CN105133347B - A kind of preparation method and application of resistance to hydrostatic pressure extinguishing waterborn polyurethane - Google Patents
A kind of preparation method and application of resistance to hydrostatic pressure extinguishing waterborn polyurethane Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method and application of resistance to hydrostatic pressure extinguishing waterborn polyurethane, belongs to technical field of textile chemical engineering.Methods described step is as follows：Vacuum dehydration after polyether Glycols, hydrophilic chain extender are mixed with trihydroxy polyethers, under nitrogen protection, adds solvent dilution, adds aromatic isocyanates and reacted, obtain performed polymer A；To in performed polymer A, add response type phosphonium flame retardant to be reacted, obtain solution B；To in solution B, add lipophile chain extender to be reacted, obtain solution C；To in solution C in addition triethylamine with after, stirring is lower to add deionized water emulsifying, standing then to remove solvent, obtain the aqueous polyurethane.The aqueous polyurethane of preparation can be applied to textile as textile coating agent and cover with paint, lacquer, colour wash, etc. field, and when being particularly applied to low elastic polyester filament coating, resistance to hydrostatic pressure performance is good, and its resistance to hydrostatic pressure value can reach 10～23KPa；Good flame retardation effect, can pass through the B1 levels during 1997 textile combustion performance vertical methods of GB/T5455 are tested.
Description
Technical field
The present invention relates to a kind of preparation method and application of resistance to hydrostatic pressure extinguishing waterborn polyurethane, belongs to weaving Chemical Engineering Technology
Field.
Background technology
Waterborne Polyurethane Fabric Coatings are a kind of macromolecule compounds that can be spread evenly across fabric face, can be led to
Crossing adhesive effect and one or more layers thin film being formed in fabric face, it can not only improve appearance of fabrics and style, and can make
Fabric functional so as to the specific function such as waterproof, moisture-inhibiting, fire-retardant.Aqueous polyurethane is with water as dispersant, friendly with environment
Good, nontoxic, safe the advantages of.However, there is many lacking in the covering with paint application of textile in the single aqueous polyurethane of feature
Point, such as resistance to hydrostatic pressure ability, inflammable, weatherability are poor etc., and the combination property of material cannot meet the demand of people.Therefore, grind
Study carefully the functional modification of aqueous polyurethane, make aqueous polyurethane be provided simultaneously with resistance to hydrostatic pressure and the function such as fire-retardant, both met fabric
The development trend of coating agent, can also meet demand of the people to material, with huge economic and social benefit prospect.
The preparation method of the high hydrostatic pressure resistance anion aqueous polyurethane textile coating agent that patent CN102418274B is announced,
The polyurethane loomage coating agent is that the form of emulsion process is prepared from addition in the presence of emulsifying agent dodecylbenzene sodium sulfonate,
This kind of method since it is desired that additional emulsifying agent easily make Waterborne Polyurethane Fabric Coatings storage it is unstable, affect application performance (such as
Feel, mechanical property etc.), and because the polyurethane loomage coating agent is linear structure, the lasting holding of its resistance to hydrostatic pressure
There are problems that larger.In the article that Li Haibei et al. is delivered (Li Haibei magnifies human relations, Luo Yunjun etc. high hydrostatic pressure resistance it is cloudy from
The development [J] of subtype Waterborne Polyurethane Fabric Coatings. printing and dyeing assistant, 2004,21 (1)：45-47), although employ interior crosslinking
Technology is prepared for the Waterborne Polyurethane Fabric Coatings with high hydrostatic pressure resistance, and resistance to hydrostatic pressure value is up to 21600Pa, but the friendship
It is excessive that the addition of connection agent easilys lead to prepolymerization reaction viscosity so that reaction is difficult to control to.Chen He of seminar of Luo Yun armies etc. is adopted
A series of halogen-free flameproof aqueous polyurethane, fire-retardant effect are synthesized with a kind of phosphorous response type halogen-free flame retardants ExolitOP550
It is really relatively good, the B1 levels during GB/T5455-1997 textile combustion performance verticals method is tested can be passed through, but, its resistance to hydrostatic
Pressure energy power can not meet market use requirement.
At present, the polyurethane for being provided simultaneously with resistance to hydrostatic pressure performance and fire resistance yet there are no someone's report.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane
Preparation method and application, aqueous polyurethane storage stability prepared by methods described are good, and asepsis environment-protecting possesses fire-retardant and resistance to hydrostatic
Pressure dual-use function, can be applied to textile as textile coating agent and cover with paint, lacquer, colour wash, etc. field.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of resistance to hydrostatic pressure extinguishing waterborn polyurethane textile coating agent, methods described step are as follows：
Step one, polyether Glycols, hydrophilic chain extender are mixed with trihydroxy polyethers after, the vacuum at 100～120 DEG C
0.5～1.5h of dehydration；
Step 2,60～75 DEG C are naturally cooling to, under nitrogen protection, add solvent dilution, add aromatic different
Cyanate, removes nitrogen and temperature of reaction system is risen to 75～90 DEG C and reacted, with di-n-butylamine method test-NCO content,
React to-NCO content and be close to theoretical value, obtain performed polymer A；
Step 3, in performed polymer A add response type phosphonium flame retardant reacted, with di-n-butylamine method test-NCO contain
Amount, reacts to-NCO content and is close to theoretical value, obtain solution B；
Step 4, in solution B lipophile chain extender is added to be reacted, with di-n-butylamine method test-NCO content, instead
Theoretical value should be close to-NCO content, obtain solution C；
After step 5, solution C are down to room temperature, triethylamine neutralization is added, after 0.5～5min of reaction, in 2000～3000r/
Min stirrings are lower to add 0～10 DEG C of deionized water to carry out emulsifying, stands 8～12h, then removes solvent, obtains the aqueouss and gather
Urethane.
In the corresponding reaction system of theoretical value of described-NCO content, after hydroxyl reacts completely ,-NCO is remaining to be contained
Amount.
Counted with reaction raw materials gross mass as 100%, needed for reaction, each component mass percent is：Polyether Glycols 27.8
～43.3%, trihydroxy polyethers 5.4～11.5%, hydrophilic chain extender 5.54～6.76%, aromatic isocyanates 23.4
～34.8%, response type phosphonium flame retardant 10.0～20.0%, lipophile chain extender 1.2～1.5% and triethylamine 4.2～
5.2%.
The deionized water is 1.86～2.33 with reaction raw materials total mass ratio:1.
The polyether Glycols are polytetrahydrofuran diol (PTMG) and/or polypropylene glycol (PPG).
The hydrophilic chain extender is dihydromethyl propionic acid or dimethylolpropionic acid.
The solvent is acetone, butanone or tetrahydrofuran.
The aromatic isocyanates are liquefaction methyl diphenylene diisocyanate (liquefied mdi), diphenyl methane two
Isocyanates (MDI) or toluene di-isocyanate(TDI) (TDI).
The preferred Germany Clariant ExolitOP550 of the response type phosphonium flame retardant.
The lipophile chain extender is 1,4- butanediols, diglycol, trimethylolpropane or tetramethylolmethane.
A kind of application of resistance to hydrostatic pressure extinguishing waterborn polyurethane of the present invention, prepared aqueous polyurethane can conduct
Textile coating agent is applied to textile and covers with paint, lacquer, colour wash, etc. field.
Beneficial effect
According to the method for the invention prepare aqueous polyurethane storage stability is good, asepsis environment-protecting and possess fire-retardant and resistance to
Hydrostatic pressing dual-use function；After being applied to textile finishing, have the advantages that coating transparent, good hand touch, caking property are good and safe.Especially
Which is that, when which is applied to low elastic polyester filament is coated with, its resistance to hydrostatic pressure value can reach 10～23KPa, meet market use requirement；
Good flame retardation effect, can pass through the B1 levels during GB/T5455-1997 textile combustion performance verticals method is tested.
Specific embodiment
With reference to specific embodiment, the present invention is further elaborated.
In following examples：
Agents useful for same and instrument：
Reaction vessel used is the four-hole boiling flask with tetrafluoro stirring paddle；
Di-n-butylamine method measure-NCO content：The sample for accurately weighing 3g or so is put in clean conical flask, adds 20mL
Dry toluene, dissolves sample, pipettes 10.00mL di-n-butylamines-toluene solution with pipet, and rocking makes liquid mixing in bottle equal
Even, room temperature places 25min, adds 45mL isopropanols, adds a few drop bromocresol greens to be indicator, molten with 0.5mol/L HCl standards
Drop is fixed, when solution by the blue yellow that becomes into terminal, and does blank assay.Its computing formula is：
W in formula-NCOThe mass fraction of-NCO in-reaction system；
V0- blank titration consumes the volume of hydrochloric acid standard solution, mL；
V1The titration of-sample consumes the volume of hydrochloric acid standard solution, mL；
The concentration of c-hydrochloric acid standard solution, mol/L；
M-sample quality, g；
The molal weight of 42-- NCO, g/mol.
Embodiment 1
PTMG, 4.05g trihydroxy polyethers N330 and 4.6g dihydromethyl propionic acid that 21g molecular weight is 2000 is taken in four mouthfuls
In flask, after 120 DEG C of dehydrated under vacuum 1h, 60 DEG C are naturally cooling to, lead to nitrogen, condensing reflux pipe is installed, add the fourth of 40g
Ketone, after temperature stabilization, constant pressure funnel Deca 26.25g liquefied mdi controls speed, 0.5h or so and adds, removes nitrogen,
75 DEG C are warming up to, about 2h is reacted, during detection shows solution-NCO content is close to theoretical value, adds 15.1g ExolitOP550,
Reaction about 3h, during detection shows solution-NCO content is close to theoretical value, adds 1g BDOs, reacts about 1h, detection is aobvious
In showing solution-NCO content is close to theoretical value, is down to room temperature, in adding 3.5g triethylamines and after 30s, stir in 2000r/min
Lower addition 140g temperature is that 0 DEG C of deionized water carries out emulsifying, stands 12h.Butanone is removed with Rotary Evaporators, aqueouss is obtained and is gathered
Urethane.
The aqueous polyurethane 40g for obtaining, then adds 3 drop ammonia, 1 drop defoamer K3 and 1g thickening agent 601H,
After stirring, it is coated on low elastic polyester filament, after coating, makes low elastic polyester filament weightening 30g/m2.Determined with digital seepage of water
Instrument is tested to the low elastic polyester filament after coating, and its resistance to hydrostatic pressure meansigma methods is 19886Pa.Low elastic polyester filament after coating can
B1 levels in being tested by GB/T5455-1997 textile combustion performance verticals method.
Embodiment 2
PTMG, 6.35g trihydroxy polyethers N330 and 4.6g dimethylolpropionic acid that 33g molecular weight is 2000 is taken in four mouthfuls
In flask, after 100 DEG C of dehydrated under vacuum 1.5h, 70 DEG C are naturally cooling to, lead to nitrogen, condensing reflux pipe is installed, add the four of 40g
Hydrogen furan, after temperature stabilization, constant pressure funnel Deca 26.25g MDI controls speed, 0.5h or so and adds, removes nitrogen
Gas, is warming up to 85 DEG C, reacts about 1.5h, during detection shows solution-NCO content is close to theoretical value, adds 8.3g
ExolitOP550, reacts about 3h, during detection shows solution-NCO content is close to theoretical value, adds 1g BDOs, instead
Should about 0.5h, during detection shows solution-NCO content is close to theoretical value, is down to room temperature, in adding 3.5g triethylamines and 5min
Afterwards, under 2500r/min stirrings add the deionized water that 154g temperature is 0 DEG C to carry out emulsifying, stand 8h.Removed with Rotary Evaporators
Tetrahydrofuran is removed, aqueous polyurethane is obtained.
The aqueous polyurethane 40g for obtaining, then adds 3 drop ammonia, 1 drop defoamer K3 and 1g thickening agent 601H,
After stirring, it is coated on low elastic polyester filament, after coating, makes low elastic polyester filament weightening 30g/m2.Determined with digital seepage of water
Instrument is tested to the low elastic polyester filament after coating, and its resistance to hydrostatic pressure meansigma methods is 22387Pa.Low elastic polyester filament after coating can
B1 levels in being tested by GB/T5455-1997 textile combustion performance verticals method.
Embodiment 3
Take PPG, 9g trihydroxy polyethers N330 and 4.6g dihydromethyl propionic acid that 33.8g molecular weight is 2000 to burn in four mouthfuls
In bottle, after 100 DEG C of dehydrated under vacuum 1.5h, 75 DEG C are naturally cooling to, lead to nitrogen, condensing reflux pipe is installed, add 50g tetrahydrochysene furans
Mutter, after temperature stabilization, constant pressure funnel Deca 18.3gTDI controls speed, 0.5h or so and adds, remove nitrogen, heats up
To 80 DEG C, about 2h is reacted, during detection shows solution-NCO content is close to theoretical value, adds 7.8g ExolitOP550, react
About 3.5h, during detection shows solution-NCO content is close to theoretical value, adds 1g diglycols, reacts about 1h, detection is aobvious
In showing solution-NCO content is close to theoretical value, is down to room temperature, in adding 3.5g triethylamines and after 2min, stir in 3000r/min
Mixing the deionized water that lower addition 182g temperature is 10 DEG C carries out emulsifying, stands 10h.Tetrahydrofuran is removed with Rotary Evaporators, is obtained
To aqueous polyurethane.
The aqueous polyurethane 40g for obtaining, then adds 3 drop ammonia, 1 drop defoamer K3 and 1g thickening agent 601H,
After stirring, it is coated on low elastic polyester filament, after coating, makes low elastic polyester filament weightening 30g/m2.Determined with digital seepage of water
Instrument is tested to the low elastic polyester filament after coating, and its resistance to hydrostatic pressure meansigma methods is 17935Pa.Low elastic polyester filament after coating can
B1 levels in being tested by GB/T5455-1997 textile combustion performance verticals method.
Embodiment 4
Take PPG, 5g trihydroxy polyethers N330 that PTMG, 12.35g molecular weight that 20g molecular weight is 2000 is 2000 and
4.6g dimethylolpropionic acids after 120 DEG C of dehydrated under vacuum 0.5h, are naturally cooling to 70 DEG C in four-hole boiling flask, lead to nitrogen, install
Condensing reflux pipe, adds 50g acetone, and after temperature stabilization, constant pressure funnel Deca 18.3g TDI controls speed, and 0.5h is left
The right side adds, and removes nitrogen, is warming up to 90 DEG C, reacts about 1.5h, during detection shows solution-NCO content is close to theoretical value, and add
13.6gExolitOP550, reacts about 3h, during detection shows solution-NCO content is close to theoretical value, adds 1g trihydroxy methyls third
Alkane, reacts about 0.5h, during detection shows solution-NCO content is close to theoretical value, is down to room temperature, adds the neutralization of 3.5g triethylamines
After 30s, under 3000r/min stirrings add the deionized water that 158g temperature is 0 DEG C to carry out emulsifying, stand 12h.Use rotary evaporation
Instrument removes acetone, obtains aqueous polyurethane.
The aqueous polyurethane 40g for obtaining, then adds 3 drop ammonia, 1 drop defoamer K3 and 1g thickening agent 601H,
After stirring, it is coated on low elastic polyester filament, after coating, makes low elastic polyester filament weightening 30g/m2.Determined with digital seepage of water
Instrument is tested to the low elastic polyester filament after coating, and its resistance to hydrostatic pressure meansigma methods is 10965Pa.Low elastic polyester filament after coating can
B1 levels in being tested by GB/T5455-1997 textile combustion performance verticals method.
The present invention includes but is not limited to above example, every any equivalent carried out under the principle of spirit of the present invention
Replace or local improvement, all will be regarded as within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of resistance to hydrostatic pressure extinguishing waterborn polyurethane, it is characterised in that：Methods described step is as follows：
Step one, polyether Glycols, hydrophilic chain extender are mixed with trihydroxy polyethers after, the vacuum dehydration at 100～120 DEG C
0.5～1.5h；
Step 2,60～75 DEG C are naturally cooling to, under nitrogen protection, add solvent dilution, add aromatic Carbimide.
Ester, removes nitrogen and temperature of reaction system is risen to 75～90 DEG C and reacted, and with di-n-butylamine method test-NCO content, reacts
Extremely-NCO content is close to theoretical value, obtains performed polymer A；
Step 3, in performed polymer A response type phosphonium flame retardant is added to be reacted, with di-n-butylamine method test-NCO content,
React to-NCO content and be close to theoretical value, obtain solution B；
Step 4, in solution B add lipophile chain extender to be reacted, with di-n-butylamine method test-NCO content, react to-
NCO content is close to theoretical value, obtains solution C；
After step 5, solution C are down to room temperature, triethylamine neutralization are added, after 0.5～5min of reaction, is stirred in 2000～3000r/min
Mixing the lower deionized water for adding 0～10 DEG C carries out emulsifying, stands 8～12h, then removes solvent, obtain the aqueous polyurethane；
In the corresponding reaction system of theoretical value of described-NCO content, after hydroxyl reacts completely ,-NCO remaining content；
Counted with reaction raw materials gross mass as 100%, needed for reaction, each component mass percent is：Polyether Glycols 27.8～
43.3%, trihydroxy polyethers 5.4～11.5%, hydrophilic chain extender 5.54～6.76%, aromatic isocyanates 23.4～
34.8%, response type phosphonium flame retardant 10.0～20.0%, lipophile chain extender 1.2～1.5% and triethylamine 4.2～
5.2%；
The deionized water is 1.86～2.33 with reaction raw materials total mass ratio:1.
2. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Polyether Glycols are polytetrahydrofuran diol and/or polypropylene glycol.
3. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Hydrophilic chain extender is dihydromethyl propionic acid or dimethylolpropionic acid.
4. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Solvent is acetone, butanone or tetrahydrofuran.
5. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Aromatic isocyanates are liquefaction methyl diphenylene diisocyanate or toluene di-isocyanate(TDI).
6. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Response type phosphonium flame retardant is German Clariant ExolitOP550.
7. the preparation method of a kind of resistance to hydrostatic pressure extinguishing waterborn polyurethane according to claim 1, it is characterised in that：It is described
Lipophile chain extender is 1,4- butanediols, diglycol, trimethylolpropane or tetramethylolmethane.
8. a kind of application of resistance to hydrostatic pressure extinguishing waterborn polyurethane as claimed in claim 1, it is characterised in that：Prepared water
Property polyurethane can as textile coating agent be applied to textile cover with paint, lacquer, colour wash, etc. field.
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| CN102226314A (en) * | 2011-04-29 | 2011-10-26 | 北京理工大学 | Environmentally-friendly halogen-free reaction type soft and hard segment co-modified flame retardant waterborne polyurethane fabric coating agent and preparation method thereof |
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| CN104018354A (en) * | 2014-06-24 | 2014-09-03 | 北京理工大学 | Hyperbranched waterborne polyurethane/organic phosphorus hard segment flame-retardant modified waterborne polyurethane coating agent and preparation method thereof |
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