CN107573778B - Low PVC dark color water paint and preparation method thereof - Google Patents
Low PVC dark color water paint and preparation method thereof Download PDFInfo
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- CN107573778B CN107573778B CN201710827701.6A CN201710827701A CN107573778B CN 107573778 B CN107573778 B CN 107573778B CN 201710827701 A CN201710827701 A CN 201710827701A CN 107573778 B CN107573778 B CN 107573778B
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Abstract
The present invention relates to low PVC dark color water paints and preparation method thereof, the water paint is by component A: accounting for 30.0~38.0% high molecular dye graft of total weight, 2.5~8.5% polyether-modified dimethyl silicone polymer wetting agents, 6.0~15.0% high-molecular block copolymer dispersing agents, 8~15% acrylic resins, 12.0~22.0% water-miscible organic solvents, 0.8~3.0% functional aid and balance deionized water；Component B: 46~53% acrylic resin of total weight is accounted for, 0.6~1.0% polyether-modified dimethyl silicone polymer wetting agent, 0.3~0.6% polyether-modified Dimethicone Copolyol body levelling agent, 5.0~12.0% water-miscible organic solvents, 0.8~3.0% functional aid and balance deionized water.Low PVC dark color water paint prepared by the present invention has good tinctorial strength, color fastness to water and flexibility.
Description
[technical field]
The present invention relates to a kind of low PVC dark color water paints and preparation method thereof.
[background technique]
The preparation of dark water paint needs to be added a large amount of pigment, dyestuff, under high PVC, can just embody dark effect
Fruit.But largely addition pigment, dyestuff then will affect the performances such as the water resistance, flexibility, gloss of water paint, become paint film
Crisp, compatibility poor；And as the environmental consciousness for developing people of society is more and more stronger, dyestuff is largely added, not only not ring
It protects, and the patience of paint film can also decline.
If we improve its performance the method that the monomer of the structure of high molecular dye film-forming resin is grafted.With at
The high molecular dye of film resin grafting, makes chemical bonds, that is, improves the tinctorial strength of dyestuff, and guarantee color fastness to water；Separately
One side acrylic resin does parent, ensure that compatibility, so as to improve flexibility.
Usually if not by the way of grafting, pigment, by simple physical mixed, forms a film with resin in resin
Afterwards, some pigment is bound on the surface of film, and fastness to rubbing can be relatively low at this time, and uses dyestuff and film-forming resin
After learning bond conjunction, fastness can be especially high.
[summary of the invention]
It is a kind of with brilliant idea intensity of colour, excellent compatibility, storage stability it is an object of the invention to be provided under low PVC
The environment-friendly water-based paint of ideal.
To overcome above-mentioned technological deficiency, the present invention provides a kind of low PVC dark color water paint, preparation method includes following
Step:
Step 1: high molecular dye graft is prepared, by the way that hydroxy acrylate grafting polymer dyestuff to be saponified to obtain；
Step 2: component A is prepared,
The acrylic resin of component A total weight 8~15%, 2.5~8.5% polyether-modified dimethyl silicone polymer will be accounted for
Wetting agent, 6.0~15.0% high-molecular block copolymer dispersing agents, 12.0~22.0% water-miscible organic solvents are scattered in part
In deionized water, premix is obtained；
Under stirring conditions, 30.0~38.0% high molecular dye grafts, dispersion are added in Xiang Suoshu premix
0.8~3.0% functional aid is added after uniformly, adjusting pH value is 8.0~9.0, obtains high molecular dye graft dispersion
Mixed liquor；
The high molecular dye graft dispersion mixed liquor is dispersed under the revolving speed of 2000~3000rpm, and
Remaining deionized water is added, obtains pre-grinding high molecular dye graft dispersion；
The pre-grinding high molecular dye graft dispersion is subjected to continuously grinding with zirconium oxide bead, until high molecular dye
After the average grain diameter of graft is no more than 1um, it is filtered, deaeration, obtains the component A, the surplus in said ratio is institute
The deionized water stated,
Step 3: component B is prepared,
46~53% acrylic resin of component B total weight, 0.6~1.0% polyether-modified poly dimethyl silicon will be accounted for
Oxygen alkane wetting agent, 0.3~0.6% polyether-modified Dimethicone Copolyol body levelling agent, 5.0~12.0% water solubility have
Solvent, 0.8~3.0% functional aid, surplus deionized water be mixed to get component B,
Step 4: component A and component B are mixed
The dosage relation B/A=(2.5~5)/1 times of component A and component B, wherein acrylic resin is in terms of 40% solid content.
This method also has following optimization processing step:
The high molecular dye is selected from polyamide, at least one of polyimide dyestuff dyestuff.
High-molecular block copolymer dispersing agent is at least one of BYK190, EFKA4585.
The functional aid is mildewproof sterilized dose and pH adjusting agent.
Mildewproof sterilized dose of the dosage is the 0.5~0.8% of high molecular dye weight, and pH adjusting agent dosage is high score
The 0.3~0.6% of sub- dyestuff weight.
Water-miscible organic solvent in component A is selected from least one of ethylene glycol, propylene glycol, polypropylene glycol.
The partial size of the zirconium oxide bead is 0.8~1.0mm.
Water-miscible organic solvent in component B is selected from least one of b propanol, n-butanol alcohol, dipropylene glycol methyl ether.
The step of by the saponification of hydroxy acrylate grafting polymer dyestuff are as follows: condenser is housed, blender and thermometer
In three-necked flask, a certain amount of high molecular dye, butanone, hydroxy acrylate and BPO is added, is warming up to 80 DEG C, it is anti-to constant temperature
It should terminate, the complete BPO of unreacted is washed to the greatest extent with acetone, deionized water is added, is heated to reflux, adjusting pH value to 6.5~8,
Obtain the high molecular dye graft.
Compared with prior art, the present invention have it is following the utility model has the advantages that
1, the present invention using high molecular dye structure film-forming resin monomer grafting method, dyestuff color strength
Degree, and guarantee color fastness to water；Another aspect acrylic resin does parent, ensure that compatibility, so as to improve flexibility；
2, if not by the way of grafting, pigment with resin by simple physical mixed, after resin film forming,
Some pigment be bound on the surface of film, fastness to rubbing can be relatively low at this time, and uses dyestuff and film-forming resin chemistry
After bond is closed, fastness can be especially high.
[specific embodiment]
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
The monomer of the structure acrylic resin of high molecular dye used in Examples 1 to 6 component A is grafted, reaction mechanism such as I
It is shown:
Wherein R is the compound of band-NH- group, such as polyamide, polyimides, wherein n=2000-8000, preferably
3000-4000
Non-grafted high molecular dye used in 1~6 component A of comparative example；
Component B used in Examples 1 to 6 and comparative example 1~6 is with an example component B.
Specific preparation process is as follows for Examples 1 to 6 and comparative example 1~6:
Component A:
One, the 20wt.% for reserving deionized water total amount, by the 80wt.% of deionized water total amount, whole acrylic acid trees
Rouge, whole polyether-modified dimethyl silicone polymer wetting agents, whole high-molecular block copolymers and whole water solubilitys have
Solvent disperses 15~20min in dispersion machine with 500~800r/min revolving speed, obtains premix；
Two, dispersing speed is adjusted to 300~400r/min, whole high molecular dye grafts is added in step 1
In resulting premix, it is stirring evenly and then adding into whole functional aids, it is mixed to adjust high molecular dye graft dispersion
Between the pH to 8.0~9.0 for closing liquid, high molecular dye graft dispersion mixed liquor is obtained；
Three, by gained high molecular dye graft dispersion mixed liquor in step 2 in the revolving speed of 2000~3000r/min
Under carry out dispersion 30min, and in dispersion process be added step 1 in reserve 20wt.% deionized water, obtain pre-grinding height
Molecular dye graft dispersion；
Four, pre-grinding high molecular dye graft dispersion obtained by step 3 is ground in horizontal mill, is ground
Grinding media is the zirconium oxide bead of 0.8~1.0mm of partial size, and continuously grinding is tested with laser particle instrument, when high molecular dye connects
Terminate to grind when the average grain diameter 1um of branch object, obtains high molecular dye graft dispersion；
Five, high molecular dye graft dispersion obtained by step 4 is filtered, deaeration, obtains required component A.
Six, 46~53% acrylic resin of component B total weight, 0.6~1.0% polyether-modified poly dimethyl will be accounted for
Polysiloxane wetting agents, 0.3~0.6% polyether-modified Dimethicone Copolyol body levelling agent, 5.0~12.0% water solubility
Organic solvent, 0.8~3.0% functional aid, surplus deionized water in dispersion machine with 500~800r/min revolving speed dispersion
15~20min obtains premix；Water-miscible organic solvent therein is in b propanol, n-butanol alcohol, dipropylene glycol methyl ether
At least one,
Seven, it by premix obtained by step 6, adjusts between pH to 8.0~9.0, obtains component B；
Eight, the component A for obtaining step 5 is added in proportion in the component B that step 7 obtains, in dispersion machine with
500~800r/min revolving speed disperses 15~20min, obtains a kind of low PVC dark color water paint.
Examples 1 to 6 group is grouped as shown in table 1.Wherein aqueous organic solvent propylene glycol, antimildew disinfectant are selected dense
Degree is 1,2- benzisothiazole-3-ketone, the pH adjusting agent triethanolamine of 1.0wt.%.
The composition of 1. Examples 1 to 6 of table
(unit: mass percent)
Comparative example 1~6 is compared mainly for embodiment 1 and embodiment 6, and table 2 is that each component accounts in comparative example 1~6
The mass percent of high molecular dye total composition.Wherein aqueous organic solvent propylene glycol, antimildew disinfectant select concentration
1,2- benzisothiazole-3-ketone, pH adjusting agent triethanolamine for 1.0wt.%.
The test method of component A prepared by Examples 1 to 6 and comparative example 1~6 is as follows: limited with Britain's Malvern instrument
The 3000 type laser particle size measurement of Mastersizer of the company component particle diameter distribution, D50 indicates surveyed particle in test result
In 50% the minimum grain size that can be transferred through of particle, average grain diameter is indicated with D50；Component A and component B is pressed into PVC1.0 painting,
It is sprayed at tinplate with electrostatic gun, after band paint film is dry, according to GB/T9286-1998 paint and varnish, paint film lattice drawing is real
It tests and carries out adhesive force test, impact resistance test is carried out according to GB/T1732-1993 paint film impact resistance measuring method, according to GB/T
1733-1993 paint film water resistance measuring method carries out water resistance test, according to the measurement method of GB 11186-1989 paint film color,
Color difference is beaten, judges △ L value and tinctorial strength, tinctorial strength is using embodiment as standard specimen 100%.Table 3 and table 4 are respectively embodiment 1
The result tested according to the above method of water paint under~the 6 and different PVC that prepare of comparative example 1~6.
The composition of 2. comparative example 1~6 of table
(unit: mass percent)
The high molecular dye of 3. Examples 1 to 6 of table preparation is grafted water paint the performance test results
Note: " 0 grade " indicates preferably, and " 1 grade " indicates general, and " 2 grades " expressions are poor.
The high molecular dye of 4. comparative example 1~6 of table preparation does not connect branch water paint the performance test results
Note: " 0 grade " indicates preferably, and " 1 grade " indicates general, and " 2 grades " expressions are poor.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (10)
1. a kind of preparation method of low PVC dark color water paint, it is characterised in that the following steps are included:
Step 1: high molecular dye graft is prepared, by the way that hydroxy acrylate grafting polymer dyestuff to be saponified to obtain；
Step 2: component A is prepared,
To account for the acrylic resin of component A total weight 8 ~ 15%, 2.5 ~ 8.5% polyether-modified dimethyl silicone polymer wetting agent,
6.0 ~ 15.0% high-molecular block copolymer dispersing agents, 12.0 ~ 22.0% water-miscible organic solvents are scattered in portions of de-ionized water,
Obtain premix；
Under stirring conditions, 30.0 ~ 38.0% high molecular dye grafts are added in Xiang Suoshu premix, after being uniformly dispersed
0.8 ~ 3.0% functional aid is added, adjusting pH value is 8.0 ~ 9.0, obtains high molecular dye graft dispersion mixed liquor；
The high molecular dye graft dispersion mixed liquor is dispersed under the revolving speed of 2000 ~ 3000rpm, and is added surplus
Remaining deionized water obtains pre-grinding high molecular dye graft dispersion；
The pre-grinding high molecular dye graft dispersion is subjected to continuously grinding with zirconium oxide bead, until high molecular dye is grafted
After the average grain diameter of object is no more than 1 μm, it is filtered, deaeration, obtains the component A, the surplus in said ratio is described
Deionized water,
Step 3: component B is prepared,
46 ~ 53% acrylic resin of component B total weight, 0.6 ~ 1.0% polyether-modified dimethyl silicone polymer wetting will be accounted for
Agent, 0.3 ~ 0.6% polyether-modified Dimethicone Copolyol body levelling agent, 5.0 ~ 12.0% water-miscible organic solvent, 0.8 ~
3.0% functional aid, surplus deionized water be mixed to get component B,
Step 4: component A and component B are mixed,
Dosage relation B/A=(2.5 ~ 5)/1 times of component A and component B, wherein acrylic resin is in terms of 40% solid content.
2. a kind of preparation method of low PVC dark color water paint as described in claim 1, it is characterised in that the high molecular dye
Select polyamide, at least one of polyimide dyestuff dyestuff.
3. a kind of preparation method of low PVC dark color water paint as described in claim 1, which is characterized in that the macromolecule is embedding
Section copolymer dispersant is at least one of BYK190, EFKA4585.
4. a kind of preparation method of low PVC dark color water paint as described in claim 1, which is characterized in that the functionality helps
Agent is mildewproof sterilized dose and pH adjusting agent.
5. a kind of preparation method of low PVC dark color water paint as claimed in claim 4, it is characterised in that described mildewproof sterilized dose
Dosage be high molecular dye weight 0.5 ~ 0.8%, pH adjusting agent dosage be high molecular dye weight 0.3 ~ 0.6%.
6. a kind of preparation method of low PVC dark color water paint as described in claim 1, it is characterised in that water-soluble in component A
Property organic solvent be selected from least one of ethylene glycol, propylene glycol, polypropylene glycol.
7. a kind of preparation method of low PVC dark color water paint as described in claim 1, it is characterised in that the zirconium oxide bead
Partial size is 0.8 ~ 1.0mm.
8. a kind of preparation method of low PVC dark color water paint as described in claim 1, it is characterised in that water-soluble in component B
Property organic solvent be selected from least one of b propanol, n-butanol, dipropylene glycol methyl ether.
9. a kind of preparation method of low PVC dark color water paint as described in claim 1, it is characterised in that by hydroxy acrylate
The step of grafting polymer dyestuff is saponified are as follows: equipped with condenser, in the three-necked flask of blender and thermometer, be added a certain amount of
High molecular dye, butanone, hydroxy acrylate and BPO are warming up to 80 DEG C, with acetone that unreacted is complete to the end of isothermal reaction
Full BPO is washed to the greatest extent, is added deionized water, is heated to reflux, and is adjusted pH value to 6.5 ~ 8, is obtained the high molecular dye graft.
10. a kind of using low PVC dark color water paint made from any preparation method of claim 1 ~ 9.
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| CN201710827701.6A CN107573778B (en) | 2017-09-14 | 2017-09-14 | Low PVC dark color water paint and preparation method thereof |
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| CN102732103A (en) * | 2012-07-23 | 2012-10-17 | 上海睿途新材料科技有限公司 | High-printing-property environment-friendly water-based back surface coating for packaging materials as well as preparation method thereof |
| CN103709834A (en) * | 2013-12-20 | 2014-04-09 | 苏州世名科技股份有限公司 | Phthalocyanine pigment water-based color paste for coloring synthetic leather and preparation method thereof |
| CN103725131A (en) * | 2013-12-30 | 2014-04-16 | 东莞光群雷射科技有限公司 | Gold stamping coating and preparation process thereof |
| CN104927064A (en) * | 2015-05-28 | 2015-09-23 | 齐鲁工业大学 | Preparation method for polymeric dye based on hyperbranched polyamine-ester |
| CN105220534A (en) * | 2015-10-26 | 2016-01-06 | 江南大学 | A kind of UV synchronously realizing textile coloration and anti-crease finishing solidifies the preparation method of azobenzene-polyurethane-base high molecular dye |
-
2017
- 2017-09-14 CN CN201710827701.6A patent/CN107573778B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102732103A (en) * | 2012-07-23 | 2012-10-17 | 上海睿途新材料科技有限公司 | High-printing-property environment-friendly water-based back surface coating for packaging materials as well as preparation method thereof |
| CN103709834A (en) * | 2013-12-20 | 2014-04-09 | 苏州世名科技股份有限公司 | Phthalocyanine pigment water-based color paste for coloring synthetic leather and preparation method thereof |
| CN103725131A (en) * | 2013-12-30 | 2014-04-16 | 东莞光群雷射科技有限公司 | Gold stamping coating and preparation process thereof |
| CN104927064A (en) * | 2015-05-28 | 2015-09-23 | 齐鲁工业大学 | Preparation method for polymeric dye based on hyperbranched polyamine-ester |
| CN105220534A (en) * | 2015-10-26 | 2016-01-06 | 江南大学 | A kind of UV synchronously realizing textile coloration and anti-crease finishing solidifies the preparation method of azobenzene-polyurethane-base high molecular dye |
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