CN105086807B - A kind of preparation method of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent - Google Patents

A kind of preparation method of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent Download PDF

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CN105086807B
CN105086807B CN201510584705.7A CN201510584705A CN105086807B CN 105086807 B CN105086807 B CN 105086807B CN 201510584705 A CN201510584705 A CN 201510584705A CN 105086807 B CN105086807 B CN 105086807B
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asphalt
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polyurethane prepolymer
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CN105086807A (en
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施新民
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Nantong Wanbangcai Coating Co., Ltd.
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Nantong Wanbangcai Coating Co Ltd
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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
    • C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72—Polyisocyanates or polyisothiocyanates
    • C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
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    • C08G18/40—High-molecular-weight compounds
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    • C08G18/40—High-molecular-weight compounds
    • C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
    • C08G18/6476—Bituminous materials, e.g. asphalt, coal tar, pitch; derivatives thereof
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    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666—Compounds of group C08G18/48 or C08G18/52
    • C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6685—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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    • C08K3/00—Use of inorganic substances as compounding ingredients
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    • 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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    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
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    • 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
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract

The invention discloses a kind of preparation method of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent, belong to water-repellent paint preparing technical field.Coating of the invention is to be vacuum dried polyoxypropyleneglycol and polytetrahydrofuran diol, stirring forms polyether polyols mixed alkoxide solution, mix with toluene di-isocyanate(TDI), flow back to obtain base polyurethane prepolymer for use as, survey its nco value, during for certain wavelength, stopping heating being cooled to room temperature and obtains base polyurethane prepolymer for use as component；ZnO powder high pressure sieve of milling is taken, is mixed with pitch, dimethylethanolamine etc., be vacuum dried, be slowly stirred, sonic oscillation, obtain asphalt component.The beneficial effects of the invention are as follows：The method is modified by nano-ZnO, improves both asphalt and polyurethane coating compatibility, and raising film is weather-proof, tensile property, film tensile strength is risen to 5~6MPa, and elongation at break is up to 550~600%, and compatible sexual compatibility and water resistance are good.

Description

A kind of preparation of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent Method
Technical field
The present invention relates to a kind of preparation method of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent, belong to Water-repellent paint preparing technical field.
Background technology
Polyurethane water-proof paint has that intensity is high, elongation percentage big and the construction material ground cementability such as cement mortar is strong, resistance to Long property is long, easy construction the features such as.But because the prices of raw materials of polyurethane are expensive, only answered in some special occasions With.What is commonly used in waterproofing work is the polyurethane water-proof paint being made up of the component of first, second two containing filler.First group It is the performed polymer synthesized by polyethers and toluene di-isocyanate(TDI) to divide, and end group is isocyanate group；Second component is by curing agent, filling plasticising Agent, diluent etc. are constituted.The first and second components are pressed into a certain amount of mixing and stirring during construction, waterproof surface of bottom material is applied to, through changing Reaction is learned, rich caoutchouc elasticity and continuous integral waterproofing layer can be formed within 12 h.China polyurethane water-proof paint grinds Study carefully exploitation and start from beginning of the eighties late 1970s, generally make to add to fill plasticising thing using the remarkable coal tar of cheap and performance Matter, makes polyurethane water-proof paint be widely used in increasing engineering, and it has been used for Beijing market place builet below the ground, the Asian Games Village, the Great Hall of the People are overhauled, in the key state project such as Diaoyutai State Guesthouse.The research of polyurethane water-proof paint in 1991 should With being once classified as key popularized project by country.With expanding economy and the progress of society, Minstry of Housing and Urban-Rural Development of People Republic of China (MOHURD) made in 1998 Limitation simultaneously progressively forbids being used in polyurethane water-proof paint the decision of coal tar.Within the time in recent years, non-coal is worked out Tar filled-type polyurethane water-proof paint with double-component asphalt and polyurethane water-proof paint be main developing direction, but due to Asphalt double-composition polyurethane waterproof paint has that compatibility is poor, and the acidproof weather-proof water resistance of film is poor, hardness of film The relatively low problem of tensile property, constrains its development.Therefore, compatibility is developed, the asphalt of good waterproof performance increases as filling The polyurethane water-proof paint for moulding the asphalt filling plasticising of material all has great importance in theory and in practice.
The content of the invention
The technical problems to be solved by the invention：It is poor for asphalt Two-component Waterproof Polyurethane Coating compatibility, Cause the drawbacks of acidproof weather-proof water resistance of film is poor, and hardness of film tensile property is relatively low, there is provided a kind of nano-ZnO oil The preparation method of asphalt polyurethane double-component is affine water-repellent paint, is modified by nano-ZnO, improves both compatibilities, is carried Film high is weather-proof, tensile property and water resistance.
In order to solve the above technical problems, the present invention is using technical scheme as described below：A kind of nano-ZnO asphalt The preparation method of polyurethane bicomponent is affine water-repellent paint, its specific preparation process is：
（1）After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 2~3h, in mass ratio 1:2 are delayed Slow stirring mixing, is placed in formation polyether polyols mixed alkoxide solution in there-necked flask, and by polyether polyols mixed alkoxide solution and toluene Diisocyanate mass ratio 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, And 30~40 DEG C, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise, then to three are warming up to there-necked flask during dropwise addition Mouth flask is warming up to 70~80 DEG C, and flow back 2~3h, obtains base polyurethane prepolymer for use as；
（2）Base polyurethane prepolymer for use as after backflow is detected using infrared spectrum, detection is sampled every 30min, When sample is 2272cm in infrared wave number-1When, after there is strong absworption peak, you can above-mentioned base polyurethane prepolymer for use as is stopped to heat, It is naturally cooled to room temperature, base polyurethane prepolymer for use as component is prepared into by being drawn off；
（3）By ZnO powder by high pressure milling device, in the case where pressure is 15~20MPa, carries out high pressure draught and mill, shape Into the nanometer ZnO powder that particle size is 5~10 μm, then, count by weight, choose 6~10 parts of phthalic acid two （2- ethyl hexyls）Ester, 20~65 parts of pitch, 5~10 parts of dimethylethanolamine, the 3,3 of 15~20 parts,- two chloro- 4,4,- two Aminodiphenylmethane, 7~32 parts of precipitated calcium carbonate, 2~8 parts of nano-ZnO are matched, and above-mentioned material vacuum is done Dry 5~8h；
（4）During the material that above-mentioned vacuum drying is completed sequentially added into there-necked flask, at 20~30 DEG C, rotating speed is 300~ Be slowly stirred to it under 500r/min and be thoroughly mixed, after 5~10min to be mixed, by ultrasonic wave carry out auxiliary oscillating 2~ 3min, makes component fully dispersed, you can asphalt component is obtained, and finally can be prepared by a kind of nano-ZnO asphalt polyurethane double Component is affine water-repellent paint.
The affine water-repellent paint base polyurethane prepolymer for use as group of nano-ZnO asphalt polyurethane bicomponent that the present invention is prepared It is divided into brown color, clear viscous liquid, viscosity is 300~500mPa. s；Asphalt component is black, emulsion.
Application process of the invention：Before brushing by base treatment is smooth, dust out and oil stain, it is then poly- by what is prepared Urethane performed polymer component and asphalt component in mass ratio 1:2 ratios are well mixed, with hairbrush that well mixed coating is straight Brushing is connect on basal plane, keeps dynamics uniform, brushing thickness is 0.5~0.8mm, after 1~2h, uses clear water wetting coating, then use Once, brushing thickness is 0.5~0.8mm to the vertical right-angled intersection brushing of hairbrush, treats that it solidifies；Measuring film tensile strength is 5~6MPa, elongation at break is up to 550~600%, and compatible sexual compatibility and water resistance are good.
Compared with other method, Advantageous Effects are the present invention：
（1）The method is modified by nano-ZnO, improves both asphalt and polyurethane coating compatibility, is improved Film is weather-proof, tensile property；
（2）Oozing out for water is effectively prevented, impermeability is improved, waterproof action continues for a long time.
Specific embodiment
After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 2~3h first, in mass ratio 1:2 are delayed Slow stirring mixing, is placed in formation polyether polyols mixed alkoxide solution in there-necked flask, and by polyether polyols mixed alkoxide solution and toluene Diisocyanate mass ratio 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, And 30~40 DEG C, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise, then to three are warming up to there-necked flask during dropwise addition Mouth flask is warming up to 70~80 DEG C, and flow back 2~3h, obtains base polyurethane prepolymer for use as；Then the base polyurethane prepolymer for use as after backflow is used Infrared spectrum detected, detection is sampled every 30min, when sample is 2272cm in infrared wave number-1When, there is strong suction After receiving peak, you can above-mentioned base polyurethane prepolymer for use as is stopped to heat, it is naturally cooled to room temperature, be prepared into by being drawn off poly- Urethane performed polymer component；ZnO powder, in the case where pressure is 15~20MPa, is carried out into high pressure draught stone roller by high pressure milling device again Mill, forms the nanometer ZnO powder that particle size is 5~10 μm, then, counts by weight, chooses 6~10 parts of O-phthalic Acid two（2- ethyl hexyls）Ester, 20~65 parts of pitch, 5~10 parts of dimethylethanolamine, the 3,3 of 15~20 parts,- two chloro- 4, 4,- diaminodiphenyl-methane, 7~32 parts of precipitated calcium carbonate, 2~8 parts of nano-ZnO are matched, and by above-mentioned material 5~8h of vacuum drying；During the material that above-mentioned vacuum drying is completed finally sequentially added into there-necked flask, in 20~30 DEG C, rotating speed It is thoroughly mixed to be slowly stirred to it under 300~500r/min, after 5~10min to be mixed, auxiliary oscillating is carried out by ultrasonic wave 2~3min, makes component fully dispersed, you can asphalt component is obtained, a kind of nano-ZnO asphalt polyurethane is finally can be prepared by Double-component is affine water-repellent paint.
Example 1
After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 2h first, in mass ratio 1:2 are carried out slowly Stirring mixing, is placed in formation polyether polyols mixed alkoxide solution in there-necked flask, and by polyether polyols mixed alkoxide solution and toluene two Isocyanate compares 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, and 30 DEG C are warming up to there-necked flask during dropwise addition, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise, then to there-necked flask 70 DEG C are warming up to, flow back 2h, obtains base polyurethane prepolymer for use as；Base polyurethane prepolymer for use as after backflow is detected using infrared spectrum, Detection is sampled every 30min, when sample is 2272cm in infrared wave number-1When, after there is strong absworption peak, you can to above-mentioned Base polyurethane prepolymer for use as stops heating, it is naturally cooled to room temperature, and base polyurethane prepolymer for use as component is prepared into by being drawn off；Again By ZnO powder by high pressure milling device, in the case where pressure is 15MPa, carries out high pressure draught and mill, form particle size for 5 μm Nanometer ZnO powder, then, count by weight, choose 8 parts of phthalic acid two（2- ethyl hexyls）Ester, 35 parts of pitch, 8 parts of dimethylethanolamine, the 3,3 of 15 parts,- two chloro- 4,4,- diaminodiphenyl-methane, 28 parts of precipitated calcium carbonate, 6 parts Nano-ZnO is matched, and above-mentioned material is vacuum dried into 5h；The material that above-mentioned vacuum drying is completed finally is sequentially added three In mouth flask, at 20 DEG C, rotating speed is thoroughly mixed to be slowly stirred to it under 300r/min, after 5min to be mixed, by ultrasonic wave Auxiliary oscillating 2min is carried out, makes component fully dispersed, you can asphalt component is obtained, a kind of nano-ZnO oil is finally can be prepared by Asphalt polyurethane double-component is affine water-repellent paint.
Before brushing by base treatment is smooth, dust out and oil stain, then the base polyurethane prepolymer for use as component that will be prepared and Asphalt component in mass ratio 1:2 ratios are well mixed, and are directly brushed on basal plane well mixed coating with hairbrush, are protected Holding force degree is uniform, and brushing thickness is 0.5mm, after 1h, uses clear water wetting coating, then with the vertical right-angled intersection brushing of hairbrush once, Brushing thickness is 0.5mm, treats that it solidifies；Film tensile strength is measured for 5MPa, elongation at break is up to 550%, and compatibility is close It is good with property and water resistance.
Example 2
After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 2.5h first, in mass ratio 1:2 are delayed Slow stirring mixing, is placed in formation polyether polyols mixed alkoxide solution in there-necked flask, and by polyether polyols mixed alkoxide solution and toluene Diisocyanate mass ratio 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, And 35 DEG C, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise are warming up to there-necked flask during dropwise addition, then three mouthfuls are burnt Bottle is warming up to 75 DEG C, and flow back 2.5h, obtains base polyurethane prepolymer for use as；Base polyurethane prepolymer for use as after backflow is examined using infrared spectrum Survey, detection is sampled every 30min, when sample is 2272cm in infrared wave number-1When, after there is strong absworption peak, you can right Above-mentioned base polyurethane prepolymer for use as stops heating, it is naturally cooled to room temperature, and base polyurethane prepolymer for use as group is prepared into by being drawn off Point；ZnO powder, in the case where pressure is 18MPa, is carried out high pressure draught and milled by high pressure milling device again, particle size is formed It is 5 μm of nanometer ZnO powder, then, counts by weight, chooses 10 parts of phthalic acid two（2- ethyl hexyls）Ester, 45 parts Pitch, 5 parts of dimethylethanolamine, the 3,3 of 15 parts,- two chloro- 4,4,- diaminodiphenyl-methane, 20 parts of lightweight carbonic acid Calcium, 5 parts of nano-ZnO are matched, and above-mentioned material are vacuum dried into 7h；Finally by above-mentioned vacuum drying complete material according to In secondary addition there-necked flask, at 25 DEG C, rotating speed is thoroughly mixed to be slowly stirred to it under 400r/min, after 8min to be mixed, leads to Crossing ultrasonic wave carries out auxiliary oscillating 3min, makes component fully dispersed, you can asphalt component is obtained, a kind of nanometer is finally can be prepared by ZnO asphalt polyurethane bicomponents are affine water-repellent paint.
Before brushing by base treatment is smooth, dust out and oil stain, then the base polyurethane prepolymer for use as component that will be prepared and Asphalt component in mass ratio 1:2 ratios are well mixed, and are directly brushed on basal plane well mixed coating with hairbrush, are protected Holding force degree is uniform, and brushing thickness is 0.7mm, after 1.5h, uses clear water wetting coating, then with the vertical right-angled intersection brushing one of hairbrush Secondary, brushing thickness is 0.6mm, treats that it solidifies；Film tensile strength is measured for 5.5MPa, elongation at break is up to 570%, phase Capacitive compatibility and water resistance are good.
Example 3
After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 3h first, in mass ratio 1:2 are carried out slowly Stirring mixing, is placed in formation polyether polyols mixed alkoxide solution in there-necked flask, and by polyether polyols mixed alkoxide solution and toluene two Isocyanate compares 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, and 40 DEG C are warming up to there-necked flask during dropwise addition, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise, then to there-necked flask 80 DEG C are warming up to, flow back 3h, obtains base polyurethane prepolymer for use as；Base polyurethane prepolymer for use as after backflow is detected using infrared spectrum, Detection is sampled every 30min, when sample is 2272cm in infrared wave number-1When, after there is strong absworption peak, you can to above-mentioned Base polyurethane prepolymer for use as stops heating, it is naturally cooled to room temperature, and base polyurethane prepolymer for use as component is prepared into by being drawn off；Again By ZnO powder by high pressure milling device, in the case where pressure is 20MPa, carries out high pressure draught and mill, form particle size for 5 μm Nanometer ZnO powder, then, count by weight, choose 6 parts of phthalic acid two（2- ethyl hexyls）Ester, 55 parts of pitch, 7 parts of dimethylethanolamine, the 3,3 of 18 parts,- two chloro- 4,4,- diaminodiphenyl-methane, 10 parts of precipitated calcium carbonate, 4 parts Nano-ZnO is matched, and above-mentioned material is vacuum dried into 8h；The material that above-mentioned vacuum drying is completed finally is sequentially added three In mouth flask, at 30 DEG C, rotating speed is thoroughly mixed to be slowly stirred to it under 500r/min, after 10min to be mixed, by ultrasonic wave Auxiliary oscillating 3min is carried out, makes component fully dispersed, you can asphalt component is obtained, a kind of nano-ZnO oil is finally can be prepared by Asphalt polyurethane double-component is affine water-repellent paint.
Before brushing by base treatment is smooth, dust out and oil stain, then the base polyurethane prepolymer for use as component that will be prepared and Asphalt component in mass ratio 1:2 ratios are well mixed, and are directly brushed on basal plane well mixed coating with hairbrush, are protected Holding force degree is uniform, and brushing thickness is 0.8mm, after 2h, uses clear water wetting coating, then with the vertical right-angled intersection brushing of hairbrush once, Brushing thickness is 0.8mm, treats that it solidifies；Film tensile strength is measured for 6MPa, elongation at break is up to 600%, and compatibility is close It is good with property and water resistance.

Claims (1)

1. a kind of preparation method of the affine water-repellent paint of nano-ZnO asphalt polyurethane bicomponent, it is characterised in that specific system It is for step：
（1）After polyoxypropyleneglycol and polytetrahydrofuran diol are vacuum dried into 2~3h, in mass ratio 1:2 are slowly stirred Mixing is mixed, formation polyether polyols mixed alkoxide solution in there-necked flask is placed in, and it is different by polyether polyols mixed alkoxide solution and toluene two Cyanate mass ratio 50:1 ratio, toluene di-isocyanate(TDI) is slowly added dropwise in there-necked flask by the speed of 3s/ drops, and 30~40 DEG C are warming up to during dropwise addition to there-necked flask, after the completion for the treatment of that toluene di-isocyanate(TDI) is slowly added dropwise, then three mouthfuls are burnt Bottle is warming up to 70~80 DEG C, and flow back 2~3h, obtains base polyurethane prepolymer for use as；
（2）Base polyurethane prepolymer for use as after backflow is detected using infrared spectrum, detection is sampled every 30min, worked as sample Product are 2272cm in infrared wave number-1When, after there is strong absworption peak, you can above-mentioned base polyurethane prepolymer for use as is stopped to heat, makes it Room temperature is naturally cooled to, base polyurethane prepolymer for use as component is prepared into by being drawn off；
（3）By ZnO powder by high pressure milling device, in the case where pressure is 15~20MPa, carries out high pressure draught and mill, form grain Footpath size is 5~10 μm of nanometer ZnO powder, then, is counted by weight, chooses 6~10 parts of phthalic acid two（2- second Base oneself）Ester, 20~65 parts of pitch, 5~10 parts of dimethylethanolamine, the 3,3 of 15~20 parts,- two chloro- 4,4,- diaminourea two Phenylmethane, 7~32 parts of precipitated calcium carbonate, 2~8 parts of nano-ZnO are matched, and by above-mentioned material be vacuum dried 5~ 8h；
（4）During the material that above-mentioned vacuum drying is completed sequentially added into there-necked flask, at 20~30 DEG C, rotating speed is 300~500r/ It is slowly stirred to it under min and is thoroughly mixed, after 5~10min to be mixed, 2~3min of auxiliary oscillating is carried out by ultrasonic wave, makes group Divide fully dispersed, you can asphalt component is obtained, finally can be prepared by a kind of nano-ZnO asphalt polyurethane bicomponent affine anti- Water paint.
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