CN106752880A - A kind of glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate - Google Patents
A kind of glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate Download PDFInfo
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- CN106752880A CN106752880A CN201710154932.5A CN201710154932A CN106752880A CN 106752880 A CN106752880 A CN 106752880A CN 201710154932 A CN201710154932 A CN 201710154932A CN 106752880 A CN106752880 A CN 106752880A
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- agent
- ultraviolet light
- polyurethane acrylate
- leather finishing
- finishing agent
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
- C09D175/16—Polyurethanes having carbon-to-carbon unsaturated bonds having terminal carbon-to-carbon unsaturated bonds
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- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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- 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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- C08G18/22—Catalysts containing metal compounds
- C08G18/24—Catalysts containing metal compounds of tin
- C08G18/244—Catalysts containing metal compounds of tin tin salts of carboxylic acids
- C08G18/246—Catalysts containing metal compounds of tin tin salts of carboxylic acids containing also tin-carbon bonds
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- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
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- C08G18/30—Low-molecular-weight compounds
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- C08G18/348—Hydroxycarboxylic acids
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- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
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- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
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- C08G18/40—High-molecular-weight compounds
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6633—Compounds of group C08G18/42
- C08G18/6637—Compounds of group C08G18/42 with compounds of group C08G18/32 or polyamines of C08G18/38
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- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
Abstract
The invention discloses a kind of glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate, it is mixed by following components by weight percentage:Polyalcohol 10~30%, isocyanates 10~40%, small molecule dihydroxylic alcohols 2~10% of the molecular weight below 150, hydrophilic chain extender 2~5%, chain extension modifying agent 2~5%, acrylate ended agent 3~8%, catalyst 0.01~0.1%, radical polymerization inhibitor 0.01~0.5%, nertralizer 1~3%, water-based thickener 0.5~1%, hand feeling agent 3~5%, wetting agent 0.5~1%, levelling agent 0.04~0.1%, light trigger 0.01~0.5%, deionized water surplus.The characteristics of present invention has low viscosity, environmental protection, fast curing rate, is especially suitable for use as the finishing agent of leather or artificial leather.
Description
Technical field
The present invention relates to a kind of leather finishing agent, more particularly to a kind of ultraviolet light solidfication water polyurethane acrylate is glossy
Leather finishing agent.
Background technology
An important link is exactly to cover with paint, lacquer, colour wash, etc. in the production process of leather, and the attractive in appearance of leather can be increased in this process
With durable performance, the class of leather is improved, dermatine is more nearly corium.Aqueous Polyurethane Leather Finishing Agent is obtained in recent years
Widely paid close attention to people, liked by people because its is pollution-free, low cost, wearability are good and stores conveniently.And water
Property polyurethane be used for leather finish when, there is good good leveling property, filming performance, strong covering power and firmness.Cover with paint, lacquer, colour wash, etc.
The features such as leather afterwards has bright, plentiful, wear-resisting, while having the advantages that elastic good, low temperature resistant, folding.
UV-curing technology is using light trigger under ultraviolet light, to trigger unsaturated organic monomers to be gathered
The chemical reactions such as conjunction, grafting, crosslinking are so as to reach a kind of rapid emerging technology for solidifying.Due to hardening time is short, equipment
Simply, capacity usage ratio is high, solidification temperature is low, it is free from environmental pollution the features such as, so it once occur receive the extensive of people
Concern.
Late 1960s, Beyer Co., Ltd of West Germany develops photocuring unsaturated polyester (UP) adhesive first, ultraviolet from this
The features such as light-cured resin is with its solvent-free volatilization, fast solidification rate and save energy is favored by people, is obtained in recent years
Quick swift and violent development.But because esters of acrylic acid reactive diluent usual in conventional oil-based UV curing systems is to the skin of people
Skin and eyes have stronger stimulation, and influence operator's is healthy;And many reactive diluents are in ultraviolet light spoke
It is difficult to react completely according to during, residual monomer directly influences the long-term behaviour of cured film, also limit it in food hygiene
Application in industry, and aqueous UV curing coating combines the advantage of traditional UV curing technologies and water paint technology, especially
It is environmentally safe, good without influence, nonflammable, security on health, is rapidly progressed nearly ten years, and into
It is a Main way of paint development.Wherein, aqueous polyurethane acrylate (WPUA) is most class of current research
UV-curable waterborne system, is either still all paid much attention to by people at home abroad.Urethane acrylate
There are carbamate and carboxylic ester structural units simultaneously in the macromolecular structure of photosensitive resin, it combines polyurethane and acrylic acid
The premium properties of resin, while also have can easily be accommodated viscosity and rheological characteristic, environmentally safe or contaminative very little, nonhazardous
And it is missing of ignition the features such as, be worth Devoting Major Efforts To Developing coating variety.
What is reported patent both at home and abroad at present is the preparation method on ultraviolet light solidfication water polyurethane resin more.Such as patent
Photocuring Waterborne Polyurethane Prepolymer is prepared using in-situ method in the patent of application number 201110178207.6, acrylic acid fourth is selected
Ester (BA) and tripropylene glycol double methacrylate (TPGDA) adjust soft and hard segments ratio as reactive diluent, and obtained emulsion is equal
First, stabilization, with preferable mechanical property.But light-cured polyurethane double bond content prepared by the method is not very high, is caused
Hardening time is more long, and gel content is not also high.The patent of application number 200610038981.4 increases double bond using reactive diluent
The method of content, causes adhesive force poor, and the excitant of reactive diluent causes damage to workmen's body.
The content of the invention
It is an object of the invention to provide a kind of glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate, tool
The characteristics of having low viscosity (range of viscosities is in 20~100MPas), environmental protection, curing rate fast (10~30s can just solidify),
It is especially suitable for use as the finishing agent of leather or artificial leather.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate, by weight percentage by with the following group
Divide and be mixed:Polyalcohol 10~30%, isocyanates 10~40%, small molecule dihydroxylic alcohols 2 of the molecular weight below 150~
10%, hydrophilic chain extender 2~5%, chain extension modifying agent 2~5%, acrylate ended agent 3~8%, catalyst 0.01~
0.1%, radical polymerization inhibitor 0.01~0.5%, nertralizer 1~3%, water-based thickener 0.5~1%, hand feeling agent 3~5%, profit
Humectant 0.5~1%, levelling agent 0.04~0.1%, light trigger 0.01~0.5%, deionized water surplus.
The effect of small molecule dihydroxylic alcohols of the molecular weight below 150 is small molecule chain extender, increases hard segment content.
Preferably, the polyalcohol is selected from PPG, PEPA, response type end hydroxy polyether being modified poly- silicon
Siloxane compound (Tech-2147, Tech-2127), terminal hydroxy group alkyl-modified organo-silicon compound (Tech-2120, Tech-
2140) one or more in, the number-average molecular weight of the polyalcohol is 2000g/mol;The isocyanates is selected from different Fu Er
Ketone diisocyanate, hexamethylene diisocyanate, 2,4 toluene diisocyanate, 2,6- toluene di-isocyanate(TDI)s, diphenyl
Methane diisocyanate, hexamethylene diisocyanate, 4,4- diphenyl-methane-group diisocyanates, PPDI, tetramethyl
Base XDI, XDI, one kind of 1,4- dicyclohexyl methyl hydride diisocyanates
Or it is several.
PPG is propane diols polyethers, the trihydroxy methyl that molecular weight is 400~4000 that molecular weight is 800~2000
Propane polyethers, the polytetrahydrofuran diol (molecular weight is 1000~2000) of terminal hydroxy group, tetrahydrofuran-propylene oxide copolymerization two
One or more of alcohol, trihydroxy polyethers (330N, 303).
PEPA is aliphatic diacid, butanedioic acid, the adjacent benzene two of the aliphatic diol by C2~C10 and C6~C14
The PEPA that the polycondensations such as formic acid, hexahydro-phthalic acid, tetrahydrophthalic acid are obtained
Preferably, the hydrophilic chain extender is 2,2- dihydromethyl propionic acids, one kind of 2,2- dimethylolpropionic acids or several
Kind;Small molecule dihydroxylic alcohols of the molecular weight below 150 is selected from 1,4- butanediols, 1,6-HD, one kind of propane diols or several
Kind;The catalyst is organic metal class compound or tertiary amine compounds.
Organic metal class compound:Dibutyl tin laurate, dibutyltin diacetate, stannous octoate, zinc naphthenate, ring
The organic metal class compound such as alkanoic acid cobalt, lead naphthenate, bismuth naphthenate, barium naphthanate.
Tertiary amine compounds:Methyl diethanolamine, triethanolamine, triethylamine, dimethylethanolamine, triethylenediamine,
The tertiary amine compounds such as N, N- dimethyl cyclohexyl amine, N-methylmorpholine.
Preferably, the chain extension modifying agent be extraordinary castor oil (castor oil modified polyalcohol, model 941#, 912#, extensively
Xin Ye trade Co., Ltds of state city), one or two in tung oil.The effect of chain extension modifying agent be increase product the degree of cross linking with
And the content of double bond improves the curing rate of product and the performance of film forming.
Preferably, described acrylate ended agent has following structural formula:
In formula, R is H or CH3, X is C1~C6Aliphatic chain.The effect of this composition is that system kind-NCO is complete
React away, terminating reaction.
Preferably, the radical polymerization inhibitor be nitrotoleune, hydroquinones, 1,4-benzoquinone, hydroquinone monomethyl ether,
In tetrachloroquinone, 1,3,5- trinitrobenzens, 2,6 di tert butyl 4 methyl phenol or 1,1- diphenyl -2- trinitrophenyl-hydrazines
One or more;The light trigger be selected from light trigger 1173, light trigger 184, light trigger 2959, light trigger 369,
One or more in light trigger 1500.
Preferably, the nertralizer is triethylamine.
Preferably, the levelling agent is one or more in BYK-333, BYK-349, BYK-348 of Bi Ke chemistry;
The wetting agent is in wetting agent EW-328, wetting agent EW-327, wetting agent EW-320, the wetting agent EW-312 of road profit chemistry
One or more.
Preferably, water-based thickener is cellulose ether (hydroxyethyl cellulose, methyl hydroxyethylcellulose, methyl hydroxy propyl
Base cellulose etc.), association type alkali swollen thickener (TF-330, TF-938, ASE-60), nonionic polyurethane thickener (AT-
90) one or more in;Hand feeling agent is bridging property organic modified polyorganosiloxane (Silok-9532), extraordinary bridging property organosilicon
In resin (Silok-4148, Silok-3316), cross linkable macromolecule polysiloxanes dispersion (Silok-9166) one
Plant or several.
A kind of preparation method of the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate, including following step
Suddenly:
(1) polyalcohol is added in reaction vessel, is stirred and the vacuum dehydration at 110 DEG C, be less than its moisture content
0.03%;
(2) 20~50 DEG C are adjusted the temperature to, isocyanates is added, catalyst is added dropwise after stirring, temperature control is existed
60~90 DEG C, react 1~2h;
(3) the small molecule dihydroxylic alcohols and chain extension modifying agent of hydrophilic chain extender, molecular weight below 150 are subsequently adding, continue anti-
1~3h is answered, reaction temperature is controlled at 75~85 DEG C;
(4) after after the hydroxyl in system and isocyano total overall reaction, temperature is reduced to 30~45 DEG C, is slowly added to third
Olefin(e) acid ester end-capping reagent, radical polymerization inhibitor, are passed through inert gas, continue 3~5h of stirring reaction, and reaction temperature is controlled 50~60
℃;
(5) step (4) reaction stirs cooling after terminating, and nertralizer is dissolved in into DMF or acetone (quantity of solvent of solute dissolving)
In, in addition system and after 10min, deionized water dispersion being added under high-speed stirred (rotating speed 2000r/min), temperature control is 30
Below DEG C, aqueous polyurethane acrylate is obtained;
(6) levelling agent, hand feeling agent, wetting agent, light trigger and water are added in the aqueous polyurethane acrylate for obtaining
Property thickener, high speed dispersor (rotating speed 1500r/min) dispersion 30min, obtain ultraviolet light solidfication water polyurethane acrylate
Glossy leather finishing agent.
The beneficial effects of the invention are as follows:
The present invention is passed through using the advantage of uV curable and polyurethane the softness adjustability of double bond in acrylate
The ratio of the hydroxyl in isocyano and polyalcohol in adjustment isocyanates, adds extraordinary castor oil and hydrophilic chain extender etc.
It is modified, being subsequently adding acrylate ended agent carries out end capping reaction, the polyurethane acrylate leather coating for finally giving
Agent has large arch dam, environmental protection, curing rate fast etc. advantage;Organic solvent is not used in preparation process, therefore is not deposited
Solvent recovery, it is safe and environment-friendly the problems such as.
Specific embodiment
Below by specific embodiment, technical scheme is described in further detail.
In the present invention, if not refering in particular to, raw material and equipment for being used etc. is commercially available or commonly used in the art.
Method in following embodiments, unless otherwise instructed, is the conventional method of this area.
Embodiment 1
100g PTMG dihydroxylic alcohols is added in equipped with agitating paddle, the four-hole boiling flask of thermometer, in true at 110 DEG C
Sky dehydration 2h, then takes 36g isofoer diisocyanates and adds four-hole boiling flask, adds the catalyst dibutyltin cinnamic acid two of 0.018g
Butyl tin, 2h is reacted at 80 DEG C;Measured after NCO group content reaches theoretical value 3.46% with toluene-di-n-butylamine method, by temperature
Degree is down to 50 DEG C, is subsequently adding 2,2- dihydromethyl propionic acids (DMPA) 7g, BDO (BDO) 4g, castor oil modified polynary
Alcohol (941#) 10g, is warming up to 80 DEG C of reaction 2h again;Then 50 DEG C are cooled the temperature to, end-capping reagent hydroxy-ethyl acrylate is added
(HEA) 6.5g, radical polymerization inhibitor hydroquinones 0.3g, are warming up to 65 DEG C of reaction 3h;30 DEG C are cooled the temperature to, addition is dissolved in third
With system 10min in triethylamine (TEA) 4.23g in ketone;Finally, ice deionized water 205g is rapidly joined under high velocity agitation,
Rapid dispersion 1h, you can obtain the ultraviolet light solidfication water polyurethane acrylate resin of solid content 40%.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1173, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, hand feeling agent Silok-3316 0.9g, wetting agent EW-312 0.5g, use height
Fast dispersion machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment 2
Add 50g polycaprolactone diolss, terminal hydroxy group response type organic in equipped with agitating paddle, the four-hole boiling flask of thermometer
Silicon Tech-2120 5g, in vacuum dehydration 2h at 110 DEG C, then take 78g isofoer diisocyanates and add four-hole boiling flask, plus
Enter the catalyst dibutyltin dilaurylate of 0.02g, 2h is reacted at 80 DEG C;NCO group is measured with toluene-di-n-butylamine method to contain
After amount reaches theoretical value 13.8%, 50 DEG C are cooled the temperature to, be subsequently adding 2,2- dihydromethyl propionic acids (DMPA) 10g, Isosorbide-5-Nitrae-fourth
Glycol (BDO) 12.9g, castor oil modified polyalcohol (941#) 10g, are warming up to 80 DEG C of reaction 2h again;Then cool the temperature to
50 DEG C, end-capping reagent hydroxy-ethyl acrylate (HEA) 14g, radical polymerization inhibitor hydroquinones 0.3g is added, be warming up to 65 DEG C of reactions
3h;30 DEG C are cooled the temperature to, addition is dissolved in the triethylamine in acetone (TEA) 6.04g and system 10min;Finally, in high-speed stirring
Mix down and rapidly join ice deionized water 280g, rapid dispersion 1h, you can obtain the poly- ammonia of UV-curable water-borne of solid content 40%
Ester acrylate.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1173, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, hand feeling agent Silok-3316 0.9g, wetting agent EW-312 0.5g, use height
Fast dispersion machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment 3
50g polycaprolactone diolss are added in equipped with agitating paddle, the four-hole boiling flask of thermometer, it is de- in vacuum at 110 DEG C
Water 2h, then takes 76g isofoer diisocyanates and adds four-hole boiling flask, adds the catalyst dibutyltin cinnamic acid dibutyl of 0.018g
Tin, 2h is reacted at 80 DEG C;Measured after NCO group content reaches theoretical value 6.77% with toluene-di-n-butylamine method, temperature is dropped
To 50 DEG C, 2,2- dihydromethyl propionic acids (DMPA) 11g, BDO (BDO) 8g, castor oil modified polyalcohol are subsequently adding
(912#) 11g, is warming up to 80 DEG C of reaction 2h again;Then 50 DEG C are cooled the temperature to, end-capping reagent hydroxy-ethyl acrylate (HEA) is added
13.5g, radical polymerization inhibitor hydroquinones 0.25g, are warming up to 65 DEG C of reaction 3h;30 DEG C are cooled the temperature to, addition is dissolved in acetone
In triethylamine (TEA) 6.65g in and system 10min;Finally, ice deionized water 227g is rapidly joined under high velocity agitation, soon
Speed dispersion 1h, you can obtain the ultraviolet light solidfication water polyurethane acrylate resin of solid content 45%.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1173, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, hand feeling agent Silok-3316 0.9g, wetting agent EW-312 0.5g, use height
Fast dispersion machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment 4
30g polycaprolactone diolss, 5g trihydroxy polyethers are added in equipped with agitating paddle, the four-hole boiling flask of thermometer
330N, 5g trihydroxy PPG 303, in vacuum dehydration 2h at 110 DEG C, then takes 76g isofoer diisocyanates and adds
Enter four-hole boiling flask, add the catalyst dibutyltin dilaurylate of 0.018g, 2h is reacted at 80 DEG C;With toluene-di-n-butylamine
Method is measured after NCO group content reaches theoretical value 21.2%, cools the temperature to 50 DEG C, is subsequently adding 2,2- dihydromethyl propionic acids
(DMPA) 10.5g, BDO (BDO) 15.2g and tung oil 11g, are warming up to 80 DEG C of reaction 2h again;Then cool the temperature to
50 DEG C, end-capping reagent hydroxy-ethyl acrylate (HEA) 12.76g, radical polymerization inhibitor hydroquinones 0.20g is added, be warming up to 65 DEG C instead
Answer 3h;30 DEG C are cooled the temperature to, addition is dissolved in the triethylamine in acetone (TEA) 6.34g and system 10min;Finally, at a high speed
Ice deionized water 170g, rapid dispersion 1h are rapidly joined under stirring, you can the UV-curable water-borne for obtaining solid content 50% gathers
Chlorinated polyethylene.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1103, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, hand feeling agent Silok-3316 0.9g, wetting agent EW-312 0.5g, use height
Fast dispersion machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment 5
51.5g polycaprolactone diolss, terminal hydroxy group response type are added in equipped with agitating paddle, the four-hole boiling flask of thermometer to be had
Machine silicon Tech-2140 2g, in vacuum dehydration 2h at 110 DEG C, then take 78g isofoer diisocyanates and add four-hole boiling flask,
The catalyst dibutyltin dilaurylate of 0.02g is added, 2h is reacted at 80 DEG C;NCO group is measured with toluene-di-n-butylamine method
After content reaches theoretical value 13.8%, 50 DEG C are cooled the temperature to, be subsequently adding chain extender 2,2- dihydromethyl propionic acids (DMPA)
10g, BDO (BDO) 12.9g, castor oil modified polyalcohol (941#) 11g, are warming up to 80 DEG C of reaction 2h again;Then
50 DEG C are cooled the temperature to, end-capping reagent hydroxy-ethyl acrylate (HEA) 14g, radical polymerization inhibitor hydroquinones 0.3g is added, is warming up to
65 DEG C of reaction 3h;30 DEG C are cooled the temperature to, addition is dissolved in the triethylamine in acetone (TEA) 6.04g and system 10min;Finally,
Ice deionized water 189g, rapid dispersion 1h are rapidly joined under high velocity agitation, you can obtain the ultraviolet light polymerization of solid content 50%
Aqueous polyurethane acrylate resin.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1173, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, hand feeling agent Silok-3316 0.9g, wetting agent EW-312 0.5g, use height
Fast dispersion machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment 6
40g PTMGs dihydroxylic alcohols, 5g trihydroxy polyethers are added in equipped with agitating paddle, the four-hole boiling flask of thermometer
Polyalcohol 330N, in vacuum dehydration 2h at 110 DEG C, then takes 76g isofoer diisocyanates and adds four-hole boiling flask, adds
0.02g catalyst dibutyltin dilaurylates, 2h is reacted at 80 DEG C;NCO group content is measured with toluene-di-n-butylamine method to reach
To after theoretical value 14.2%, 50 DEG C are cooled the temperature to, be subsequently adding 2,2- dihydromethyl propionic acids (DMPA) 11g, BDO
(BDO) 15g and castor oil modified polyalcohol (912#) 11g, is warming up to 80 DEG C of reaction 2h again;Then 50 DEG C are cooled the temperature to,
End-capping reagent hydroxy-ethyl acrylate (HEA) 14g, radical polymerization inhibitor hydroquinones 0.2g is added, 65 DEG C of reaction 3h are warming up to;By temperature
Degree is down to 30 DEG C, and addition is dissolved in the triethylamine in acetone (TEA) 6.65g and system 10min;Finally, under high velocity agitation soon
Speed adds ice deionized water 178g, rapid dispersion 1h, you can obtain the ultraviolet light solidfication water polyurethane propylene of solid content 50%
Acid ester resin.
Take 50g ultraviolet light solidfication water polyurethane acrylate resins, plus the 2.5g of light trigger 1173, water-based thickener
ASE-60 0.3g, levelling agent BYK-347 0.2g, the 0.9g of hand feeling agent 0301, wetting agent EW-312 0.5g, are disperseed using high speed
Machine is disperseed, you can the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate is obtained.
Embodiment described above is a kind of preferably scheme of the invention, not makees any formal to the present invention
Limitation, also has other variants and remodeling on the premise of without departing from the technical scheme described in claim.
Claims (10)
1. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate, it is characterised in that by weight percentage
Meter is mixed by following components:Polyalcohol 10~30%, isocyanates 10~40%, small molecule two of the molecular weight below 150
First alcohol 2~10%, hydrophilic chain extender 2~5%, chain extension modifying agent 2~5%, acrylate ended agent 3~8%, catalyst 0.01
~0.1%, radical polymerization inhibitor 0.01~0.5%, nertralizer 1~3%, water-based thickener 0.5~1%, hand feeling agent 3~5%,
Wetting agent 0.5~1%, levelling agent 0.04~0.1%, light trigger 0.01~0.5%, deionized water surplus.
2. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the polyalcohol is selected from PPG, PEPA, response type end hydroxy polyether modified polyorganosiloxane chemical combination
One or more in the alkyl-modified organo-silicon compound of thing, terminal hydroxy group, the number-average molecular weight of the polyalcohol is 2000g/
mol;The isocyanates be selected from isofoer diisocyanate, hexamethylene diisocyanate, 2,4 toluene diisocyanate,
2,6- toluene di-isocyanate(TDI)s, methyl diphenylene diisocyanate, hexamethylene diisocyanate, the isocyanide of 4,4- diphenylmethane groups two
Acid esters, PPDI, tetramethylxylylene diisocyanate, XDI, the rings of 1,4- bis-
One or more of hexyl methane diisocyanate.
3. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the hydrophilic chain extender is one or more of 2,2- dihydromethyl propionic acids, 2,2- dimethylolpropionic acids;The molecule
The small molecule dihydroxylic alcohols of amount less than 150 is selected from one or more of 1,4- butanediols, 1,6-HD, propane diols;The catalysis
Agent is organic metal class compound or tertiary amine compounds.
4. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the chain extension modifying agent is one or two in extraordinary castor oil, tung oil.
5. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, described acrylate ended agent has following structural formula:
In formula, R is H or CH3, X is C1~C6Aliphatic chain.
6. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the radical polymerization inhibitor be nitrotoleune, hydroquinones, 1,4-benzoquinone, hydroquinone monomethyl ether, tetrachloroquinone,
One kind or several in 1,3,5- trinitrobenzens, 2,6 di tert butyl 4 methyl phenol or 1,1- diphenyl -2- trinitrophenyl-hydrazines
Kind;The light trigger is selected from light trigger 1173, light trigger 184, light trigger 2959, light trigger 369, light trigger
One or more in 1500.
7. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the nertralizer is triethylamine.
8. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, the levelling agent is one or more in BYK-333, BYK-349, BYK-348 of Bi Ke chemistry;The wetting agent
It is the one kind or several in wetting agent EW-328, wetting agent EW-327, wetting agent EW-320, the wetting agent EW-312 of road profit chemistry
Kind.
9. the glossy leather finishing agent of a kind of ultraviolet light solidfication water polyurethane acrylate according to claim 1, it is special
Levy and be, water-based thickener be cellulose ether, association type alkali swollen thickener, nonionic polyurethane thickener in one kind or
It is several;Hand feeling agent is bridging property organic modified polyorganosiloxane, extraordinary bridging property organic siliconresin, the poly- silicon of cross linkable macromolecule
One or more in oxygen alkane dispersion.
10. a kind of preparation of the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate as claimed in claim 1
Method, it is characterised in that comprise the following steps:
(1) polyalcohol is added in reaction vessel, is stirred and the vacuum dehydration at 110 DEG C, its moisture content is less than 0.03%;
(2) adjust the temperature to 20~50 DEG C, add isocyanates, catalyst is added dropwise after stirring, by temperature control 60~
90 DEG C, react 1~2h;
(3) it is subsequently adding the small molecule dihydroxylic alcohols and chain extension modifying agent of hydrophilic chain extender, molecular weight below 150, continue to react 1~
3h, reaction temperature is controlled at 75~85 DEG C;
(4) after after the hydroxyl in system and isocyano total overall reaction, temperature is reduced to 30~45 DEG C, is slowly added to acrylic acid
Ester end-capping reagent, radical polymerization inhibitor, are passed through inert gas, continue 3~5h of stirring reaction, and reaction temperature is controlled at 50~60 DEG C;
(5) step (4) reaction stirs cooling after terminating, during nertralizer is dissolved in into DMF or acetone, in addition system and after 10min,
Under high velocity agitation plus deionized water dispersion, temperature control obtains aqueous polyurethane acrylate below 30 DEG C;
(6) levelling agent, hand feeling agent, wetting agent, light trigger and aqueous increasing are added in the aqueous polyurethane acrylate for obtaining
Thick dose, high speed dispersor dispersion 30min obtains the glossy leather finishing agent of ultraviolet light solidfication water polyurethane acrylate.
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CN107384081A (en) * | 2017-08-29 | 2017-11-24 | 安徽乐踏鞋业有限公司 | A kind of finishing agent for improving the low temperature resistant dry environment of leather |
CN109679484A (en) * | 2018-12-24 | 2019-04-26 | 清远市美佳乐环保新材股份有限公司 | A kind of leather water-based temperature resistant foaming pre-treatment finishing agent and preparation method thereof |
CN111850179A (en) * | 2020-07-30 | 2020-10-30 | 浙江奥康鞋业股份有限公司 | First layer cowhide leather making process and first layer cowhide leather shoes |
CN113916417A (en) * | 2021-10-18 | 2022-01-11 | 天津科技大学 | Novel flexible stress sensor and preparation method thereof |
CN113956784A (en) * | 2021-10-18 | 2022-01-21 | 丽水学院 | Water-based visible light driven film-forming finishing agent for ecological synthetic leather |
CN115491118A (en) * | 2022-10-13 | 2022-12-20 | 浙江南龙皮业有限公司 | Water-based leather finishing agent, preparation method thereof and leather finishing process |
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CN107384081A (en) * | 2017-08-29 | 2017-11-24 | 安徽乐踏鞋业有限公司 | A kind of finishing agent for improving the low temperature resistant dry environment of leather |
CN109679484A (en) * | 2018-12-24 | 2019-04-26 | 清远市美佳乐环保新材股份有限公司 | A kind of leather water-based temperature resistant foaming pre-treatment finishing agent and preparation method thereof |
CN111850179A (en) * | 2020-07-30 | 2020-10-30 | 浙江奥康鞋业股份有限公司 | First layer cowhide leather making process and first layer cowhide leather shoes |
CN113916417A (en) * | 2021-10-18 | 2022-01-11 | 天津科技大学 | Novel flexible stress sensor and preparation method thereof |
CN113956784A (en) * | 2021-10-18 | 2022-01-21 | 丽水学院 | Water-based visible light driven film-forming finishing agent for ecological synthetic leather |
CN115491118A (en) * | 2022-10-13 | 2022-12-20 | 浙江南龙皮业有限公司 | Water-based leather finishing agent, preparation method thereof and leather finishing process |
CN115491118B (en) * | 2022-10-13 | 2023-08-08 | 浙江南龙皮业有限公司 | Water-based leather finishing agent, preparation method thereof and leather finishing process |
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Application publication date: 20170531 |