during currently manufactured aqueous dumb light woodcare paint: first: extinction material needs
High speed dispersion, to cause production process energy consumption high；Second: extinction material disperses extremely difficult control batch gloss quality, causes water
Property woodcare paint gloss is inconsistent；Third: extinction material easily influences product transparency, so that transparency variation influence product
Energy；4th: extinction material needs to add compared with multi-dispersant and wetting agent, and then influence product is water-fast, alcohol resistance；5th: directly
In coating manufacture, addition fumed silica is easy precipitating, influences coating storage stability.
The technical solution adopted by the present invention is that the aqueous dumb light self-crosslinking acrylic lotion of woodcare paint, raw material include monomer,
Functional monomer, solvent, neutralizer, buffer, initiator, emulsifier and delustering agent, by weight:
Wherein monomer includes 3-12 parts of methacrylic acid, 120-300 parts of methyl methacrylate, 2-20 parts of butyl acrylate, benzene
10-50 parts and Isooctyl acrylate monomer 40-120 parts of ethylene；
Functional monomer is Diacetone Acrylamide 4-14 parts, 3-10 parts of adipic dihydrazide and vinyltrimethoxysilane 1-
10 parts；
Solvent is deionized water 500-800 parts；
Neutralizer is ammonium hydroxide 2-10 parts；
Buffer is sodium bicarbonate 0.2-1 parts；
Initiator is ammonium persulfate 0.5-3 parts, 0.1-2 parts of tert-butyl hydroperoxide and 0.1-2 parts of ascorbic acid；
Emulsifier is lauryl sodium sulfate 0.5-8 parts；
Delustering agent is fumed silica 5-35 parts.
Further, the fumed silica is Degussa TS100.
Further, the monomer further includes 80-180 parts of butyl methacrylate, 2-10 parts of acrylic acid, metering system
Any one of 40-100 parts of acetoacetic ester or several combinations.For improving water solubility, film forming, paint film flexibility.Methyl-prop
Olefin(e) acid butyl ester and ethyl methacrylate are used for some or all of substitution methyl methacrylate, butyl acrylate, styrene
And Isooctyl acrylate monomer；Acrylic acid is for substituting methacrylic acid.
Further, the functional monomer further includes 3-10 parts of succinic acid hydrazide ii and/or vinyl triethoxyl silicon
1-20 parts of alkane.For improving the degree of cross linking, enhancing paint film intensity, resistance to acid and alkali, water resistance, alcohol resistance.Wherein succinic acid hydrazide ii
Part or all of alternative functions monomer adipic dihydrazide, some or all of alternative functions monomer of vinyltriethoxysilane
Vinyltrimethoxysilane.
Further, the neutralizer further includes 2-10 parts of 2-amino-2-methyl-1-propanol.During the purpose of addition is
And water-base resin, improve water-soluble and stability.2-amino-2-methyl-1-propanol partly or entirely substitutes neutralizer ammonium hydroxide.
Further, the initiator further includes 0.5-5 parts of sodium peroxydisulfate.The purpose of addition is that causing monomer carries out certainly
It is reacted by base, produces aqueous high molecular lotion.The part or all of alternative initiator ammonium persulfate of sodium peroxydisulfate.
Further, the emulsifier further includes 0.4-6 parts of isomeric alcohol polyethenoxy ether.The purpose of addition is to prepare steady
Fixed monomer pre-emulsion, so that pre-emulsion is stably and controllable.Selected component can replace emulsifier sodium lauryl sulfate completely.
Further, the delustering agent is 5-35 parts of Degussa TS100 fumed silicas, further includes 4-30 parts of Degussas
OK520 fumed silica.For manufacturing the water-based emulsion for having Extinction Characteristic.
The invention further relates to the woodcare paint synthetic method of aqueous dumb light self-crosslinking acrylic lotion, including it is following
Step:
1) first deionized water, part lauryl sodium sulfate, sodium bicarbonate are mixed, as bottom, is then warming up to 80 DEG C；
2) ionized water, part lauryl sodium sulfate, part methyl acrylic acid, butyl acrylate, part methyl acrylic acid are removed
Methyl esters, part styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) resulting material is added by the 5% of step 2 stratum nucleare pre-emulsion quality, is added at one time part mistake after five minutes
Then the mixed liquor A of ammonium sulfate and deionized water keeps the temperature 15 minutes for 85 DEG C；Water is added to prepare mixed liquor using remaining ammonium persulfate again
B；
4) reaction kettle is added in step 2 residue stratum nucleare pre-emulsion, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) it is different pungent that ionized water, remaining lauryl sodium sulfate, Diacetone Acrylamide, remaining methacrylic acid, acrylic acid are removed
Ester, residual styrene, vinyltrimethoxysilane, remaining methyl methacrylate, delustering agent (Degussa TS100) mixing are stirred
It mixes 20-40 minutes and obtains shell pre-emulsion；
6) after to stratum nucleare pre-emulsion addition heat preservation in step 4), reaction kettle, drop is added in step 5) shell pre-emulsion
85 DEG C of heating degree, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the shell pre-emulsion time is added, this period needs simultaneously
The mixed liquid B of preparation is added dropwise always, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are cooled to；
10) the mixed liquor C for preparing tert-butyl hydroperoxide and water, prepares the mixed liquor D of ascorbic acid and water；
11) after step 9) cools to 70 DEG C, by the mixed liquor of the mixed liquor C and ascorbic acid and water of tert-butyl hydroperoxide and water
Reaction kettle is added in D simultaneously, and time for adding is 20 minutes, then keeps the temperature 30 minutes for 60-70 DEG C；
12) the mixed liquor E for preparing ammonium hydroxide and water will cool to 50-55 DEG C obtained by step 11), mixed liquor E then be added, and stir
It mixes 10 minutes；
13) the mixed liquor F for preparing adipic dihydrazide and water will be cooled to lower than 50 DEG C obtained by step 12), then by mixed liquor
F is added in obtained by step 12), and stirs 20 minutes, and filtering obtains a kind of aqueous dumb light self-crosslinking acrylic cream of woodcare paint
Liquid.
Meteorological silica (Degussa TS100) is added in the invention when manufacturing water-based emulsion, enables to product
It is more stable, and solve the problems, such as five present on aspects.Vinyl trimethoxy is introduced in shell structurre simultaneously
Silane, the vinyl in vinyltrimethoxysilane carry out radical reaction, vinyl three with acrylic monomers in the reaction
Alkoxy hydrolysis in methoxy silane generates silicone hydroxyl, and silicone hydroxyl can further be reacted with fumed silica, so make
It has a distinct increment in terms of product patience produced, overcomes the disadvantage of degradation caused by outer addition extinction material.The production
Product are core-shell structure, and the glass transition temperature of core is high, ensure that the coating hardness after film forming, and the glass transition temperature of shell is low, are protected
It has demonstrate,proved film easily to form a film at normal temperature, has thereby reduced the dosage of coalescing agent.Simultaneously introduce Diacetone Acrylamide-oneself
The self-crosslinking system of dihydrazi.It is comprehensive to solve the problems, such as the aqueous dumb light woodcare paint of manufacture.
When preparation, deionized water, lauryl sodium sulfate, sodium bicarbonate are firstly added as bottom, by deionized water, ten
Sodium dialkyl sulfate, methacrylic acid, methyl methacrylate, butyl acrylate, styrene are stirred the production pre- cream of stratum nucleare
Stratum nucleare pre-emulsion is added dropwise in liquid while initiator ammonium persulfate aqueous solution is added dropwise.Then by deionized water, dodecyl sulphate
Sodium, Diacetone Acrylamide, methacrylic acid, Isooctyl acrylate monomer, styrene, vinyltrimethoxysilane, metering system
Sour methyl esters, delustering agent (Degussa TS100) are stirred production shell pre-emulsion, and initiator ammonium persulfate aqueous solution is being added dropwise
Shell pre-emulsion is added dropwise simultaneously.It prepares tert-butyl hydroperoxide aqueous solution and aqueous ascorbic acid is added dropwise simultaneously, aoxidized
Reduction reaction, and then make monomer reaction abundant, PH finally is adjusted with ammonia spirit, and adipic dihydrazide aqueous solution is added, obtained
To core-shell structure aqueous woodware paint dumb light self-crosslinking acrylic lotion.
Producing aqueous dumb light woodcare paint varnish at present is directly using flatting silica high speed dispersion, to reach the effect of delustring
Fruit.However there are problems in dispersion process for flatting silica；Product of the present invention, which can arrange in pairs or groups, manufactures any gloss aqueous wooden ware
Paint, and the above problem is solved, in dumb light woodcare paint aqueous with the invention product manufacturing, it is not necessarily to high speed dispersion, energy can be reduced
Consumption guarantees batch products gloss consistency, facilitates large-scale industrial production, reduces comprehensive production cost.Because not adding
More wetting agents, dispersing agent, can correspondingly increase the comprehensive performance of manufactured aqueous dumb light woodcare paint, thus have very big product
Advantage.
Beneficial effects of the present invention:
1, extinction material needs high speed dispersion to cause production process energy consumption during solving the aqueous dumb light woodcare paint of manufacture
High problem, to reduce the production cost of aqueous dumb light woodcare paint.
2, extinction material disperses extremely difficult control batch gloss quality, causes during solving the aqueous dumb light woodcare paint of manufacture
The inconsistent problem of aqueous woodware paint gloss.
3, it solves extinction material during the aqueous dumb light woodcare paint of manufacture and easily influences product transparency and make transparency
The problem of variation influence properties of product.
4, it solves extinction material during the aqueous dumb light woodcare paint of manufacture to need to add compared with multi-dispersant and wetting agent, into
And the problem of influencing water-fast product, alcohol resistance.
5, solving the aqueous dumb light woodcare paint of manufacture, directly in coating manufacture, addition fumed silica holds in the process
Easily precipitating influences the problem of coating storage stability.
To sum up, the present invention the problems of satisfactorily solves during the aqueous dumb light woodcare paint of production, such as produces
Energy consumption is high, product batches are inconsistent, product poor transparency, influences properties of product, poor storage stability.To manufacture aqueous dumb light wood
Device paint provides extremely convenient solution, and can arrange in pairs or groups with conventional wood lacquer emulsion and prepare the coating of various gloss, therefore has
There is very big promotional value, meets the policy of national energy conservation and emission reduction.
Specific embodiment
Below with reference to specific implementation, the present invention is furture elucidated.These embodiments are interpreted as being merely to illustrate the present invention
Rather than for limiting the scope of the invention.After having read the content of the invention recorded, those skilled in the art can
To make various changes or modifications to the present invention, these equivalence changes and modification are equally fallen into defined by claims of the present invention
Range.
Embodiment 1: a kind of synthetic method of the aqueous dumb light self-crosslinking acrylic lotion of woodcare paint:
1) first 220kg deionized water, 1.5kg lauryl sodium sulfate, 0.6kg sodium bicarbonate are mixed, as bottom, is then risen
Temperature is to 80 DEG C；
2) by 70kg deionized water, 1kg lauryl sodium sulfate, 3kg methacrylic acid, 125kg methyl methacrylate, 8kg
Butyl acrylate, 15kg styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) is added by the 5% of step 2 stratum nucleare pre-emulsion quality, be added at one time after five minutes 1kg ammonium persulfate and
Then the mixed liquor (A) of 8kg deionized water keeps the temperature 15 minutes for 85 DEG C；Prepare the mixed of 0.5kg ammonium persulfate and 30kg deionized water
It closes liquid (B)；
4) by remaining step 2) stratum nucleare pre-emulsion addition reaction kettle, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) by 290kg deionized water, 1kg lauryl sodium sulfate, 6kg Diacetone Acrylamide, 4.5kg methacrylic acid,
70kg Isooctyl acrylate monomer, 10kg styrene, 3kg vinyltrimethoxysilane, 65kg methyl methacrylate, 28kg delustring
Agent (Degussa TS100) is mixed 20-40 minutes and obtains shell pre-emulsion；
6) after to the addition heat preservation of stratum nucleare pre-emulsion, reaction kettle, dropping temperature 85 is added in step 5) shell pre-emulsion
DEG C, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the step 5) shell pre-emulsion time is added, this period is needed
The mixed liquor of ammonium persulfate and deionized water (B) is added dropwise always simultaneously, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are then cooled to；
10) mixed liquor (C) for preparing 0.5kg tert-butyl hydroperoxide and 5kg deionized water, prepares 0.4kg ascorbic acid and 5kg
The mixed liquor (D) of deionized water；
11) after step 9) cools to 70 DEG C, by the mixed liquor (C) of 0.5kg tert-butyl hydroperoxide and 5kg deionized water and
Reaction kettle is added in 0.4kg ascorbic acid and the mixed liquor (D) of 5kg deionized water simultaneously, and time for adding is 20 minutes, then 60-
70 DEG C keep the temperature 30 minutes；
12) mixed liquor (E) for preparing 4kg ammonium hydroxide and 8kg deionized water, cools to 50-55 DEG C for step 11), then quickly adds
Enter step (E), and stirs 10 minutes；
13) mixed liquor (F) for preparing 5kg adipic dihydrazide and 20kg deionized water, step 12) is cooled to lower than 50 DEG C,
Then step 12) is added in mixed liquor (F), and stirred 20 minutes, filtering can be obtained a kind of woodcare paint and is selfed with aqueous dumb light
Bipropenyl yogurt liquid.
The aqueous dumb light resin made is scratched on black and white covering power paper jam and glass plate respectively from after dry place 7 days
It is tested, which is placed in 50 DEG C of baking ovens and is stored 15 days.
Test performance is as follows:
Adhesive force: 0 grade
Gloss (60 ° of LOOK RIGHTs): 2.3 ° (complete mute)
Hardness: H(China pencil)
Water resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception
Alcohol resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception (dehydrated alcohol: water=1:1)
Storage stability (50 DEG C * 15 days): (no precipitating, without layering) without exception
It can analyze out from experimental data, the product is complete mute, and water resistance, alcohol resistance, adhesive force, hardness, stable storing
Property is not all affected, admittedly any gloss aqueous woodware paint can be prepared with the product mix conventional emulsions.
Embodiment 2:
1) first 210kg deionized water, 1.8kg lauryl sodium sulfate, 0.8kg sodium bicarbonate are mixed, as bottom, is then risen
Temperature is to 80 DEG C；
2) by 80kg deionized water, 1.1kg lauryl sodium sulfate, 3.5kg acrylic acid, 120kg methyl methacrylate, 7kg
Butyl acrylate, 18kg styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) is added by the 5% of step 2 stratum nucleare pre-emulsion quality, be added at one time after five minutes 1.2kg ammonium persulfate and
Then the mixed liquor (A) of 8.8kg deionized water keeps the temperature 15 minutes for 85 DEG C；Prepare 0.6kg ammonium persulfate and 35kg deionized water
Mixed liquor (B)；
4) by remaining step 2) stratum nucleare pre-emulsion addition reaction kettle, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) by 280kg deionized water, 1.2kg lauryl sodium sulfate, 6.5kg Diacetone Acrylamide, 4.8kg acrylic acid,
75kg Isooctyl acrylate monomer, 10kg styrene, 5kg vinyltriethoxysilane, 60kg methyl methacrylate, 28.5kg disappear
Photo etching (Degussa OK520) is mixed 20-40 minutes and obtains shell pre-emulsion；
6) after to the addition heat preservation of stratum nucleare pre-emulsion, reaction kettle, dropping temperature 85 is added in step 5) shell pre-emulsion
DEG C, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the step 5) shell pre-emulsion time is added, this period is needed
The mixed liquor of ammonium persulfate and deionized water (B) is added dropwise always simultaneously, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are then cooled to；
10) prepare 0.55kg tert-butyl hydroperoxide and 5kg deionized water mixed liquor (C), prepare 0.45kg ascorbic acid and
The mixed liquor (D) of 5kg deionized water；
11) after step 9) cools to 70 DEG C, by the mixed liquor (C) of 0.55kg tert-butyl hydroperoxide and 5kg deionized water and
Reaction kettle is added in 0.45kg ascorbic acid and the mixed liquor (D) of 5kg deionized water simultaneously, and time for adding is 20 minutes, then 60-
70 DEG C keep the temperature 30 minutes；
12) mixed liquor (E) for preparing 4.2kg ammonium hydroxide and 8.4kg deionized water, cools to 50-55 DEG C for step 11), then fastly
Step (E) is added in speed, and stirs 10 minutes；
13) mixed liquor (F) for preparing 5.2kg adipic dihydrazide and 20.8kg deionized water, step 12) is cooled to lower than 50
DEG C, step 12) then is added in mixed liquor (F), and stir 20 minutes, filtering can be obtained a kind of woodcare paint with aqueous dumb light oneself
Crosslinking acrylic acid emulsion.
The aqueous dumb light resin made is scratched on black and white covering power paper jam and glass plate respectively from after dry place 7 days
It is tested, which is placed in 50 DEG C of baking ovens and is stored 15 days.
Test performance is as follows:
Adhesive force: 0 grade
Gloss (60 ° of LOOK RIGHTs): 1.3 ° (complete mute)
Hardness: H(China pencil)
Water resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception
Alcohol resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception (dehydrated alcohol: water=1:1)
Storage stability (50 DEG C * 15 days): (no precipitating, without layering) without exception
Embodiment 3:
1) first 220kg deionized water, 1.2kg lauryl sodium sulfate, 0.75kg sodium bicarbonate are mixed, as bottom, then
It is warming up to 80 DEG C；
2) by 80kg deionized water, 0.8kg lauryl sodium sulfate, 3.5kg methacrylic acid, 100kg methyl methacrylate,
10kg butyl acrylate, 18kg styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) is added by the 5% of step 2 stratum nucleare pre-emulsion quality, be added at one time after five minutes 0.8kg ammonium persulfate and
Then the mixed liquor (A) of 6.4kg deionized water keeps the temperature 15 minutes for 85 DEG C；Prepare 0.6kg ammonium persulfate and 33kg deionized water
Mixed liquor (B)；
4) by remaining step 2) stratum nucleare pre-emulsion addition reaction kettle, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) by 300kg deionized water, 1.2kg lauryl sodium sulfate, 8kg Diacetone Acrylamide, 5kg methacrylic acid,
80kg Isooctyl acrylate monomer, 12kg styrene, 3.8kg vinyltrimethoxysilane, 70kg methyl methacrylate, 5kg disappear
Photo etching (Degussa OK520) is mixed 20-40 minutes and obtains shell pre-emulsion；
6) after to the addition heat preservation of stratum nucleare pre-emulsion, reaction kettle, dropping temperature 85 is added in step 5) shell pre-emulsion
DEG C, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the step 5) shell pre-emulsion time is added, this period is needed
The mixed liquor of ammonium persulfate and deionized water (B) is added dropwise always simultaneously, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are then cooled to；
10) mixed liquor (C) for preparing 0.3kg tert-butyl hydroperoxide and 3kg deionized water, prepares 0.3kg ascorbic acid and 3kg
The mixed liquor (D) of deionized water；
11) after step 9) cools to 70 DEG C, by the mixed liquor (C) of 0.3kg tert-butyl hydroperoxide and 3kg deionized water and
Reaction kettle is added in 0.3kg ascorbic acid and the mixed liquor (D) of 3kg deionized water simultaneously, and time for adding is 20 minutes, then 60-
70 DEG C keep the temperature 30 minutes；
12) mixed liquor (E) for preparing 4.1kg ammonium hydroxide and 8.2kg deionized water, cools to 50-55 DEG C for step 11), then fastly
Step (E) is added in speed, and stirs 10 minutes；
13) mixed liquor (F) for preparing 4.8kg adipic dihydrazide and 18kg deionized water, step 12) is cooled to lower than 50
DEG C, step 12) then is added in mixed liquor (F), and stir 20 minutes, filtering.
The water-base resin made is scratched respectively and is carried out on black and white covering power paper jam and glass plate from after dry place 7 days
The lotion is placed in 50 DEG C of baking ovens and stored 15 days by test.
Test performance is as follows:
Adhesive force: 0 grade
Gloss (60 ° of LOOK RIGHTs): 78.7 °
Hardness: H(China pencil)
Water resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception
Alcohol resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception (dehydrated alcohol: water=1:1)
Storage stability (50 DEG C * 15 days): (no precipitating, without layering) without exception
Pass through experimental test data, it is known that, delustering agent, which is not added with, influences obviously the extinction effect of lotion.
Embodiment 4:
1) first 240kg deionized water, 1.3kg lauryl sodium sulfate, 0.8kg sodium bicarbonate are mixed, as bottom, is then risen
Temperature is to 80 DEG C；
2) by 80kg deionized water, 0.8kg lauryl sodium sulfate, 4.5kg methacrylic acid, 130kg methyl methacrylate,
10kg butyl acrylate, 18kg styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) is added by the 5% of step 2 stratum nucleare pre-emulsion quality, be added at one time after five minutes 1.3kg ammonium persulfate and
Then the mixed liquor (A) of 9kg deionized water keeps the temperature 15 minutes for 85 DEG C；Prepare the mixed of 0.8kg ammonium persulfate and 35kg deionized water
It closes liquid (B)；
4) by remaining step 2) stratum nucleare pre-emulsion addition reaction kettle, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) by 260kg deionized water, 1.2kg lauryl sodium sulfate, 6.5kg Diacetone Acrylamide, 4.5kg metering system
Acid, 75kg Isooctyl acrylate monomer, 13kg styrene, 4kg vinyltrimethoxysilane, 70kg methyl methacrylate, 24kg
Delustering agent (Degussa TS100) is mixed 20-40 minutes and obtains shell pre-emulsion；
6) after to the addition heat preservation of stratum nucleare pre-emulsion, reaction kettle, dropping temperature 85 is added in step 5) shell pre-emulsion
DEG C, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the step 5) shell pre-emulsion time is added, this period is needed
The mixed liquor of ammonium persulfate and deionized water (B) is added dropwise always simultaneously, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are then cooled to；
10) mixed liquor (C) for preparing 0.45kg tert-butyl hydroperoxide and 4.5kg deionized water, prepares 0.45kg ascorbic acid
With the mixed liquor (D) of 4.5kg deionized water；
11) after step 9) cools to 70 DEG C, by the mixed liquor (C) of 0.45kg tert-butyl hydroperoxide and 4.5kg deionized water and
Reaction kettle is added in 0.45kg ascorbic acid and the mixed liquor (D) of 4.5kg deionized water simultaneously, and time for adding is 20 minutes, then
60-70 DEG C keeps the temperature 30 minutes；
12) mixed liquor (E) for preparing 3.8kg ammonium hydroxide and 7.6kg deionized water, cools to 50-55 DEG C for step 11), then fastly
Step (E) is added in speed, and stirs 10 minutes；
13) mixed liquor (F) for preparing 4.8kg adipic dihydrazide and 18.6kg deionized water, step 12) is cooled to lower than 50
DEG C, step 12) then is added in mixed liquor (F), and stir 20 minutes, filtering can be obtained a kind of woodcare paint with aqueous dumb light oneself
Crosslinking acrylic acid emulsion.
The aqueous dumb light resin made is scratched on black and white covering power paper jam and glass plate respectively from after dry place 7 days
It is tested, which is placed in 50 DEG C of baking ovens and is stored 15 days.
Test performance is as follows:
Adhesive force: 0 grade
Gloss (60 ° of LOOK RIGHTs): 4.5 ° (complete mute)
Hardness: H(China pencil)
Water resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception
Alcohol resistance: 48 hours (not blistering, non-whitening, not loss of gloss) without exception (dehydrated alcohol: water=1:1)
Storage stability (50 DEG C * 15 days): (no precipitating, without layering) without exception
The above embodiments are only the preferred technical solution of the present invention, and are not construed as limitation of the invention, of the invention
Protection scope should be with the technical solution of claim record, and technical characteristic is equal in the technical solution recorded including claim
Alternative is protection scope.Equivalent replacement i.e. within this range is improved, also within protection scope of the present invention.
Claims (9)
1. the aqueous dumb light self-crosslinking acrylic lotion of woodcare paint, which is characterized in that raw material includes monomer, functional monomer, molten
Agent, neutralizer, buffer, initiator, emulsifier and delustering agent, by weight:
Wherein monomer includes 3-12 parts of methacrylic acid, 120-300 parts of methyl methacrylate, 2-20 parts of butyl acrylate, benzene
10-50 parts and Isooctyl acrylate monomer 40-120 parts of ethylene；
Functional monomer is Diacetone Acrylamide 4-14 parts, 3-10 parts of adipic dihydrazide and vinyltrimethoxysilane 1-
10 parts；
Solvent is deionized water 500-800 parts；
Neutralizer is ammonium hydroxide 2-10 parts；
Buffer is sodium bicarbonate 0.2-1 parts；
Initiator is ammonium persulfate 0.5-3 parts, 0.1-2 parts of tert-butyl hydroperoxide and 0.1-2 parts of ascorbic acid；
Emulsifier is lauryl sodium sulfate 0.5-8 parts；
Delustering agent is fumed silica 5-35 parts.
2. lotion according to claim 1, it is characterised in that: the fumed silica is Degussa TS100.
3. lotion according to claim 1, it is characterised in that: the monomer further includes butyl methacrylate 80-180
Any one of part, 2-10 parts of acrylic acid, 40-100 parts of ethyl methacrylate or several combinations；Butyl methacrylate and
Ethyl methacrylate is different for some or all of substitution methyl methacrylate, butyl acrylate, styrene and acrylic acid
Monooctyl ester；Acrylic acid is for substituting methacrylic acid.
4. lotion according to claim 1, it is characterised in that: the functional monomer further includes succinic acid hydrazide ii 3-10
Part and/or 1-20 parts of vinyltriethoxysilane；The wherein part or all of alternative functions monomer adipic acid of succinic acid hydrazide ii
Two hydrazides, some or all of alternative functions monomer vinyl trimethoxy silane of vinyltriethoxysilane.
5. lotion according to claim 1, it is characterised in that: the neutralizer further includes 2-amino-2-methyl-1-propanol
2-10 parts；2-amino-2-methyl-1-propanol partly or entirely substitutes neutralizer ammonium hydroxide.
6. lotion according to claim 1, it is characterised in that: the initiator further includes 0.5-5 parts of sodium peroxydisulfate；Over cure
The sour part or all of alternative initiator ammonium persulfate of sodium.
7. lotion according to claim 1, it is characterised in that: the emulsifier further includes isomeric alcohol polyethenoxy ether 0.4-
6 parts；Selected component can replace emulsifier sodium lauryl sulfate completely.
8. lotion according to claim 1, it is characterised in that: the delustering agent is 5-35 parts of Degussa TS100 gas phases two
Silica further includes 4-30 parts of Degussa OK520 fumed silicas.
9. the synthetic method of aqueous dumb light self-crosslinking acrylic lotion of woodcare paint described in claim 1-8 any one,
It is characterized in that, comprising the following steps:
1) first deionized water, part lauryl sodium sulfate, sodium bicarbonate are mixed, as bottom, is then warming up to 80 DEG C；
2) ionized water, part lauryl sodium sulfate, part methyl acrylic acid, butyl acrylate, part methyl acrylic acid are removed
Methyl esters, part styrene are mixed 20-40 minutes and uniformly obtain stratum nucleare pre-emulsion；
3) step 1) resulting material is added by the 5% of step 2 stratum nucleare pre-emulsion quality, is added at one time part mistake after five minutes
Then the mixed liquor A of ammonium sulfate and deionized water keeps the temperature 15 minutes for 85 DEG C；Water is added to prepare mixed liquor using remaining ammonium persulfate again
B；
4) reaction kettle is added in step 2 residue stratum nucleare pre-emulsion, 85 DEG C of dropping temperature, time for adding is 1.5 hours, is added dropwise
Continue heat preservation 0.5 hour for 85 DEG C after complete stratum nucleare pre-emulsion；
5) it is different pungent that ionized water, remaining lauryl sodium sulfate, Diacetone Acrylamide, remaining methacrylic acid, acrylic acid are removed
Ester, residual styrene, vinyltrimethoxysilane, remaining methyl methacrylate, delustering agent (Degussa TS100) mixing are stirred
It mixes 20-40 minutes and obtains shell pre-emulsion；
6) after to stratum nucleare pre-emulsion addition heat preservation in step 4), reaction kettle, drop is added in step 5) shell pre-emulsion
85 DEG C of heating degree, time for adding 2 hours；
7) from adding step 2 stratum nucleare pre-emulsion to amount to 4 hours to the shell pre-emulsion time is added, this period needs simultaneously
The mixed liquid B of preparation is added dropwise always, it is synchronous to carry out；
8) after to step 7), 85 DEG C are continued heat preservation 1 hour；
9) after to step 8) heat preservation, 70 DEG C are cooled to；
10) the mixed liquor C for preparing tert-butyl hydroperoxide and water, prepares the mixed liquor D of ascorbic acid and water；
11) after step 9) cools to 70 DEG C, by the mixed liquor of the mixed liquor C and ascorbic acid and water of tert-butyl hydroperoxide and water
Reaction kettle is added in D simultaneously, and time for adding is 20 minutes, then keeps the temperature 30 minutes for 60-70 DEG C；
12) the mixed liquor E for preparing ammonium hydroxide and water will cool to 50-55 DEG C obtained by step 11), mixed liquor E then be added, and stir
It mixes 10 minutes；
13) the mixed liquor F for preparing adipic dihydrazide and water will be cooled to lower than 50 DEG C obtained by step 12), then by mixed liquor
F is added in obtained by step 12), and stirs 20 minutes, and filtering obtains a kind of aqueous dumb light self-crosslinking acrylic cream of woodcare paint
Liquid.
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