CN109679327A - A kind of nano-organosilicon composite polyurethane water-proof emulsion - Google Patents
A kind of nano-organosilicon composite polyurethane water-proof emulsion Download PDFInfo
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- CN109679327A CN109679327A CN201811596318.5A CN201811596318A CN109679327A CN 109679327 A CN109679327 A CN 109679327A CN 201811596318 A CN201811596318 A CN 201811596318A CN 109679327 A CN109679327 A CN 109679327A
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
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- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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Abstract
The invention discloses a kind of nano-organosilicon composite polyurethane water-proof emulsions, it is characterised in that: is combined by nano-organosilicon lotion with aqueous polyurethane emulsion, by percentage to the quality, nano-organosilicon lotion is 34-47%, aqueous polyurethane emulsion 53-66%；The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer, mono-vinyl organic silicon monomer, emulsifier, water, initiator are made through emulsion polymerization；The aqueous polyurethane emulsion is made of polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy silane monomer, triethylamine, ethylenediamine, catalyst, organic solvent, water reaction.The hydrophobicity of textile surface can be by increasing its rough overshoot or in surface modification low-surface energy substance.Using polysiloxanes as low-surface-energy material, nano silica, which constructs roughness, had not only realized good water repellency in conjunction with aqueous polyurethane, but also improved the adhesive force of organosilicon.
Description
Technical field
The present invention relates to a kind of water-proof emulsions, are combined with nano-organosilicon lotion with polyaminoester emulsion, belong to nanometer
Field of functional materials.
Background technique
Polyurethane is a kind of block polymer, generally constitutes segment by the long flexible chain of oligomer dihydric alcohol, by polyisocyanate cyanogen
Acid esters and chain extender constitute hard section, have many advantages, such as that wear-resisting, flexibility is good, adhesive force is strong, are widely used in textile field.Cause
For the reason of environmental protection, aqueous polyurethane is gradually instead of solvent borne polyurethane.Contain a large amount of water in the macromolecular chain of aqueous polyurethane
Soluble group, water resistance, in terms of it is slightly insufficient.
Proposed adoption nano-organosilicon lotion of the present invention is waterborne polyurethane modified to carrying out, and Si-O-Si, Si-C are introduced lotion
System, drop low-surface-energy improve thermal stability, improve the weatherability, water resistance and mechanical property of polyurethane.
Summary of the invention
It is an object of the present invention to provide a kind of nano-organosilicon composite polyurethane water-proof emulsions, with nano-organosilicon lotion and water
Property polyaminoester emulsion composite, to promote aqueous polyurethane correlated performance.
To achieve the above object, the technical solution adopted by the present invention is as follows.
A kind of nano-organosilicon composite polyurethane water-proof emulsion, it is compound by nano-organosilicon lotion and aqueous polyurethane emulsion
It forms, by percentage to the quality, nano-organosilicon lotion is 34-47%, aqueous polyurethane emulsion 53-66%；
The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer are (such as 1 institute of formula
Show), mono-vinyl organic silicon monomer (as shown in Equation 2), emulsifier, water, initiator be made through emulsion polymerization；
(H3C)3Si-O-CH2CH2NH-CH2CH=CH2Formula 2
The aqueous polyurethane emulsion is by polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy base silane list
Body (as shown in Equation 3), triethylamine, ethylenediamine, catalyst, organic solvent, water reaction are made；
The vinyl Nano-meter SiO_22Colloidal sol is made, method of vinyl silicane coupling agent, catalyst, water, emulsifier
It is as follows: 6 parts of Silane coupling reagent KH-570s, 1.4 parts of lauryl sodium sulfate, 1.8 parts of AEO-7,0.8 part of PEG-400 are added to
In 100 parts of water, stirring, dispersion are persistently stirred to react 4h then at 2.5 parts of ammonium hydroxide are added with stirring, and form vinyl Nano-meter SiO_22
Colloidal sol.
The nano-organosilicon lotion, the preparation method is as follows:
(1) 250 parts of water, 18 parts of vinyl Nano-meter SiO_2s are added into emulsifier2Colloidal sol, 24 parts of both-end alkenyl organosilicon lists
Body, 21 parts of mono-vinyl organic silicon monomers and 2 parts of AEO-9,2 parts of AEO-7,4 parts of neopelexes continue stirring and emulsifying
0.5h, at pre-emulsion；
(2) it takes half pre-emulsion to be placed in the reactor with temperature control, stirring and condensing unit, is added at 80 DEG C
The solution of 0.2 part of initiator and 4 parts of water, insulation reaction 0.5h；
(3) the other half pre-emulsion is placed in constant pressure funnel, is slowly dropped into reaction system, while being added dropwise 0.4
The solution of part initiator and 10 parts of water, drips off for about 2 hours, controls 80 DEG C of temperature, then react 2 hours, obtains nano-organosilicon lotion；
The aqueous polyurethane emulsion, the preparation method is as follows:
A, by 180 parts of polyether Glycols (N220) be added with blender, condenser, N2 protection and thermometer reactor
In, under 60 DEG C, stirring, 52 parts of IPDI are added, are warming up to 70 DEG C of reaction 1.5h；
B, 9.4 parts of DMPA for being dissolved in DMF are added, 0.28 part of dibutyl tin dilaurate is stirred to react 0.5h at 75 DEG C；
C, 55 DEG C are cooled to, 7 parts of dihydroxy silane monomers (as shown in Equation 3) are slowly added to, reaction to NCO reaches theoretical value,
Aggravate it is strong be added with stirring 6 parts of TEA, persistently stir 0.5h；
D, 25 DEG C are cooled to, 384 parts of deionized waters are added, quickly stir 15min, adds 2.4 parts of ethylenediamines, is reacted
1.5h；
E, vacuum removal acetone obtains aqueous polyurethane emulsion.
The initiator is one of sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate.
Organosilicon is widely used in textile, soft fabric, slippery feel is assigned, and organosilyl surface can be low, through it
The fabric of processing can get good hydrophobicity.But organosilicon is the adhesive force of fabric surface is weak, washability is poor.
Viscoelastic polyurethane puts forth effort by force, have good toughness, by the way that the property, it can be achieved that two kinds of materials of organic silicon polyurethane is blended
The complementation of energy.
Contain highly polar carbamate groups, urea groups in polyurethane molecular chain, there is strong cohesive force to fabric, it is organic
Silicon and polyurethane it is compound, while assigning fabric good water repellency, improve good with fabric when multiple emulsion film forming
Adhesive property.When lotion is handled fabric, in fabric surface film forming procedure, energy low silicone segments in surface are moved to surface
It moves, preferable water repellency is provided；Polyurethane segment then forms hydrogen bond by its polar group and fabric and chemical bond generates by force
Bonding, and then reach excellent water repellency and adhesive property.
The hydrophobicity of textile surface can be by increasing the rough overshoot on its surface or in its surface modification low-surface energy substance.
The present invention is using polysiloxanes as low-surface-energy material, nano silica (SiO2) construction roughness, in conjunction with aqueous polyurethane, both
Good water repellency is realized, and improves the adhesive force of organosilicon.
It participates in emulsion polymerization and is mostly vinylsiloxane coupling agent for improving the silicon-containing monomer of emulsion property, due to containing
There is hydrolyzable groups Si-O-C, in emulsion polymerization process, a degree of hydrolysis, condensation can occur for these groups, to make
It is excessively crosslinked between polymer molecule and leads to polymerization reaction unstability.Although in the course of the polymerization process, being added dropwise using delay, addition hydrolyzes
Inhibitor is still difficult to obtain effective modified effect.Present invention employs Si (CH3)3The organic-silicon-modified monomer of group, due to
Its steric hindrance is big, does not hydrolyze, and substantially increases the stability of emulsion polymerization, increases the content of silicon in polymer, and makes to have
Distribution of the machine silicon in polymer molecular chain is more balanced, effectively enhances the water repellency of polymer.
Specific embodiment
Substance unit " part " of the present invention refers to " mass parts ".
The system of both-end alkenyl organic silicon monomer, mono-vinyl organic silicon monomer, dihydroxy organic silicon monomer involved by the present invention
Preparation Method is as follows.
The preparation method of both-end alkenyl organic silicon monomer:
In the drying four-hole boiling flask equipped with thermometer, blender, a certain amount of 1,3- divinyl -1,1 of addition, 3,3-
Tetramethyl disiloxane and octamethylcy-clotetrasiloxane, warming while stirring to reaction temperature, and a certain amount of fluoroform is added
Base sulfonic acid, insulation reaction certain time.Anhydrous Na is added after reaction2CO3It is 6-7 that stirring, which is neutralized to pH, is filtered and by product
It is evaporated under reduced pressure (90 DEG C, vacuum degree -0.1Mpa or less), removes unreacted monomer, obtain colorless and transparent product liquid.It is involved
Reaction process is such as shown in (1).
Mono-vinyl organic silicon monomer, which is reacted by 2- (trimethylsiloxy group) ethanol amine with allyl chloride, to be made, preparation method
Are as follows:
In 250mL there-necked flask, sequentially add 1mol 2- (trimethylsiloxy group) ethanol amine, 1.5mol triethylamine and
100mL methylene chloride.There-necked flask is placed in ice-water bath, 1.2mol allyl chloride is slowly added dropwise at this temperature, drips
Reaction system is warming up to room temperature after finishing, and the reaction was continued at this temperature 1.5 hours, stops reaction, be filtered to remove triethylamine
After chlorate, vacuum distillation removes methylene chloride and excessive triethylamine, and the fraction collected, and obtains vinyl organosilicon monomer,
N-2 (trimethylsiloxy group) ethyl enamine.Involved reaction process is such as shown in (2).
Wherein, 2- (trimethylsiloxy group) ethanol amine the preparation method comprises the following steps: with mechanical stirring, thermometer reactor
In, ethanol amine is put into, agitation and dropping hexamethyldisilazane, in 5~50 DEG C of 0.5~2h of reaction, end of reaction is filtered through decompression
Obtain 2- (trimethylsiloxy group) ethanol amine.The molar ratio of ethanol amine and hexamethyldisilazane is 2:1.
The dihydroxy organic silicon monomer is reacted by diethanol amine, NaOH, trim,ethylchlorosilane to be made, and preparation method is such as
Under:
The NaOH aqueous solution of diethanol amine and 0.4mol/L are added to the three-necked flask with blender, reflux condensing tube
In, it is then slowly added to trim,ethylchlorosilane into flask, after charging, 80min is reacted at 70 DEG C, is evaporated under reduced pressure, removes
Extra water and unreacted diethanol amine are removed, N- diethanol-trimethyl silicane (dihydroxy organic silicon monomer) is obtained；Wherein, institute
The diethanol amine of addition and the molar ratio of trim,ethylchlorosilane are 1.1:1, and trim,ethylchlorosilane and NaOH molar ratio are 1:1.Instead
Answer process such as shown in (3).
Embodiment 1
A kind of nano-organosilicon composite polyurethane water-proof emulsion, it is compound by nano-organosilicon lotion and aqueous polyurethane emulsion
It forms, by percentage to the quality, nano-organosilicon lotion is 34%, aqueous polyurethane emulsion 66%；
The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer are (such as 1 institute of formula
Show), mono-vinyl organic silicon monomer (as shown in Equation 2), emulsifier, water, initiator be made through emulsion polymerization；
(H3C)3Si—O-CH2CH2NH-CH2CH=CH2Formula 2
The aqueous polyurethane emulsion is by polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy base silane list
Body (as shown in Equation 3), triethylamine, ethylenediamine, catalyst, organic solvent, water reaction are made；
The vinyl Nano-meter SiO_22Colloidal sol is made, method of vinyl silicane coupling agent, catalyst, water, emulsifier
It is as follows: 6 parts of Silane coupling reagent KH-570s, 1.4 parts of lauryl sodium sulfate, 1.8 parts of AEO-7,0.8 part of PEG-400 are added to
In 100 parts of water, stirring, dispersion are persistently stirred to react 4h then at 2.5 parts of ammonium hydroxide are added with stirring, and form vinyl Nano-meter SiO_22
Colloidal sol.
The nano-organosilicon lotion, the preparation method is as follows:
(1) 250 parts of water, 18 parts of vinyl Nano-meter SiO_2s are added into emulsifier2Colloidal sol, 24 parts of both-end alkenyl organosilicon lists
Body, 21 parts of mono-vinyl organic silicon monomers and 2 parts of AEO-9,2 parts of AEO-7,4 parts of neopelexes continue stirring and emulsifying
0.5h, at pre-emulsion；
(2) it takes half pre-emulsion to be placed in the reactor with temperature control, stirring and condensing unit, is added at 80 DEG C
The solution of 0.2 part of initiator and 4 parts of water, insulation reaction 0.5h；
(3) the other half pre-emulsion is placed in constant pressure funnel, is slowly dropped into reaction system, while being added dropwise 0.4
The solution of part initiator and 10 parts of water, drips off for about 2 hours, controls 80 DEG C of temperature, then react 2 hours, obtains nano-organosilicon lotion；
The aqueous polyurethane emulsion, the preparation method is as follows:
A, by 180 parts of polyether Glycols (N220) be added with blender, condenser, N2 protection and thermometer reactor
In, under 60 DEG C, stirring, 52 parts of IPDI are added, are warming up to 70 DEG C of reaction 1.5h；
B, 9.4 parts of DMPA for being dissolved in DMF are added, 0.28 part of dibutyl tin dilaurate is stirred to react 0.5h at 75 DEG C；
C, 55 DEG C are cooled to, 7 parts of dihydroxy silane monomers (as shown in Equation 3) are slowly added to, reaction to NCO reaches theoretical value,
Aggravate it is strong be added with stirring 6 parts of TEA, persistently stir 0.5h；
D, 25 DEG C are cooled to, 384 parts of deionized waters are added, quickly stir 15min, adds 2.4 parts of ethylenediamines, is reacted
1.5h；
E, vacuum removal acetone obtains aqueous polyurethane emulsion.
The initiator is sodium peroxydisulfate.
Embodiment 2
A kind of nano-organosilicon composite polyurethane water-proof emulsion, it is compound by nano-organosilicon lotion and aqueous polyurethane emulsion
It forms, by percentage to the quality, nano-organosilicon lotion is 41%, aqueous polyurethane emulsion 59%；
The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer are (such as 1 institute of formula
Show), mono-vinyl organic silicon monomer (as shown in Equation 2), emulsifier, water, initiator be made through emulsion polymerization；
(H3C)3Si-O-CH2CH2NH-CH2CH=CH2Formula 2
The aqueous polyurethane emulsion is by polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy base silane list
Body (as shown in Equation 3), triethylamine, ethylenediamine, catalyst, organic solvent, water reaction are made；
The vinyl Nano-meter SiO_22Colloidal sol is made, method of vinyl silicane coupling agent, catalyst, water, emulsifier
It is as follows: 6 parts of Silane coupling reagent KH-570s, 1.4 parts of lauryl sodium sulfate, 1.8 parts of AEO-7,0.8 part of PEG-400 are added to
In 100 parts of water, stirring, dispersion are persistently stirred to react 4h then at 2.5 parts of ammonium hydroxide are added with stirring, and form vinyl Nano-meter SiO_22
Colloidal sol.
The nano-organosilicon lotion, the preparation method is as follows:
(1) 250 parts of water, 18 parts of vinyl Nano-meter SiO_2s are added into emulsifier2Colloidal sol, 24 parts of both-end alkenyl organosilicon lists
Body, 21 parts of mono-vinyl organic silicon monomers and 2 parts of AEO-9,2 parts of AEO-7,4 parts of neopelexes continue stirring and emulsifying
0.5h, at pre-emulsion；
(2) it takes half pre-emulsion to be placed in the reactor with temperature control, stirring and condensing unit, is added at 80 DEG C
The solution of 0.2 part of initiator and 4 parts of water, insulation reaction 0.5h；
(3) the other half pre-emulsion is placed in constant pressure funnel, is slowly dropped into reaction system, while being added dropwise 0.4
The solution of part initiator and 10 parts of water, drips off for about 2 hours, controls 80 DEG C of temperature, then react 2 hours, obtains nano-organosilicon lotion；
The aqueous polyurethane emulsion, the preparation method is as follows:
A, by 180 parts of polyether Glycols (N220) be added with blender, condenser, N2 protection and thermometer reactor
In, under 60 DEG C, stirring, 52 parts of IPDI are added, are warming up to 70 DEG C of reaction 1.5h；
B, 9.4 parts of DMPA for being dissolved in DMF are added, 0.28 part of dibutyl tin dilaurate is stirred to react 0.5h at 75 DEG C；
C, 55 DEG C are cooled to, 7 parts of dihydroxy silane monomers (as shown in Equation 3) are slowly added to, reaction to NCO reaches theoretical value,
Aggravate it is strong be added with stirring 6 parts of TEA, persistently stir 0.5h；
D, 25 DEG C are cooled to, 384 parts of deionized waters are added, quickly stir 15min, adds 2.4 parts of ethylenediamines, is reacted
1.5h；
E, vacuum removal acetone obtains aqueous polyurethane emulsion.
The initiator is potassium peroxydisulfate.
Embodiment 3
A kind of nano-organosilicon composite polyurethane water-proof emulsion, it is compound by nano-organosilicon lotion and aqueous polyurethane emulsion
It forms, by percentage to the quality, nano-organosilicon lotion is 47%, aqueous polyurethane emulsion 53%；
The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer are (such as 1 institute of formula
Show), mono-vinyl organic silicon monomer (as shown in Equation 2), emulsifier, water, initiator be made through emulsion polymerization；
(H3C)3Si-O-CH2CH2NH-CH2CH=CH2Formula 2
The aqueous polyurethane emulsion is by polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy base silane list
Body (as shown in Equation 3), triethylamine, ethylenediamine, catalyst, organic solvent, water reaction are made；
The vinyl Nano-meter SiO_22Colloidal sol is made, method of vinyl silicane coupling agent, catalyst, water, emulsifier
It is as follows: 6 parts of Silane coupling reagent KH-570s, 1.4 parts of lauryl sodium sulfate, 1.8 parts of AEO-7,0.8 part of PEG-400 are added to
In 100 parts of water, stirring, dispersion are persistently stirred to react 4h then at 2.5 parts of ammonium hydroxide are added with stirring, and form vinyl Nano-meter SiO_22
Colloidal sol.
The nano-organosilicon lotion, the preparation method is as follows:
(1) 250 parts of water, 18 parts of vinyl Nano-meter SiO_2s are added into emulsifier2Colloidal sol, 24 parts of both-end alkenyl organosilicon lists
Body, 21 parts of mono-vinyl organic silicon monomers and 2 parts of AEO-9,2 parts of AEO-7,4 parts of neopelexes continue stirring and emulsifying
0.5h, at pre-emulsion；
(2) it takes half pre-emulsion to be placed in the reactor with temperature control, stirring and condensing unit, is added at 80 DEG C
The solution of 0.2 part of initiator and 4 parts of water, insulation reaction 0.5h；
(3) the other half pre-emulsion is placed in constant pressure funnel, is slowly dropped into reaction system, while being added dropwise 0.4
The solution of part initiator and 10 parts of water, drips off for about 2 hours, controls 80 DEG C of temperature, then react 2 hours, obtains nano-organosilicon lotion；
The aqueous polyurethane emulsion, the preparation method is as follows:
A, by 180 parts of polyether Glycols (N220) be added with blender, condenser, N2 protection and thermometer reactor
In, under 60 DEG C, stirring, 52 parts of IPDI are added, are warming up to 70 DEG C of reaction 1.5h；
B, 9.4 parts of DMPA for being dissolved in DMF are added, 0.28 part of dibutyl tin dilaurate is stirred to react 0.5h at 75 DEG C；
C, 55 DEG C are cooled to, 7 parts of dihydroxy silane monomers (as shown in Equation 3) are slowly added to, reaction to NCO reaches theoretical value,
Aggravate it is strong be added with stirring 6 parts of TEA, persistently stir 0.5h；
D, 25 DEG C are cooled to, 384 parts of deionized waters are added, quickly stir 15min, adds 2.4 parts of ethylenediamines, is reacted
1.5h；
E, vacuum removal acetone obtains aqueous polyurethane emulsion.
The initiator is ammonium persulfate.
Above-mentioned 3 embodiments nano-organosilicon composite polyurethane water-proof emulsion, appearance are in light blue translucent shape, warp
3000r/min is centrifuged 1h, is not layered, also has no precipitating.(referring to<GB/T11175-2002 synthetic resin emulsion test method>side
Method test)
The nano-organosilicon composite polyurethane water-proof emulsion of above-mentioned 3 embodiments is used for the water-proof finish of polyester fabric,
Prescription are as follows: 20 parts of nano-organosilicon composite polyurethane water-proof emulsion, 2 parts of thickener, 78 parts of water；Technique are as follows: coating → preliminary drying (90
DEG C, 3min) → bake (160 DEG C, 90s), polyester fabric ingredient and specification are 100% terylene, 150D*150D.Referring to GB/
T4745-2012, GB/T4744-2013 method have carried out water resistance, water repellency test to the polyester fabric after coating, as a result
As shown in table 1.
1 terylene coating sample of table is water-fast, waterproof performance
| Sample | Water repellency/grade | Water repellency/grade (after washing) | Waterproofness (hydrostatic pressing)/KPa |
| Embodiment 1 | 4 | 3 | 47.3 |
| Embodiment 2 | 5 | 4 | 51.6 |
| Embodiment 3 | 5 | 4 | 54.2 |
Polyester fabric is after the nano-organosilicon composite polyurethane water-proof emulsion top finish of embodiment, water repellent class 4 grade
More than, hydrostatic pressing 47KPa or more, waterproof, water repellency are excellent.
Claims (4)
1. a kind of nano-organosilicon composite polyurethane water-proof emulsion, it is characterised in that: by nano-organosilicon lotion and aqueous poly- ammonia
Ester lotion is combined, and by percentage to the quality, nano-organosilicon lotion is 34-47%, aqueous polyurethane emulsion 53-66%；
The nano-organosilicon lotion is by vinyl Nano-meter SiO_22Colloidal sol, both-end alkenyl organic silicon monomer (as shown in Equation 1), list
Vinyl organosilicon monomer (as shown in Equation 2), emulsifier, water, initiator are made through emulsion polymerization；
(H3C)3Si—O—CH2CH2NH—CH2CH=CH2Formula 2
The aqueous polyurethane emulsion is by polyether Glycols, diisocyanate, dihydromethyl propionic acid, dihydroxy silane monomer
(as shown in Equation 3), triethylamine, ethylenediamine, catalyst, organic solvent, water reaction are made；
The vinyl Nano-meter SiO_22Colloidal sol is made of vinyl silicane coupling agent, catalyst, water, emulsifier, the method is as follows:
6 parts of Silane coupling reagent KH-570s, 1.4 parts of lauryl sodium sulfate, 1.8 parts of AEO-7,0.8 part of PEG-400 are added to 100 parts
In water, stirring, dispersion are persistently stirred to react 4h then at 2.5 parts of ammonium hydroxide are added with stirring, and form vinyl Nano-meter SiO_22Colloidal sol.
2. a kind of nano-organosilicon composite polyurethane water-proof emulsion according to claim 1, it is characterised in that: described receives
Rice organic silicon emulsion, the preparation method is as follows:
(1) 250 parts of water, 18 parts of vinyl Nano-meter SiO_2s are added into emulsifier2Colloidal sol, 24 parts of both-end alkenyl organic silicon monomers, 21
Part mono-vinyl organic silicon monomer and 2 parts of AEO-9,2 parts of AEO-7,4 parts of neopelexes continue stirring and emulsifying 0.5h,
At pre-emulsion；
(2) it takes half pre-emulsion to be placed in the reactor with temperature control, stirring and condensing unit, 0.2 part is added at 80 DEG C
The solution of initiator and 4 parts of water, insulation reaction 0.5h；
(3) the other half pre-emulsion is placed in constant pressure funnel, is slowly dropped into reaction system, while be added dropwise 0.4 part and drawing
The solution for sending out agent and 10 parts of water, drips off for about 2 hours, controls 80 DEG C of temperature, then react 2 hours, obtains nano-organosilicon lotion.
3. a kind of nano-organosilicon composite polyurethane water-proof emulsion according to claim 1, it is characterised in that: the water
Property polyaminoester emulsion, the preparation method is as follows:
A, 180 parts of polyether Glycols (N220) are added in the reactor with blender, condenser, N2 protection and thermometer,
Under 60 DEG C, stirring, 52 parts of IPDI are added, are warming up to 70 DEG C of reaction 1.5h；
B, 9.4 parts of DMPA for being dissolved in DMF are added, 0.28 part of dibutyl tin dilaurate is stirred to react 0.5h at 75 DEG C；
C, 55 DEG C are cooled to, 7 parts of dihydroxy silane monomers (as shown in Equation 3) are slowly added to, reaction to NCO reaches theoretical value, aggravation
It is strong to be added with stirring 6 parts of TEA, persistently stir 0.5h；
D, 25 DEG C are cooled to, 384 parts of deionized waters are added, quickly stir 15min, adds 2.4 parts of ethylenediamines, reacts 1.5h；
E, vacuum removal acetone obtains aqueous polyurethane emulsion.
4. a kind of nano-organosilicon composite polyurethane water-proof emulsion according to claim 1 to 4, it is characterised in that: institute
The initiator stated is one of sodium peroxydisulfate, potassium peroxydisulfate, ammonium persulfate.
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