CN109721704A - A kind of light shield extinguishing waterborn polyurethane and preparation method thereof - Google Patents
A kind of light shield extinguishing waterborn polyurethane and preparation method thereof Download PDFInfo
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- CN109721704A CN109721704A CN201910026028.5A CN201910026028A CN109721704A CN 109721704 A CN109721704 A CN 109721704A CN 201910026028 A CN201910026028 A CN 201910026028A CN 109721704 A CN109721704 A CN 109721704A
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- light shield
- extinguishing waterborn
- polyurethane
- chain extender
- isocyanates
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Abstract
The present invention relates to a kind of light shield extinguishing waterborn polyurethanes and preparation method thereof, belong to flame retardant polyurethane technical field of material；The polyurethane is one kind using hydrophilic nanoparticles, polyether Glycols, isocyanates, hydrophilic chain extender as raw material, solvent is added to reduce system viscosity, through, with synthesis Waterborne Polyurethane Prepolymer, emulsifying the light shield extinguishing waterborn polyurethane being prepared by high-speed stirred in parlkaline；The ultravioletlight screening effect for the light shield extinguishing waterborn polyurethane that the present invention is prepared is good, and glossiness is low, and flame retardant property is good, and limit oxygen index is 29.0% or more.
Description
Technical field
The invention belongs to organic material technical fields, and in particular to a kind of preparation side of light shield extinguishing waterborn polyurethane
Method.
Background technique
Aqueous polyurethane is to replace organic solvent as the new polyurethane system of decentralized medium using water, and also referred to as water dispersion is poly-
Urethane, aqueous polyurethane or water-based polyurethane.Aqueous polyurethane takes water as a solvent, pollution-free, safe and reliable, mechanical performance is excellent
Good, the advantages that compatibility is good, easily modified, therefore be widely used.The most common purposes of aqueous polyurethane is used as coating.It is logical
Cross cross-linking modified aqueous polyurethane coating with good storage stability, coating machinery performance, water resistance, solvent resistance and
Ageing-resistant performance, and the similar performance with traditional solvent borne polyurethane coating.
The materials such as woodenware are based on moisture-proof, loss prevention and beauty etc. and consider, and generally can spray organic coating on surface and be protected.
And aqueous polyurethane it is safe and environment-friendly and functional with its advantages that, become the first choice of woodenware surface protection coating.Such as middle promulgated by the State Council
Bright patent application (application number 2017111686418) discloses a kind of polyurethane environmental protection water-borne woodwork coating and preparation method thereof,
Including raw material: modified aqueous polyurethane, sodium citrate, dibutyl tin dilaurate, polycarboxylic acids glycine betaine methyl methacrylate,
Polycarbonate glycol, filler, defoaming agent, auxiliary rheological agents, increases sliding anti-wear agent, deionized water at hydroxyethyl cellulose.The coating is water-fast
Property is good, stability is good, solid component is high, smearing is smooth, plentiful, bright, therefore is widely portable to the coating of woodenware substrate.But
It is the materials such as woodenware, it is easy to lignin degradation occur under the ultraviolet light in shortwave area and medium wave area, damage woodenware.On
State the ineffective of coating antiultraviolet injury.Therefore, require study a kind of good aqueous polyurethane coating of light shielding effect.
Summary of the invention
The present invention is intended to provide a kind of preparation method of light shield extinguishing waterborn polyurethane, passes through adding for photomask agent
Add, substantially increases the shield effectiveness to ultraviolet light of aqueous polyurethane.
In order to solve the above technical problems, The technical solution adopted by the invention is as follows:
As one aspect of the present invention, the present invention provides a kind of light shield extinguishing waterborn polyurethane, raw material includes such as
Lower component: photomask agent, polyether Glycols, soft segment flame-proof modifier, isocyanates, antalkali and hydrophilic chain extender；
Wherein, in the isocyanates in-NCO group and polyether Glycols, soft segment flame-proof modifier and hydrophilic chain extender
- OH group molar ratio be 1.1:1~2.0:1；
The quality and polyether Glycols, soft segment flame-proof modifier, hydrophilic chain extender, isocyanates and alkali of the photomask agent
Property neutralizer quality summation ratio be 1:1000~2:100.
As a further improvement of the present invention, the antalkali is identical as the additive amount of hydrophilic chain extender, for except light
5.5% of other components quality summation except screener.
As a further improvement of the present invention, photomask agent is hydrophilic titanium dioxide (TiO2) or hydrophilic oxidation
Zinc (ZnO).Hydrophilic titanium dioxide (TiO2) or hydrophilic zinc oxide (ZnO) be nano-titanium dioxide or nano zine oxide
It is obtained by surface hydrophilicity modification, hydrophilically modified process belongs to the prior art, should obtain for those skilled in the art
The common knowledge known, and not invention main points, this will not be repeated here.
As a further improvement of the present invention, the isocyanates is aliphatic polyisocyante and/or aromatic series polyisocyanate
Cyanate.It is furthermore preferred that isocyanates is isophorone diisocyanate (IPDI).
As a further improvement of the present invention, the hydrophilic chain extender is 2,2- hydroxymethyl propionic acid (DMPA), 2,2- hydroxyl first
Base butyric acid (DMBA), 1,2- propylene glycol -3-3 sodium sulfonate, 1,4- butanediol -2- sodium sulfonate, N, N- dimethyl diethanol amine, benzyl
Dimethyl (2- ethoxy) ammonium chloride, dodecyl dimethyl (2- ethoxy) ammonium bromide, Polyoxyethylene glycol, trihydroxy third
Alkoxy polyalkylene glycol monoether, N, N- dimethyl-N-(2- ethoxy) glycine betaine or N- methyl-N, N- bis- (2- ethoxy) glycine betaine.
It is furthermore preferred that hydrophilic chain extender is 2,2- hydroxymethyl propionic acid (DMPA) or 2,2- hydroxymethylbutyrate (DMBA).
As a further improvement of the present invention, the soft segment flame-proof modifier is phosphorous polyether polyol (OP550).
As another aspect of the present invention, the present invention also provides a kind of preparation sides of light shield extinguishing waterborn polyurethane
Method includes the following steps: photomask agent, polyether Glycols, soft segment flame-proof modifier and isocyanates being added to reaction vessel,
It is passed through inert gas or nitrogen into reaction system and keeps, is reacted 2.5~3.5 hours in 80~90 DEG C of oil bath；It is added
Hydrophilic chain extender and solvent, the reaction was continued 2.5~3.5 hours, is cooled to 35~45 DEG C, and antalkali is added and neutralize instead
It answers, stopping is passed through inert gas or nitrogen, obtains the performed polymer product for being dissolved in solvent；After revolving removes solvent, pre-polymerization is isolated
Deionized water is added in body product thereto, stirs the emulsified 30~40min of shearing condition, obtains product.
Further, the quality of the solvent and polyether Glycols (PPG), soft segment flame-proof modifier, isocyanates, hydrophilic
The gross mass of chain extender and antalkali is equal.
Further, the rate of the stirring shearing is 3000-3500rpm.
Further, the solvent is acetone, butanone, ethyl acetate, methylene chloride, tetrahydrofuran or N, N- dimethyl methyl
Amide；The antalkali is ammonium hydroxide, 2-amino-2-methyl-1-propanol (AMP-95), diethanol amine, triethanolamine, diethyl
Amine, triethylamine (TEA), sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium acetate, sodium pyrophosphate or sodium carbonate.It is furthermore preferred that molten
Agent is acetone, and antalkali is triethylamine (TEA).
Further, the mass ratio of the quality of the deionized water and the performed polymer product of taking-up is 7:3.
Light shield extinguishing waterborn polyurethane of the present invention can be used directly, and light shield extinguishing waterborn can also be made
It is used after polyurethane film, property remains unchanged after film forming.
A kind of film build method of light shield extinguishing waterborn polyurethane of the present invention, the method comprises the following steps: this is sent out
The bright light shield extinguishing waterborn polyurethane stands 7 days in polyfluortetraethylene plate at room temperature and forms a film naturally, slow to moisture
Vacuum drying 24 hours at 80 DEG C are placed into vacuum oven after volatilization, obtain a kind of light shield extinguishing waterborn polyurethane
Film.
Compared with prior art, the present invention has the following technical effect that
The photomask agent added in Raw Materials for Waterborne Polyurethane of the invention is inorganic photomask agent, is not only had to ultraviolet light
There is stronger absorption, ultraviolet light can also be made to scatter, therefore, imitates water-base polyurethane material to the shielding of ultraviolet light
Fruit greatly improves.And inorganic photomask agent has many advantages, such as that environment-protecting and non-poisonous, thermal stability is high, is particularly suitable for being used as woodenware table
Face protective coating.
Photomask agent particle size is an important factor for influencing light shielding effect, and the present invention is using hydrophilic dioxy
Change titanium (TiO2) or hydrophilic zinc oxide (ZnO) screener, belong to semiconductor material, it is full there are one in electronic structure
Valence band and an empty conduction band, there are forbidden bands between valence band and conduction band.After nanoparticle, which absorbs, is more than the light radiation of black pigment used by women in ancient times to paint their eyebrows west energy,
Nano-oxide can be excited to excitation state from ground state.In this course, electrons rush valence band and transit to conduction band, in valence band shape
At positively charged hole.And the service life of electrons and holes is very short, therefore in transition process, most electrons and holes
Will be again compound, heat is released, luminous energy has been converted to thermal energy, has reached light shielding effect with this.Additionally due to inorganic matter
It is not soluble in water, it is easy to happen isolation in aqueous polyurethane, causes dispersion uneven, not only influences the mechanicalness of polyurethane material
Can, it is also greatly reduced light shielding effect.The hydrophilic titanium dioxide (TiO2) or hydrophilic zinc oxide that the present invention uses
(ZnO) have and pass through hydrophilic surface modification, therefore disperse in aqueous polyurethane more uniform, improve light shielding effect.
Flame-retardant modified soft segment is the polyether polyol that will have fire-retardant segment or polyester polyol as reactive matrix, is introduced
Into polyurethane.The flame retardant property of the flame-retardant modified aqueous polyurethane of soft segment is good, and ignition-proof element content is high, and glue film is soft.It is burning
When, phosphate can be generated phosphoric acid and metaphosphoric acid by thermal decomposition on strand, can also be heated and hydroxyl dehydrogenation polycondensation reaction production occurs
Raw polyphosphoric acid and poly-metaphosphoric acid, polyphosphoric acid and poly-metaphosphoric acid can not only accelerate dehydration carbonization, but also will form non-ignitibility liquid
Film is covered on charcoal layer surface, and imflammable gas is inhibited to release, and hinders its heat transmitting from surface, protects layer of charcoal, prevent its continuation
Burning, plays fire retardation.
The ultravioletlight screening effect of light shield extinguishing waterborn polyurethane of the present invention is good, uv transmittance down to
10.0%, it is seen that light transmission rate causes glossiness low down to 89.0%, since photomask agent particle weakens mirror-reflection, favorably
In the transmission for hindering visible light.For the rate of drying of its latex film within 7 days, limit oxygen index is fire retardant 28.0% or more
Material.
Light shield extinguishing waterborn polyurethane of the present invention, operating procedure is simple, safe, has preferable industrial application
Value.
Specific embodiment
It is clearly and completely described below in conjunction with the technical solution in the embodiment of the present invention, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general
Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected
Range.
Embodiment 1:
Take the hydrophilic nano TiO of 1.24g2, by its 80 DEG C at a temperature of it is dry for 24 hours, with 100.00g PPG,
37.45g OP550 and 83.18gIPDI are added in the four-hole boiling flask equipped with thermometer, and nitrogen is passed through into reaction system, will
React reaction system 3 hours；Then, 13.67g is added into reaction system
DMPA and 247.97g acetone, the reaction was continued 3 hours；Then 40 DEG C are cooled to, 13.67g TEA progress neutralization reaction 30 is added and divides
Clock stops logical nitrogen, obtains the performed polymer product for being dissolved in acetone；After revolving removes acetone, the performed polymer for taking out 210.00g is produced
The deionized water of 490.00g is added in object, shears emulsified 30 minutes in the stirring of 3000rpm, it is poly- to obtain light shield extinguishing waterborn
Urethane.
The uv transmittance of test gained light shield extinguishing waterborn polyurethane is 13.4%；Test gained light shield is fire-retardant
The visible light transmittance of aqueous polyurethane is 92.2%；The glossiness of test gained light shield extinguishing waterborn polyurethane is 120.7；
The LOI index of test gained light shield extinguishing waterborn polyurethane film is 30.1%.
Embodiment 2:
Take 2.34g hydrophilic nano TiO2, by its under the conditions of 80 DEG C of temperature it is dry for 24 hours, will with 100.00gPPG,
35.38gOP550 and 73.17gIPDI is added in the four-hole boiling flask equipped with thermometer, and nitrogen is passed through into reaction system, by four
Reaction system is reacted 3 hours in the oil bath environment that mouth flask is placed at 85 DEG C；Then, it is added 12.92g's into reaction system
The acetone of DMPA and 234.39g, the reaction was continued 3 hours；Then 40 DEG C are cooled to, the TEA that 12.92g is added carries out neutralization reaction
30 minutes, stops logical nitrogen, obtain the performed polymer product for being dissolved in acetone；After revolving removes acetone, the performed polymer of 210.00g is taken out
The deionized water of 490.00g is added in product, shears emulsified 30 minutes in the stirring of 3000rpm, obtains light shield extinguishing waterborn
Polyurethane.
The uv transmittance of test gained light shield extinguishing waterborn polyurethane: 11.9%；Test gained light shield is fire-retardant
The visible light transmittance of aqueous polyurethane is 89.6%；The glossiness of test gained light shield extinguishing waterborn polyurethane is 115.8；
The LOI index of test gained light shield extinguishing waterborn polyurethane film is 30.4%.
Embodiment 3:
Take the hydrophily TiO of 6.00g2, by its 80 DEG C at a temperature of it is dry for 24 hours, PPG, 45.37g with 100.00g
OP550 and the IPDI of 121.54g be added in the four-hole boiling flask equipped with thermometer, nitrogen is passed through into reaction system, by four
Mouth flask is placed in the oil bath environment at 85 DEG C, reacts reaction system 3 hours；Then, be added 16.54g DMPA and
The acetone of 299.99g, the reaction was continued 3 hours；Then 40 DEG C are cooled to, the TEA that 16.54g is added is carried out neutralization reaction 30 minutes,
Stop logical nitrogen, obtains the performed polymer product for being dissolved in acetone；After revolving removes acetone, the performed polymer product of 240.00g is taken out, is added
The deionized water for entering 560.00g is sheared emulsified 30 minutes in the stirring of 3000rpm, obtains light shield extinguishing waterborn polyurethane.
The uv transmittance of test gained light shield extinguishing waterborn polyurethane: 10.5%；Test gained light shield is fire-retardant
The visible light transmittance of aqueous polyurethane is 90.8%；The glossiness of test gained light shield extinguishing waterborn polyurethane is 103.4；
The LOI index of test gained light shield extinguishing waterborn polyurethane film is 30.6%.
Comparative example 1:
Hydrophilic nano TiO is not added in this comparative example2, rest materials are same as Example 2 with step, compared with this
Light shield extinguishing waterborn polyurethane is prepared in the method for example.
The uv transmittance 62.7% of test gained light shield extinguishing waterborn polyurethane；Test gained light shield flame-retardant water
Property polyurethane visible light transmittance be 92.5%；The glossiness of test gained light shield extinguishing waterborn polyurethane is 109.2；It surveys
The LOI index of examination gained light shield extinguishing waterborn polyurethane film is 29.3%.
Comparative example 2:
Soft segment flame-proof modifier is not added in this comparative example, rest materials are same as Example 2 with step, compared with this
Light shield extinguishing waterborn polyurethane is prepared in the method for example.
The uv transmittance of test gained light shield extinguishing waterborn polyurethane: 11.2%；Test gained light shield is fire-retardant
The visible light transmittance of aqueous polyurethane is 91.6%；The glossiness of test gained light shield extinguishing waterborn polyurethane is 107.8；
The LOI index of test gained light shield extinguishing waterborn polyurethane film is 26.7%.
Test method in above-described embodiment is as follows:
The test of LOI value: referring to GB/T 5454-1997 combustibility oxygen index method, with TTech-GBT2406-2 type intelligence
Critical oxygen index analyzer (Tyke (Suzhou) detecting instrument Science and Technology Ltd. is thought by Thailand) is tested.By embodiment 1-3 and right
The light shield extinguishing waterborn polyurethane that ratio 1-2 is obtained stands 5-7 days in polyfluortetraethylene plate at room temperature and forms a film naturally, to
Moisture places into vacuum oven vacuum drying 24 hours at 80 DEG C after slowly volatilizing, obtain a kind of light shield flame-retardant water
Property polyurethane film.150 × 50mm is made in light shield extinguishing waterborn polyurethane film2Batten, every group 15, flame of getting fire is away from top
Hold oxygen concentration when just extinguishing at 50mm for the oxygen index (OI) of institute's test sample item.
Light transmission rate test: embodiment is obtained into light shield extinguishing waterborn polyurethane and is diluted to 1% with deionized water, is obtained
Lotion tests the light transmission rate of lotion using F-2500 type ultra-violet and visible spectrophotometer (Hitachi, Japan),
The quartz colorimetric utensil for selecting 10 × 10 × 50mm3, is tested at room temperature.
Glossiness test: by embodiment obtain light shield extinguishing waterborn polyurethane spin-coating method coated in 25.6 × 72.4 ×
The glass slide of 2mm3, after 60 DEG C of vacuum drying, using the small-sized 60 ° of gloss meters of Ref101N (Sheen company, Britain), in room
Under temperature, the glossiness of lotion is tested, 60 ° of glossiness of glass slide are 154.2.
The laboratory the SDF400 Multi-functional dispersion machine that stirring shearing is produced using Shanghai Farfly Energy Technology Co., Ltd
It completes, the use of temperature is room temperature.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention
It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Various changes and improvements, should all fall into claims of the present invention determine protection scope in.
Claims (10)
1. a kind of light shield extinguishing waterborn polyurethane, which is characterized in that raw material includes following component: photomask agent, polyethers binary
Alcohol, soft segment flame-proof modifier, isocyanates, antalkali and hydrophilic chain extender；
Wherein, in the isocyanates-the OH in-NCO group and polyether Glycols, soft segment flame-proof modifier and hydrophilic chain extender
The molar ratio of group is 1.1:1~2.0:1；
In the quality and polyether Glycols, soft segment flame-proof modifier, hydrophilic chain extender, isocyanates and alkalinity of the photomask agent
Ratio with agent quality summation is 1:1000~2:100.
2. a kind of light shield extinguishing waterborn polyurethane according to claim 1, it is characterised in that: the antalkali with
The additive amount of hydrophilic chain extender is identical, is 5.5% of the other components quality summation in addition to photomask agent.
3. a kind of light shield extinguishing waterborn polyurethane according to claim 1, it is characterised in that: photomask agent is hydrophilic receives
Rice titanium dioxide or hydrophilic zinc oxide.
4. a kind of light shield extinguishing waterborn polyurethane according to claim 1, it is characterised in that: the isocyanates is rouge
Fat race polyisocyanates and/or aromatic polyisocyanate.
5. a kind of light shield extinguishing waterborn polyurethane according to claim 1, it is characterised in that: the hydrophilic chain extender is
2,2- hydroxymethyl propionic acid, 2,2- hydroxymethylbutyrate, 1,2- propylene glycol -3-3 sodium sulfonate, 1,4- butanediol -2- sodium sulfonate, N, N- bis-
Methyl diethanolamine, benzyl dimethyl (2- ethoxy) ammonium chloride, dodecyl dimethyl (2- ethoxy) ammonium bromide, polyoxygenated
Ethylene glycol, Glycerin polyethylene glycol monoether, N, N- dimethyl-N-(2- ethoxy) glycine betaine or N- methyl-N, N- bis-
(2- ethoxy) glycine betaine.
6. a kind of light shield extinguishing waterborn polyurethane according to claim 1, it is characterised in that: the soft segment is flame-retardant modified
Agent is phosphorous polyether polyol.
7. a kind of preparation method of light shield extinguishing waterborn polyurethane as claimed in any one of claims 1 to 6, which is characterized in that
Include the following steps:
Photomask agent, polyether Glycols, soft segment flame-proof modifier and isocyanates are added to reaction vessel, into reaction system
It is passed through inert gas or nitrogen and keeps, reacted 2.5~3.5 hours in 80~90 DEG C of oil bath；Be added hydrophilic chain extender and
Solvent, the reaction was continued 2.5~3.5 hours, is cooled to 35~45 DEG C, and antalkali is added and carries out neutralization reaction, stops being passed through
Inert gas or nitrogen obtain the performed polymer product for being dissolved in solvent；After revolving removes solvent, performed polymer product, Xiang Qi are isolated
Middle addition deionized water stirs the emulsified 30~40min of shearing condition, obtains product.
8. preparation method according to claim 7, which is characterized in that the quality and polyether Glycols, soft segment of the solvent
Flame-proof modifier, isocyanates, the gross mass of hydrophilic chain extender and antalkali are equal.
9. preparation method according to claim 7, which is characterized in that the rate of the stirring shearing is 3000-
3500rpm。
10. preparation method according to claim 7, which is characterized in that the solvent is acetone, butanone, ethyl acetate, two
Chloromethanes, tetrahydrofuran or N,N-dimethylformamide；The antalkali be ammonium hydroxide, 2-amino-2-methyl-1-propanol,
Diethanol amine, triethanolamine, diethylamine, triethylamine, sodium hydroxide, potassium hydroxide, sodium bicarbonate, sodium acetate, sodium pyrophosphate or
Sodium carbonate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116239752A (en) * | 2023-03-24 | 2023-06-09 | 浙江梅盛新材料有限公司 | Preparation method of bio-based aqueous polyurethane, textile and leather |
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|---|---|---|---|---|
| CN102199274A (en) * | 2011-04-14 | 2011-09-28 | 武汉纺织大学 | Preparation method of nanometer in situ composite reaction type organic silicone modified cationic water-based polyurethane and product thereof |
| CN103073696A (en) * | 2013-01-30 | 2013-05-01 | 段宝荣 | Preparation method of light-resistant waterborne polyurethane |
| CN106432676A (en) * | 2016-09-28 | 2017-02-22 | 齐鲁工业大学 | Preparation method of N/P/nano synergistic flame-retardant waterborne polyurethane dispersion liquid |
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2019
- 2019-01-11 CN CN201910026028.5A patent/CN109721704A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199274A (en) * | 2011-04-14 | 2011-09-28 | 武汉纺织大学 | Preparation method of nanometer in situ composite reaction type organic silicone modified cationic water-based polyurethane and product thereof |
| CN103073696A (en) * | 2013-01-30 | 2013-05-01 | 段宝荣 | Preparation method of light-resistant waterborne polyurethane |
| CN106432676A (en) * | 2016-09-28 | 2017-02-22 | 齐鲁工业大学 | Preparation method of N/P/nano synergistic flame-retardant waterborne polyurethane dispersion liquid |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116239752A (en) * | 2023-03-24 | 2023-06-09 | 浙江梅盛新材料有限公司 | Preparation method of bio-based aqueous polyurethane, textile and leather |
| CN116239752B (en) * | 2023-03-24 | 2024-04-30 | 浙江梅盛新材料有限公司 | Preparation method of bio-based aqueous polyurethane, textile and leather |
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