CN106750080A - It is a kind of from extinction type modified aqueous polyurethane coating and preparation method and application - Google Patents

It is a kind of from extinction type modified aqueous polyurethane coating and preparation method and application Download PDF

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Publication number
CN106750080A
CN106750080A CN201710044087.6A CN201710044087A CN106750080A CN 106750080 A CN106750080 A CN 106750080A CN 201710044087 A CN201710044087 A CN 201710044087A CN 106750080 A CN106750080 A CN 106750080A
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China
Prior art keywords
castor oil
aqueous polyurethane
epoxy
organosilicon
modified aqueous
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CN201710044087.6A
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Chinese (zh)
Inventor
庞浩
雍奇文
黄健恒
廖兵
莫文蔚
黄福仁
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Foshan Function High Polymer Materials & Fine Chemicals Professional Center
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Foshan Function High Polymer Materials & Fine Chemicals Professional Center
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Priority to CN201710044087.6A priority Critical patent/CN106750080A/en
Publication of CN106750080A publication Critical patent/CN106750080A/en
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Abstract

The invention belongs to water paint field, disclose a kind of from extinction type modified aqueous polyurethane coating and preparation method thereof.By regulating and controlling, castor oil and epoxy resin synthesize the crosslinking of aqueous polyurethane to the method during the course of the reaction and degree of branching controls the purpose of emulsion particle diameter to reach, and it is selectively introducing organosilicon, synthesize particle diameter 400~2000nm castor oil epoxy Modified Waterborne Polyurethane and particle diameter 50~200nm organosilicon castor oil Modified Waterborne Polyurethane, and above-mentioned two component that will be obtained carry out physical blending and compounding be obtained paint film.Compared to one-component from extinction type aqueous polyurethane, synthesis from extinction type modified aqueous polyurethane coating due to the branched and crosslinked action of castor oil and epoxy resin, make it have hardness higher, the introducing of more preferable scratch resistance, hydrolytic resistance and heat endurance, especially organosilicon is also imparted from the good sense of touch of extinction type modified aqueous polyurethane paint film.

Description

It is a kind of from extinction type modified aqueous polyurethane coating and preparation method and application
Technical field
It is more particularly to a kind of from extinction type modified aqueous polyurethane coating and its preparation the invention belongs to water paint field Method and application.
Background technology
The article with extinction effect is seen everywhere in daily life：At home, on the road being on duty, or at night All visible its trace in restaurant.Employ delustring face more indoor furniture, be covered in the wooden boards also delustring substantially outside restaurant Appearance.When the effect of selection light or delustring is faced, we are not limited solely to fashion and outward appearance demand.Practice card Bright, property easy to clean, the requirement of the aspect such as brightness effect and touch perception also contributes to our selection.When we arrive at office Room, whether drives, and by bus or by train, can all find the upholstery face substantially delustring of all kinds of vehicles 's.From from the aspect of practical and safety, the blackboard of school be all avoided using frosting it is dazzling.The inside of car is also adopted by The decoration of this kind of design, some economical and practical devices and inside employs not dazzling delustring paint for security consideration. Reflection-proof is a problem.The general not bright coating of scratch brushing in skyscraper surface, but with painting in advance on the base material of steel or aluminium The sheet material of paint is covered, and uses antiglossing pigment, to avoid producing dangerous reflective, the eye of stimulation pedestrian or driver Eyeball.Additionally, economical and practical is another key factor of selection coating surface state.Such as, it is scratched when some base materials, has light When nick is cheated and made dirty, these defects can be covered up using antiglossing pigment, and coat polish lacquer and be difficult to cover such flaw.
So-called extinction effect is exactly few light for receiving of human eye, is the subjective print of one kind that our sense organ is formed As.Specifically, exactly when a branch of light source (sunshine, light etc.) is radiated on certain object at an angle, portion big absolutely Divide incident ray that absorption, refraction, scattering etc. are mainly there occurs according to physical surface characteristics, only few some light is reflected away Received by human eye, people go out whether this object has extinction effect further according to subjective judgement.Studies have found that, light line reflection Intensity depends on the flatness of body surface.Such as mirror, it is commonly known that its surface is very moist, to light reflectance pole Height, with high gloss.On the contrary, the coating surface scattering light of micro-rough, a repellel small part light, realize tool There is the outward appearance of extinction effect.
Ground pumice was used for the outer surface of dried paint of polishing in the past.Trickle scratch is obtained by processing, there is paint film Fine, noble delustring appearance.It is used to manufacture frosting now with more materials.Although some process are more multiple It is miscellaneous, but it is but very quick.Additive based on silica, paraffin, organic material even filler, can add in coating In, the coating surface of micro-rough can be formed after the drying.For example, United States Patent (USP) US9353271B2 combines untreated silicon, has The collaboration photoextinction of three kinds of delustering agents of machine modified silicon and wax modified silicon imparts the low gloss of acrylic coating and excellent Physical property.United States Patent (USP) US8986791B2 invented water dissolvable polyethylene oxide resin serve as organic matting agent with After acrylic resin stirring mixing lustrous surface can be reduced for the surface treatment of natural or synthetic leather.Traditionally by drying of polishing The outer surface of paint film or additional a certain amount of delustering agent make coating surface produce micro-rough, so as to realize its table in coating The effect of face low gloss.Requirement of the former approach to labour cost and construction technology is too high, the latter's method be limited to delustering agent with The matching (different base resins is different to parameter requests such as particle diameter, porosity, the indexs of refraction of delustering agent) of base resin, disappear The problems such as compatibility, cost of delustering agent of photo etching and base resin, and additional delustering agent will necessarily cause paint film loss section The spectroscopy transparency and some physical and chemical performances.
As world industry technology is maked rapid progress, follow the technology of the conventionally manufactured antiglossing pigment for getting off the 80s and 90s seemingly Do not realize fundamentally changing, be faced with the difficult situation do not fitted mutually with contemporary advanced industrial technology demand.Therefore, Increasing countries in the world coating experts and scholars open the new industrial research for inquiring into manufacture antiglossing pigment.They expect profit With the means such as chemical reactive synthesis control, ultraviolet light step curing realize building the coating surface of micro- fold or micro-rough without Needing again additional delustering agent just can produce good extinction effect, and this new technology is referred to as chemical quenching or from delustring, So that the physics extinction method with traditional additional delustering agent is distinguished.United States Patent (USP) US20140371384A1, US8906468B2 is military using the antiglossing pigment and low gloss that dual-beam uviol lamp step curing principle has respectively obtained scratch-resistant Aircraft coating, is to carry out radiation curing to coating surface first with the mercury lamp that wavelength is more long, energy is relatively low to produce micro- fold, Recycling the xenon lamp that wavelength is shorter, energy is higher carries out the complete radiation curing of depth of paint film.The shortcoming of this method is paint film Thickness be preferably controlled within 20 μm, otherwise ultra-violet curing is incomplete；It is also required to specific ultraviolet equipment simultaneously and raw material is matched somebody with somebody Ultra-violet curing film forming can be realized just now.Chinese patent CN103865031A, CN104193946A, CN103936959A are using chemistry The aqueous polyurethane of control consecutive publications one-component is synthesized from matting resin, its glossiness is low, and synthesis technique is simple, but Hardness of paint film not enough, is easily scratched, and water resistance and heat endurance are poor.Chinese patent CN103626930A has delivered a kind of with phase point From the preparation method of Aqueous acrylic urethane's matting resin of structure, its complex process, it is necessary to simultaneously synthesizing anionic is sealed Polyurethane and nonionic polyurethane are closed, then triggers esters of acrylic acid to be polymerized and reacted, it is difficult to industrially apply.
The content of the invention
In order to overcome the hardness of paint film from extinction type aqueous polyurethane coating of existing one-component low, easily scratch, it is water-fast Property and the shortcomings of heat endurance difference with it is not enough.The present invention is intended to provide one kind is from extinction type modified aqueous polyurethane coating.The painting Material is formed micro-coarse structured and produces extinction effect after film-forming by surface, it is not necessary to add silica flatting silica again Or traditional physics delustering agent such as delustring wax.Additionally, the paint film that the modified aqueous polyurethane coating is formed is due to castor oil and ring The branched and crosslinked action of oxygen tree fat, makes it have hardness higher, more preferable scratch resistance, hydrolytic resistance and heat endurance, The especially introducing of organosilicon also imparts the good sense of touch of paint film.
Another object of the present invention is to provide the above-mentioned preparation method from extinction type modified aqueous polyurethane coating.The method It is simple controllable, the modified aqueous polyurethane of different hardness and various luster degree can be also obtained by the usage ratio for adjusting two components Paint film.
Still a further object of the present invention is to provide the above-mentioned application from extinction type modified aqueous polyurethane coating.
The purpose of the present invention is achieved through the following technical solutions：
It is a kind of from extinction type modified aqueous polyurethane coating, including castor oil epoxy Modified Waterborne Polyurethane and organic Silicon castor oil Modified Waterborne Polyurethane.
Preferably, the castor oil epoxy Modified Waterborne Polyurethane component is dual modified with organosilicon castor oil aqueous The mass ratio of polyurethane component is 0.6~1.5:1.
A kind of above-mentioned preparation method from extinction type modified aqueous polyurethane coating, comprises the following specific steps that：
S1. the preparation of castor oil epoxy Modified Waterborne Polyurethane：
A () leads to N at isocyanates, castor oil, polymer polyatomic alcohol, catalyst are blended in into 60~90 DEG C2Reaction 2~3 Hour；
B () continues to react 2~4 hours during small molecule hydrophilic monomer, epoxy resin are added into step S1 (a), and use acetone The viscosity of reaction system is adjusted, the generation of gel is prevented；
C the reaction solution that step S1 (b) is obtained is down to 30~50 DEG C by (), add nertralizer, is reacted 10~30 minutes, is obtained Castor oil epoxy Modified Waterborne Polyurethane performed polymer；
D castor oil epoxy Modified Waterborne Polyurethane performed polymer that () obtains step S1 (c) is added drop-wise to and contains chain extension Abundant chain extension is carried out in the aqueous solution of agent, and is stirred 0.5~1 hour under 1000~2000r/min rotating speeds, obtain castor-oil plant oil ring Oxygen Modified Waterborne Polyurethane；
S2. the preparation of organosilicon castor oil Modified Waterborne Polyurethane：
A () leads to N at isocyanates, castor oil, polymer polyatomic alcohol, catalyst are blended in into 60~90 DEG C2Reaction 2~3 Hour；
B () continues to react 2~4 hours during small molecule hydrophilic monomer is added into step S2 (a), reaction system is adjusted with acetone Viscosity, prevent the generation of gel；
C the reaction solution that step S2 (b) is obtained is down to 30~50 DEG C by (), add nertralizer, is reacted 10~30 minutes, is obtained Castor oil modified Waterborne Polyurethane Prepolymer；
D () then mixes organosilicon with deionized water after, be added drop-wise to that step S2 (c) obtains is castor oil modified aqueous poly- Stirred 0.5~1 hour in urethane performed polymer and under 1000~2000r/min rotating speeds, organosilicon castor oil is obtained dual modified Aqueous polyurethane；
S3. it is step S1 gained castor oil epoxy Modified Waterborne Polyurethanes and step S2 gained organosilicon castor oil is double Weight modified aqueous polyurethane blending, 2~4 hours are stood after being stirred 15~30 minutes under 1000~2000r/min rotating speeds, are obtained final product From extinction type modified aqueous polyurethane coating.
Preferably, step S1 (a) and isocyanates described in S2 (a) are trimethyl hexamethylene diisocyanate, different Buddhist That ketone diisocyanate or hexamethylene diisocyanate；
Preferably, step S1 (a) and polymer polyatomic alcohol described in S2 (a) are polyoxypropyleneglycol, polycaprolactone two One or more of alcohol, PCDL or polytetrahydrofuran diol, the polyoxypropyleneglycol, polycaprolactone glycol, The molecular weight of PCDL or polytetrahydrofuran diol is 400~4000；
Preferably, step S1 (a) and the hydroxyl value content of castor oil described in S2 (a) are 175~185mg/g；The catalysis Agent is any one in dibutyl tin laurate, isooctyl acid bismuth, laurate bismuth, bismuth neodecanoate.
Preferably, step S1 (b) and small molecule hydrophilic monomer described in S2 (b) are dihydromethyl propionic acid or dihydroxymethyl fourth Acid；Epoxy resin described in step S1 (b) is bisphenol type epoxy E-44 resins or epoxy E-51 resins；Step S1 (c) and S2 C nertralizer described in () is triethylamine or tripropyl amine (TPA).
Preferably, chain extender described in step S1 (d) is ethylenediamine or hydrazine hydrate；Organosilicon is described in step S2 (d) Containing amino, hydroxyl, epoxy radicals small molecule organosiloxane class.
It is further preferable that the small molecule organosiloxane class is the KH550 containing mono amino functional group, epoxy functionality KH560, the KH792 of the KH602 of double amido functional groups or double amido functional groups.
Preferably, isocyanates described in step S1 (a) and the mol ratio of polymer polyatomic alcohol are 1.2~1.8:1, it is described The consumption of castor oil is the 5~8% of the quality of polymer polyatomic alcohol, and the consumption of the catalyst is isocyanates, polymer is more The 0.3~0.6% of first alcohol and castor oil gross mass；
Preferably, the consumption of small molecule hydrophilic monomer described in step S1 (b) is the total of isocyanates and polymer polyatomic alcohol The 4~8% of quality, the consumption of the epoxy resin is the 4~6% of the gross mass of isocyanates and polymer polyatomic alcohol；
Preferably, nertralizer described in step S1 (c) and the mol ratio of small molecule hydrophilic monomer are 0.8~1.2：1.
Preferably, the consumption of chain extender described in step S1 (d) is castor oil epoxy Modified Waterborne Polyurethane pre-polymerization The molal weight of remaining isocyano in body, the solid content of the castor oil epoxy Modified Waterborne Polyurethane for 15~ 30%.
Preferably, isocyanates described in step S2 (a) and the mol ratio of polymer polyatomic alcohol are 1.4~2:1, the castor The consumption of sesame oil is the 3~5% of the quality of polymer polyatomic alcohol；
Preferably, the consumption of small molecule hydrophilic monomer described in step S2 (b) is isocyanates and polymer polyatomic alcohol The 3~6% of gross mass；
Preferably, nertralizer described in step S2 (c) and the mol ratio of small molecule hydrophilic monomer are 0.8~1.2：1；
Preferably, the consumption of organosilicon described in step S2 (d) is the 3~4% of the quality of polymer polyatomic alcohol, is obtained Organosilicon castor oil Modified Waterborne Polyurethane solid content is 30~40%.
It is above-mentioned from extinction type modified aqueous polyurethane coating in automotive trim, woodenware, furniture, paper gloss oil, natural and people Application in fabricate-leather field of surface treatment.
The present invention synthesizes the crosslinking of aqueous polyurethane and branched during the course of the reaction by regulating and controlling castor oil and epoxy resin Degree is selectively introducing organosilicon to reach the purpose of control emulsion particle diameter, is respectively synthesized out particle diameter 400~2000nm's The dual modified aqueous poly- ammonia of organosilicon castor oil of castor oil epoxy Modified Waterborne Polyurethane and particle diameter in 50~200nm Ester.Both are all polyurethane resin series, and with extremely similar physico-chemical property and structure of functional groups, compatibility is preferable, refractive power Rate is approached, film forming is covered with paint, lacquer, colour wash, etc. after blending has preferable penetrating degree, it is to avoid the coating surface that additional delustering agent occurs turns white The problems such as flower phenomenon and poor storage stability.Because the molecular structure side chain of castor oil epoxy Modified Waterborne Polyurethane is more, Crosslinking degree is big, and emulsion micelles particle has larger volume, and proportion is small, and easily coating surface is floated in film forming procedure, there is provided The extinction effect of modified aqueous polyurethane paint film.Organosilicon castor oil Modified Waterborne Polyurethane is due to having introduced simultaneously Machine silicon and castor oil, make paint film have the performances such as preferable water resistance, heat endurance and excellent sense of touch.
Compared with prior art, the present invention has advantages below and beneficial effect：
1. the present invention prepare from extinction type modified aqueous polyurethane coating, it is aqueous poly- from extinction type compared to one-component Urethane, synthesis from extinction type modified aqueous polyurethane coating due to the branched and crosslinked action of castor oil and epoxy resin and The features such as high-modulus, high intensity of epoxy resin, make it have hardness higher, more preferable scratch resistance, hydrolytic resistance and heat The introducing of stability, especially organosilicon also imparts the good sense of touch of modified aqueous polyurethane paint film.
2. what prepared by the present invention has preferable penetrating degree from extinction type modified aqueous polyurethane coating after film forming is covered with paint, lacquer, colour wash, etc., The coating surface that additional delustering agent occurs is avoided to turn white the problems such as growing dim phenomenon and poor storage stability.
3. the present invention synthesizes crosslinking and the branch of aqueous polyurethane by regulating and controlling castor oil and epoxy resin during the course of the reaction Change degree, and introduce organic-silicon-modified, extinction type modified aqueous polyurethane coating is come from synthesis.The method is simply controllable, into This is cheap, it is not necessary to complicated production equipment, and different hardness and various luster can be obtained by the usage ratio for adjusting two components The paint film of degree.Its extinction effect is automatically generated by coating sheet after film forming, it is not required that additional physics delustering agent.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but embodiments of the present invention not limited to this.
Adopt in the examples below and tested with the following method：
1. the test of the solid content of emulsion：The present invention is dual according to GB/T 1725-79 measurement standards test castor oil epoxy The solid content of modified aqueous polyurethane and organosilicon castor oil Modified Waterborne Polyurethane emulsion.
2. the test of emulsion particle diameter：The present invention is using Malvern instrument company Nano-60 nano particle sizes analyzer at 25 DEG C Under measure the particle diameter of castor oil epoxy Modified Waterborne Polyurethane and organosilicon castor oil Modified Waterborne Polyurethane emulsion.
3. the test of viscosity：It is double that the present invention measures castor oil epoxy using NDJ-1A viscosity measuring instruments at 20rpm-25 DEG C The viscosity of weight modified aqueous polyurethane and organosilicon castor oil Modified Waterborne Polyurethane emulsion.
4. the test of glossiness：The present invention uses KGZ-60 ° of standard glossiness instrument, is measured according to standard GB 9754 and painted The glossiness of film.
Embodiment 1
1. the synthesis of castor oil epoxy Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with nitrogen Added in the 500ml four-hole boiling flasks of gas 2000 molecular weight polyoxyethylene propylene glycol 40g, IPDI 17.58g, Castor oil 1.38g and dibutyltin dilaurate catalyst 0.01g, 2h is reacted at 70 DEG C.Then dihydroxymethyl third is added The acetone soln of sour 3.85g and E-44 epoxy resin 3.69g continues to react 3h, and period adds acetone regulation viscosity.It is cooled to 40 DEG C, it is transferred in dropping funel in addition triethylamine 2.91g and after 30min, under the high-speed stirred of 2000r/min, dropwise soon Speed is added drop-wise to ethylenediamine (1.72g) aqueous dispersion 30min, and to obtain milky castor oil epoxy Modified Waterborne Polyurethane standby. Emulsion is measured admittedly containing being 20%, viscosity is 3500mPa.s, and particle diameter is 500~1000nm.
2. the synthesis of organosilicon castor oil Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with 2000 molecular weight polyoxyethylene propylene glycol 20g, 2000 molecular weight polycaprolactone glycol are added in the 500ml four-hole boiling flasks of nitrogen 20g, IPDI 17.58g, castor oil 1.2g and dibutyltin dilaurate catalyst 0.01g, at 70 DEG C Reaction 2h.Then the acetone soln for adding dimethylolpropionic acid 3.51g continues to react 3h, and period adds acetone regulation viscosity. It is cooled to 50 DEG C, adds in triethylamine 2.4g and 30min.Then, organic silicon is added under the high-speed stirred of 2000r/min KH792 mass 1.2g and the mixed liquor of deionized water, disperse 0.5~1h to obtain organosilicon castor oil Modified Waterborne Polyurethane standby With.Emulsion is measured admittedly containing being 30%, viscosity is 500mPa.s, and particle diameter is 50~100nm.
3. castor oil epoxy Modified Waterborne Polyurethane is compounded with organosilicon castor oil Modified Waterborne Polyurethane：With High speed shearing emulsification agent is under the speed of 2000r/min by castor oil epoxy Modified Waterborne Polyurethane 100g and organosilicon castor Sesame oil Modified Waterborne Polyurethane 80g mixes 15min, after standing froth breaking 2h, derives from extinction type modified aqueous polyurethane Coating.Viscosity is measured for 2500mPa.s, centrifugation test is without deposited phenomenon.
4. apply：To obtain being coated in from extinction type modified aqueous polyurethane coating bar spreader undressed On natural leather, 50 DEG C of constant temperature 2h in an oven, after 1 day, it is 3 to measure 60 ° of lower glossiness to drying at room temperature.
Embodiment 2
1. the synthesis of castor oil epoxy Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with nitrogen Added in the 500ml four-hole boiling flasks of gas 2000 molecular weight polyoxyethylene propylene glycol 40g, IPDI 17.58g, Castor oil 2.07g and catalyst dibutyltin dilaurylate 0.01g, 2h is reacted at 75 DEG C.Then dihydroxymethyl third is added The acetone soln of sour 3.85g and E-51 epoxy resin 3.18g continues to react 3h, and period adds acetone regulation viscosity.It is cooled to 50 DEG C, it is transferred in dropping funel in addition triethylamine 2.91g and after 30min, under the high-speed stirred of 2000r/min, dropwise soon Speed is added drop-wise to ethylenediamine water (1.58g) solution dispersion 30min, obtains milky castor oil epoxy Modified Waterborne Polyurethane standby With.Emulsion is measured admittedly containing being 15%, viscosity is 3200mPa.s, and particle diameter is 400~1200nm.
2. the synthesis of organosilicon castor oil Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with 2000 molecular weight polycarbonate glycol 40g, IPDI 17g, castor-oil plant are added in the 500ml four-hole boiling flasks of nitrogen Oily 1.6g and dibutyltin dilaurate catalyst 0.01g, 2h is reacted at 70 DEG C.Then dimethylolpropionic acid is added The acetone soln of 3.31g continues to react 3h, and period adds acetone regulation viscosity.50 DEG C are cooled to, add triethylamine 2.26g to neutralize 30min.Then, the KH550 mass 1.2g of organic silicon is added under the high-speed stirred of 2000r/min with the mixing of deionized water Liquid stirs 1h, obtains organosilicon castor oil Modified Waterborne Polyurethane standby.Measure emulsion to contain admittedly is 30%, and viscosity is 800mPa.s, particle diameter is 50~200nm.
3. castor oil epoxy Modified Waterborne Polyurethane is compounded with organosilicon castor oil Modified Waterborne Polyurethane：With High speed shearing emulsification agent is organic by 100g castor oil epoxy Modified Waterborne Polyurethanes and 60g under the speed of 2000r/min Silicon castor oil Modified Waterborne Polyurethane mixes 15min, after standing froth breaking 3h, derives from extinction type modified aqueous polyurethane Coating.Viscosity is measured for 2800mPa.s, centrifugation test is without deposited phenomenon.
4. apply：To obtain being coated in from extinction type modified aqueous polyurethane coating spreader undressed natural On leather, 50 DEG C of constant temperature 2h in an oven, after 1 day, it is 4 to measure 60 ° of lower glossiness to drying at room temperature.
Embodiment 3
1. the synthesis of castor oil epoxy Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with nitrogen Added in the 500ml four-hole boiling flasks of gas 2000 molecular weight polyoxyethylene propylene glycol 40g, IPDI 17.58g, Castor oil 2.76g and organo-bismuth class catalyst-laurate bismuth 0.01g, 2h is reacted at 70 DEG C.Then dihydroxymethyl third is added The acetone soln of sour 3.85g and E-44 epoxy resin 1.85g continues to react 3h, and period adds acetone regulation viscosity.It is cooled to 50 DEG C, it is transferred in dropping funel in addition triethylamine 3.01g and after 30min, under the high-speed stirred of 2000r/min, dropwise soon Speed be added drop-wise to ethylenediamine (1.58g) aqueous dispersion 30 minutes milky castor oil epoxy Modified Waterborne Polyurethane is standby With.Emulsion is measured admittedly containing being 20%, viscosity is 3000mPa.s, and particle diameter is 800~1500nm.
2. the synthesis of organosilicon castor oil Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with 2000 molecular weight polyoxyethylene propylene glycol 40g, trimethyl hexamethylene diisocyanate are added in the 500ml four-hole boiling flasks of nitrogen 13g, castor oil 1.4g and dibutyltin dilaurate catalyst 0.01g, react 2 hours at 75 DEG C.Then dihydroxy is added The acetone soln of methylbutanoic acid 4.51g continues to react 3h, and period adds acetone regulation viscosity.50 DEG C are cooled to, triethylamine is added In 3.1g and 30min.Then, the KH560 mass 1.4g and deionization of organic silicon are added under the high-speed stirred of 1500r/min The mixed liquor dispersion 1h of water, obtains organosilicon castor oil Modified Waterborne Polyurethane standby.Measure emulsion to contain admittedly is 30%, viscosity It is 600mPa.s, particle diameter is 50~100nm.
3. castor oil epoxy Modified Waterborne Polyurethane is compounded with castor oil epoxy Modified Waterborne Polyurethane：With height Fast shearing emulsifier is under the speed of 1800r/min by castor oil epoxy Modified Waterborne Polyurethane 100g and castor oil epoxy Modified Waterborne Polyurethane 100g mixes 15min, after standing froth breaking 2h, derives from the painting of extinction type modified aqueous polyurethane Material.Viscosity is measured for 2000mPa.s, centrifugation test is without deposited phenomenon.
4. apply：To obtain being coated in from extinction type modified aqueous polyurethane coating spreader undressed natural On leather, 50 DEG C of constant temperature 2h in an oven, after 1 day, it is 4 to measure 60 ° of lower glossiness to drying at room temperature.
Embodiment 4
1. the synthesis of castor oil epoxy Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with nitrogen Added in the 500ml four-hole boiling flasks of gas 2000 molecular weight polyoxyethylene propylene glycol 40g, IPDI 17.58g, Castor oil 2.76g and dibutyltin dilaurate catalyst 0.01g, 2h is reacted at 70 DEG C.Then dihydroxymethyl fourth is added The acetone soln of sour 3.31g and E-51 epoxy resin 3.75g continues to react 3h, and period adds acetone regulation viscosity.It is cooled to 40 DEG C, it is transferred in dropping funel in addition triethylamine 2.26g and after 30min, under the high-speed stirred of 2000r/min, dropwise soon Speed is added drop-wise to ethylenediamine (1.8g) aqueous dispersion 30min, obtains milky castor oil epoxy Modified Waterborne Polyurethane standby. Emulsion is measured admittedly containing being 25%, viscosity is 3500mPa.s, and particle diameter is 500~1000nm.
2. the synthesis of organosilicon castor oil Modified Waterborne Polyurethane：To equipped with agitator, reflux condensing tube and being connected with 2000 molecular weight polyisoprene erythritan 40g, IPDI 17g, castor are added in the 500ml four-hole boiling flasks of nitrogen Sesame oil 1.8g and catalyst dibutyltin dilaurylate 0.01g, 2h is reacted at 70 DEG C.Then dimethylolpropionic acid is added The acetone soln of 3.51g continues to react 3h, and period adds acetone regulation viscosity.50 DEG C are cooled to, add triethylamine 2.4g to neutralize 30min.Then, the KH792 mass 1.2g of organic silicon is added under the high-speed stirred of 2000r/min with the mixing of deionized water Liquid stirs 1h, obtains organosilicon castor oil Modified Waterborne Polyurethane standby.Measure emulsion to contain admittedly is 30%, and viscosity is 800mPa.s, particle diameter is 50~150nm.
3. castor oil epoxy Modified Waterborne Polyurethane is compounded with castor oil epoxy Modified Waterborne Polyurethane：With height Fast shearing emulsifier is under the speed of 2200r/min by castor oil epoxy Modified Waterborne Polyurethane 100g and organosilicon castor-oil plant Oily Modified Waterborne Polyurethane 60g mixes 15min, after standing froth breaking 2h, derives from the painting of extinction type modified aqueous polyurethane Material.Viscosity is measured for 1800mPa.s, centrifugation test is without deposited phenomenon.
4. apply：To obtain being coated in from extinction type modified aqueous polyurethane coating spreader undressed natural On leather, 50 DEG C of constant temperature 2h in an oven, after 1 day, it is 5 to measure 60 ° of lower glossiness to drying at room temperature.
Embodiment 5
The present embodiment is with the difference of embodiment 1：
Castor oil consumption in described synthetic castor oil epoxy Modified Waterborne Polyurethane is 2.07g.
Catalyst in described synthetic castor oil epoxy Modified Waterborne Polyurethane is laurate bismuth 0.01g.
Nertralizer in described synthetic castor oil epoxy Modified Waterborne Polyurethane is tripropyl amine (TPA) 4.12g.
Containing admittedly for described synthetic castor oil epoxy Modified Waterborne Polyurethane is 20%, and viscosity is 2000mPa.s, grain Footpath is 600~1500nm.
The polymer polyatomic alcohol of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 2000 molecular weight Polycaprolactone glycol 40g.
The reaction temperature of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 80 DEG C.
Containing admittedly for described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 35%, and viscosity is 800mPa.s, Particle diameter is 100~200nm.
Described preparation technology is obtained from the extinction type modified aqueous polyurethane coating light obtained on natural leather Damp degree is 5.
Embodiment 6
This implementation is with the difference of example embodiment 1：
Reaction temperature in described synthetic castor oil epoxy Modified Waterborne Polyurethane is 80 DEG C.
Catalyst in described synthetic castor oil epoxy Modified Waterborne Polyurethane is isooctyl acid bismuth 0.01g.
Chain extender in described synthetic castor oil epoxy Modified Waterborne Polyurethane is hydrazine hydrate 1.4g.
The solid content of described synthetic castor oil epoxy Modified Waterborne Polyurethane is 20%, and viscosity is 3000mPa.s, Particle diameter is 600~1000nm.
The polymer polyatomic alcohol of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 2000 molecular weight Polycaprolactone glycol 40g.
The isocyanates of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is the isocyanic acid of hexa-methylene two Ester 12.9g.
The organic silicon of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is KH602 mass 1.4g.
Containing admittedly for described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 35%, and viscosity is 600mPa.s, Particle diameter is 50~200nm.
Described preparation technology is obtained from the extinction type modified aqueous polyurethane coating light obtained on natural leather Damp degree is 3.5.
Embodiment 7
The present embodiment is with the difference of embodiment 1：
Epoxy resin in described synthetic castor oil epoxy Modified Waterborne Polyurethane is E-51 epoxy resin 3.18g。
Chain extender in described castor oil epoxy Modified Waterborne Polyurethane is hydrazine hydrate 1.4g.
Containing admittedly for described synthetic castor oil epoxy Modified Waterborne Polyurethane is 20%, and viscosity is 3500mPa.s, grain Footpath is 500~1500nm.
The polymer polyatomic alcohol of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 2000 molecular weight The polytetrahydrofuran diol 10g of polyoxypropyleneglycol 20g and 1000 molecular weight.
The isocyanates of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is tri-methyl hexamethylene two Isocyanates 15.5g.
The organic silicon of described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is KH560 mass 1.2g.
Containing admittedly for described synthesizing organo-silicon castor oil Modified Waterborne Polyurethane is 35%, and viscosity is 600mPa.s, Particle diameter is 50~100nm.
Described preparation technology is obtained from the extinction type modified aqueous polyurethane coating light obtained on natural leather Damp degree is 4.5.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine and simplification, Equivalent substitute mode is should be, is included within protection scope of the present invention.

Claims (10)

1. one kind is from extinction type modified aqueous polyurethane coating, it is characterised in that dual modified aqueous poly- including castor oil epoxy Urethane and organosilicon castor oil Modified Waterborne Polyurethane.
2. according to claim 1 from extinction type modified aqueous polyurethane coating, it is characterised in that the castor oil epoxy is double Weight modified aqueous polyurethane is 0.6~1.5 with the mass ratio of organosilicon castor oil Modified Waterborne Polyurethane:1.
3. a kind of preparation method from extinction type modified aqueous polyurethane coating according to claim 1 or claim 2, its feature exists In comprising the following specific steps that：
S1. the preparation of castor oil epoxy Modified Waterborne Polyurethane：
A () leads to N after mixing isocyanates, castor oil, polymer polyatomic alcohol, catalyst at 60~90 DEG C2Reaction 2~3 is small When；
B () continues to react 2~4 hours during small molecule hydrophilic monomer, epoxy resin are added into step S1 (a),
And with the viscosity of acetone regulation reaction system, prevent the generation of gel；
C the reaction solution that step S1 (b) is obtained is down to 30~50 DEG C by (), add nertralizer, is reacted 10~30 minutes, obtains castor-oil plant Oil ring oxygen Modified Waterborne Polyurethane performed polymer；
D castor oil epoxy Modified Waterborne Polyurethane performed polymer that () obtains step S1 (c) is added drop-wise to and contains chain extender Abundant chain extension is carried out in the aqueous solution, and is stirred 0.5~1 hour under 1000~2000r/min rotating speeds, obtain castor oil epoxy double Weight modified aqueous polyurethane；
S2. the preparation of organosilicon castor oil Modified Waterborne Polyurethane：
A () leads to N after mixing isocyanates, castor oil, polymer polyatomic alcohol, catalyst at 60~90 DEG C2Reaction 2~3 is small When；
B () continues to react 2~4 hours during small molecule hydrophilic monomer is added into step S2 (a), the viscous of reaction system is adjusted with acetone Degree, prevents the generation of gel；
C the reaction solution that step S2 (b) is obtained is down to 30~50 DEG C by (), add nertralizer, is reacted 10~30 minutes, obtains castor-oil plant Oily modified aqueous polyurethane performed polymer；
D () then mixes organosilicon with deionized water after, the castor oil modified aqueous polyurethane that step S2 (c) is obtained is added drop-wise to In performed polymer, and stirred 0.5~1 hour under 1000~2000r/min rotating speeds, organosilicon castor oil is obtained dual modified aqueous Polyurethane；
S3. by step S1 gained castor oil epoxy Modified Waterborne Polyurethanes and step S2 gained, organosilicon castor oil is dual changes Property aqueous polyurethane blending, stirring stands 2~4 hours after 15~30 minutes under 1000~2000r/min rotating speeds, that is, derive from and disappear Light type modified aqueous polyurethane coating.
4. according to claim 3 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that step S1 A isocyanates described in () and S2 (a) is trimethyl hexamethylene diisocyanate, IPDI or six methylenes Group diisocyanate；
Polymer polyatomic alcohol described in step S1 (a) and S2 (a) is polyoxypropyleneglycol, polycaprolactone glycol, makrolon One or more of glycol or polytetrahydrofuran diol, the polyoxypropyleneglycol, polycaprolactone glycol, PCDL Or the molecular weight of polytetrahydrofuran diol is 400~4000；
The hydroxyl value content of castor oil described in step S1 (a) and S2 (a) is 175~185mg/g；The catalyst is tin dilaurate Dibutyl tin, isooctyl acid bismuth, any one in laurate bismuth or bismuth neodecanoate.
5. according to claim 3 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that step S1 B small molecule hydrophilic monomer described in () and S2 (b) is dihydromethyl propionic acid or dimethylolpropionic acid；Ring described in step S1 (b) Oxygen tree fat is bisphenol type epoxy E-44 resins or epoxy E-51 resins；Nertralizer described in step S1 (c) and S2 (c) is three second Amine or tripropyl amine (TPA).
6. according to claim 3 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that step S1 D chain extender described in () is ethylenediamine or hydrazine hydrate；Organosilicon described in step S2 (d) be containing amino, hydroxyl, epoxy radicals it is small Molecule organosiloxane class.
7. according to claim 6 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that described small Molecule organosiloxane class is the KH550 containing mono amino functional group, the KH560 of epoxy functionality, double amido functional groups The KH792 of KH602 or double amido functional groups.
8. according to claim 3 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that step S1 A isocyanates described in () is 1.2~1.8 with the mol ratio of polymer polyatomic alcohol:1, the consumption of the castor oil is polymer The 5~8% of the quality of polyalcohol, the consumption of the catalyst is isocyanates, polymer polyatomic alcohol and castor oil gross mass 0.3~0.6%；
The consumption of small molecule hydrophilic monomer described in step S1 (b) be the gross mass of isocyanates and polymer polyatomic alcohol 4~ 8%, the consumption of the epoxy resin is the 4~6% of the gross mass of isocyanates and polymer polyatomic alcohol；
Nertralizer described in step S1 (c) is 0.8~1.2 with the mol ratio of small molecule hydrophilic monomer：1；
The consumption of chain extender described in step S1 (d) is remaining isocyanide in castor oil epoxy Modified Waterborne Polyurethane performed polymer The mole of acid group, the solid content of the castor oil epoxy Modified Waterborne Polyurethane is 15~30%.
9. according to claim 3 from the preparation method of extinction type modified aqueous polyurethane coating, it is characterised in that step S2 A isocyanates described in () is 1.4~2 with the mol ratio of polymer polyatomic alcohol:1, the consumption of the castor oil is that polymer is more The 3~5% of the quality of first alcohol；
The consumption of small molecule hydrophilic monomer described in step S2 (b) be the gross mass of isocyanates and polymer polyatomic alcohol 3~ 6%；
Nertralizer described in step S2 (c) is 0.8~1.2 with the mol ratio of small molecule hydrophilic monomer：1；
The consumption of organosilicon described in step S2 (d) is the 3~4% of the quality of polymer polyatomic alcohol, the organosilicon castor-oil plant for obtaining Oily Modified Waterborne Polyurethane solid content is 30~40%.
10. described in claim 1 or 2 from extinction type modified aqueous polyurethane coating in automotive trim, woodenware, furniture, paper light Application in oil, natural and artificial leather field of surface treatment.
CN201710044087.6A 2017-01-19 2017-01-19 It is a kind of from extinction type modified aqueous polyurethane coating and preparation method and application Pending CN106750080A (en)

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CN108276551A (en) * 2017-12-26 2018-07-13 合肥科天水性科技有限责任公司 A kind of multiple cross-linked modified aqueous polyurethane resin of biology base and its preparation method and application
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CN109651588A (en) * 2018-11-21 2019-04-19 万华化学集团股份有限公司 Castor oil modified cation self-crosslinkable polyurethane polyurea water dispersion and preparation method and application
CN110976247A (en) * 2019-12-16 2020-04-10 江苏靓时新材料科技股份有限公司 Device of super mute skin sense panel of lamp system
CN111848914A (en) * 2020-06-10 2020-10-30 华南理工大学 Self-extinction light-cured waterborne polyurethane acrylate cured film with low water absorption rate and preparation method and application thereof
CN111849337A (en) * 2020-07-22 2020-10-30 清远市美佳乐环保新材股份有限公司 Preparation method of self-extinction emulsion taking oily extinction resin as core
CN111849337B (en) * 2020-07-22 2021-11-23 清远市美佳乐环保新材股份有限公司 Preparation method of self-extinction emulsion taking oily extinction resin as core
CN114181577A (en) * 2020-09-15 2022-03-15 广东华润涂料有限公司 Aqueous wood coating composition and wood product made therefrom
CN112852278A (en) * 2021-03-16 2021-05-28 天津中晶建筑材料有限公司 Water-based plant-based fingerprint-resistant varnish and preparation method and application thereof
CN112852278B (en) * 2021-03-16 2022-02-25 天津中晶建筑材料有限公司 Water-based plant-based fingerprint-resistant varnish and preparation method and application thereof
CN115819984A (en) * 2022-12-29 2023-03-21 江西阿璐达新材料有限公司 High-resilience fluorosilicone rubber material and preparation method thereof
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