CN109666148A - A kind of preparation method of aqueous dispersion - Google Patents
A kind of preparation method of aqueous dispersion Download PDFInfo
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- CN109666148A CN109666148A CN201811640103.9A CN201811640103A CN109666148A CN 109666148 A CN109666148 A CN 109666148A CN 201811640103 A CN201811640103 A CN 201811640103A CN 109666148 A CN109666148 A CN 109666148A
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- Prior art keywords
- aqueous dispersion
- preparation
- styrene
- dispersion according
- maleic anhydride
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- 239000006185 dispersion Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 27
- 229920000570 polyether Polymers 0.000 claims abstract description 26
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229920000147 Styrene maleic anhydride Polymers 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 239000000080 wetting agent Substances 0.000 claims abstract description 16
- 239000000049 pigment Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 230000001603 reducing effect Effects 0.000 claims abstract description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 54
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 36
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- 239000007864 aqueous solution Substances 0.000 claims description 10
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 229920001577 copolymer Polymers 0.000 claims description 8
- 229920001400 block copolymer Polymers 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 5
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 5
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000012752 auxiliary agent Substances 0.000 claims description 4
- 239000002585 base Substances 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- JRBPAEWTRLWTQC-UHFFFAOYSA-N dodecylamine Chemical compound CCCCCCCCCCCCN JRBPAEWTRLWTQC-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000001476 alcoholic effect Effects 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000009736 wetting Methods 0.000 claims description 3
- DTCCVIYSGXONHU-CJHDCQNGSA-N (z)-2-(2-phenylethenyl)but-2-enedioic acid Chemical compound OC(=O)\C=C(C(O)=O)\C=CC1=CC=CC=C1 DTCCVIYSGXONHU-CJHDCQNGSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 claims 1
- 229940092714 benzenesulfonic acid Drugs 0.000 claims 1
- 239000003906 humectant Substances 0.000 claims 1
- 150000002576 ketones Chemical class 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000004094 surface-active agent Substances 0.000 claims 1
- 239000002270 dispersing agent Substances 0.000 abstract description 14
- 239000011248 coating agent Substances 0.000 abstract description 10
- 238000000576 coating method Methods 0.000 abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000945 filler Substances 0.000 abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000032050 esterification Effects 0.000 description 5
- 238000005886 esterification reaction Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 150000003384 small molecules Chemical class 0.000 description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 4
- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229920001223 polyethylene glycol Polymers 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- -1 acrylic ester Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical class CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- 239000004606 Fillers/Extenders Substances 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 238000004873 anchoring Methods 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical group [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- 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
- C08G81/024—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G
- C08G81/025—Block or graft polymers containing sequences of polymers of C08C or C08F and of polymers of C08G containing polyether sequences
-
- 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
- C09D133/00—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 at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
-
- 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
- C09D7/41—Organic pigments; Organic dyes
-
- 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
-
- 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
- C09D7/65—Additives macromolecular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention relates to a kind of preparation methods of aqueous dispersion, and styrene-maleic anhydride copolymer is dissolved in atent solvent, and monomethyl polyethers and catalyst is added;60~110 DEG C are heated to, is reacted 2.5~6.0 hours, solvent is boiled off, neutralizer is added and neutralizes, then mixes and stirs evenly with thinner, wetting agent, aqueous dispersion is prepared.Compared with prior art, dispersing agent prepared by the present invention has good water solubility, there is good dispersibility and color developing to pigment, filler, and viscosity reducing effect is good, will form colour paste system of good performance, can be widely used in coating, ink addition agent field.
Description
Technical field
The invention belongs to coating, ink addition agent field, more particularly, to a kind of preparation method of aqueous dispersion.
Background technique
Currently, increasingly stringent with national environmental protection policy, coating, ink product Water-borne modification process increasingly step up, be
Meet this kind of product Water-borne modification process, the research of Water-borne modification auxiliary agent becomes hot spot.
The requirement of coating and ink this kind of product to color is even more almost harsh, so the dispersion one of pigment and filler
Where being directly key problem in technology, such issues that solution rely heavily on high performance dispersing agent, traditional small molecule dispersion
Agent tool has disadvantages that, for example dispersion is unstable, and storage time is short, reunion sedimentation easy to form.Polymer type surpasses
These drawbacks of dispersing agent very good solution.
For the hyper-dispersant of phenylethylene-maleic anhydride class system, since styrene has benzene ring structure, to phthalocyanines
Pigment dispersion effect is good, and anchoring group of the maleic anhydride as dispersion inorganic filler disperses inorganic pigment and extender pigment
Effect is obvious.But styrene-maleic anhydride copolymer is water-soluble and bad, the system after this kind of macromolecule dispersing agent dispersion
Viscosity is higher, affects the fluid properties of mill base product below;Generally come real by the way of by the inorganic alkali neutralization of maleic acid
Existing Water-borne modification, but the dispersion being formed by, can make a big impact to the water-resistant coating formed below.
Summary of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide cost is relatively low and has for one kind
For the preparation method of good pigment, the aqueous dispersion of filler dispersibility.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of aqueous dispersion, styrene-maleic anhydride copolymer is dissolved in atent solvent, is added
Monomethyl polyethers and catalyst;60~110 DEG C are heated to, is reacted 2.5~6.0 hours, solvent is boiled off, neutralizer is added, by body
System neutralizes to pH between 6~8, then mixes and stir evenly with thinner, wetting agent, and aqueous dispersion is prepared.
Molecular weight (the M of the styrene-maleic anhydride copolymerwtWeight is equal) it is 2000~10000, molecular weight distributing index
Between 1.0~2.0, the structure of copolymer is any one of trackless, block or alternating structure.
The atent solvent is to be not involved in esterification, and the lower atent solvent of boiling point, preferably can using acetone or
Ethyl acetate.
The monomethyl polyethers is the block copolymer of propylene glycol and ethylene glycol, and the molar ratio of propylene glycol and ethylene glycol is 1:
1~6, and blocked by methyl in ethylene glycol side, molecular weight (Mn number is equal) is 500~3000.
The catalyst is the catalyst for capableing of catalytic esterification, can preferably use p-methyl benzenesulfonic acid.
The ratio between the molal quantity of maleic anhydride and the molal quantity of monomethyl polyethers are in the styrene-maleic anhydride copolymer
1:0.5~1.5 when reaction temperature, generate main polymer styrene-maleic acid polyether ester, catalyst under catalyst
Additional amount be reactant weight 3wt%.
The neutralizer is the aqueous solution or alcoholic solution of potassium hydroxide, ammonium hydroxide or triethanolamine.
The thinner is the nonionic surfactants object such as ethoxylated dodecyl alcohol or lauryl amine polyoxyethylene ether
Matter.
The wetting agent is the auxiliary agent that Hydropalat 875 etc. can be such that pigment particle surface soaks.
Above-mentioned wetting agent and thinner are commercially available water-soluble small molecule wetting agent and thinner, additive amount are totality
0~30wt% of content is subject to and guarantees that dispersing agent arbitrary proportion aqueous solution is transparent.
Aqueous dispersion in the present invention, the raw material used for styrene-maleic anhydride copolymer resin and end capped polyether,
It is relatively inexpensive raw material, has mature supply chain and industrialization basis, be conducive to promote and industrialize.
Aqueous dispersion in the present invention introduces the polyethers esterification chain of polypropylene glycol and polyethylene glycol in molecule branch
Section, increase it is water-soluble reduce the dosage of neutralizer simultaneously, reduce the influence to follow-up coating water resistance.
The small molecule thinner and wetting agent being added in the present invention, due to playing the peptizaiton to macromolcular dispersant,
The water solubility for increasing macromolecular has achieved the effect that aqueous solution clear, while drops the viscosity of dispersion further
It is low, improve the rheological equationm of state of subsequent dispersion.
Compared with prior art, the invention has the following advantages that
1) combine macromolecule hyper-dispersant dispersion stabilization and small molecule wetting dispersing agent it is Viscosity-reducing, water-soluble
Advantage, increases the dispersion effect of dispersing agent, and reduces the viscosity of dispersion;
2) use for reducing neutralizer effectively reduces the influence to the water resistance and alkali resistance of follow-up coating;
3) raw material sources are extensive, cheap, there is industrialization basis well.
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.
A kind of preparation method of aqueous dispersion, styrene-maleic anhydride copolymer is dissolved in atent solvent, benzene second
The ratio between molal quantity of the molal quantity of maleic anhydride and monomethyl polyethers is 1:0.5~1.5 in alkene-copolymer-maleic anhydride, is added
Monomethyl polyethers and catalyst, the additional amount of catalyst are the 3wt% of reactant weight, system are heated to 60~110 DEG C, instead
Answer 2.5~6.0 hours, boil off solvent, neutralizer is added and neutralizes system to pH between 6~8, then with thinner, wetting agent
Mixing stirs evenly, and aqueous dispersion is prepared.
In above-mentioned preparation process, the molecular weight (M for the styrene-maleic anhydride copolymer that can be usedwtWeight is equal) it is 2000
~10000, for molecular weight distributing index between 1.0~2.0, the structure of copolymer is appointing in trackless, block or alternating structure
It is a kind of.The relatively inexpensive raw material of the raw material have mature supply chain and industrialization basis, are conducive to promote and industrialize.
The atent solvent used is to be not involved in esterification, and the lower atent solvent of boiling point, can use acetone or ethyl acetate.It is single
Methyl polyethers is the block copolymer of propylene glycol and ethylene glycol, and the molar ratio of propylene glycol and ethylene glycol is 1:1~6, and by methyl
It is blocked in ethylene glycol side, molecular weight (MnNumber is equal) 500~3000.Polypropylene glycol and poly- second two are introduced in molecule branch
The polyethers of alcohol is esterified segment, increase it is water-soluble reduce the dosage of neutralizer simultaneously, reduce to follow-up coating water resistance
Influence.Catalyst is the catalyst for capableing of catalytic esterification, can use p-methyl benzenesulfonic acid.Neutralizer is hydroxide
The aqueous solution or alcoholic solution of potassium, ammonium hydroxide or triethanolamine.Thinner is poly- for nonionic surfactants substance such as laruyl alcohol
Ethylene oxide ether, lauryl amine polyoxyethylene ether etc., wetting agent are the auxiliary agent that pigment particle surface can be made to soak, such as Hydropalat
875 etc..Above-mentioned wetting agent and thinner are commercially available water-soluble small molecule wetting agent and thinner, and additive amount is overall contains
0~30wt% of amount, is subject to and guarantees that dispersing agent arbitrary proportion aqueous solution is transparent.
More detailed case study on implementation below, by following case study on implementation further illustrate technical solution of the present invention with
And the technical effect that can be obtained.
Embodiment 1:
A kind of preparation of aqueous dispersion, specifically includes the following steps:
Styrene-maleic anhydride copolymer (maleic anhydride ratios 20%) is dissolved in acetone;By monomethyl block
Polyethers (polypropylene glycol: polyethylene glycol=1:5) and p-methyl benzenesulfonic acid (3%) are added in above-mentioned system;80 DEG C are heated to, reaction
4.0 hours, acetone is boiled off, the aqueous solution that potassium hydroxide is then added is neutralized to solution into faintly acid, adds 20%
AC1210 is to get aqueous dispersion.
Dispersion is prepared according to following ratios:
Phthalocyanine blue: 5%
Barium sulfate: 25%
Calcium carbonate: 25%
Titanium dioxide: 15%
Dispersing agent: 2.5%
Water: 27.5%
After 1h grinding is dispersed with stirring, system viscosity is 0.987 × 10-3Pas,
For color developing compared with pure phthalocyanine blue mill base, color difference is no more than 5%.
Above-mentioned dispersion is added in acrylic ester aquosity coating, spraying plate-making, test result is as follows:
Embodiment 2:
A kind of preparation of aqueous dispersion, specifically includes the following steps:
Styrene-maleic anhydride copolymer (block copolymer that maleic anhydride ratios are 10%) is dissolved in ethyl acetate
In;Monomethyl block polyether (polypropylene glycol: polyethylene glycol=1:3) and p-methyl benzenesulfonic acid (3%) are added in above-mentioned system;
80 DEG C are heated to, reacts 4.0 hours, boils off ethyl acetate, the aqueous solution that triethanolamine is then added is neutralized to solution into weak acid
Property adds 25% AC1210 to get aqueous dispersion.
Dispersion is prepared according to following ratios:
Phthalocyanine blue: 5%
Barium sulfate: 25%
Calcium carbonate: 25%
Titanium dioxide: 15%
Dispersing agent: 2.5%
Water: 27.5%
After 1h grinding is dispersed with stirring, system viscosity is 1.02 × 10-3Pas,
For color developing compared with pure phthalocyanine blue mill base, color difference is no more than 5%.
Above-mentioned dispersion is added in acrylic ester aquosity coating, spraying plate-making, test result is as follows:
Embodiment 3:
A kind of preparation method of aqueous dispersion, styrene-maleic anhydride copolymer is dissolved in atent solvent acetone,
Molecular weight (the M of the styrene-maleic anhydride copolymer usedwtWeight is equal) be 2000, molecular weight distributing index 1.0~2.0 it
Between, copolymer is trackless structure, and monomethyl polyethers and catalyst toluenesulfonic acid is added, and the monomethyl polyethers used is propylene glycol
With the block copolymer of ethylene glycol, the molar ratio of propylene glycol and ethylene glycol is 1:1, and is blocked by methyl in ethylene glycol side, point
Son amount (MnNumber is equal) molal quantity of the molal quantity of maleic anhydride and monomethyl polyethers in 500, styrene-maleic anhydride copolymer
The ratio between be 1:0.5, the additional amount of catalyst is the 3wt% of reactant weight
System is heated to 60 DEG C, is reacted 6.0 hours, solvent is boiled off, neutralizer potassium hydroxide is added and arrives system neutralization
Aqueous dispersion is prepared 6 in pH.
Embodiment 4:
Styrene-maleic anhydride copolymer is dissolved in atent solvent acetic acid second by a kind of preparation method of aqueous dispersion
In ester, the molecular weight (M of the styrene-maleic anhydride copolymer usedwtWeight is equal) be 5000, molecular weight distributing index 1.0~
Between 2.0, copolymer is block structure, and monomethyl polyethers is added and catalyst toluenesulfonic acid, the monomethyl polyethers used are
The molar ratio of the block copolymer of propylene glycol and ethylene glycol, propylene glycol and ethylene glycol is 1:3, and by methyl in one side seal of ethylene glycol
End, molecular weight (MnNumber is equal) molal quantity of maleic anhydride and monomethyl polyethers in 2000, styrene-maleic anhydride copolymer
The ratio between molal quantity is 1:1, and the additional amount of catalyst is the 3wt% of reactant weight, system is heated to 90 DEG C, reaction 4.0 is small
When, boil off solvent, neutralizer ammonium hydroxide be added and neutralizes system to pH 7, then with thinner ethoxylated dodecyl alcohol, wetting agent
The mixing of Hydropalat 875 stirs evenly, and the additive amount of wetting agent and thinner is the 10wt% of overall content, guarantees dispersing agent
Subject to arbitrary proportion aqueous solution is transparent, aqueous dispersion is prepared.
Embodiment 5:
Styrene-maleic anhydride copolymer is dissolved in atent solvent acetic acid second by a kind of preparation method of aqueous dispersion
In ester, the molecular weight (M of the styrene-maleic anhydride copolymer usedwtWeight is equal) be 5000, molecular weight distributing index 1.0~
Between 2.0, copolymer is block structure, and monomethyl polyethers is added and catalyst toluenesulfonic acid, the monomethyl polyethers used are
The molar ratio of the block copolymer of propylene glycol and ethylene glycol, propylene glycol and ethylene glycol is 1:6, and by methyl in one side seal of ethylene glycol
End, molecular weight (MnNumber is equal) molal quantity of maleic anhydride and monomethyl polyethers in 3000, styrene-maleic anhydride copolymer
The ratio between molal quantity is 1:1.5, and the additional amount of catalyst is the 3wt% of reactant weight.System is heated to 110 DEG C, reaction 2.5
Hour, boil off solvent, neutralizer ammonium hydroxide be added and neutralizes system to pH 8, then with thinner lauryl amine polyoxyethylene ether, wetting
The mixing of agent Hydropalat 875 stirs evenly, and the additive amount of wetting agent and thinner is the 30wt% of overall content, guarantees dispersion
Subject to agent arbitrary proportion aqueous solution is transparent, aqueous dispersion is prepared.
The above description of the embodiments is intended to facilitate ordinary skill in the art to understand and use the invention.
Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein general
Principle is applied in other embodiments without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments, ability
Field technique personnel announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be of the invention
Within protection scope.
Claims (10)
1. a kind of preparation method of aqueous dispersion, which is characterized in that it is molten that styrene-maleic anhydride copolymer is dissolved in inertia
In agent, monomethyl polyethers and catalyst is added;It is heated to 60~110 DEG C, reacts 2.5~6.0 hours, boil off solvent, in addition
Neutralizing with agent to pH value is 6.0~8.0, then mixes and stir evenly with thinner, wetting agent, and aqueous dispersion is prepared.
2. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the styrene-Malaysia
The weight average molecular weight of acid anhydride copolymer is 2000~10000, and molecular weight distributing index is between 1.0~2.0, the structure of copolymer
For any one of trackless, block or alternating structure.
3. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the atent solvent is third
(boiling point is lower than 100 to the volatile solvent of the low boiling point that ketone or ethyl acetate etc. are not reacted with styrene-maleic anhydride copolymer
℃)。
4. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the monomethyl polyethers is
The molar ratio of the block copolymer of propylene glycol and ethylene glycol, propylene glycol and ethylene glycol is 1:1~6, and by methyl in ethylene glycol one
Side seal end, number-average molecular weight are 500~3000.
5. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the catalyst is to first
Base benzene sulfonic acid.
6. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the styrene-Malaysia
The molar ratio of the molal quantity of maleic anhydride and monomethyl polyethers is 1:0.5~1.5 in acid anhydride copolymer, is acted in catalyst
Lower generation main polymer styrene-maleic acid polyether ester, the additional amount of catalyst are the 3wt% of reactant weight.
7. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the neutralizer is hydrogen-oxygen
Change the aqueous solution or alcoholic solution of potassium, ammonium hydroxide or triethanolamine.
8. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the thinner be with
The nonionic surface active agent class substance for reducing system viscosity, including but not limited to lauryl amine polyoxyethylene ether or laruyl alcohol
Polyoxyethylene ether.
9. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the wetting agent is can
The surface of pigment microscopic particles is set to be easier to the auxiliary agent of wetting, the wetting agent for being Hydropalat 875 including the commercially available trade mark.
10. a kind of preparation method of aqueous dispersion according to claim 1, which is characterized in that the thinner and profit
The additive amount of humectant is 0~30wt%.
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