CN106978059A - Silane end-cappers modified double components polyurethane water-proof paint and preparation method thereof - Google Patents
Silane end-cappers modified double components polyurethane water-proof paint and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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- 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
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- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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Abstract
The present invention relates to silane end-cappers modified double components polyurethane water-proof paint and preparation method thereof, raw material includes component A and B component, component A is by the PPG of relative molecular mass 2000, the PPG of relative molecular mass 3000, polyisocyanates, isocyanatosilanes end-capping reagent is constituted, and B component is by the PPG of relative molecular mass 2000, the PPG of relative molecular mass 3000, chlorinated paraffin, aromatic naphtha, catalyst, defoamer, filler, pigment, plasticizer, environmentally friendly solvent composition.Compared with prior art, the present invention does not have bubble formation, the polyisocyanates also not remained after reaction, environmental protection, and curing rate is fast, and film-formation result is good, and pollution is not resulted in base material and environment.
Description
Technical field
The present invention relates to technical field of coatings, applied more particularly, to a kind of silane end-cappers modified double components polyurethane water-proof
Material and preparation method thereof.
Background technology
Polyurethane water-proof paint is with its excellent product properties and processing diversity, it has also become global coatings industry last decade
Carry out one of kind with fastest developing speed, among traditional double-composition polyurethane waterproof paint, component A is typically by polyisocyanates
It is excessive, then polyurethane coating is mixed to get with B component, so have unnecessary polyisocyanates and evaporate into air and pollute empty
Gas, unnecessary polyisocyanates can also so have bubble with water reaction generation carbon dioxide, influence polyurethane coating product
Various performances, may make product lose waterproof effect when serious.
Chinese patent CN104194608A discloses a kind of organosilane-modified mono-composition poyurethane water-proof paint, utilizes
Crosslinked with silicane mechanism replaces the mechanism of crosslinking of isocyanates, after there is the prepolymer end of the chain alkoxy silane of reactivity to hydrolyze
It is condensed into stable siloxanes (Si-O-Si) cross-linked network, it is to avoid NCO group with moisture reaction releases CO2Gas, reduces and applies
Film pin hole and bubble problem, increase film compactness, reduce the environmental factor dependence of product construction, solve traditional one-component and gather
The insoluble construction problem of urethane water-repellent paint.And this patent is to be used in double-component polyurethane coating first to synthesize end group and be
The silane end-cappers of isocyanate group utilize the end-capping reagent mechanism of crosslinking of isocyanates as performed polymer.Compared with organosilane-modified
Mono-composition poyurethane water-proof paint it is more environmentally friendly, bubble is less, is evaporate into without volatile polyisocyanates among air.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide one kind is environment-friendly, reduce
Silane end-cappers modified double components polyurethane water-proof paint that bubble is produced after film forming and preparation method thereof.
The purpose of the present invention can be achieved through the following technical solutions：
Silane end-cappers modified double components polyurethane water-proof paint, is mixed by component A and B component,
Described component A is prepared by the raw material of following weight percent content：
The hydroxyl PPOX ether 20%-60% of relative molecular mass 2000, the hydroxyl of relative molecular mass 3000 gather
Propylene oxide ether 20%-50%, isocyanatosilanes end-capping reagent 10%-25%, chlorinated paraffin 2%-30%, polyisocyanates 2%-
10%,
Described B component is prepared by the raw material of following weight percent content：
Aromatic naphtha 5%-20%, the hydroxyl PPOX ether 2%-15% of relative molecular mass 2000, average molecular matter
Hydroxyl PPOX ether 2%-15%, chlorinated paraffin 15%-25%, filler 30%-65%, the pigment 0.2%- of amount 3000
1%th, plasticizer 3%-10%, catalyst 0.1%-0.5%, defoamer 0.1%-0.5%, solvent 5%-10%.
The raw material of described component A preferably following weight percent content is prepared：
The hydroxyl that hydroxyl PPOX ether 30%-55% that relative molecular mass is 2000, relative molecular mass are 3000
Base PPOX ether 30%-50%, isocyanatosilanes end-capping reagent 10%-23%, polyisocyanates 2%-8%, chlorinated paraffin
2%-25%；
The raw material of described B component preferably following weight percent content is prepared：
Hydroxyl PPOX ether 2%-13%, the average molecular of aromatic naphtha 6%-18%, relative molecular mass for 2000
Quality is 3000 hydroxyl PPOX ether 2%-13%, chlorinated paraffin 17%-25%, filler 30%-58%, pigment
0.2%-1%, plasticizer 3%-8%, catalyst 0.1%-0.3%, defoamer 0.1%-0.3%, solvent 5%-10%.
Described polyisocyanates is toluene di-isocyanate(TDI) or methyl diphenylene diisocyanate.
Described isocyanatosilanes end-capping reagent is the alkoxy silane with Isocyanato functional group, described alkane
Epoxide is methoxy or ethoxy, is prepared using following methods：
(1) hybrid reaction：Potassium cyanate, N,N-dimethylformamide, caprolactam are added sequentially to stir in reactor
It is mixed thoroughly, 120-130 DEG C is to slowly warm up to, control programming rate can destroy very much raw material soon in 5 DEG C/min, heating
Structure, heating causes whole reaction process oversize very much slowly, and chloropropyl triethoxysilane is then added dropwise into mixture, and speed is added dropwise
Degree control is in 3kg/min, and reaction temperature is maintained at 120-130 DEG C, and addition can make very much reaction not exclusively soon, influence final performance,
After completion of dropwise addition, continue insulation reaction 4-5h, wherein potassium cyanate, DMF, caprolactam, the ethoxy of chloropropyl three
The weight of base silicon is 12-18 than control:30-35:12-16:35-40, potassium cyanate, DMF, caprolactam, chlorine
The weight of propyl-triethoxysilicane is than control 15:33:15:37.
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum controls bottom temp 130~160
DEG C, the cut under the conditions of 130~135 DEG C and 2~10kPa is collected, that is, has obtained isocyanatosilanes end-capping reagent.
Described catalyst is organo-metallic catalyst, selected from dibutyl tin laurate, stannous octoate or isooctyl acid lead
In one or more.
Described plasticizer is selected from dioctyl phthalate, dibutyl phthalate, diisononyl phthalate
Or the one or more in citric acid ester plasticizer.
Described solvent is malonic acid methyl ether acetate.
In kaolin of the described filler for the coarse whiting, the talcum powder of 600-1250 mesh or 600-1250 mesh of 600-1250 mesh
One or several kinds of mixing,
Described pigment be iron oxide brown or iron oxide red,
Described chlorinated paraffin is the one or two kinds of in chlorinated paraffin -42 or chlorinated paraffin -52,
Described defoamer is universal organic silicon defoamer.
The preparation method of silane end-cappers modified double components polyurethane water-proof paint, using following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX of relative molecular mass 3000
Ether is added sequentially in reactor, and stirring is warming up to 100 DEG C~115 DEG C, and vacuum is small for dehydration 3~4 under conditions of -0.01MPa
When；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 75~85 DEG C of stirrings, reacted 2~3 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 60~70 DEG C of stirrings, occurs silicon
Alkanisation end capping reaction, reacts 1~2 hour；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially to reaction
In kettle, stirring is warming up to 100 DEG C~115 DEG C, and vacuum is dehydration 3~4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 1 under 75~85 DEG C of stirrings
~2 hours；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:2-3 uniformly after mixing, will smear construction part, within 24 hours
Film-forming is polyurethane water-proof paint.
Compared with prior art, the present invention has advantages below：
(1) addition of PPG is excessive in reaction system, first generates performed polymer with polyisocyanates, then
Again plus the silane agent containing NCO carry out end capping reaction, the polyisocyanates not remained thus evaporate into air work as
In, air is polluted, the generation of bubble among reaction film forming is decreased.
(2) conventional aromatic solvent is replaced using environmentally friendly solvent malonic acid methyl ether acetate, bi-component is so solved with this
The problem of polyurethane water-proof paint environmental protection and aeration properties of product.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following examples will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that to the ordinary skill of this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
A kind of silane end-cappers modified double components polyurethane coating is divided into component A and B component：
Component A composition of raw materials：40% PPG 2000,35% PPG 3000,2% toluene diisocynate
Ester, 17%3- NCO propyl-triethoxysilicanes, 4% chlorinated paraffin -42.
B component composition of raw materials：5% aromatic naphtha, 5% PPG 2000,3% PPG 3000,15% chlorination
Paraffin -42,45% coarse whiting, 15% talcum powder, 1% cologne earth, 3.6% plasticizer, catalyst 0.2%, defoamer 0.2%, 7% ring
Protect solvent malonic acid methyl ether acetate.
Component A and B component raw material are individually placed in agitator successively, then by A, B component is according to mass ratio 1：2 is uniform
Mixing, film-forming.
Embodiment 2
A kind of silane end-cappers modified double components polyurethane coating is divided into component A and B component：
Component A composition of raw materials：35% PPG 2000,39% PPG 3000,2.5% toluene diisocynate
Ester, 19%3- NCO propyl-triethoxysilicanes, 4.5% chlorinated paraffin -42.
B component composition of raw materials：7% aromatic naphtha, 3% PPG 2000,5% PPG 3000,18% chlorination
Paraffin -42,40% coarse whiting, 15% talcum powder, 1% cologne earth, 3.6% plasticizer, catalyst 0.2%, defoamer 0.2%, 7% ring
Protect solvent malonic acid methyl ether acetate.
Component A and B component raw material are individually placed in agitator successively, then by A, B component is according to mass ratio 1：2.5
Even mixing, film-forming.
Embodiment 3
A kind of silane end-cappers modified double components polyurethane coating is divided into component A and B component：
Component A composition of raw materials：30% PPG 2000,45% PPG 3000,3% toluene diisocynate
Ester, 20%3- NCO propyl-triethoxysilicanes, 2% chlorinated paraffin -42.
B component composition of raw materials：5% aromatic naphtha, 4% PPG 2000,4% PPG 3000,15% chlorination
Paraffin -42,40% coarse whiting, 20% talcum powder, 1% cologne earth, 3.6% plasticizer, catalyst 0.2%, defoamer 0.2%, 7% ring
Protect solvent malonic acid methyl ether acetate.
Component A and B component raw material are individually placed in agitator successively, then by A, B component is according to mass ratio 1：2.5
Even mixing, film-forming.
Embodiment 4
A kind of silane end-cappers modified double components polyurethane coating is divided into component A and B component：
Component A composition of raw materials：42% PPG 2000,30% PPG 3000,2% toluene diisocynate
Ester, 21%3- NCO propyl-triethoxysilicanes, 5% chlorinated paraffin -42.
B component composition of raw materials：5% aromatic naphtha, 5% PPG 2000,3% PPG 3000,15% chlorination
Paraffin -42,35% coarse whiting, 25% talcum powder, 1% cologne earth, 3.6% plasticizer, catalyst 0.2%, defoamer 0.2%, 7% ring
Protect solvent malonic acid methyl ether acetate.
Component A and B component raw material are individually placed in agitator successively, then by A, B component is according to mass ratio 1：3 is uniform
Mixing, film-forming.
Embodiment 1-4 is subjected to film, performance test is carried out by national standard GB/T 19250-2013, see the table below one：
Table one
The present invention is prepared for a kind of silane end-cappers modified double components polyurethane water-proof paint, is imitated with excellent waterproof
Really, make PPG excessive, add first with a small amount of polyisocyanates with adding excessive PPG and crosslinking
Into reaction, carbamate is generated, is then sealed with 3- NCOs propyl-triethoxysilicane with unnecessary hydroxyl
End reaction, the ratio of strict control each group raw material, generates the polyurethane of high intensity.So it also avoid in the past using excessive
Polyisocyanates, construction when pollute air.Conventional aromatic solvent is replaced using environmentally friendly solvent malonic acid methyl ether acetate,
And with DINP as plasticizer, it is hypotoxicity, and plasticization effect is good, all plays environmental-protection function effect.Polyethers using excess is more
First alcohol and polyisocyanates reaction first synthesizes hydroxyl-terminated polyurethane performed polymer, and the silane for then adding isocyanato group containing is sealed
End reaction, has obtained silane end capped polyurethane polymer, has then uniformly been mixed according to a certain percentage with B component, and so we are just
Silane end-cappers modified double components polyurethane water-proof paint is obtained.But in the silane epoxide absorption air in silane end-cappers
Moisture hydrolysis generation silicone hydroxyl and small molecular alcohol, small molecular alcohol can be typically dissolved in polymer, do not have bubble formation,
The polyisocyanates also not remained after reaction, environmental protection, curing rate is fast, and film-formation result is good, will not to base material and environment
Pollute.So the present invention is a kind of feature of environmental protection silane end-cappers modified double components polyurethane water-proof paint.
Embodiment 5
Silane end-cappers modified double components polyurethane water-proof paint, is mixed by component A and B component,
Wherein, component A is prepared by the raw material of following weight percent content：
The hydroxyl PPOX ether 20% of relative molecular mass 2000, the hydroxyl polyoxygenated third of relative molecular mass 3000
Alkene ether 20%, isocyanatosilanes end-capping reagent 25%, chlorinated paraffin 30%, polyisocyanates 5%,
B component is prepared by the raw material of following weight percent content：
Hydroxyl PPOX ether 2%, the hydroxyl of relative molecular mass 3000 of aromatic naphtha 5%, relative molecular mass 2000
Base PPOX ether 3.8%, chlorinated paraffin 15%, filler 65%, pigment 1%, plasticizer 3%, catalyst 0.1%, froth breaking
Agent 0.1%, solvent 5%.
Wherein, the polyisocyanates used is toluene di-isocyanate(TDI), and catalyst is dibutyl tin laurate, plasticizer
Pungent for phthalic acid two, solvent is malonic acid methyl ether acetate, and filler is the coarse whiting of 600-1250 mesh, and pigment is iron oxide
Palm fibre, chlorinated paraffin is chlorinated paraffin -42, and defoamer is universal organic silicon defoamer.
Isocyanatosilanes end-capping reagent is the alkoxy silane with Isocyanato functional group, using following methods system
It is standby to obtain：
(1) hybrid reaction：Potassium cyanate, N,N-dimethylformamide, caprolactam are added sequentially to stir in reactor
It is mixed thoroughly, it is 5 DEG C/min to control heating rate, is to slowly warm up to 120 DEG C, chloropropyl three is added dropwise into mixture
Ethoxysilane, rate of addition is controlled in 3kg/min, and reaction temperature is maintained at 120 DEG C, after completion of dropwise addition, continues insulation reaction
4h, wherein potassium cyanate, DMF, caprolactam, the weight of chloropropyl triethoxy silicon are 12 than control:30:
12:35；
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum, control bottom temp is collected at 130 DEG C
Cut under the conditions of 130 DEG C and 2kPa, that is, obtained isocyanatosilanes end-capping reagent.
The preparation method of silane end-cappers modified double components polyurethane water-proof paint, using following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX of relative molecular mass 3000
Ether is added sequentially in reactor, and stirring is warming up to 100 DEG C, and vacuum is dehydration 3 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 75 DEG C of stirrings, reacted 2 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 60 DEG C of stirrings, occurs silanization
End capping reaction, reacts 1 hour；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially to reaction
In kettle, stirring is warming up to 100 DEG C~115 DEG C, and vacuum is dehydration 3 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 1 small under 75 DEG C of stirrings
When；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:After 2 uniform mixing, construction part will be smeared, it is solid within 24 hours
Chemical conversion film is polyurethane water-proof paint.
Embodiment 6
Silane end-cappers modified double components polyurethane water-proof paint, is mixed by component A and B component,
Component A is prepared by the raw material of following weight percent content：
The hydroxyl PPOX ether 60% of relative molecular mass 2000, the hydroxyl polyoxygenated third of relative molecular mass 3000
Alkene ether 26%, isocyanatosilanes end-capping reagent 10%%, chlorinated paraffin 2%, polyisocyanates 2%,
B component is prepared by the raw material of following weight percent content：
Aromatic naphtha 20%, the hydroxyl PPOX ether 15% of relative molecular mass 2000, relative molecular mass 3000
Hydroxyl PPOX ether 5%, chlorinated paraffin 15%, filler 30%, pigment 0.2%, plasticizer 3.8%, catalyst 0.5%,
Defoamer 0.5%, solvent 10%.
Wherein, polyisocyanates is methyl diphenylene diisocyanate, and catalyst is stannous octoate, and plasticizer is adjacent benzene two
Formic acid dibutyl ester, solvent is malonic acid methyl ether acetate, and filler is the coarse whiting of 600-1250 mesh, the talcum powder of 600-1250 mesh
Mixture, pigment is iron oxide red, and chlorinated paraffin is the mixture of chlorinated paraffin -42 and chlorinated paraffin -52, and defoamer is general
Type organic silicon defoamer.
Isocyanatosilanes end-capping reagent is the alkoxy silane with Isocyanato functional group, using following methods system
It is standby to obtain：
(1) hybrid reaction：Potassium cyanate, N,N-dimethylformamide, caprolactam are added sequentially to stir in reactor
It is mixed thoroughly, it is 5 DEG C/min to control heating rate, is to slowly warm up to 125 DEG C, chloropropyl three is added dropwise into mixture
Ethoxysilane, rate of addition is controlled in 3kg/min, and reaction temperature is maintained at 125 DEG C, after completion of dropwise addition, continues insulation reaction
5h, wherein potassium cyanate, DMF, caprolactam, the weight of chloropropyl triethoxy silicon are 15 than control:33:
15:37。
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum, control bottom temp is collected at 135 DEG C
Cut under the conditions of 135 DEG C and 5kPa, that is, obtained isocyanatosilanes end-capping reagent.
The preparation method of silane end-cappers modified double components polyurethane water-proof paint, using following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX of relative molecular mass 3000
Ether is added sequentially in reactor, and stirring is warming up to 110 DEG C, and vacuum is dehydration 3 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 80 DEG C of stirrings, reacted 2 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 65 DEG C of stirrings, occurs silanization
End capping reaction, reacts 1 hour；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially to reaction
In kettle, stirring is warming up to 110 DEG C, and vacuum is dehydration 3 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 1 small under 80 DEG C of stirrings
When；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:After 2 uniform mixing, construction part will be smeared, it is solid within 24 hours
Chemical conversion film is polyurethane water-proof paint.
Embodiment 7
Silane end-cappers modified double components polyurethane water-proof paint, is mixed by component A and B component,
Component A is prepared by the raw material of following weight percent content：
The hydroxyl PPOX ether 20% of relative molecular mass 2000, the hydroxyl polyoxygenated third of relative molecular mass 3000
Alkene ether 50%, isocyanatosilanes end-capping reagent 10%, chlorinated paraffin 10%, polyisocyanates 10%,
B component is prepared by the raw material of following weight percent content：
Aromatic naphtha 12%, the hydroxyl PPOX ether 10% of relative molecular mass 2000, relative molecular mass 3000
Hydroxyl PPOX ether 2%, chlorinated paraffin 25%, filler 30%, pigment 0.5%, plasticizer 10%, catalyst 0.2%, disappear
Infusion 0.3%, solvent 10%.
Polyisocyanates is methyl diphenylene diisocyanate, and described catalyst is isooctyl acid lead, and plasticizer is selected from neighbour
The mixture of dioctyl phthalate, dibutyl phthalate.Solvent is malonic acid methyl ether acetate.Filler is 600-1250
Purpose kaolin, pigment is iron oxide brown, and chlorinated paraffin is chlorinated paraffin -42, and defoamer is universal organic silicon defoamer.
Isocyanatosilanes end-capping reagent is the alkoxy silane with Isocyanato functional group, and described alkoxy is
Methoxy or ethoxy, is prepared using following methods：
(1) hybrid reaction：Potassium cyanate, N,N-dimethylformamide, caprolactam are added sequentially to stir in reactor
It is mixed thoroughly, it is 5 DEG C/min to control heating rate, is to slowly warm up to 125 DEG C, chloropropyl three is added dropwise into mixture
Ethoxysilane, rate of addition is controlled in 3kg/min, and reaction temperature is maintained at 125 DEG C, after completion of dropwise addition, continues insulation reaction
5h, wherein potassium cyanate, DMF, caprolactam, the weight of chloropropyl triethoxy silicon are 15 than control:33:
15:37。
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum, control bottom temp is collected at 150 DEG C
Cut under the conditions of 135 DEG C and 10kPa, that is, obtained isocyanatosilanes end-capping reagent.
The preparation method of silane end-cappers modified double components polyurethane water-proof paint, using following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX of relative molecular mass 3000
Ether is added sequentially in reactor, and stirring is warming up to 115 DEG C, and vacuum is dehydration 4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 85 DEG C of stirrings, reacted 3 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 70 DEG C of stirrings, occurs silanization
End capping reaction, reacts 2 hours；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially to reaction
In kettle, stirring is warming up to 115 DEG C, and vacuum is dehydration 4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 2 small under 85 DEG C of stirrings
When；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:After 2.5 uniform mixing, construction part will be smeared, within 24 hours
Film-forming is polyurethane water-proof paint.
Embodiment 8
Silane end-cappers modified double components polyurethane water-proof paint, is mixed by component A and B component,
Component A is prepared by the raw material of following weight percent content：
The hydroxyl PPOX ether 20% of relative molecular mass 2000, the hydroxyl polyoxygenated third of relative molecular mass 3000
Alkene ether 50%, isocyanatosilanes end-capping reagent 10%, chlorinated paraffin 10%, polyisocyanates 10%,
B component is prepared by the raw material of following weight percent content：
Aromatic naphtha 13%, the hydroxyl PPOX ether 12% of relative molecular mass 2000, relative molecular mass 3000
Hydroxyl PPOX ether 15%, chlorinated paraffin 15%, filler 30%, pigment 1%, plasticizer 4%, catalyst 0.5%, froth breaking
Agent 0.5%, solvent 9%.
Polyisocyanates is methyl diphenylene diisocyanate, and described catalyst is isooctyl acid lead, and plasticizer is selected from neighbour
The mixture of dioctyl phthalate, dibutyl phthalate.Solvent is malonic acid methyl ether acetate.Filler is 600-1250
Purpose kaolin, pigment is iron oxide brown, and chlorinated paraffin is chlorinated paraffin -42, and defoamer is universal organic silicon defoamer.
Isocyanatosilanes end-capping reagent is the alkoxy silane with Isocyanato functional group, using following methods system
It is standby to obtain：
(1) hybrid reaction：Potassium cyanate, N,N-dimethylformamide, caprolactam are added sequentially to stir in reactor
It is mixed thoroughly, it is 5 DEG C/min to control heating rate, is to slowly warm up to 130 DEG C, chloropropyl three is added dropwise into mixture
Ethoxysilane, rate of addition is controlled in 3kg/min, and reaction temperature is maintained at 130 DEG C, after completion of dropwise addition, continues insulation reaction
5h, wherein potassium cyanate, DMF, caprolactam, the weight of chloropropyl triethoxy silicon are 18 than control:35:
16:40；
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum, control bottom temp is collected at 160 DEG C
Cut under the conditions of 135 DEG C and 10kPa, that is, obtained isocyanatosilanes end-capping reagent.
The preparation method of silane end-cappers modified double components polyurethane water-proof paint, using following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX of relative molecular mass 3000
Ether is added sequentially in reactor, and stirring is warming up to 115 DEG C, and vacuum is dehydration 4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 85 DEG C of stirrings, reacted 3 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 70 DEG C of stirrings, occurs silanization
End capping reaction, reacts 2 hours；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially to reaction
In kettle, stirring is warming up to 115 DEG C, and vacuum is dehydration 4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 2 small under 85 DEG C of stirrings
When；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:After 3 uniform mixing, construction part will be smeared, it is solid within 24 hours
Chemical conversion film is polyurethane water-proof paint.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (10)
1. silane end-cappers modified double components polyurethane water-proof paint, it is characterised in that mixed by component A and B component,
Described component A is prepared by the raw material of following weight percent content：
The hydroxyl that hydroxyl PPOX ether 20%-60% that relative molecular mass is 2000, relative molecular mass are 3000 gathers
Propylene oxide ether 20%-50%, isocyanatosilanes end-capping reagent 10%-25%, chlorinated paraffin 2%-30%, polyisocyanates 2%-
10%,
Described B component is prepared by the raw material of following weight percent content：
Hydroxyl PPOX ether 2%-15%, the relative molecular mass of aromatic naphtha 5%-20%, relative molecular mass for 2000
3000 hydroxyl PPOX ether 2%-15%, chlorinated paraffin 15%-25%, filler 30%-65%, pigment 0.2%-1%,
Plasticizer 3%-10%, catalyst 0.1%-0.5%, defoamer 0.1%-0.5%, solvent 5%-10%.
2. silane end-cappers modified double components polyurethane water-proof paint according to claim 1, it is characterised in that
The raw material of described component A preferably following weight percent content is prepared：
The hydroxyl that hydroxyl PPOX ether 30%-55% that relative molecular mass is 2000, relative molecular mass are 3000 gathers
Propylene oxide ether 30%-50%, isocyanatosilanes end-capping reagent 10%-23%, polyisocyanates 2%-8%, chlorinated paraffin 2%-
25%；
The raw material of described B component preferably following weight percent content is prepared：
Hydroxyl PPOX ether 2%-13%, the relative molecular mass of aromatic naphtha 6%-18%, relative molecular mass for 2000
For 3000 hydroxyl PPOX ether 2%-13%, chlorinated paraffin 17%-25%, filler 30%-58%, pigment 0.2%-
1%th, plasticizer 3%-8%, catalyst 0.1%-0.3%, defoamer 0.1%-0.3%, solvent 5%-10%.
3. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The polyisocyanates stated is toluene di-isocyanate(TDI) or methyl diphenylene diisocyanate.
4. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The isocyanatosilanes end-capping reagent stated is the alkoxy silane with Isocyanato functional group, and described alkoxy is methoxy
Base or ethyoxyl.
5. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The isocyanatosilanes end-capping reagent stated is prepared using following methods：
(1) hybrid reaction：Potassium cyanate, DMF, caprolactam are added sequentially into stirring in reactor makes it
It is mixed thoroughly, is to slowly warm up to 120-130 DEG C, control programming rate adds chloropropyl three into mixture in 5 DEG C/min
Ethoxysilane, rate of addition is controlled in 3kg/min, and reaction temperature is maintained at 120-130 DEG C, after raw material addition terminates, continues
Insulation reaction 4-5h, wherein potassium cyanate, DMF, caprolactam, the weight of chloropropyl triethoxy silicon are than control
It is made as 12-18:30-35:12-16:35-40.
(2) rectification and purification：After reaction terminates, filtrate is filtrated to get, rectification under vacuum, control bottom temp is received at 130~160 DEG C
Cut under the conditions of 130~135 DEG C and 2~10kPa of collection, that is, obtained isocyanatosilanes end-capping reagent.
6. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The catalyst stated is organo-metallic catalyst, one kind in dibutyl tin laurate, stannous octoate or isooctyl acid lead or
It is several.
7. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The plasticizer stated is selected from dioctyl phthalate, dibutyl phthalate, diisononyl phthalate or citrate
One or more in class plasticizer.
8. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that institute
The solvent stated is malonic acid methyl ether acetate.
9. silane end-cappers modified double components polyurethane water-proof paint according to claim 1 or 2, it is characterised in that
Described filler is one in the kaolin of the coarse whiting, the talcum powder of 600-1250 mesh or 600-1250 mesh of 600-1250 mesh
Plant or several mixing,
Described pigment be iron oxide brown or iron oxide red,
Described chlorinated paraffin is the one or two kinds of in chlorinated paraffin -42 or chlorinated paraffin -52,
Described defoamer is universal organic silicon defoamer.
10. the preparation method of silane end-cappers modified double components polyurethane water-proof paint as claimed in claim 1, its feature exists
In this method uses following steps：
The preparation of component A：
A. the hydroxyl PPOX ether of relative molecular mass 2000, the hydroxyl PPOX ether of relative molecular mass 3000 according to
Secondary to be added in reactor, stirring is warming up to 100 DEG C~115 DEG C, and vacuum is dehydration 3~4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, isocyanates is added, under 75~85 DEG C of stirrings, reacted 2~3 hours；
C. less than 50 DEG C are reduced the temperature to, isocyanatosilanes end-capping reagent is added, under 60~70 DEG C of stirrings, occurs silanization
End capping reaction, reacts 1~2 hour；
D. less than 40 DEG C are reduced the temperature to, discharging obtains component A；
The preparation of B component：
A. by aromatic naphtha, PPG, chlorinated paraffin, plasticizer, coarse whiting, talcum powder, pigment is added sequentially in reactor,
Stirring is warming up to 100 DEG C~115 DEG C, and vacuum is dehydration 3~4 hours under conditions of -0.01MPa；
B. less than 60 DEG C are reduced the temperature to, catalyst is added, defoamer, solvent stirs 1~2 under 75~85 DEG C of stirrings
Hour；
C. less than 40 DEG C are reduced the temperature to, discharging obtains B component；
The preparation of water-repellent paint：
Component A and B component are made into 1 by weight:2-3 uniformly after mixing, will smear construction part, solidify within 24 hours
Film forming is polyurethane water-proof paint.
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