Stabilized water dispersions of curing agent

FIELD: chemistry.

SUBSTANCE: scope of invention covers stabilized water dispersions of curing agent suitable for coating preparation. Dispersion dispersed in water contains the following components: A1) at least one organic polyisocyanate with isocyanate groups connected in aliphatic, cycloaliphatic, araliphatic and/or aromatic manner, A2) ionic or potentially ionic and/or non-ionic substance, A3) blocking agent, B) stabilizer containing a) at least one amine with structural element of common formula (I) without any hydrazide group, b) substance with formula (IV) .

EFFECT: resistance to thermal yellowing increases.

6 cl, 5 tbl, 11 ex

 

The invention relates to new, stable to thermopolae, dispersible in water or water-soluble blocked polyisocyanates, their preparation and use.

Industrial coatings are increasingly used aqueous one-component and two-component polyurethane system in combination with blocked isocyanates. This often leads to an thermopolae caused by the blocking means, which is undesirable.

However, to date known such a blocking means, which cause only a slight thermopolae, such as, for example, 3,5-dimethylpyrazole, 1,2,4-triazole and ε-caprolactam. However, their disadvantage is that they are either costly, cannot always be used due to certain properties of the products. For example, the blocked polyisocyanates based on HDI 1,2,4-triazole leads to highly crystallized products that are not suitable for use in varnishes and coatings. ε-Caprolactam for comparison has a markedly higher temperature release and therefore also not suitable for all applications.

From patent US-A 5216078 known stabilizing agent, which reduces thermopolae blocked polyisocyanates, in particular blocked by butanonoxime isocyanate is in, and if we are talking about the adduct with hydrazine.

In EP-A 0829500 as a stabilizing means for blocked polyisocyanates is described, the combination of connections, and one of the compounds has at least 2,2,6,6-tetramethylpiperidinyloxy the remainder, the so-called SSA-balance (svedeteliami hindered amine), and the other structure hydrazides.

The disadvantage of the above-mentioned stabilized blocked polyisocyanates is that they are only suitable for solvent-containing paints and coatings and are not suitable for water systems.

Getting dispersible in water or water-soluble blocked polyisocyanates generally known and described, for example, in patents DE-A 2456469 and DE-A 2853937. However, the problem of thermopolae for these systems is not solved in a satisfactory manner.

The objective of the present invention is therefore the preparation of isocyanates, which, on the one hand, are blocked, and can dispergirujutsja in water or dissolve in water and, on the other hand, a sufficiently stable to possible thermopolae and suitable for structuring water one - and two-component binder or varnish especially on the basis of polyurethane and/or polyacrylate.

However, it is found that gidratirovannye and blocking the nye polyisocyanates, capable of dispergirujutsja in water or soluble in water due to a particular combination of hydrazides and some sterically obstructed amines, can significantly protect against thermopolae.

The subject of this invention is dispersible in water composition of a crosslinking agent containing

A) at least one blocked and gidratirovannyi the polyisocyanate

B) at least one stabilizer, containing a) at least one amine with a structural unit of General formula (I),

no one hydrazide group,

b) at least one connection with the structural unit of General formula (II)

C) if necessary, different from a) and b) a stabilizing component, and

C) if necessary, an organic solvent.

Component a) of the composition, cross-linking means is a reaction product of at least one organic MDI A1) with isocyanate groups connected with aliphatic, cycloaliphatic, alifaticheskimi and/or aromatic residue, ionic or potentially ionic and/or nonionic compounds A2) and blocking means A3). Potentially ionic in the context of this invention means that the compound has a group which is capable of images of the TB ion group.

The composition of a crosslinking agent according to this invention contains from 78,0 to 99.8 wt.%, better from 84,0 to 99.6 wt.%, even better from 90,0 up to 99.0 wt.% component A), from 0.2 to 22.0 wt.%, better from 0.4 to 16.0 wt.%, even better from 1.0 to 10.0 wt.% component B), and sum of components is 100 wt.% and makes all the solids content of the composition of a crosslinking agent according to this invention.

The subject of this invention is also an aqueous solution or dispersion containing the composition of a crosslinking agent according to the invention, characterized in that the solution or dispersion, the solids content is from 10 to 70 wt.%, better from 20 to 60 wt.% and better still from 25 to 50 wt.%, and the proportion of the component In the total composition, preferably less than 15 wt.% and especially preferably less than 5 wt.%.

In the calculation on the total solids content of the composition of a crosslinking agent according to this invention contains from 0.1 to 11.0 wt.%, better from 0.2 to 8.0 wt.%, better still from 0.5 to 4.0 wt.% Amin (a) with a structural unit of formula (I), from 0.1 to 11.0 wt.%, better from 0.2 to 8.0 wt.%, better still from 0.5 to 4.0 wt.% connection b) with a structural unit of formula (II) and, if necessary, from 0 to 5.0 wt.% another, different from a) and b), stabilizer).

Polyisocyanate component a) has an (average) NCO functionality of from 2.0 to 5.0, preferably from 2.3 on the 4,5, the content of isocyanate groups (non-blocked and blocked) from 5.0 to 27.0 wt.%, preferably of 14.0 to 24.0 wt.%, and a content of Monomeric diisocyanates of less than 1 wt.%, preferably less than 0.5 wt.%. Isocyanate groups in the polyisocyanate component (a) of the composition according to this invention there are at least 50%, ideally not less than 60% and better still at least 70% in blocked form.

Suitable polyisocyanates A1) is obtained by modifying simple aliphatic, cycloaliphatic, alifaticheskih and/or aromatic diisocyanates, constructed from at least two diisocyanates of the polyisocyanates with uretdione, which, allophanate, biuret, iminoimidazolidine and/or oxidization structure, which is described, for example, in the Journal of Practical Chemistry, 1994, vol 336, str-200.

Suitable diisocyanates for more polyisocyanates A1) are all available by vosganian or using bestsennyh ways, for example, by thermal decomposition of urethanes, diisocyanate with a molecular weight in the range from 140 to 400 and isocyanate groups associated with the aliphatic, cycloaliphatic, analiticheskie and/or aromatic residues, such as 1,4-diisocyanatobutane, 1,6-diisocyanatohexane (HDI), methyl-1,5-diisocyanatobutane, 1,5-diisocyanato-2,2-dimethylpentane, 2,2,4 - or 2,4,4-trimethyl-1,6-diisocyanatohexane, 1,10-diisocyanatohexane, 1,3 - and 1,4-diisocyanatohexane, 1,3 - and 1,4-bis-(isocyanatomethyl)-cyclohexane, 1-isocyanato-3,3,5-trimethyl-5-isocyanatomethyl (isophorondiisocyanate, IPDI), 4,4'-diisocyanatohexane, 1-isocyanato-1-methyl-4(3)-isocyanato-methylcyclohexane, bis-(isocyanatomethyl)-norbornane, 1,3 - and 1,4-bis-(2-isocyanato-prop-2-yl)-benzene (TMXDI), 2,4 - and 2,6-diisocyanates (TDI), 2,4'- and 4,4'-diisocyanatobutane, 1,5-diisocyanatomethyl or any mixtures of these diisocyanates.

In the case of the starting components A1) preferably it is about the polyisocyanates or mixtures of polyisocyanates mentioned type exclusively with isocyanate groups associated with aliphatic and/or cycloaliphatic groups.

Particularly preferred source components A1) are polyisocyanates or mixtures of polyisocyanates structure isocyanurate and/or biureta based on HDI, IPDI and/or 4,4'-diisocyanatohexane.

Suitable compounds of component A2) are ionic or potentially ionic and/or nonionic compounds.

Non-ionic compounds are, for example, monovalent simple polyalkylene alcohols having on average 5 to 70, preferably from 7 to 55 ethyleneoxide chains on the molecule, which itself is on its own available known method by alkoxysilane suitable starting compounds (for example, in the Encyclopedia of technical chemistry Ullman (Ullmanns Encyclopadie der technischen Chemie), 4th edition, t, p.31-38 (in Russian) Chemistry (Chemie), Weinheim (Weinheim)). Suitable parent compounds are, for example, saturated monosperma, such as methanol, ethanol, n-propanol, ISO-propanol, n-butanol, ISO-butanol, sec.- butanol, isomers of pentanol, hexanol, octanol and nonanol, n-decanol, n-dodecanol, n-tetradecanol, n-hexadecanol, n-octadecanol, cyclohexanol, isomers of methylcyclohexanol or hydroxymethylcellulose, 3-ethyl-3-hydroxyethyloxy, or tetrahydrofurfuryl alcohol; monoalkyl ethers of diethylene glycol such as, for example, monobutyl ether of diethylene glycol; unsaturated alcohols such as allyl alcohol, 1,1-dimethylallyl alcohol or oleic alcohol, aromatic alcohols such as phenol, cresol isomers or methoxyphenol, analiticheskie alcohols such as benzyl alcohol, anise alcohol or cinnamic alcohol; secondary monoamines such as dimethylamine, diethylamine, dipropylamine, Diisopropylamine, dibutylamine, bis(2-ethylhexyl)-amine, N-methyl - and N-ethylcyclohexylamine or dicyclohexylamine, and also heterocyclic secondary amines such as morpholine, pyrrolidine, piperidine or 1H-pyrazole.

Preferred parent compounds are saturated monosperma and simple monoalkylamines EPE is s diethylene glycol. Particularly preferably used as the starting compound simple monobutyl ether of diethylene glycol.

Suitable for reaction alkoxysilane acceleratedly are, in particular, ethylene oxide and propylene oxide, which can be used for the reaction of alkoxysilane in any sequence or in a mixture.

In the case of polyalkyleneglycol alcohols it is either pure polyalkyleneglycols or mixtures polyalkyloxy-polyesters, acceleratedly links which are not less than 30 mol.%, better of not less than 40 mol.% from ethylenoxide links.

Preferred nonionic compounds are monofunctional mixed polyalkyleneglycols with at least 40 mol.% ethyleneoxide units and a maximum of 60 mol.% propylenoxide links.

Suitable compounds of component A2) are ionic or potentially ionic compounds that can be used in addition to or instead of the non-ionic compounds, such as, for example, mono - and dihydroxycinnamate acid, mono - and diaminocarbenes acid, mono - and dihydroxyanthraquinone, mono - and diaminoalkylene, and mono - and dihydroxyacetone acids or mono - and diaminooctane acids and their salts, such as dimethylolpropionic acid, hydroxypivalic acid, N-(2-what aminoethyl)-β -alanine, 2-(2-aminoethylamino)-econsultation, ethylene-diaminopropan or butylsulfonyl, 1,2 - or 1,3-Propylenediamine-β-ethylsulfonyl, lysine, 3,5-diaminobenzoic acid, Hydrophilidae tool according to example 1 of EP-A 0916647 and its alkali metal salts and/or ammonium salts; the adduct of sodium bisulfite and butene-2-diol-1,4, simple polyethersulfone, propoxycarbonyl adduct of 2-butandiol and NaHSO3(for example, in DE-A 2446440, p.5-9, formula I-III), as well as hydrophilic structural component is able to translate in cationic group structural group, such as N-methyl-diethanolamine. Preferred ionic or potentially ionic compounds A2) are such compounds which have a carboxyl or carboxylate and/or sulphonate groups and/or ammonium groups. The most preferred ionic compounds A2) are such compounds which contain carboxyl and/or sulphonate groups as ionic or potentially ionic groups, such as the salts of N-(2-amino-ethyl)-β-alanine, 2-(2-amino-ethylamino)-ethane-sulfonic acids, hydrophiloidea funds according to example 1 of EP-A 0916647 and dimethylolpropionic acid.

Component A2) is preferred as the combination of non-ionic and ionic gidrofilnami funds. Especially preferred ablauts the combination of nonionic and anionic gidrofilnami funds.

Suitable locking means A3) are known to the present time, we are talking about, for example, alcohols, lactams, oximes, esters of malonic acid, alkylaromatic, triazole, phenols, imidazoles, pyrazoles, and amines have had, such as, for example, butanonoxime, Diisopropylamine, 1,2,4-triazole, dimethyl-1,2,4-triazole, imidazole, diethyl ester of malonic acid, acetoacetic ester, acetonates, 3,5-dimethylpyrazole, ε-caprolactam and any mixtures of these blocking means. Preferably as a blocking means A3) apply butanonoxime, 3,5-dimethylpyrazol and ε-caprolactam. Particularly preferred blocking means A3) are butanonoxime and ε-caprolactam.

Compositions according to this invention contain a mixture of stabilizers B), which contains (a) amine with a structural unit of General formula (I). Suitable compounds a) are compounds that have 2,2,6,6-tetramethylpiperidinyloxy balance (the so-called SSA-cycle). Piperidinyl nitrogen in SSA-cycle is not replaced and is not included in any of hydrazide structure. Preferred compounds (a) are the following:

Table 1: Compounds (a)
CAS-Per. No.Structure
24860-22-8
79720-19-7
64338-16-5
52829-07-9
99473-08-2
71029-16-8
71878-19-8

CAS-Reg. No.Structure
90751-07-8
154636-38-1
100631-44-5
115810-23-6

CAS-Reg. No.Structure
164648-93-5
96204-36-3

Especially predpochtitelnei is a compound of formula (III), which is sold by the firm Ciba Spezialitaten (Ciba Spezialitäten) (Lampertheim, Germany) under the name Tinuvin®770 DF

Stabilizer B) in the composition according to this invention contains the compound (b) of General formula (II). Suitable compounds b) are, for example, hydrazides and dihydrazide acids, such as acetic acid hydrazide, adipic acid hydrazide or dehydrated adipic acid or adducts of hydrazine and cyclic carbonates, which, for example as in EP-A 654490 (page 3, line 48 to page 4 line 3). Preferably used dehydrated adipic acid or an adduct of 2 moles of propylene carbonate and 1 mole of hydrazine of General formula (IV)

Especially preferred is the adduct of 2 moles of propylene carbonate and 1 mole of hydrazine of General formula (IV).

Suitable compounds b) are, for example, antioxidants, such as 2,6-diretti-4-METHYLPHENOL, UV absorbers type 2-hydroxyphenyl-benzotriazole or snow tools of the type substituted at the nitrogen atom of SSA-compounds such as Tinuvin® 292 (Ciba Spezialitaten (Cuba Spezialitäten), Lampertheim, Germany) and other trade quality stabilizers, which, for example, described in the books "the Light shielding means for varnishes" ("Lichtschutzmittel für Lacke") Avale (A.Valet), Izd-vo Vincentz (Vincentz, Hannover, 1996) and "Stabilization of polymeric materials" ("Stabilization of Polymeric Materials") (Htuyfl (H.Zweifel), published by Springer (Springer, Berlin, 1997, g is the group of 3, str-213). Preferred compounds C) are shown in table 2.

Table 2: Connection)
CAS-Reg. No.Structure
10191-41-0
128-37-0
2082-79-3
12643-61-0
119-47-1
35074-77-2

CAS-Reg. No.Structure
23128-74-7
976-56-7
65140-91-2
36443-68-2
85-60-9
90498-90-1
1709-70-2

Structure
CAS-Reg. No.
1843-03-4
34137-09-2
27676-62-6
40601-76-1
6683-19-8
32509-66-3

CAS-Reg. No.Structure
31851-03-3
96-69-5
90-66-4
110553-27-0
41484-35-9
991-84-4
103-99-1

CAS-Reg. No.Structure
63843-89-0
4221-80-1
67845-93-6
61167-58-6
128961-68-2
135-88-6
26780-96-1
101-72-4

CAS-Reg. No.Structure
90-30-2
68411-46-1
10081-67-1
32687-78-8
70331-94-1
6629-10-3
26523-78-4
31570-04-4
26741-53-7
80693-00-1

CAS-Reg. No.Structure
140221-14-3
38613-77-3
118337-09-0
3806-34-6
80410-33-9
693-36-7

CAS-Reg. No.Structure
123-28-4
16545-54-3
2500-88-1
131-57-7
1843-05-6
2985-59-3
43221-33-6
57472-50-1

CAS-Reg. No.Structure
2440-22-4
3147-75-9
3896-11-5
3846-71-7
23328-53-2
25973-55-1
36437-37-3
3864-99-1

CAS-Reg. No.Structure
70321-86-7
103597-45-1
84268-08-6
147315-50-2
2725-22-6
23949-66-8

CAS-Reg. No.Structure
35001-52-6
7443-25-6
106917-30-0
41556-26-7
65447-77-0
78276-66-1

CAS-Reg. No.Structure
130277-45-1

As organic solvents) suitable conventional in themselves solvents for varnishes, such as, for example, utilitate, butyl acetate, 1-methoxypropyl-2-acetate, 3-methoxy-n-butyl acetate, acetone, 2-butanone, 4-methyl-2-pentanone, cyclohexanone, toluene, xylene, chlorobenzene or white spirit. Suitable mixtures that contain primarily multiply substituted aromatic compounds which are available in Commerce under the names Solvent Naphtha, Solvesso®(Exxon chemicals (Exxon Chemicals, Houston, USA), Cypar (shell chemicals Shell Chemicals, Eschborn, Germany), Cyclo Sol®(Shell chemicals Shell Chemicals, Eschborn, Germany), The Sol®(Shell chemicals Shell Chemicals, Eschborn, Germany), Shellsol®(Shell Chemicals Shell Chemicals, Eschborn, Germany). Other solvents are, for example, esters of carbonic acid, such as dimethylcarbonate, diethylcarbamyl, 1,2-ethylene carbonate resulting and 1,2-propylene carbonate, lactones, such as β-propiolactone, γ-butyrolactone, ε-caprolacton, ε-methylcaprolactam, propilenglikolstearat, dimethyl ether of diethylene glycol, ketelbey broadcast dipropyleneglycol, ethyl - and butylaminoethyl diethylene glycol, N-organic N-medicalrelated or any mixture of these solvents. Preferred solvents are acetone, 2-butanone, 1-methoxypropyl-2-acetate, xylene, toluene, mixtures, which primarily contain highly substituted aromatic compounds which, for example, known under the names Solvent Naphtha, Solvesso®(Exxon chemicals (Exxon Chemicals, Houston, USA), Cypar®(Shell chemicals Shell Chemicals, Eschborn, Germany), Cycle Sol®(Shell chemicals Shell Chemicals, Eschborn, Germany), Tolu Sol® (shell chemicals Shell Chemicals, Eschborn, Germany), Shellsol®(Shell chemicals Shell Chemicals, Eschborn, Germany)and N-organic. Particularly preferred acetone, 2-butanone and N-organic.

Dispersible in water composition cross-linking agents according to this invention can be obtained by known methods (for example, described in DE-A 2456469, columns 7-8, examples 1-5 and DE-A 2853937 columns 21-26, examples 1-9).

Get dispersible in water composition cross-linking agents according to this invention, in which components A1), A2), A3), (a), (b) and, if necessary, in) is converted in any sequence and, if needed, by using organic solvent).

Preferably at the beginning of the converted A1) component b) and if necessary the value of the nonionic component A2). Then there is the block with the help of component A3), then the transformation using (a) and, if necessary, with a containing an ionic group, a part of component A2). To the reaction mixture, if needed, can be added to the solvent). The following operation is added, if necessary, another component).

The preparation of an aqueous solution or water dispersion is the fact that the dispersible composition of a crosslinking agent by adding water is transferred into the aqueous dispersion or aqueous solution. Used, if necessary, an organic solvent) can be removed at the end of the dispersion by distillation.

For the preparation of aqueous solutions or dispersions containing composition cross-linking agents according to this invention in the General case, using the same quantities of water, the resulting dispersion or solution containing from 10 to 70 wt.% solids, better from 20 to 60 wt.% and better still from 25 to 50 wt.%.

The composition of a crosslinking agent according to this invention can be used in combination with suitable reactive partners who possess groups capable to react with isocyanate groups, for example, with an aqueous binder, such as polyurethane and/or polyacrylate dispersions or mixtures or hybrids. Suitable reaction is about-capable partners are also low molecular weight amines, which can be recycled by being dissolved in water, cured by heating from the aqueous phase means for coating capable processed. Further, the composition of a crosslinking agent according to this invention can be placed in one-component binder, such as polyurethane and/or polyacrylate dispersion, and hybrid polyurethane-polyacrylate dispersions.

Aqueous solutions or dispersions containing composition of a crosslinking agent according to this invention can also be applied without the addition of other reactive partners, for example for impregnating substrates, which have hydrogen atoms capable of reacting with isocyanate groups.

Another object of this invention is an aqueous vehicle for coatings containing composition of a crosslinking agent according to this invention.

Means for coatings containing composition of a crosslinking agent according to this invention is applied to a suitable substrate known methods, such as, for example, an application using a doctor knife, spray or roller applicators or wire wrapped squeegee.

Suitable substrates are, for example, selected from the group of metal, wood, glass, fiberglass, carbon fiber, stone, ceramic watch, the ski minerals, concrete, rigid and flexible plastics of various types, woven and nonwoven textiles, leather, paper, hard fibers, straw and bitumen, which before coating, if needed, can be provided with conventional primers. Preferred substrates are glass fiber, carbon fiber, metals, textiles and leather. Particularly preferred substrate is glass.

The subject of the invention is also the use of cross-linking agent compositions according to this invention in varnishes and means for coating.

Preferred is the use of cross-linking agent compositions according to this invention in dressing for optical fibers. When this dispersion can be used alone or preferably together with a binder, such as, for example, polyurethane dispersions, polyacrylate dispersion, hybrid polyurethane-polyacrylate dispersions, dispersions of simple and complex polyvinyl esters, polystyrene or acrylic dispersions, as well as in combination with other blocked polyisocyanates and aminobenzamide hardeners, such as melamine-formaldehyde resin.

The composition of a crosslinking agent according to the invention or the coating obtained with their help, can contain usual auxiliary materials and additives, such as, for example, ant is the blowing agent, thickener, a means to spill, auxiliary dispersant, catalysts, preventing the formation of film, anticapital, emulsifiers, biocides, adhesion promoter, for example, on the basis of known low - and high-molecular silanes, external lubricant, lubricant, antistatic agents.

Coatings can be applied by any method, for example, by means of suitable devices, such as spray and roller coating alligatory. They can be applied to the extruded at high speed from the nozzles steklofiliny immediately after solidification, i.e. before winding. Coatings can be applied to the fiber at the end of the spinning process in the bath for coating by immersion. Fiberglass coated can be further processed either wet or dry cutting of glass. Drying final or intermediate product is at temperatures of from 80 to 250°C. Under a drying it is important to understand not only the removal of other volatile components, but, for example, the solidification of the components of the dressing. The share of dressing per covered with fiberglass is from 0.1 to 4 wt.%, preferably from 0.2 to 2 wt.%.

As matrix polymers can be used as thermoplastics and thermosets.

The subject of this invention are also the fiberglass, covered means coatings containing composition of a crosslinking agent according to this invention.

Examples

Definition thermopolae

Below the composition of a crosslinking agent applied to the control plate, covered with transparent lacquer-based trading quality, for example, company Spies & Hecker (shpis und the Hecker), with a thickness in the wet state 120 μm Plates are dried for 30 min at room temperature and then subjected to a hot dryer for 30 minutes at 170°in a drying Cabinet. After this happens the color measurement according to the method of CIELAB. More than a certain positive value of b*, the more yellow colored coating composition cross-linking agent.

Example 1 (according to the invention):

To 1445,7 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0%at a temperature of 40°C, for 10 min added under stirring 1215,0 g of polyether LB 25 (Bayer AG (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)) and 16.5 g of the above-mentioned adduct of 1 mole of hydrazine hydrate is added and 2 moles of propylene carbonate has a molecular weight of 236 formula IV. Then the reaction mixture is heated to 90°and peremeci is up at this temperature until until it reaches theoretical NCO value. After cooling to 65°with stirring, added dropwise within 30 min 628,1 g butanonoxime so that the temperature of the mixture did not exceed 80°C. Then add 16.5 g Tinuvin®770 DF (Ciba Spezialitaten GmbH (Ciba Spezialitäten GmbH, Lampertheim, Germany), stirred for further 10 min and the reaction mixture cooled down to 60°C. the Dispersion is by adding 7751,0 g of water (20° (C) at 60°C for 30 minutes subsequent stirring at 40°C is 1 hour.

Get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 30.0%.

Example 2: (example for comparison)

To 677,6 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0%at a temperature of 40°C, for 10 min added under stirring 558,9 g of polyether LB 25 (Bayer AG (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)). Then the reaction mixture is heated to 90°C and stirred at this temperature until, until it reaches theoretical NCO value. After cooling to 65°with stirring, added dropwise within 30 min 274,5g butanonoxime so, to the temperature of the mixture did not exceed 80°C. Then add at 65°From 20.1 g dihydrazide adipic acid for 5 min and the reaction mixture cooled down to 60°C. the Dispersion is by adding 3390,5 g of water (20° (C) at 60°C for 30 minutes subsequent stirring at 40°C is 1 hour.

Get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 30%.

Example 3: (example for comparison)

To 147.4 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0%at a temperature of 40°C, for 10 min added under stirring to 121.0 g of polyether LB 25 (Bayer AG (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)). Then the reaction mixture is heated to 90°C and stirred at this temperature until, until it reaches theoretical NCO value. After cooling to 65°with stirring, added dropwise within 30 min of 62.8 g butanonoxime so that the temperature of the mixture did not exceed 80°C. Then add 1.7 g brganox®245 (Ciba Spezialitaten GmbH (Ciba Spezialitäten GmbH, Lampertheim, Germany) and 1.7 g of Tinuvin®765 (Ciba Speciality the ten GmbH (Ciba Spezialitä ten GmbH, Lampertheim, Germany), stirred for further 10 min and the reaction mixture cooled down to 60°C. the Dispersion is by adding 726,0 g of water (20° (C) at 60°C for 30 minutes subsequent stirring at 40°C is 1 hour.

Get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 31.4%.

Example 4: (example for comparison)

To 147.4 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0%at a temperature of 40°C, for 10 min added under stirring to 121.0 g of polyether LB 25 (Bayer AG (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molekulyarnym weight of 2250 (hydroxyl number=25)). Then the reaction mixture is heated to 90°C and stirred at this temperature until, until it reaches theoretical NCO value. After cooling to 65°with stirring, added dropwise within 30 min of 62.8 g butanonoxime so that the temperature of the mixture did not exceed 80°C. the Dispersion is by adding 726,0 g of water (20° (C) at 60°C for 30 minutes subsequent stirring at 40°C is 1 hour.

Get stable during storage of the aqueous dispersion to block the data MDI with a solids content of 30%.

Example 5: (example for comparison)

To 147.4 g containing biuret groups MDI based on 1,6-diisocyanatohexane(HDI) with a content of NCO-groups 23,0%at a temperature of 40°C, for 10 min added under stirring to 121.0 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)) and 1.7 g of the above-mentioned adduct of 1 mole of hydrazine hydrate is added and 2 moles of propylene carbonate has a molecular weight of 236. Then the reaction mixture is heated to 90°C and stirred at this temperature until, until it reaches theoretical NCO value. After cooling to 65°with stirring, added dropwise within 30 min of 62.8 g butanonoxime so that the temperature of the mixture did not exceed 80°C. Then add 1.7 g Tinuvin®765. Stirred for 10 min and the reaction mixture cooled down to 60°C. the Dispersion is by adding 726,0 g of water (20° (C) at 60°C for 30 minutes subsequent stirring at 40°C is 1 hour.

Get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 30%.

Table 3
Blocked by butanonoxime composition of a crosslinking agent with various stabilizers
Example 1Example 2 (comparison)Example 3 (comparison)Example 4 (comparison)Example 5 (comparison)
The blocking toolButanone-oximeButanone-oximeButanone-oximeButanone-oximeButanone-oxime
The compound of formula IVx---x
Irganox 245--x--
Tinuvin 765--x-x
Tinuvin 770 DFx
Dehydrated adipic acid-x---
CIE-LAB*1)b*-value : 4,46,4the 5.79,95,2

*1)The film thickness of 120 μm in the wet state after 30 min of drying at room temperature and 30 min drying at 170°C.

The cross-linking composition Agay is that according to the invention from example 1 (see table 3) in comparison with the compositions of examples 2-5 has a much better resistance to yellowing.

Example 6 (according to the invention):

963,0 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0% stirred for 30 min at 100°from 39.2 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)) and 7.8 g of the above-mentioned adduct of 1 mole of hydrazine hydrate is added and 2 moles of propylene carbonate has a molecular weight of 236 formula IV. Then added dropwise within 20 min 493,0 g ε-caprolactam so that the temperature of the reaction mixture did not exceed 110°C. is Stirred at a temperature of 110°until then, until it reaches theoretical NCO value and then cooled to 90°C. After adding 7.9 g Tinuvin®770 DF (Ciba Spezialitaten GmbH (Ciba Spezialitäten GmbH, Lampertheim, Germany) and subsequent stirring for 5 min add for 2 min, the mixture of 152.5 g hydrophiloidea funds KV 1386 (BASF AG (BASF AG, Ludwigshafen, Germany) and 235,0 g of water and stirred for another 7 min without change of temperature. In conclusion happens after this dispersion by adding 3341,4 g of water. After subsequent stirring during the 4 hour get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 29.9%.

Example 7 (example for comparison):

963,0 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0% stirred for 30 min at 100°from 39.2 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)). Then added dropwise within 20 min 493,0 g ε-caprolactam so that the temperature of the reaction mixture did not exceed 110°C. is Stirred at a temperature of 110°until then, until it reaches theoretical NCO value and then cooled to 90°C. After further stirring for 5 min add for 2 min, the mixture of 152.5 g hydrophiloidea funds KV 1386 (AT BASF (BASF AG, Ludwigshafen, Germany) and 235,0 g of water and stirred for another 7 min without changing the temperature. In conclusion happens after this dispersion by adding 3325,1 water. After subsequent stirring for 4 hours get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 30.0%.

Example 8 (example for comparison):

192,6 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with a content of NCO-groups 23,0% stirred at 100°With 7.8 g of polyether LB 25 (Bayer AT (Bayer AG),Germany, monofunctional simple polyester based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)). Then added dropwise within 20 min to 98.6 g ε-caprolactam so that the temperature of the reaction mixture did not exceed 110°C. is Stirred at a temperature of 110°until then, until it reaches theoretical NCO value and then cooled to 90°C. After the parallel added within 5 min 4.1 g dihydrazide adipic acid, dissolved in of 20.0 g of water, and the mixture of 22.4 g hydrophiloidea funds KV 1386 (BASF AG (BASF AG, Ludwigshafen, Germany) and and 47.0 g of water stirred the reaction mixture for 7 min without change of temperature. In conclusion happens after this dispersion by adding 647,8 water for 3 minutes After subsequent stirring for 4 hours get stable during storage of the aqueous dispersion of the blocked MDI with a solids content of 28.8%.

Example 9 (according to the invention):

to 13.5 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)) and an 85.1 g ε-caprolactam with stirring, heated to 90°C. Then add 193,0 g, which contains groups of MDI, based on 1,6-Hai is alantolactone (HDI) with a content of NCO-groups to 21.8% for 30 min so to the temperature of the reaction mixture did not exceed 110°C. After the addition is stirred for further 3 hours at 120°add 11.1 g of the above-mentioned adduct of 1 mole of hydrazine hydrate is added and 2 moles of propylene carbonate has a molecular weight of 236 formulas IV and stirred until then, until it reaches theoretical NCO value. Then for 5 min at 100°With added 3.1 g Tinuvin®770 DF (Ciba Spezialitaten GmbH (Ciba Spezialitäten GmbH, Lampertheim, Germany) and the reaction mixture is cooled to 80°C. for 2 min add to 24.6 g hydrophiloidea funds KV 1386 (BASF AG (BASF AG, Ludwigshafen, Germany) and the reaction mixture is stirred for further 15 minutes the Dispersion by adding 648,1 g of water (T=60° (C) within 10 minutes of Subsequent stirring is 2 hours. Get stable during storage of the dispersion with a solids content of 30.0%.

Table 4
Blocked ε-caprolactam composition of a crosslinking agent with various stabilizers
Example 6Example 7 (comparison)Example 8 (comparison)Example 9
The blocking toolε-Caprolactamε-Caprolactamε-Caprolactam the ε-Caprolactam
Type polyisocyanateBiuretBiuretBiuretIsocyanurate
The compound of formula(IV)x--x
Tinuvin 770 DFx--x
Dehydrated adipic acid--x-
CIE-LAB*1)b*-value : 1,35,35,01,4

*1)The film thickness of 120 μm in the wet state after 30 min of drying at room temperature and 30 min drying at 170°C.

The composition of a crosslinking agent according to the invention from examples 6 and 9 (see table 4) compared with the compositions of examples 7-8 has a much better resistance to yellowing.

Example 10 (according to the invention):

231,1 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with an NCO content of 23.0 per cent mixed with 9.4 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molecular weight of 2250 (hydroxyl number=25)) and 1.9 g of the above-mentioned adduct of 1 mole hydrating the rata, and 2 moles of propylene carbonate has a molecular weight of 236 formula IV within 30 min at 100° C. Then at 90°C for 20 min is added to 91.1 g butanonoxime so that the temperature of the reaction mixture did not exceed 110°C. Stirred at 100°until then, until it reaches theoretical NCO value and then cooled to 90°C. After the addition of 1.9 g of Tinuvin®770 DF (Ciba Spezialitaten GmbH (Ciba Spezialitäten GmbH, Lampertheim, Germany) and subsequent stirring for 5 minutes added for 2 min the mixture out of 36.6 g hydrophiloidea funds KV 1386 (AT BASF (BASF AG, Ludwigshafen, Germany) and 56.4 g of water and stirred without changing the temperature for 7 minutes and then in conclusion is the dispersion by adding 738,4 g of water. After additional stirring for 4 hours get stable during storage of the aqueous dispersion with a solids content of 28.0%.

Example 11 (example for comparison):

154,1 g containing biuret groups MDI based on 1,6-diisocyanatohexane (HDI) with an NCO content of 23.0 per cent mixed with 6.3 g of polyether LB 25 (Bayer AT (Bayer AG), Germany, simple monofunctional polyether based on ethylene oxide/propylene oxide with an average molekulyarnym weight of 2250 (hydroxyl number=25)) for 30 min at 100°C. Then at 90°C for 20 min is added to 60.6 g butanonoxime so that the temperature of the reaction mixture did not exceed 110&#HWS. Stirred at 100°until then, until it reaches theoretical NCO value and then cooled to 90°C. After further stirring for 5 minutes added for 2 min, the mixture of 22.0 g hydrophiloidea funds KV 1386 (AT BASF (BASF AG, Ludwigshafen, Germany) and 37.5 g of water and stirred without changing the temperature for 7 minutes and then in conclusion is the dispersion by adding 485,5 g of water. After additional stirring for 4 hours get stable during storage of the aqueous dispersion with a solids content 29,8%.

Table 5
Blocked by butanonoxime composition cross-linkable assets in comparison
Example 10Example 11 (comparison)
The blocking toolButanonoximeButanonoxime
The compound of formula (IV)x-
Tinuvin 770 DFx-
CIE-LAB*1)b*-value : 5,27,2

*1)The film thickness of 120 μm in the wet state after 30 min of drying at room temperature and 30 min drying at 170°C.

Composition cross-linking agents is as according to this invention from example 10 (see table 5) compared with example 11 has a much better resistance to yellowing.

1. Dispersible in water composition of a crosslinking agent containing

A1) at least one organic polyisocyanate with alifaticheskii, cycloaliphatic, analiticheskii and/or aromaticheski bound isocyanate groups,

A2) ionic or potentially ionic and/or nonionic compound,

A3) a blocking means,

B) a stabilizer, containing

a) at least one amine with a structural unit of General formula (I)

no one hydrazide group,

b) the compound of formula (IV)

.

2. Dispersible in water composition of a crosslinking agent according to claim 1, characterized in that it contains the reaction product of at least one organic MDI with alifaticheskii, cycloaliphatic, analiticheskii and/or aromaticheski bound isocyanate groups A1), one ionic or potentially ionic and/or nonionic compounds A2) and blocking means A3) as component (A).

3. Dispersible in water composition of a crosslinking agent according to claim 2, characterized in that component A) a content of isocyanate groups (non-blocked and blocked) is 5.0-27,0 ve the.%.

4. Dispersible in water composition of a crosslinking agent according to claim 2, characterized in that the isocyanate group of the component (A) not less than 50% are in blocked form.

5. Dispersible in water composition of a crosslinking agent according to claim 1, characterized in that as component (B) contains from 0.1 to 11.0 wt.% Amin (a) with a structural unit of formula (I), from 0.1 to 11.0 wt.% connection b) with a structural unit of formula (IV), and the data refer to the total solid content in the composition of a crosslinking agent.

6. Dispersible in water composition of a crosslinking agent according to claim 1, wherein the amine (a) is a compound of formula (III)

.



 

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