CN109503789A - A kind of polyurethane-modified silicone resin emulsion and its preparation method and application - Google Patents
A kind of polyurethane-modified silicone resin emulsion and its preparation method and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/38—Low-molecular-weight compounds having heteroatoms other than oxygen
- C08G18/3893—Low-molecular-weight compounds having heteroatoms other than oxygen containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/2805—Compounds having only one group containing active hydrogen
- C08G18/288—Compounds containing at least one heteroatom other than oxygen or nitrogen
- C08G18/289—Compounds containing at least one heteroatom other than oxygen or nitrogen containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3225—Polyamines
- C08G18/3228—Polyamines acyclic
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Abstract
The present invention relates to a kind of technical field of novel high polymer material, including but not limited to leather and textile auxiliary field, more particularly, to a kind of polyurethane-modified silicone resin emulsion/performed polymer and its preparation method and application.The present invention provides a kind of polyurethane-modified silicone resin emulsion (can also be a kind of polyurethane-modified organosilicon performed polymer) and its preparation method and application.There is silicone resin emulsion of the invention excellent water repellent to wash, the performances such as high resiliency, fold resistant, it thoroughly solves existing for traditional amido silicon oil easily demulsification, floating oil, roll banding, be not easy the problems such as returning something for repairs, a kind of high-elastic, smooth, waterproof and the good polyurethane-modified silicone resin emulsion of durability are provided, make the feel style of the leather after arranging and the existing organic silicone finishing agent of fabric surface, and the special feel with polyurethane.
Description
Technical field
The present invention relates to a kind of high molecular material new technical fields, including but not limited to leather and textile auxiliary field, especially
It is to be related to a kind of polyurethane-modified silicone resin emulsion/performed polymer and its preparation method and application.
Background technique
Organic silicon emulsion can improve the feel of textile and leather surface as finishing agents such as fabric, leathers, assign
Fabric and leather surface is soft, the performances such as smooth, in addition to this, organic silicon emulsion has become high-end apparel industry as finishing agent
Essential processing articles.Domestic and international company selects similar with fabric (terylene etc.) structure according to the similar principle that mixes
Terephthalate macrogol ester finish fabric and leather select polyamide polyether copolymer to arrange nylon fabric, can
To obtain excellent hydrophilic effect, but often feel is general, and wearing comfort is poor.
Some enterprises are in order to improve added value of product, and introducing silicon oxygen segment can get excellent in polyether polyester block object structure
The finishing agent of matter feel.Such as moral treasured chemical industry dimethyl terephthalate (DMT), ethylene glycol, polyethylene glycol and special organosilicon polymer
Polyester polyether silicones ternary polymerization type multifunctional hydrophilic finishing agent is synthesized, but due to not forming firm combination with fiber
Power, washability is poor, and hydrophilic effect is not lasting.
Polyurethane can carry out a variety of excellent performances to webbing as fabric weaving auxiliary agent, such as soft, crease-resistant, anti-
Electrostatic, hydrophily, these performances improve the appearance and wearing comfort of fabric, while also leather surface can be made more smooth
Resistant.By polyurethane-modified organosilicon polymer, the dual property of polyurethane and organosilicon can be effectively utilized, organic
Urea ester group and urethano are introduced in silicon and reinforces anchoring effect, are assigned fabric and the excellent permanent hydrophilic feel of leather surface, are mentioned
The economic value of high product.A kind of existing Chinese patent " preparation of polyurethane-modified organosilicon multiple copolymer fabric softener
Method " (publication No. CN103951809A), discloses following steps: using two isocyanide of polyethylene glycol 2000 and isophorone first
Acid esters prepares base polyurethane prepolymer for use as；Then alkane is prepared using di-n-butylamine, epoxy double-seal head and octamethylcy-clotetrasiloxane
Hydroxy silicon oil；Base polyurethane prepolymer for use as and hydroxyl-containing silicone are reacted again to obtain polyurethane organosilicon multiple copolymer；Finally
Be added deionized water and emulsify to get.The product of this method synthesis has certain hydrophilic soft fluffy performance, but the scope of application
It is narrow, washability is poor, be not able to satisfy the demand in market.
Aqueous polyurethane makes it have good elasticity and special feel style, application field due to its special construction
Cover leather, papermaking, weaving and coating etc..External existing research person carries out aqueous polyurethane emulsion and hydroxy-silicone-oil emulsion
It is blended, and finds that this co-mixing system has good freexing tolerance and heat-resistant stability.Studies in China person is on this basis by this
Kind blending emulsion is applied in leather and textile finishing, and the leather and fabric after making arrangement are not only soft, smooth, elasticity is good,
And there is certain antistatic, anti-fluffing and anti-pilling effect.But this blending emulsion is simple physical mixed, has been difficult
To durable effect.
Summary of the invention
In view of the above existing problems in the prior art, the present invention provides a kind of polyurethane-modified silicone resin emulsion (
A kind of polyurethane-modified organosilicon performed polymer can be) and its preparation method and application.Silicone resin emulsion tool of the invention
There is excellent water repellent to wash, the performances such as high resiliency, fold resistant, thoroughly solves existing for traditional amido silicon oil easily demulsification, floating oil, viscous
Roller is not easy the problems such as returning something for repairs, and provides a kind of high-elastic, smooth, waterproof and the good polyurethane-modified silicone resin emulsion of durability,
Make the feel style of the leather after arranging and the existing organic silicone finishing agent of fabric surface, and the special feel with polyurethane.
To achieve the above object, the invention adopts the following technical scheme:
A kind of polyurethane-modified silicone resin emulsion, is made by following methods:
Step 1:OH-R-Si-R-OH and isocyanates synthesize NCO-Si-PU-NCO performed polymer；
Step 2: NCO-Si-PU-NCO performed polymer and R '-Si-R-OH composite part prepared by step 1 is silicone terminated
NCO-organic silicon polyurethane performed polymer；
Step 3: the silicone terminated NCO-organic silicon polyurethane performed polymer in the part that step 2 synthesizes and DMPA carry out chain extension again
After reaction, triethylamine and water is added, after being eventually adding ethylenediamine chain extension, obtains polyurethane-modified silicone resin emulsion.
The R is EO and/or PO polyethers, the preferred 2500-2000 of degree of polymerization M=1000-4000, M；R ' is C1-C12Alkyl
Or phenyl, preferably C1-C3 alkyl and phenyl, most preferably isopropyl and phenyl.
Isocyanates is isocyanates generally in the art, preferably toluene di-isocyanate(TDI) (TDI), two isocyanide of isophorone
Acid esters (IPDI), methyl diphenylene diisocyanate (MDI), dicyclohexyl methyl hydride diisocyanate (HMDI), hexa-methylene two
Isocyanates (HDI), lysine diisocyanate (LDI), most preferably isophorone diisocyanate (IPDI).
The molar ratio of OH-R-Si-R-OH and isocyanates is 1:1-2.5, preferably 1:1.2-1.8, step in step 1
1 reaction temperature is 80-150 DEG C, and preferably 105-115 DEG C, reaction pressure is -0.1-2Mpa, preferably -0.05-0.5Mpa, when reaction
Between 2-5 hours, preferably 3-4 hours, be cooled to room temperature after reaction, obtain NCO-Si-PU-NCO performed polymer.
NCO-Si-PU-NCO performed polymer and R '-Si-R-OH are mixed in step 2 and are added into reaction vessel, two
Person's molar ratio is 1:2.5-5.5, preferably 1:3-4, is to slowly warm up to 140-180 DEG C, insulation reaction 1-3 hours, preferably 2-3 was small
When, control reaction pressure is -0.1-2Mpa, and preferably -0.05-0.5Mpa is slowly dropped to room temperature after reaction, obtains part silicon
The NCO of sealing end-organic silicon polyurethane performed polymer.
The silicone terminated NCO in part-organic silicon polyurethane performed polymer and dihydromethyl propionic acid (DMPA) first carry out in step 3
Chain extending reaction again, the two molar ratio be 1:10-40, preferably 1:15-25, reaction temperature be 80-150 DEG C, preferably 105-115 DEG C,
Synthesis under normal pressure, reaction time 1-3 hour, preferably 2-3 hour, wherein DMPA is added by high speed dispersing device；After reaction,
It is added water at room temperature, the molar ratio of water and DMPA are 1:0.5-0.8, are carried out after being sufficiently stirred 0.5-2 hour to lotion, addition
Ethylenediamine carries out chain extension again, and the molar ratio of ethylenediamine and triethylamine is 1:0.8-2.2, and preferably 1:1-1.2 adds ethylenediamine
While, in order to improve reaction rate, it is that (organo-tin compound is that this field is normal to catalyst that organotin, which can be added, to make compound
Organo-tin compound, preferably dibutyl tin, stannous octoate), it can also be added without, be added without and have no effect on final product
It generates, the dosage of organotin catalysts is the 0.01-0.03% of ethylenediamine quality.
Polyurethane-modified silicone resin emulsion is prepared the invention also includes a kind of, is included the following steps:
Step 1:OH-R-Si-R-OH and isocyanates synthesize NCO-Si-PU-NCO performed polymer；
Step 2: NCO-Si-PU-NCO performed polymer and R '-Si-R-OH composite part prepared by step 1 is silicone terminated
NCO-organic silicon polyurethane performed polymer；
Step 3: the silicone terminated NCO-organic silicon polyurethane performed polymer in the part that step 2 synthesizes and DMPA carry out chain extension again
After reaction, triethylamine and water is added, after being eventually adding ethylenediamine chain extension, obtains polyurethane-modified silicone resin emulsion.
Raw material of the present invention is purchased from Yu Shenyao (Xianghe) Science and Technology Ltd., and the purchase date is in January, 2018.
In addition, skin can be used in the invention also includes a kind of purposes for preparing polyurethane-modified silicone resin emulsion
Leather and fabric surface, use as finishing agent.Simultaneously also can be widely applied to other defoaming agents, levelling agent, coating, ink,
Smooth dose, the fields such as anti-wear agent.
The present invention compared with the existing technology, has the advantage that
1. it is poly- to react synthesis Amino End Group using amino closure agent for polyurethane-modified silicone resin emulsion prepared by the present invention
Siloxanes, then with triethylamine, the polyurethane-modified organosilicon polymer of reacting ethylenediamine synthesis hydrophilic, pass through compounding high feel addition
Agent emulsifies out finishing agent microemulsion, and performance is substantially better than polyester polyether-type finishing agent, more with fiber and leather surface binding force
By force, durability is more prominent.
2. polyurethane-modified silicone resin emulsion prepared by the present invention assigns various fabrics splendid durable hydrophilic property
Can, washable effect outstanding, feel is better than most hydrophilic block silicone oil, while can effectively solve under amino hot conditions
The problem of easy xanthochromia, fabric xanthochromia is small after processing, is suitable for white or light-colored textile finishing.
3. being modified using Waterborne Polyurethane Prepolymer to organic silicon emulsion, remaining isocyanate groups in performed polymer
It can react with the amino on organosilicon chain, form the network structure of three-dimensional interpenetrating, improve film forming of the lotion on fiber
With the durability of film, make the feel style of the fabric after arranging or the existing organic silicone finishing agent of leather surface, and there is polyurethane
Special feel.
4. since polyurethane differs larger with polysiloxanes solubility, during pyroreaction, polyurethane with it is organic
Silicon is easy to happen light microphase-separated, can effectively increase the elasticity of fabric and the toughness of leather surface after arranging.Simultaneously as film forming
Property improvement, but also arrange after fabric slipping and waterproofness further increase.
Specific embodiment
In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention is carried out below further detailed
It describes in detail bright.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention, it is not limited to this hair
Bright range.Raw material in specific embodiment can pass through commercially available acquisition.
Embodiment 1
Step 1: taking OH-(EO)M—Si—(EO)M- OH 0.1mol (M=2000), IPDI 0.12mol, 110 DEG C, instead
Pressure 0.05Mpa is answered, is reacted 3 hours, is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
Step 2: taking NCO-Si-PU-NCO performed polymer 0.1mol, CH3- Si-EO-OH 0.3mol mixing is added extremely
In reaction vessel, 140 DEG C are to slowly warm up to, insulation reaction 2 hours, control reaction pressure was -0.05Mpa, was delayed after reaction
Slowly it is down to room temperature, obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
Step 3: the NCO for taking part silicone terminated-organic silicon polyurethane performed polymer 0.1mol, DMPA1.5mol passes through high speed
Dispersal device is added in the silicone terminated NCO-organic silicon polyurethane performed polymer in part, and chain extending reaction, reaction temperature are again for progress
105 DEG C, synthesis under normal pressure, the reaction time 2 hours；After reaction, the water of 0.75mol is added at room temperature, lotion is filled
After dividing stirring 0.5 hour, the ethylenediamine and 0.01g dibutyl tin that 1.65mol is added carry out chain extension again, obtain after reaction
Polyurethane-modified silicone resin emulsion.
Embodiment 2
Step 1: taking OH-(PO)M—Si—(PO)M- OH 0.1mol (M=2500), TDI 0.25mol, 115 DEG C, instead
Pressure 0.5Mpa is answered, is reacted 4 hours, is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
Step 2: taking NCO-Si-PU-NCO performed polymer 0.1mol, CH3CH2- Si-PO-OH0.4mol mixing is added
Into reaction vessel, 160 DEG C are to slowly warm up to, insulation reaction 3 hours, control reaction pressure was 0.5Mpa, was delayed after reaction
Slowly it is down to room temperature, obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
Step 3: the NCO for taking part silicone terminated-organic silicon polyurethane performed polymer 0.1mol, DMPA2.5mol passes through high speed
Dispersal device is added in the silicone terminated NCO-organic silicon polyurethane performed polymer in part, and chain extending reaction, reaction temperature are again for progress
115 DEG C, synthesis under normal pressure, the reaction time 3 hours；After reaction, the water of 2mol is added at room temperature, lotion is sufficiently stirred
After mixing 1 hour, the ethylenediamine and 0.008g stannous octoate that 2.7mol is added carry out chain extension again, obtain polyurethane after reaction
Modified organic silicone resin lotion.
Embodiment 3
Step 1: taking OH-(EO)M—Si—(EO)M- OH 0.1mol, HMDI 0.2mol, 110 DEG C, reaction pressure
0.05Mpa reacts 3 hours, is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
Step 2: NCO-Si-PU-NCO performed polymer 0.1mol, phenyl-Si-EO-OH 0.22mol mixing being taken to be added
Into reaction vessel, 140 DEG C are to slowly warm up to, insulation reaction 1 hour, control reaction pressure was 2Mpa, after reaction slowly
It is down to room temperature, obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
Step 3: the NCO for taking part silicone terminated-organic silicon polyurethane performed polymer 0.1mol, DMPA3.5mol passes through high speed
Dispersal device is added in the silicone terminated NCO-organic silicon polyurethane performed polymer in part, carries out chain extending reaction again, reaction temperature 80
DEG C, synthesis under normal pressure, the reaction time 1 hour；After reaction, the water of 3mol is added at room temperature, lotion is carried out to be sufficiently stirred 2
After hour, the ethylenediamine that 3.5mol is added carries out chain extension again, obtains polyurethane-modified silicone resin emulsion after reaction.
Embodiment 4
Step 1: taking OH-(PO)M—Si—(PO)M- OH 0.1mol (M=2200), LDI 0.15mol, react by 80 DEG C
Pressure 1Mpa reacts 2.5 hours, is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
Step 2: taking NCO-Si-PU-NCO performed polymer 0.1mol, (CH3)2CH-Si-PO-OH0.55mol mixing adds
Enter into reaction vessel, is to slowly warm up to 170 DEG C, insulation reaction 1.5 hours, control reaction pressure was 2Mpa, after reaction
It is slowly dropped to room temperature, obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
Step 3: the NCO for taking part silicone terminated-organic silicon polyurethane performed polymer 0.1mol, DMPA3.5mol passes through high speed
Dispersal device is added in the silicone terminated NCO-organic silicon polyurethane performed polymer in part, and chain extending reaction, reaction temperature are again for progress
105 DEG C, synthesis under normal pressure, the reaction time 2 hours；After reaction, the water of 2.8mol is added at room temperature, lotion is carried out abundant
After stirring 0.5 hour, the ethylenediamine that 6mol is added carries out chain extension again, obtains polyurethane-modified organic siliconresin after reaction
Lotion.
Embodiment 5
Step 1: taking OH-(EO)M—Si—(EO)M- OH 0.1mol, HMDI 0.25mol, 150 DEG C, reaction pressure-
0.1Mpa reacts 5 hours, is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
Step 2: NCO-Si-PU-NCO performed polymer 0.1mol, phenyl-Si-EO-OH 0.25mol mixing being taken to be added
Into reaction vessel, 180 DEG C are to slowly warm up to, insulation reaction 3 hours, control reaction pressure was -0.05Mpa, after reaction
It is slowly dropped to room temperature, obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
Step 3: the NCO for taking part silicone terminated-organic silicon polyurethane performed polymer 0.1mol, DMPA1mol passes through high speed point
In bulk set is added in the silicone terminated NCO-organic silicon polyurethane performed polymer in part, carries out chain extending reaction again, reaction temperature 105
DEG C, synthesis under normal pressure, the reaction time 2 hours；After reaction, the water of 0.75mol is added at room temperature, lotion is sufficiently stirred
After mixing 0.5 hour, the ethylenediamine that 1.65mol is added carries out chain extension again, obtains polyurethane-modified organosilicon tree after reaction
Fat liquor.
Present invention embodiment raw material described above is purchased from Yu Shenyao (Xianghe) Science and Technology Ltd., and the purchase date is 2018
January in year.
6 application performance test of embodiment
It is that auspicious hundred million (RuIyi) fur clothing of commercial product nurses spray to mark example
Embodiment 1-5 lotion and commercial product are measured after leather surface use according to standard QB/T2714-2005, leather
Folding degree.
Embodiment 1-5 lotion and commercial product are measured after fabric surface use according to KESFB-AUTO-A, the pressure of fabric
Elasticity is retracted, numerical value is bigger, shows that elasticity is better.
Embodiment 1-5 lotion and commercial product are measured after fabric surface use according to FZ/T 01054-2012, fabric table
The smoothness in face, numerical value is smaller, shows that smoothness is better.
Waterproofness is tested with reference to GB/T 4745-1997.
Above-mentioned the performance test results see the table below 1.
1 performance test of table
Conclusion (of pressure testing): the polyurethane-modified silicone resin emulsion performance of the present invention is more excellent.
Claims (10)
1. a kind of polyurethane-modified silicone resin emulsion, which is characterized in that be made by following methods:
Step 1:OH-R-Si-R-OH and isocyanates synthesize NCO-Si-PU-NCO performed polymer；
Step 2: NCO-Si-PU-NCO performed polymer and R '-Si-R-OH composite part prepared by step 1 is silicone terminated
NCO-organic silicon polyurethane performed polymer；
Step 3: the silicone terminated NCO-organic silicon polyurethane performed polymer in the part that step 2 synthesizes and DMPA carry out chain extending reaction again
Afterwards, triethylamine and water is added, after being eventually adding ethylenediamine chain extension, obtains polyurethane-modified silicone resin emulsion；
The R is EO and/or PO polyethers, degree of polymerization M=1000-4000；R ' is C1-C12 alkyl or phenyl.
2. polyurethane-modified silicone resin emulsion according to claim 1, it is characterised in that: the R is EO and/or PO
Polyethers, degree of polymerization M are 2500-2000；R ' is C1-C3 alkyl and phenyl.
3. polyurethane-modified silicone resin emulsion according to claim 1, it is characterised in that: the isocyanates is first
Phenylene diisocyanate, isophorone diisocyanate, methyl diphenylene diisocyanate, dicyclohexyl methyl hydride diisocyanate,
Hexamethylene diisocyanate, lysine diisocyanate.
4. polyurethane-modified silicone resin emulsion according to claim 1, it is characterised in that: OH-R-in step 1
The molar ratio of Si-R-OH and isocyanates is 1:1-2.5, and reaction temperature is 80-150 DEG C, reaction pressure is -0.1-2Mpa,
In reaction time 2-5 hour, it is cooled to room temperature after reaction, obtains NCO-Si-PU-NCO performed polymer.
5. polyurethane-modified silicone resin emulsion according to claim 1, it is characterised in that: by NCO-in step 2
Si-PU-NCO performed polymer and R '-Si-R-OH mixing are added into reaction vessel, and the two molar ratio is 1:2.5-5.5, is delayed
Slowly it is warming up to 140-180 DEG C, insulation reaction 1-3 hours, control reaction pressure was -0.1-2Mpa, was slowly dropped to after reaction
Room temperature obtains the silicone terminated NCO in part-organic silicon polyurethane performed polymer.
6. polyurethane-modified silicone resin emulsion according to claim 1, it is characterised in that: part silicon seals in step 3
The NCO at end-organic silicon polyurethane performed polymer and dihydromethyl propionic acid first carry out chain extending reaction again, and the two molar ratio is 1:10-
40, reaction temperature is 80-150 DEG C, synthesis under normal pressure, and in reaction time 1-3 hour, DMPA is added by high speed dispersing device；Reaction
After, it is added water at room temperature, the molar ratio of water and DMPA are 1:0.5-0.8, be sufficiently stirred 0.5-2 hours to lotion
Afterwards, ethylenediamine is added and carries out chain extension again, the molar ratio of ethylenediamine and triethylamine is 1:0.8-2.2.
7. polyurethane-modified silicone resin emulsion according to claim 6, it is characterised in that: second two is added in step 3
Organotin catalysts are added while amine, the dosage of organotin catalysts is the 0.01-0.03% of ethylenediamine quality.
8. polyurethane-modified silicone resin emulsion according to claim 7, it is characterised in that: organotin catalysts two
Butyl tin or stannous octoate.
9. a kind of preparation method of polyurethane-modified silicone resin emulsion as described in claim 1, the preparation method step is such as
Under:
Step 1:OH-R-Si-R-OH and isocyanates synthesize NCO-Si-PU-NCO performed polymer；
Step 2: NCO-Si-PU-NCO performed polymer and R '-Si-R-OH composite part prepared by step 1 is silicone terminated
NCO-organic silicon polyurethane performed polymer；
Step 3: the silicone terminated NCO-organic silicon polyurethane performed polymer in the part that step 2 synthesizes and DMPA carry out chain extending reaction again
Afterwards, triethylamine and water is added, after being eventually adding ethylenediamine chain extension, obtains polyurethane-modified silicone resin emulsion；
The R is EO and/or PO polyethers, degree of polymerization M=1000-4000；R ' is C1-C12 alkyl or phenyl.
10. a kind of purposes of polyurethane-modified silicone resin emulsion as described in claim 1, can be used in leather and fabric
Surface is used as finishing agent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112679695A (en) * | 2020-04-03 | 2021-04-20 | 胡黎明 | Preparation method of high-stability organic silicon modified waterborne polyurethane |
| CN114015241A (en) * | 2022-01-06 | 2022-02-08 | 北京智天新航科技有限公司 | Polyurethane modified organic silicon damping material and preparation method thereof |
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| CN114015241A (en) * | 2022-01-06 | 2022-02-08 | 北京智天新航科技有限公司 | Polyurethane modified organic silicon damping material and preparation method thereof |
| CN114015241B (en) * | 2022-01-06 | 2022-03-11 | 北京智天新航科技有限公司 | Polyurethane modified organic silicon damping material and preparation method thereof |
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