CN1878835A - Aqueous compositions - Google Patents
Aqueous compositions Download PDFInfo
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- CN1878835A CN1878835A CNA2005800011397A CN200580001139A CN1878835A CN 1878835 A CN1878835 A CN 1878835A CN A2005800011397 A CNA2005800011397 A CN A2005800011397A CN 200580001139 A CN200580001139 A CN 200580001139A CN 1878835 A CN1878835 A CN 1878835A
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/54—Polycondensates of aldehydes
- C08G18/548—Polycondensates of aldehydes with ketones
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/703—Isocyanates or isothiocyanates transformed in a latent form by physical means
- C08G18/705—Dispersions of isocyanates or isothiocyanates in a liquid medium
- C08G18/706—Dispersions of isocyanates or isothiocyanates in a liquid medium the liquid medium being water
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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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/102—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds
- C09D11/103—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions other than those only involving unsaturated carbon-to-carbon bonds of aldehydes, e.g. phenol-formaldehyde resins
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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
- C09D11/00—Inks
- C09D11/16—Writing inks
- C09D11/18—Writing inks specially adapted for ball-point writing instruments
-
- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/32—Inkjet printing inks characterised by colouring agents
- C09D11/322—Pigment inks
-
- 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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/001—Pigment pastes, e.g. for mixing in paints in aqueous medium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Paints Or Removers (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to aqueous compositions comprised of: a) colorants and/or fillers; B) functionalized aqueous ketone, ketone/aldehyde or urea/aldehyde resin dispersions; C) optionally, additional binding agents and/or; D) auxiliary and accessory agents.
Description
The present invention relates to aqueous composition, wherein contain A) tinting material and/or filler, the B) ketone resin of functionalization, ketone/urea formaldehyde or urea/urea formaldehyde water dispersion, and C) other tackiness agent and/or D when needing) assistant agent and additive.
The polycondensation that generates ketone resin, ketone/urea formaldehyde and/or urea/urea formaldehyde be known (Ulmann ' s Encyclopedia of Industril Chemistry.VCHVerlagsgesellschaft mbH Weinheim 1993, Vol.23, PP.99-105).This resinoid is generally water insoluble.
DE-A 25 42 090 has described the water-soluble cpds that has sulfonic acid group, and is different with method of the present invention, and this compound can be obtained through the associating polycondensation by naphthenone, formaldehyde and basic metal hydrosulphite.
DE-A 31 44 673 has showed it is the water-soluble polycondensation product that the association response of the compound by ketone, aldehyde and introducing acidic-group obtains equally.Back one examples for compounds is the salt of sulphite and thionamic acid, Padil and phosphoric acid.
DE-A 25 42 090 and DE-A 31 44 673 have prepared the product that contains ionogen (for example Na ion).But one of effect of this resin is the corrosion control effect that weakens coating system.
DE 0 617 103 A1 have described polymeric polyisocyanate (a) and molecular weight is the reaction of the dihydroxy compound (b) of 500-5000, compound (b) does not contain the group that can change into ionic group (for example hydroxy-acid group), but contain other functional group, for example ester group or ether (seeing that page 3 17-21 is capable).The urethane that obtains like this is further with the compound (c) that also contains certain group that can change into ionic group except the NCO-active group and glycol when needing or polyvalent alcohol (d) reaction, (d) molecular weight is 60-500, and the functional group (see page 4,5-15 is capable) that does not contain other.This reaction product and a kind of condensation resin reaction is subsequently also introduced in the water.Not mentioned resin as basis of the present invention.
DE-A 24 08 865 has described and can dilute in water or dispersive melamine-formaldehyde-urethane resin.The main component of this urethane resin is (the seeing the 1st section of page 2) that is made of the polycondensation product based on Synolac.Synolac is by carboxylic acid, unsaturated fatty acids and two pure and mild polyvalent alcohol preparations.
DE-A 34 06 473 and DE-A 34 06 474 or EP-A-0 154 835 have described the method for the stable water dispersion of preparation urea/urea formaldehyde and ketone (/ aldehyde) resin respectively; according to this method; with resin melt or its highly spissated solution in the presence of organic protective colloid; add or do not add emulsifying agent, be scattered in the water.A shortcoming of these methods is that organic protective colloid and emulsifying agent hinder the application in paint field of water base ketone (/ aldehyde) resin or urea/urea formaldehyde.Hydrophilic protective colloid and the emulsifying agent that may use can be retained in the coating, therefore make it have secular moisture sensitive.This coating swelling when making moist, forfeiture hardness, its corrosion control effect is impaired.
The dispersible polycondensation product of water has been described in EP 0 838 486 A1, EP 0 838 485, EP 0 498 301, DE 25 42090, DE 31 44 673 and EP 0 154 835.These patent applications are not mentioned and are the special compound of the directed introducing of functionalization widely.
DE 102004034303.9 has described resin water dispersion and its preparation method, and it can obtain by the reaction or the partial reaction of following material:
1) ketone resin of hydroxyl, ketone/urea formaldehyde, urea/urea formaldehyde or its hydrogenated derivatives and
2) isocyanic ester and/or the polymeric polyisocyanate of at least a modification of at least one free NCO group are arranged, it can obtain by at least a isocyanic ester and/or polymeric polyisocyanate and compound reaction, this compound except wetting ability or potential hydrophilic radical, also have at least one can with the functional group of isocyanate groups reaction, and also have at least one hydrophilic radical and/or a potential hydrophilic radical
3) and at least aly have and with the functional group of isocyanic ester radical reaction and to have the compound of other functional group,
Subsequently with this resin (being neutralized when needing) and water combination.
An object of the present invention is exploitation such as aqueous compositions such as pigment paste, coating material and printing-inks, they are based on ketone, ketone/aldehyde or the urea/urea formaldehyde dispersion of functionalization, film forming pigment paste resin for example, and being in harmonious proportion very with bright color, dark colour is characteristics.The said composition plan contains the lower molecular weight dispersing auxiliary of extremely low ratio, and enough stable when storing.
According to these requirements, as this target on basis of the present invention unexpectedly by in the presence of the water dispersion that below at least a, describes in detail with tinting material and/or fillers dispersed and accomplished.
Different with the known architectures in the prior art, aqueous composition of the present invention contains the lower molecular weight dispersion agent and the wetting agent of low ratio, and it is extremely low that its ratio will keep, and this is particularly owing to the reason of cost.In addition, different with above-mentioned assistant agent, they have good film forming character.Said composition is substantially free of formaldehyde.
Composition of the present invention can be used for water base coating material especially, and for example trowel is coated with compound, whole coating materials, base paint and/or top coating, and printing-ink.Their purposes is not limited to for example coating of metal, plastics, paper, cardboard, textiles, leather or timber of particular substrate.The present composition can be used for indoor and outdoor all thinkable application.
The invention provides aqueous composition, it mainly contains
A) at least a tinting material of 1-70% weight and/or filler and
B) water dispersion of the ketone resin of at least a functionalization of 30-99% weight, ketone/urea formaldehyde or urea/urea formaldehyde and
C) the another kind of at least aqueous-based adhesive of 0-69% weight and
D) at least a assistant agent of 0-69% weight,
Component A) to D) quantity sum total be 100% weight.
Have been found that the following component A that contains) to D) composition, for example coating material and printing-ink meet all relevant criterion.
Component A)
Component A as center of the present invention component), its consumption is a 1-70% weight, preferred 10-40% weight.All tinting material and/or fillers that are used in varnish, paint and the printing-ink industry all are suitable in principle.They will be according to color situation and requirement, and for example, tone, brightness, saturation ratio, transparency, obscurity, photostabilization, bleeding resistance wait to be selected.
That uses has mineral dye and a filler; for example; milori blue; titanium dioxide; ferric oxide; metallic pigment; pigment carbon black; carbonate (chalk for example; the levigated Wingdale; calcite; rhombspar and barium carbonate); vitriol (barite for example; process white and calcium sulfate); silicate (talcum for example; pyrophyllite; chlorite; mica; kaolinite; slate flour; feldspar; sedimentary Ca; Al; Ca/Al and Na/Al silicate); silica is (for example quartzy; fused quartz; cristobalite; diatomite; precipitation and/or fumed silica); glass powder; oxide compound (for example oxide compound of the oxide compound of magnesium and oxyhydroxide and aluminium and oxyhydroxide); and pigment dyestuff; isoindole for example; azo and phthalocyanine pigment; metal effect pigments (aluminium for example; copper; copper/zinc and zinc pigment; the oxidation bronze; ferric oxide-aluminium pigment); interference pigment and pearly pigment (metal oxide-pigments, mica for example; Bismuth Oxychloride; white lead carbonate; pearlescence or micronised titanium dioxide; strip graphite; the strip ferric oxide); with PVD membrane process or the multi-layer effect pigment that obtains with CVD (chemical vapour deposition) method, and liquid crystal (polymkeric substance) pigment.Also can use dyestuff.In " R mpp Lexikon, Lacke and Druckfarben " (Dr.UlrichZorll compiles, Georg Thieme Verlag, Stuttgart, 1998), listed the compilation of the pigment that uses.
B component)
B component) be basal component of the present invention, its consumption is a 30-99% weight, preferred 30-60% weight.As B component), can use the resin water dispersion that can obtain by the reaction or the partial reaction of following material.
I) a kind of ketone resin of hydroxyl, ketone/urea formaldehyde, urea/urea formaldehyde or its hydrogenated derivatives and
II) at least a isocyanic ester and/or the polymeric polyisocyanate that contains the modification of at least one free NCO group, it can obtain by at least a isocyanic ester and/or polymeric polyisocyanate and compound reaction, this compound is except wetting ability or potential hydrophilic radical, contain at least one can with the functional group of isocyanate groups reaction, and contain at least one wetting ability and/or potential hydrophilic radical.
III) have respond active group and contain at least a compound of other functional group of isocyanate group,
Subsequently with this resin or resin that neutralized and water combination.
All resins of statement all are suitable as component I among DE-A 102,004,005 208.5 and the DE-A 10 2,004 005 204.7).Preferred ketone/urea formaldehyde, urea/urea formaldehyde, phenol/urea formaldehyde and the hydrogenated derivatives thereof that uses hydroxyl.II) mixture of hydrophilic modifying by (gathering) isocyanic ester and/or different (gathering) isocyanic ester reacts with the compound with (except that hydrophilic or potential hydrophilic radical) at least one functional group (for example OH or NH) that can react with isocyanate groups and at least one wetting ability and/or potential wetting ability (that is, becoming hydrophilic after the neutralization) group to be finished.This type of is used for the ester modified examples for compounds of polyisocyanate is aminocarboxylic acid, hydroxyl sulfoacid, thionamic acid and hydroxycarboxylic acid.
Hydrophilic modifying also can carry out with the compound that has been neutralized.Hydroxycarboxylic acid, for example dimethylol propionic acid, dimethylolpropionic acid, two (hydroxyphenyl) valeric acid and/or hydroxy new pentane acid are suitable especially because when in volatile alkali (for example amine) and the time, they demonstrate strong hydrophilic interaction, but suddenly descend in volatile alkali evaporation back wetting ability; In this way, coating softening or whiting at the Shi Buhui that makes moist.In addition, dihydroxy first propionic acid and 2-[(2-aminoethyl) amino] ethyl sulfonic acid, to carry out (potential) hydrophilic modifying to two hydrophobicity polymeric polyisocyanates desirable especially because of it.
Suitable preparation II) polymeric polyisocyanate preferably has the polymeric polyisocyanate that 2-4 functionality, molar mass are lower than 800g/mol and have the isocyanate groups that connects with aliphatic series, (ring) aliphatic series and/or alicyclic form, those that usually in polyurethane coated material field, use and composition thereof for example: 1-isocyanato-3,3,5-trimethylammonium-5-isocyanato methyl cyclohexanol (isophorone diisocyanate; IPDI), trimethyl hexamethylene diisocyanate (TMDI), 1,6-two isocyanato hexanes (HDI), two (4-isocyanato base) methane (H
12MDI) reach at DE-A 24 56 469 the 5th and the 6th page of other polymeric polyisocyanate of listing.
The suitable oligopolymer that can obtain and obtain according to prior art by monomeric isocyanic ester (polyisocyanates) in addition, these oligopolymer are at for example Journal f ü lpraktischeChemie 336 (1994), 185-200 and Farbe und Lack 100,5 (1994), 330-335 reaches in the reference of wherein quoting introduction.They are the polymeric polyisocyanates with biuret, uretdione or isocyanurate structure, and the latter can obtain by monomeric cyclic trimerization.In addition, other suitable polymeric polyisocyanate is the product as polyvalent alcohol and/or amine and monomeric diisocyanate, for example as the polymeric polyisocyanate of TriMethylolPropane(TMP) and isophorone diisocyanate reaction product.
Also can utilize polyethers to carry out the hydrophilization of nonionic, for example, polyethers can with above-mentioned polymeric polyisocyanate and component I) reaction.
Especially preferably by dimethylol propionic acid and/or 2-[(2-amino-ethyl) amino] ethyl sulfonic acid or derivatives thereof and IPDI and/or H
12MDI and/or TMDI and/or HDI are by the polymeric polyisocyanate II of the hydrophilic modifying of 1: 2 mol ratio formation).
Function ingredients III) mixture that can be by (gathering) isocyanic ester and/or different (gathering) isocyanic ester with have at least a can the reaction and introduce with the functional group's (for example OH or NH) of isocyanate groups reaction compound, this compound also has another functional group at least, so stay next NCO functional group at least, subsequently with II) reaction before or after with I) reaction.Component III) also can during the preparation preadduct, original position make.In principle, except the NCO active group, also have another functional group's aliphatic series or aromatic alcohol and/or amine or aromatics or the heteroaromatic ring system can be as component III) use.The preferred embodiment of this compounds is dimethylamino propylamine, diethanolamine, pyrrolidone and/or hydroxy new pentane acid.The unsaturated part of introducing described in DE-A 103 38 560, DE-A 103 38 562, DE-A 10 2,004 005 208.5 and DE-A 10 2,004 005 207.7 is not a research contents of the present invention.
I) with II) and/or reaction III) can become piece ground (solvent-free) to carry out, perhaps preferably, in the presence of suitable secondary solvent, carry out.The quantity of organic solvent is lower than 20% weight, preferably is lower than 10% weight, more preferably less than 2% weight.When using secondary solvent, preferred solids content is the 50-95% quality, more preferably the 60-80% quality.
Suitable secondary solvent preferably under 1013hPa boiling point be lower than 100 ℃ solvent, they can separate with the aqueous based systems of final generation fully with distillation method, residual volume is low to moderate 0.5% quality, and can reuse, for example acetone, methylethylketone or tetrahydrofuran (THF), perhaps in due course, high boiling solvent, they are retained in the aqueous systems, for example butyl glycol, ethyl Diethylene Glycol or N-Methyl pyrrolidone.Preferred boiling point is lower than 100 ℃ secondary solvent, does not contain the therefore pure water dispersion compatible especially with environment of solvent because they can make.Boiling point surpasses 100 ℃ the high boiling solvent (suitably time in proportion) or the use of solvent mixture, though technical feasible, and inadvisable also non-effort target.An advantage of the inventive method particularly in, in the water-based resin dispersion that finally obtains, can not contain organic solvent fully, but still obtain the solid dispersion of stable height.
At an embodiment preferred i) in
As component III), for example prepare the affixture of the functional NCO-active ingredient of 1mol vulcabond and 1mol, use suitable solvent and appropriate catalyst when needing.
As component I I), can prepare 2mol vulcabond and 1mol dimethylol propionic acid and/or 2-[(2-amino-ethyl) amino] affixture of ethyl sulfonic acid or derivatives thereof, use suitable solvent and appropriate catalyst in the time of suitably.
The product of preparation respectively is added to ketone, ketone/aldehyde or urea/urea formaldehyde or its hydrogenated derivatives I of hydroxyl) solution or melt in and react.
Confirmed the 1mol component I) component III of (according to Mn) and 0.1-10mol, especially 0.25-5mol) reaction is favourable.
Confirmed the component I of 1mol) and the component I I of reaction product III) (according to Mn) and 0.1-1.0mol, preferred 0.3-0.75mol) reaction is favourable.
Temperature of reaction is selected according to component reactive behavior to each other.For all reactions steps, 30-245 ℃ temperature is suitable, preferred 50-140 ℃.
If desired, can neutralize with suitable neutralizing agent earlier, then the neutral reaction product is dispersed in the water.Or, can directly in water/neutralizing agent mixture, disperse.
If there is solvent, can after reaction finishes, it be separated when needed, generally obtain the solution or the dispersion of product of the present invention in this situation.
An embodiment preferred ii) in.
As component I I), for example can prepare 2mol vulcabond and 1mol dimethylol propionic acid and/or 2-[(2-amino-ethyl) amino] affixture of ethyl sulfonic acid or derivatives thereof, use suitable solvent and appropriate catalyst in the time of suitably.
This product is added to ketone, ketone/aldehyde or urea/urea formaldehyde or its hydrogenated derivatives I of hydroxyl) and component III) and the solution of other polymeric polyisocyanate or melt in and react.
Confirmed to make the 1mol component I) component III of (based on Mn) and 0.1-10mol, especially 0.25-5mol) reaction is favourable.
Confirmed to make component I and the III of 1mol) reaction product (based on Mn) and 0.1-1.0mol, the component I I of preferred 0.3-0.75mol) reaction is favourable.
Temperature of reaction is selected according to each component reactive behavior to each other.For all reactions steps, it is suitable that 30-245 ℃ temperature has been proved to be, preferred 50-140 ℃.
If desired, can neutralize with suitable neutralizing agent earlier, the reaction product that will neutralize is scattered in the water then.Or, can directly in water/neutralizing agent mixture, disperse.
If there is solvent, then can after reaction finishes, it be separated when needed, obtain the solution or the dispersion of product of the present invention usually in this situation.
If desired, can use appropriate catalyst to prepare resin of the present invention.Suitable compound is all compounds of known acceleration NH-or OH-NCO reaction in the document, for example diazabicyclooctane (DABCO) or dibutyl tin dilaurate (DBTL), for example titanium ester, and bismuth salt.
If hydrophilization reagent is introduced a kind of potential hydrophilic radical in polymeric polyisocyanate, for example carboxyl or tertiary amine group, then this group can change into Ionized hydrophilic radical by neutralization subsequently.
According to the present invention according to anion-modified embodiment i) and ii) the neutralization reaction of the resin of preparation can carry out for example ammonia or organic amine with organic and mineral alkali.Preferred primary amine, secondary amine and the tertiary amine of using, for example, ethamine, propylamine, dimethylamine, dibutylamine, hexahydroaniline, benzylamine, morpholine, piperidines and trolamine.Particularly preferably be the volatility tertiary amine, especially dimethylethanolamine, diethylethanolamine, 2-dimethylamino-2-methyl isophthalic acid-propyl alcohol, triethylamine, tripropyl amine and Tributylamine.
In and quantity by the potential in the polymeric polyisocyanate of hydrophilic modifying can in and the decision of the quantity of group, be preferably in the stoichiometry and the 50-130% of required dosis neutralisata.In the situation of cationic hydrophilic system, use suitable acid in the same way, for example acetate, formic acid, phenylformic acid or lactic acid neutralize.
Before adding water, can be with I), II) and reaction product III), in the time of suitably with other resin of hydrophilization not, or with other the component of water-soluble or water-dilutable, be mixed together then and disperse together.Utilize this measure, can obtain solids content technically easily and surpass 35% quality, preferred 35-40% quality is until the solid dispersion of the height of about 50% quality.
Component C)
Aqueous-based adhesive C) be basal component of the present invention, its consumption is a 0-69% weight, preferred 0-60% weight.The preferred use is selected from following aqueous-based adhesive: urethane, polyacrylic ester, polyethers, polyester, Synolac, polymeric amide, casein, ether of cellulose, derivatived cellulose, polyvinyl alcohol and derivative, polyvinyl acetate, polyvinyl chloride, Polyvinylpyrolidone (PVP), rubber, natural resin, hydrocarbon resin (coumarone resin for example, inden resin and cyclopentadiene resin), terpine resin, maleic acid resin, resol, phenolic aldehyde/urea-formaldehyde resin, aminoresin (for example melamine resin and benzoguanamine resin), epoxy acrylic resin, Resins, epoxy, silicon ester and alkalimetal silicate (for example water glass) with and/or silicone resin and/or fluoropolymer.Aqueous-based adhesive can external crosslinking and/or self-crosslinking, dry air (physical dryness) and/or oxidative cure.
Component D)
Component D) be basal component of the present invention, its consumption is a 0-69% weight, preferred 0-60% weight.Suitable component D) is assistant agent and additive, for example, co-inhibitor, organic solvent, surfactant, oxygen scavenqer and/or free-radical scavengers, catalyzer, photostabilizer, colored brightening agent, photosensitizer and light trigger are used to influence the additive (for example thixotropic agent and/or thickening material) of rheological property, flow control agent, anti, defoamer, static inhibitor, lubricant, wetting agent, dispersion agent, sanitas (comprising mycocide and/or biocides), thermoplastic additive, softening agent, matting agent, fire retardant, in execute releasing agent, filler and/or whipping agent.
By component A) to D) preparation composition, for example pigment slurry, coating material and printing-ink:
By each component thorough mixing under 20-80 ℃ temperature being prepared composition (" Lehrbuch der Lacktechnologie ", Th.Brock, M.Groteklaes, P.Mischke, V.Zorll (ed.), Vincentz Verlag, Hanover, 1998, P.229ff.).
If suitable, before mixing, earlier non-liquid component is dissolved in the suitable solvent or water, under agitation add all the other components then.In the situation of for example pigment and/or filler, disperse.
The present composition can be used for water-base pigment cream, ballpoint pen oil, ink, rumbling compound, lustering agent, trowel especially and be coated with compound, makeup, sealing agent and/or insulating compound, whole coating materials, base paint and/or top coating, and printing-ink.Substrate coated and/or printing can comprise metal, plastics, paper, cardboard, inorganic materials (for example pottery, stone, concrete and/or glass), textiles, fiber, braided material, leather and/or synthetic materials (as leatheroid), timber, plastics and/or composite material film, for example ironed film of aluminium lamination.Said composition can be used for indoor and outdoor the purposes that might expect, for example building protection, automobile, coil coating, can lacquer, textiles finishing, wood coating, decorative use etc.This based composition also is suitable for binding agent, the textiles that for example bonds, leather, paper and materials similar.
The distinguishing feature of the present composition is the very dark color of color harmony that becomes clear.Said composition contains the lower molecular weight dispersing auxiliary of low levels, and in stable upon storage.The quantity of lower molecular weight dispersing auxiliary and wetting agent is lower than 10% weight, preferably is lower than 7% weight, more preferably less than 5% weight.
The outstanding characteristic of the present composition is extra high initial drying and finish-drying speed, good resistance to blocking, good water resisting property and with the elasticity bonded high rigidity of excellence.Flowing property excellence, and surperficial zero defect, for example pit and wetting defective.
The exsiccant curing and/or the crosslinked film that are obtained by said composition have good adhesive property to following coating; Also demonstrate being coated with the favourable influence that interlayer adheres to for the coating that is positioned on the above-mentioned coating.
The solids content of the present composition is 10-80%, preferred 20-60%.Formaldehyde content in the composition is less than 100ppm, preferably is lower than 20ppm, more preferably less than 1ppm.
Following examples are to be used for further specifying the present invention, rather than limit its range of application:
Embodiment 1) B component) preparation
(1) the preparation polymeric polyisocyanate II of hydrophilic modifying), affixture III) and and I) reaction
The mixture of dibutyl tin dilaurate (DBTL) acetone soln of 60g dimethylol propionic acid (DMPA), 217g acetone and 0.3g 10% (quality) is under agitation mixed with different Buddhist diketone two isocyanic acids of 201g, and its speed should make this thermopositive reaction keep control easily.Continue down to stir at 60 ℃ subsequently, dissolve fully until DMPA, the NCO number of solution is brought down below 8.4%NCO (measuring according to DIN 53185).
45.6g IPDI is mixed under nitrogen with the 17.4g pyrrolidone, 80 ℃ of stirrings, is 13.6% until NCO content with mixture.
Be cooled to after the room temperature, two kinds of precursors are mixed under nitrogen, adding is dissolved in the ketone/urea formaldehyde (OHN 310mg KOH/g, Kunstharz SK, Degussa AG) of the 544g hydroxyl in the 508g acetone and the 10%DBTL acetone soln of 1.24g.Mixture is stirred under reflux temperature, be lower than 0.15% until NCO content.
(2) dispersion modified resin I)
The solution of preparation among the 250g (1) is used the neutralization of 6.8g triethylamine in room temperature with under stirring, add the complete deionized water of 457g, under high degree of agitation, disperse.Remove assisted solution acetone and a part of water under decompression, obtain slightly opalescent resin dispersion shelf-stable, tiny, its solids content is about 27.0% quality, and pH is 8.2, and viscosity is about 90mPas.
Embodiment 2) B component) preparation
(1) the preparation polymeric polyisocyanate II of hydrophilic modifying), affixture III) and and I) reaction
The mixture of 10% (quality) dibutyl tin dilaurate (DBTL) acetone soln of 51g dimethylol propionic acid (DMPA), 253g acetone and 0.3g is under agitation mixed with the 253g isophorone diisocyanate, and its speed should make this thermopositive reaction keep control easily.Continue to stir at 60 ℃ subsequently, dissolve fully until DMPA, the NCO number of solution is reduced to 11.8%NCO following (measuring according to DIN 53185).
Be cooled to after the room temperature, the 10%DBTL acetone soln of precursor with ketone/urea formaldehyde (OHN 310mg KOH/g, Kunstharz SK, Degussa AG) that is dissolved in the 480g hydroxyl in the 400g acetone and 0.5g mixed.This mixture is stirred under reflux temperature, be lower than 1.3% until NCO content.Be added in the 38.3g diethanolamine in the 31.2g acetone subsequently, continue stirring and be lower than 0.15% until NCO content.
(2) dispersion modified resin I)
The solution of preparation is used the neutralization of 6.3g triethylamine in room temperature with under stirring among the 250g (1), adds the complete deionized water of 335g, disperses under high degree of agitation.Secondary solvent acetone and a part of water are removed in decompression, obtain shelf-stable, tiny and slightly opalescent resin dispersion, and its solids content is about 32.9% quality, and pH is 8.3, and viscosity is about 260mPas.
Preparation of compositions and research
Be research pigment wetting character, will be with Spezialschwarz 4 (carbon blacks; Degussa AG) partly replaces for the dispersing auxiliary in the based coating prescription with the dispersion agent for preparing among two embodiment.
Pre-dispersed:
5 minutes, Pendraulik LM 34 Laboratary type high speed dispersors, 4000rpm (impeller diameter 40mm)
Disperse:
60 minutes, Skandex dispersion machine BA-S, 540g Chromanit steel ball (diameter 3mm), cooling settings 2
Coating:
Use spreading rod (slit height 200 μ m) to be coated on the sheet glass.
Drying conditions: dried under the room temperature 30 minutes, following 30 minutes in 80 ℃ in air dry oven.
| Be coated with slurry formulation | To in the same old way | A | B | |
| Deionized water | 40.0g | 40.0g | 40.0g | |
| Tego dispersion agent 760W | Degussa AG | 21.4g | ||
| Embodiment 2 dispersions | 22.8g | |||
| Embodiment 1 dispersion | 27.8g | |||
| Tego Foamex 830 | Degussa AG | 05g | 0.5g | 0.5g |
| AMP 90 | 0.5g | 0.5g | 05g | |
| Spezialschwarz 4 | Degussa AG | 15.0g | 15.0g | 15.0g |
| Amount to | 76.9g | 78.3g | 83.3g | |
| Wetting agent, solid is by Spezialschwarz 4 | 50.0％ | 50.0％ | 50.0％ | |
| Pigment concentration | 12.4％ | 12.3％ | 12.2％ | |
| Dynamic viscosity under the 800s-1 (Haake viscometer VT 550) | 50mPa·s | 40mPa·s | 55mPa·s |
| The blending stock preparation | To in the same old way | A | B |
| To in the same old way | 2.7g | ||
| Pasting A | 2.7g | ||
| Pasting B | 2.9g | ||
| Alberdingk U 710，30％ | 17.3g | 17.3g | 17.1g |
| Amount to | 20.0g | 20.0g | 20.0g |
| Press the pigment concentration (solid) that tackiness agent calculates | 10％ | 10％ | 10％ |
| Size of particles (Grindometer) | ＜10μm | ＜10μm | ＜10μm |
| (Q-Color 35, Pausch) for black number, My for color depth | 242 | 247 | 254 |
| Glossiness, 20 ° | 55 | 59 | 66 |
Claims (38)
1. an aqueous composition mainly contains
A) at least a tinting material and/or the filler of 1-70% weight,
B) water dispersion of at least a functionalization ketone resin, ketone/urea formaldehyde or the urea/urea formaldehyde of 30-99% weight,
C) the another kind of at least aqueous-based adhesive of 0-69% weight and
D) at least a assistant agent of 0-69% weight,
Component A) to D) summation be 100% weight.
2. the aqueous composition of claim 1, wherein the solids content of said composition is 10-80%, formaldehyde content is lower than 100ppm.
3. the aqueous composition of aforementioned each claim, wherein the quantity of organic solvent is lower than 20% weight, and the quantity of lower molecular weight dispersing auxiliary and wetting agent is lower than 10% weight.
4. the aqueous composition of aforementioned each claim wherein uses tinting material and/or filler as component A).
5. the aqueous composition of aforementioned each claim wherein uses pigment, dyestuff and/or filler as component A).
6. the aqueous composition of aforementioned each claim; wherein use independent or the following material of blended as component A: milori blue; titanium dioxide; ferric oxide; metallic pigment; pigment carbon black; carbonate (chalk for example; the levigated Wingdale; calcite; rhombspar and barium carbonate); vitriol (barite for example; process white and calcium sulfate); silicate (talcum for example; pyrophyllite; chlorite; mica; kaolinite; slate flour; feldspar; sedimentary Ca; Al; Ca/Al and Na/Al silicate); silica is (for example quartzy; fused silica; cristobalite; diatomite; precipitation and/or fumed silica); glass powder; oxide compound (for example magnesium oxide and oxyhydroxide; aluminum oxide and oxyhydroxide); and pigment dyestuff (isoindole for example; azo and phthalocyanine pigment); metal effect pigments (aluminium for example; copper; copper/zinc and zinc pigment); the oxidation bronze pigments; ferric oxide-aluminium pigment; interference pigment and pearly pigment (metal oxide-pigments, mica for example; Bismuth Oxychloride; white lead carbonate; pearlescence or micronized titanium dioxide); strip graphite; the strip ferric oxide; by PVD film or the multi-layer effect pigment that makes with CVD (chemical vapour deposition) method, and liquid crystal (polymkeric substance) pigment.
7. aforementioned each a kind of aqueous composition wherein uses a kind of functional resin water dispersion as B component), it can obtain by the reaction or the partial reaction of following material:
I) a kind of ketone resin of hydroxyl, ketone/urea formaldehyde, urea/urea formaldehyde or its hydrogenated derivatives,
II) at least a isocyanic ester and/or the polymeric polyisocyanate that contains the modification of at least one free NCO group, it can obtain by at least a isocyanic ester and/or polymeric polyisocyanate and compound reaction, this compound except that hydrophilic or potential hydrophilic radical, also have at least one can with the functional group of isocyanate groups reaction, and have at least one hydrophilic radical and/or a potential hydrophilic group
III) and at least aly have and with the functional group of isocyanate reaction and to also have the compound of other functional group,
Subsequently with this resin or resin that neutralized and water combination.
8. the aqueous composition of aforementioned each claim, wherein use have at least a can with the functional group of isocyanate reaction and the compound that also has another kind of functional group as being used for preparing resin dispersion B) component III).
9. the aqueous composition of aforementioned each claim wherein, uses the alcohol that also contains another functional group except the NCO active group and/or amine as being used for preparing resin dispersion B) component III).
10. the aqueous composition of aforementioned each claim wherein uses dimethylamino propylamine, diethanolamine, pyrrolidone and/or hydroxypentanoic acid as being used for preparing resin dispersion B) component III).
11. the aqueous composition of aforementioned each claim, wherein be used to prepare resin dispersion B) component III) with the mixture reaction of (gathering) isocyanic ester and/or different (gathering) isocyanic ester, at least one NCO functional group is kept, and subsequently with II) reaction before, among or afterwards and I) reaction.
12. the aqueous composition of aforementioned each claim wherein is used to prepare resin dispersion B) component I I) be with uncle amino alcohol, aminocarboxylic acid, hydroxyl sulfoacid, thionamic acid and/or hydroxycarboxylic acid preparation.
13. the aqueous composition of aforementioned each claim wherein is used to prepare resin dispersion B) component I I) with dimethylol propionic acid and/or 2-[(2-aminoethyl) amino] the ethyl sulfonic acid preparation.
14. the aqueous composition of aforementioned each claim wherein is used to prepare resin dispersion B in order to prepare) component I I), use to have the polymeric polyisocyanate of the molecular weight of 2-4 functionality less than 800g/mol.
15. the aqueous composition of aforementioned each claim wherein is used to prepare resin dispersion B in order to prepare) component I I), use polymeric polyisocyanate or its mixture have with the isocyanate groups of aromatics, aliphatic series and/or the connection of alicyclic form.
16. the aqueous composition of aforementioned each claim wherein is used to prepare resin dispersion B in order to prepare) component I I), use 1-isocyanato-3,3,5-trimethylammonium-5-isocyanato methylcyclohexane (isophorone diisocyanate; IPDI), trimethyl hexamethylene diisocyanate (TMDI), 1,6-two isocyanato hexanes (HDI) and/or two (4-isocyanato hexyl) methane (H
12MDI).
17. the aqueous composition of aforementioned each claim wherein, is used to prepare resin dispersion B in order to prepare) component I I), use polymeric polyisocyanate with connection urea, uretdione or isocyanurate structure.
18. the aqueous composition of aforementioned each claim wherein, is used to prepare resin dispersion B in order to prepare) component I I), use by polyvalent alcohol and/or amine polymeric polyisocyanate with monomeric diisocyanate reaction formation.
19. the aqueous composition of aforementioned each claim is wherein, for preparation is used to prepare resin dispersion B) component I I), using mol ratio is 1: 2 dimethylol propionic acid and isophorone diisocyanate (IPDI).
20. the aqueous composition of aforementioned each claim wherein is preparation B), component I) and II) and III) reaction and be dispersed into piece ground (not solubilizing agent) and carry out.
21. the aqueous composition of aforementioned each claim wherein is preparation B), component I) and II) and III) reaction and be dispersed in a kind of secondary solvent and carry out under existing.
22. the aqueous composition of aforementioned each claim wherein is used to prepare B) the boiling point of secondary solvent under 1013hPa be lower than 100 ℃.
23. the aqueous composition of aforementioned each claim wherein is used to prepare B) secondary solvent be N-Methyl pyrrolidone, acetone or/and methylethylketone or/and tetrahydrofuran (THF).
24. the aqueous composition of aforementioned each claim wherein is used for preparing B with organic or inorganic alkali) neutralization reaction.
25. the aqueous composition of aforementioned each claim wherein uses dimethylethanolamine and/or diethylethanolamine and/or 2-dimethylamino-2-methyl isophthalic acid-propyl alcohol and/or triethylamine and/or ammonia to be prepared B) neutralization reaction.
26. the aqueous composition of aforementioned each claim is wherein for being prepared B) neutralization reaction, use in the stoichiometry and the dosis neutralisata of the 50-130% of aequum.
27. the aqueous composition of aforementioned each claim wherein, is used to prepare B in adding) water before, add earlier one or more water-insolubles or non-water-dilutable component.
28. the aqueous composition of aforementioned each claim wherein uses aqueous-based adhesive as component C).
29. the aqueous composition of aforementioned each claim, the tackiness agent that wherein uses water base, external crosslinking and/or self-crosslinking and/or dry air (physical dryness) and/or oxidative cure is as component C).
30. the aqueous composition of aforementioned each claim wherein uses aqueous-based adhesive as component C), this tackiness agent is selected from following material independent or mixed form: urethane, polyacrylic ester, polyethers, polyester, Synolac, polymeric amide, casein, ether of cellulose, derivatived cellulose, polyvinyl alcohol and derivative, polyvinyl acetate, polyvinyl chloride, polyvinylpyrrolidone, rubber, natural resin, hydrocarbon resin (coumarone resin for example, inden resin and cyclopentadiene resin), terpine resin, maleic acid resin, resol, phenolic aldehyde/urea-formaldehyde resin, aminoresin (for example melamine resin and benzoguanamine resin), Epocryl, Resins, epoxy, silicon ester and/or alkalimetal silicate (for example water glass) and/or silicone resin with and/or fluoropolymer.
31. the aqueous composition of aforementioned each claim wherein uses assistant agent and additive as component D).
32. the aqueous composition of aforementioned each claim wherein uses to be selected from following auxiliary and additive independent or mixed form as component D): co-inhibitor, organic solvent, surfactant, oxygen scavenqer and/or free-radical scavengers, catalyzer, photostabilizer, colored brightening agent, photosensitizer and light trigger, influence the additive (for example thixotropic agent and/or thickening material) of rheological property, flow control agent, anti, defoamer, static inhibitor, lubricant, wetting agent, dispersion agent, sanitas (comprising mycocide and/or biocides), thermoplastic additive, softening agent, matting agent, execute releasing agent in the fire retardant, filler and/or whipping agent.
33. a method for preparing aqueous composition, said composition mainly contains
A) at least a tinting material and/or the filler of 1-70% weight,
B) aqueous based dispersions of at least a functionalization ketone resin, ketone/urea formaldehyde or the urea/urea formaldehyde of 30-99% weight,
C) the another kind of at least aqueous-based adhesive of 0-69% weight and
D) at least a assistant agent of 0-69% weight,
Component A) to D) the weight percentage sum be 100%, this method be with each component under+20 to+80 ℃ temperature by stirring and/or disperseing thorough mixing.
34. the aqueous composition in aforementioned at least one the claim is as the application of water-base pigment slurry, coating material and/or printing-ink.
35. the aqueous composition in aforementioned at least one the claim is coated with the application of compound, makeup, sealing agent, insulating compound, whole coating materials, base paint, top coating or printing-ink as water-base ballpoint slurry or ink, pigment paste, rumbling compound, lustering agent, trowel.
36. the coating of the aqueous composition of aforementioned at least one claim and/or the purposes of printed matter.
37. the aqueous composition of aforementioned at least one claim applies and/or the purposes of the goods that the following material of printing is made: metal, plastics, paper, cardboard, inorganic materials (for example pottery, stone, concrete and/or glass), textiles, fiber, braided material, leather and/or synthetic materials (for example leatheroid), timber, the film of plastics and/or mixture (for example ironed film of aluminium lamination).
38. the goods that apply with the aqueous composition of aforementioned at least one claim.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE200510006296 DE102005006296A1 (en) | 2005-02-11 | 2005-02-11 | Aqueous compositions |
| DE102005006296.2 | 2005-02-11 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1878835A true CN1878835A (en) | 2006-12-13 |
Family
ID=35929551
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2005800011397A Pending CN1878835A (en) | 2005-02-11 | 2005-12-20 | Aqueous compositions |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN1878835A (en) |
| DE (1) | DE102005006296A1 (en) |
| WO (1) | WO2006084523A1 (en) |
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| DE4309079A1 (en) * | 1993-03-20 | 1994-09-22 | Basf Ag | Aqueous dispersion of a polyurethane and a condensation resin |
| DE19643704A1 (en) * | 1996-10-23 | 1998-04-30 | Huels Chemische Werke Ag | Aqueous resin dispersions |
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| DE102004034303A1 (en) * | 2004-07-15 | 2006-02-09 | Degussa Ag | Functionalized, aqueous resins |
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2005
- 2005-02-11 DE DE200510006296 patent/DE102005006296A1/en not_active Withdrawn
- 2005-12-20 CN CNA2005800011397A patent/CN1878835A/en active Pending
- 2005-12-20 WO PCT/EP2005/056981 patent/WO2006084523A1/en not_active Application Discontinuation
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Also Published As
| Publication number | Publication date |
|---|---|
| DE102005006296A1 (en) | 2006-08-24 |
| WO2006084523A1 (en) | 2006-08-17 |
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