CN114958133A - Bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating and preparation method thereof - Google Patents
Bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating and preparation method thereof Download PDFInfo
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- CN114958133A CN114958133A CN202210412976.4A CN202210412976A CN114958133A CN 114958133 A CN114958133 A CN 114958133A CN 202210412976 A CN202210412976 A CN 202210412976A CN 114958133 A CN114958133 A CN 114958133A
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
- C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
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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
- C09D195/00—Coating compositions based on bituminous materials, e.g. asphalt, tar, pitch
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- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
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Abstract
The invention relates to a bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating and a preparation method thereof, wherein the bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating comprises the following raw materials in parts by weight: 40-55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion, 30-50 parts of asphalt emulsion, 0.2-1 part of defoaming agent, 5-10 parts of flame retardant and 1-4 parts of anti-precipitation auxiliary agent. The bio-based polyurethane-acrylate interpenetrating network emulsion is prepared by interpenetrating network synthesis of polyurethane and acrylate prepared from modified castor oil polyester polyol, and has the advantages of excellent low-temperature flexibility, high elongation, high tensile strength and low gel rate.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating and a preparation method thereof.
Background
The high-speed railway bridge in China is mostly of a reinforced concrete structure, and the concrete bridge structure is corroded by rain erosion and penetration, so that the service life of the bridge is shortened. The maintenance cost is higher in the operation process, and certain difficulty is provided. With the development of high-speed rail construction in China, the requirements on bridge deck water resistance are higher and higher due to different temperature difference between south and north and different rainwater.
The current common waterproof materials for high-speed rail bridge decks comprise asphalt coiled materials, rubber asphalt coatings and polyurethane elastic coatings. The construction of asphalt coiled material is mostly artifical naked light and toasts the construction, and the efficiency of construction is low, and the coiled material is difficult to toast completely for the coiled material bonds poorly with the substrate, and the easy cluster of coiled material junction is watery, and water-proof effects is relatively poor. Most of polyurethane coatings are solvent-based coatings, and organic solvents volatilize to pollute the environment. The polyurethane coating has slow curing speed, is sensitive to the environmental temperature and humidity, and has easy foaming on the surface, thereby limiting the application of the polyurethane coating. The rubber asphalt coating is a fast curing coating, and has high construction efficiency and low cost. The common rubber modified asphalt paint mainly comprises asphalt emulsion, neoprene latex, styrene-butadiene latex and a demulsifier. The mechanical construction and demulsification speed are high, a complete waterproof layer can be formed on a substrate, and the rubber asphalt coating has certain self-repairing capability, but the existing rubber asphalt coating has the defects that the low resistance is difficult to reach-40 ℃, the mechanical property is poor, and the like.
With the improvement of environmental protection consciousness of people, the environmental protection requirement is higher and higher, so that the search for the waterproof coating for the high-speed railway bridge floor, the performance index of which meets the requirement, becomes a key point and a difficult point of the research in the industry. CN112694825A discloses a special polyurethane waterproof coating for high-speed railway roads and bridges, which is prepared from A, B components, wherein the A component comprises castor oil polyol, polyether glycol and isocyanate, the B component comprises polyether triol, 3-dichloro-4, 4-diaminodiphenylmethane, a whisker material, talcum powder, silicon dioxide powder, iron oxide red and lead naphthenate, and the double-component polyurethane coating is easy to be involved in bubbles during construction, does not influence the product performance, is beneficial to spraying construction, is low in construction efficiency, long in film forming time and low in product elongation, and cannot be self-repaired.
Based on this, how to obtain a waterproof material which has ideal low temperature resistance and mechanical properties and is friendly to the environment is still an important problem to be solved in the field.
Disclosure of Invention
The invention aims to solve the problems in the prior art, provides a bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating with excellent performance and environmental protection, and also provides a preparation method thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating which is prepared from the following raw materials in parts by weight:
as some preferred embodiments of the present invention, the bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
as some preferable schemes of the invention, the bio-based polyurethane-acrylate interpenetrating network emulsion is prepared by the following method:
adding hydrophilic castor oil polyester polyol and diphenylmethane diisocyanate into a reaction container, reacting for 2-3h at a set temperature of 80-85 ℃ under the protection of nitrogen, stopping heating after the measured isocyanate group reaches a theoretical value, adding butyl acrylate, propyl acrylate, trimethylolpropane triacrylate, a polyurethane chain extender, an emulsifier CO-436 and triethylamine after the temperature is reduced to 45-50 ℃, continuously stirring for 25-30min, adding deionized water at a set stirring speed of 800-.
As some preferred embodiments of the present invention, the urethane chain extender is an oxazolidine chain extender, and the oxazolidine chain extender is prepared from the following raw materials:
33-39 parts of diethanolamine;
22-28 parts of isobutyraldehyde;
36-42 parts of isophorone diisocyanate.
As some preferred embodiments of the present invention, the preparation method of the oxazolidine chain extender is as follows:
adding diethanol amine into a reaction vessel, adding isobutyraldehyde, cooling, keeping the temperature at 40-45 ℃, keeping the temperature for 2-2.5h, heating and reacting at the set temperature of 90-95 ℃ for 3h, cooling to 50-60 ℃, decompressing and dewatering, heating to 100 ℃ and 110 ℃, keeping the vacuum degree at 0.09-0.095MPa, keeping the temperature for 1.5-2h, stopping heating, and adding isophorone diisocyanate to obtain the oxazolidine chain extender.
As some preferred embodiments of the present invention, the hydrophilic castor oil polyester polyol is prepared from the following raw materials:
as some preferred embodiments of the present invention, the modified castor oil polyester polyol is prepared by the following steps:
adding castor oil and glycerin into a reaction vessel, setting the temperature at 220-235 ℃, keeping the temperature for 2.5-3h, cooling to the temperature below 90-100 ℃, adding adipic acid, setting the temperature at 230-235 ℃, reacting for 2h, stopping heating after the acid value reaches 5mgKOH/g, cooling to the temperature of 80-85 ℃, adding phthalic anhydride, setting the temperature at 150-160 ℃, keeping the temperature for 1-1.5h, and stopping heating after the acid value reaches 45-52mgKOH/g to obtain the hydrophilic castor oil polyester polyol.
As some preferred embodiments of the present invention, the antifoaming agent is selected from FOAMEX 825.
As some preferred embodiments of the present invention, the flame retardant is selected from ZH-8024.
As some preferable schemes of the invention, the anti-precipitation auxiliary agent is selected from ECO-6000.
The invention also provides a preparation method of the bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating, which comprises the following steps:
adding other raw materials except the flame retardant and the anti-precipitation auxiliary agent into a stirring device according to the formula ratio, stirring for 20-35 minutes at 600 revolutions per minute, adding the flame retardant and the anti-precipitation auxiliary agent, stirring for 10-15 minutes at 800 revolutions per minute, and discharging to obtain the flame retardant and anti-precipitation auxiliary agent.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in:
the bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating provided by the invention is verified to have the adhesive force higher than 1.1MPa on the surface of a concrete base material, the tensile strength higher than 1.5MPa, the elongation at break higher than 1250%, and the surface has no cracks and no cracks when tested at the low temperature of minus 45 ℃, the gel rate is lower than 0.5%, and the performance requirement and the production requirement are met.
The bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating provided by the invention takes bio-based polyurethane-acrylate interpenetrating network emulsion as a raw material, can form physical crosslinking by utilizing self-carried carbamate groups with higher cohesion, and the self-made hydrophilic castor oil polyol has side groups and can provide internal plasticization, so that the coating is also excellent in low-temperature flexibility and high in mechanical strength.
The oxazolidine chain extender used in the bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating provided by the invention has secondary amine with certain steric hindrance, is low in activity, is uniformly dispersed in a system before emulsification, and can be wrapped by an emulsifier after water is added, so that the gel rate is low.
The method provided by the invention is quick and simple in construction, and can meet the requirements of construction sites.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail and fully with reference to the following embodiments.
Example 1 polyurethane chain extender
The raw materials are as follows:
| diethanolamine (DEA) | 36 portions of |
| Isobutyraldehyde | 25 portions of |
| Isophorone diisocyanate | 39 portions of |
The preparation method comprises the following steps:
adding 36 parts of diethanolamine into a four-mouth bottle with a thermometer, a mechanical stirring device and a reduced pressure distillation device, adding 25 parts of isobutyraldehyde, cooling, keeping the temperature at 45 ℃, and keeping for 2 hours. The reaction was heated at a set temperature of 95 ℃ for 3 h. Cooling to 60 deg.C, removing water under reduced pressure, heating to 100 deg.C, maintaining vacuum degree at 0.095MPa for 2 hr, and stopping heating. And adding 39 parts of isophorone diisocyanate to obtain the oxazolidine chain extender.
Example 2 hydrophilic Castor oil polyester polyol
The hydrophilic castor oil polyester polyol is prepared from the following raw materials:
the preparation method of the hydrophilic castor oil polyester polyol comprises the following steps:
82 parts of castor oil and 5 parts of glycerol are added into a four-mouth bottle with a water separator, a thermometer, mechanical stirring and nitrogen protection, the temperature is set to be 220 ℃, and the mixture is kept for 3 hours. Cooling to below 100 ℃, adding 5 parts of adipic acid, setting the temperature to 230 ℃, reacting for 2 hours, stopping heating after the acid value is measured to reach 5mgKOH/g, cooling to 80 ℃, adding 10 parts of phthalic anhydride, setting the temperature to 150 ℃, keeping for 1 hour, measuring the acid to be 45-52mgKOH/g, and stopping heating to obtain the hydrophilic castor oil polyester polyol.
Example 3-1 Bio-based polyurethane-acrylate interpenetrating network emulsion 1#
The bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
| hydrophilic castor oil polyester polyol | 30 portions of |
| Diphenylmethane diisocyanate | 7 portions of |
| Acrylic acid butyl ester | 10 portions of |
| Acrylic acid propyl ester | 3 portions of |
| Polyurethane chain extender | 2 portions of |
| Trihydroxymethyl triacrylate | 0.5 portion |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.3 part |
| Triethylamine | 1 part of |
| Sodium bicarbonate | 0.2 part |
| Deionized water | 45 portions of |
Adding 30 parts of the hydrophilic castor oil polyester polyol prepared in the example 2 and 7 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to be 80 ℃ for reaction for 2.5h, measuring isocyanate groups to reach a theoretical value, stopping heating, reducing the temperature to 45 ℃, adding 10 parts of butyl acrylate, 3 parts of propyl acrylate, 0.5 part of trimethylolpropane triacrylate, 2 parts of polyurethane chain extender, 1 part of emulsifier CO-436 and 1 part of triethylamine, continuing stirring for 30min, adding 45 parts of deionized water, setting the stirring speed to be 900r/min, stirring for 10min, adding 0.3 part of ammonium persulfate and 0.2 part of sodium bicarbonate, setting the temperature to be 85 ℃ for reaction for 2h, setting the temperature to be 90 ℃ for reaction for 1h, and stopping heating to obtain the bio-based modified acrylate interpenetrating network emulsion.
Example 3-2 Bio-based polyurethane-acrylate interpenetrating network emulsion 2#
The bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
| hydrophilic castor oil polyester polyol | 35 portions of |
| Diphenylmethane diisocyanate | 7 portions of |
| Acrylic acid butyl ester | 5 portions of |
| Acrylic acid propyl ester | 6 portions of |
| Polyurethane chain extender | 1 part of |
| Trihydroxymethyl triacrylate | 1 part of |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.2 part |
| Triethylamine | 2 portions of |
| Sodium bicarbonate | 0.1 part |
| Deionized water | 41.7 parts |
Adding 35 parts of the hydrophilic castor oil polyester polyol prepared in example 2 and 7 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to be 80 ℃ for reaction for 2.5h, measuring isocyanate groups to reach a theoretical value, stopping heating, reducing the temperature to 45 ℃, adding 5 parts of butyl acrylate, 6 parts of propyl acrylate, 1 part of trimethylolpropane triacrylate, 1 part of polyurethane chain extender, 1 part of emulsifier CO-436 and 2 parts of triethylamine, continuing stirring for 30min, adding 41.7 parts of deionized water, setting the stirring speed to be 900r/min, stirring for 10min, adding 0.2 part of ammonium persulfate and 0.1 part of sodium bicarbonate, setting the temperature to be 85 ℃ for reaction for 2h, setting the temperature to be 90 ℃ for reaction for 1h, and stopping heating to obtain the bio-based modified acrylate interpenetrating network emulsion.
Example 3-3 Bio-based polyurethane-acrylate interpenetrating network emulsion 3#
The bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
| hydrophilic castor oil polyester polyol | 30 portions of |
| Diphenylmethane diisocyanate | 10 portions of |
| Acrylic acid butyl ester | 5 portions of |
| Acrylic acid propyl ester | 3 portions of |
| Polyurethane chain extender | 1 part of |
| Trihydroxymethyl triacrylate | 0.5 portion |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.3 part |
| Triethylamine | 2 portions of |
| Sodium bicarbonate | 0.2 part |
| Deionized water | 45 portions of |
Adding 30 parts of the hydrophilic castor oil polyester polyol prepared in the example 2 and 10 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to be 80 ℃ for reaction for 2.5h, measuring isocyanate groups to reach a theoretical value, stopping heating, reducing the temperature to 45 ℃, adding 5 parts of butyl acrylate, 3-propyl acrylate, 0.5 part of trimethylolpropane triacrylate, 1 part of polyurethane chain extender, 1 part of emulsifier CO-436 and 2 parts of triethylamine, continuing stirring for 30min, adding 45 parts of deionized water, setting the stirring speed to be 900r/min, stirring for 10min, adding 0.3 part of ammonium persulfate and 0.2 part of sodium bicarbonate, setting the temperature to be 85 ℃ for reaction for 2h, setting the temperature to be 90 ℃ for reaction for 1h, and stopping heating to obtain the biological-based modified acrylate interpenetrating network emulsion.
Example 4-1 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
A bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating is prepared from the following raw materials in parts by weight:
| bio-based polyurethane-acrylate interpenetrating network emulsion 1# | 40 portions of |
| Asphalt emulsion | 50 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 6 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 3 portions of |
According to the formula mass ratio, 40 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 1, 50 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 6 parts of flame retardant, 3 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute, and discharging.
Example 4-2 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 1# | 45 portions of |
| Asphalt emulsion | 40.8 parts of |
| Defoaming agent: FOAMEX 825 digao | 0.2 part |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 10 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 4 portions of |
According to the formula mass ratio, 45 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 1, 40.8 parts of asphalt emulsion, 0.2 part of defoaming agent are stirred for 30 minutes at 500 revolutions per minute, 10 parts of flame retardant and 4 parts of anti-precipitation auxiliary agent are stirred for 15 minutes at 600 revolutions per minute, and then the materials are discharged.
Example 4-2 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 1# | 55 portions of |
| Asphalt emulsion | 38.5 portions |
| Defoaming agent: FOAMEX 825 digao | 0.5 portion |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 5 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 1 part of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 1, 38.5 parts of asphalt emulsion, 0.5 part of defoaming agent, stirring at 500 revolutions per minute for 30 minutes, 5 parts of flame retardant, 1 part of anti-precipitation auxiliary agent, stirring at 600 revolutions per minute for 15 minutes, and discharging.
Examples 4-4 Bio-based modified Low temperature resistant quick setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 1# | 55 portions of |
| Asphalt emulsion | 30 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 10 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 4 portions of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 1, 30 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 10 parts of flame retardant and 4 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute, and discharging.
Examples 4-5 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 2# | 55 portions of |
| Asphalt emulsion | 35 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 2 portions of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 2, 35 parts of asphalt emulsion, 1 part of defoaming agent, 30 parts of stirring at 50 revolutions per minute, 7 parts of flame retardant and 2 parts of anti-precipitation auxiliary agent according to the mass ratio of the formula, stirring for 15 minutes at 60 revolutions per minute, and discharging.
Examples 4-6 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 2# | 50 portions of |
| Asphalt emulsion | 40 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 2 portions of |
Stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant and 2 parts of anti-precipitation auxiliary agent according to the formula mass ratio of 50 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 2, 40 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 600 minutes, and discharging.
Examples 4-7 Bio-based modified Low temperature resistant quick-setting asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion 3# | 55 portions of |
| Asphalt emulsion | 35 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 2 portions of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion No. 3, 35 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant and 2 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute, and discharging.
Comparative example 1
Step 1) bio-based polyurethane-acrylate interpenetrating network emulsion
| Hydrophilic castor oil polyester polyol | 30 portions of |
| Diphenylmethane diisocyanate | 10 portions of |
| Acrylic acid butyl ester | 5 portions of |
| Acrylic acid propyl ester | 3 portions of |
| Butanediamine | 3 portions of |
| Trihydroxymethyl triacrylate | 0.5 portion |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.3 part |
| Triethylamine | 2 portions of |
| Sodium bicarbonate | 0.2 part |
| Deionized water | 45 portions of |
Adding 30 parts of hydrophilic castor oil polyester polyol and 10 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to 80 ℃ for reaction for 2.5h, measuring isocyanate groups to reach a theoretical value, stopping heating, cooling to 45 ℃, adding 5 parts of butyl acrylate, 3 parts of propyl acrylate, 0.5 part of trimethylolpropane triacrylate, 1 part of emulsifier CO-436 and 2 parts of triethylamine, continuously stirring for 30min, adding 45 parts of deionized water, setting the stirring speed to 900r/min, stirring for 10min, slowly adding 3 parts of butanediamine, stirring for 30min, adding 0.3 part of ammonium persulfate and 0.2 part of sodium bicarbonate, setting the temperature to 85 ℃ for reaction for 2h, setting the temperature to 90 ℃ for reaction for 1h, and stopping heating to obtain the biological-based modified acrylate interpenetrating network emulsion.
Step 2) bio-based modified low temperature resistant asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion | 55 portions of |
| Asphalt emulsion | 35 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: new Teng Ying material isLimited company ECO-6000 | 2 portions of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion, 35 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant, 2 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute and discharging.
Comparative example 2 bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating
Which is prepared from the following raw materials
According to the formula, 50 parts of neoprene latex, 5 parts of styrene-butadiene latex, 35 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant, 2 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute, and discharging.
Comparative example 3
Step 1) bio-based polyurethane-acrylate interpenetrating network emulsion
The bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
| hydrophilic castor oil polyester polyol | 30 portions of |
| Diphenylmethane diisocyanate | 10 portions of |
| Acrylic acid butyl ester | 5 portions of |
| Acrylic acid propyl ester | 3 portions of |
| 1, 4-butanediol | 1 part of |
| Trihydroxymethyl triacrylate | 0.5 portion |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.3 part |
| Triethylamine | 2 portions of |
| Sodium bicarbonate | 0.2 part |
| Deionized water | 45 portions of |
Adding 30 parts of hydrophilic castor oil polyester polyol and 10 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to 80 ℃ for reaction for 2-3h, measuring isocyanate groups to reach a theoretical value, stopping heating, cooling to 45 ℃, adding 5 parts of butyl acrylate, 3 parts of propyl acrylate, 0.5 part of trimethylolpropane triacrylate, 1 part of 1, 4-butanediol, 1 part of emulsifier CO-436 and 2 parts of triethylamine, continuously stirring for 30min, adding 45 parts of deionized water, setting the stirring speed to 900r/min, stirring for 10min, adding 0.3 part of ammonium persulfate and 0.2 part of sodium bicarbonate, setting the temperature to 85 ℃ for reaction for 2h, setting the temperature to 90 ℃ for reaction for 1h, and stopping heating to obtain the bio-based modified acrylate interpenetrating network emulsion.
Step 2) bio-based modified low temperature resistant asphalt emulsion coating
| Bio-based polyurethane-acrylate interpenetrating network emulsion | 55 portions of |
| Asphalt emulsion | 35 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 2 portions of |
55 parts of bio-based polyurethane-acrylate interpenetrating network emulsion, 35 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant, 2 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute and discharging.
Comparative example 4
Step 1) polyurethane-acrylate interpenetrating network emulsion
The polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
| castor oil polyester polyol | 30 portions of |
| Diphenylmethane diisocyanate | 10 portions of |
| Acrylic acid butyl ester | 5 portions of |
| Acrylic acid propyl ester | 3 portions of |
| Polyurethane chain extender | 1 part of |
| Trihydroxymethyl triacrylate | 0.5 portion |
| Emulsifier CO-436 | 1 part of |
| Ammonium persulfate | 0.3 part |
| Triethylamine | 2 portions of |
| Sodium bicarbonate | 0.2 part |
| Deionized water | 45 portions of |
Adding 30 parts of castor oil polyester polyol and 10 parts of diphenylmethane diisocyanate into a four-mouth bottle with a mechanical stirring, thermometer, nitrogen protection and constant-pressure dropping funnel, setting the temperature to 80 ℃ for reaction for 2.5h, measuring isocyanate groups to reach a theoretical value, stopping heating, cooling to 45 ℃, adding 5 parts of butyl acrylate, 3 parts of propyl acrylate, 0.5 part of trimethylolpropane triacrylate, 1 part of polyurethane chain extender, 1 part of emulsifier CO-436 and 2 parts of triethylamine, continuing stirring for 30min, adding 45 parts of deionized water, setting the stirring speed to 900r/min, stirring for 10min, adding 0.3 part of ammonium persulfate and 0.2 part of sodium bicarbonate, setting the temperature to 85 ℃ for reaction for 2h, setting the temperature to 90 ℃ for reaction for 1h, and stopping heating to obtain the acrylate interpenetrating network emulsion.
Step 2) modified low temperature resistant asphalt emulsion coating
| Polyurethane-acrylate interpenetrating network emulsion | 55 portions of |
| Asphalt emulsion | 35 portions of |
| Defoaming agent: FOAMEX 825 digao | 1 part of |
| Flame retardant: hao ZH-8024 in Huangshan mountain | 7 portions of |
| Anti-settling aid: ten new materials, Inc. ECO-6000 | 2 portions of |
55 parts of polyurethane-acrylate interpenetrating network emulsion, 35 parts of asphalt emulsion, 1 part of defoaming agent, stirring for 30 minutes at 500 revolutions per minute, 7 parts of flame retardant, 2 parts of anti-precipitation auxiliary agent, stirring for 15 minutes at 600 revolutions per minute and discharging.
Examples of effects
The concrete base material adhesion, tensile strength, elongation at break, low-temperature flexibility and the like of the above examples 4-1 to 4-7 and comparative examples 1 to 4 were tested according to GB/T16777-2008, and the gel fraction and the like of the modified asphalt coating were compared. The test results are given in table 1 below.
TABLE 1
As can be seen from the data in Table 1, in examples 4-1 to 4-7, the self-made hydrophilic castor oil polyol is used to react with isocyanate, the oxazolidine polyurethane chain extender is added to prepare the bio-based modified low temperature resistant asphalt emulsion coating, the adhesive force of the bio-based modified low temperature resistant asphalt emulsion coating on the surface of a concrete substrate is higher than 1.1MPa, the tensile strength is higher than 1.5MPa, the elongation at break is larger than 1250%, the surface has no cracks and no cracks in a low temperature flexibility test at-45 ℃, the gel fraction is smaller than 0.5%, and the performance requirements and the production requirements are met. Compared with the embodiments 4 to 7, in the comparative example 1, chain extension is performed by using butanediamine, and as the reactivity of aliphatic primary amine and isocyanate is too high, and butanediamine is easily soluble in water, butanediamine is reacted with isocyanate without entering emulsion particles, and the formed polyurethane polymer is difficult to be wrapped by an emulsifier, the gel rate is too high, secondary amine with certain steric hindrance is used as the oxazolidine chain extender, the activity is lower, the secondary amine is uniformly dispersed in a system before emulsification, secondary amine generated after water is added can be wrapped by the emulsifier, and the gel rate is low. Compared with the examples 4 to 7, the comparison result shows that the tensile strength and the elongation at break of the asphalt emulsion modified by the bio-based polyurethane-acrylate interpenetrating network emulsion are higher than those of the asphalt emulsion modified by the neoprene latex and the styrene-butadiene latex, because the bio-based polyurethane-acrylate interpenetrating network emulsion has carbamate groups with higher cohesive force and can form physical crosslinking, and the self-made hydrophilic castor oil polyol has a side group and can provide internal plasticization, the low-temperature flexibility is also excellent. As can be seen from comparison of comparative example 3 with examples 4-7, the strength and elongation at break of the modified asphalt coating prepared by using the self-made polyurethane chain extender are much higher than those of the modified asphalt coating prepared by using the conventional 1, 4-butanediol polyurethane chain extender. Because the self-made polyurethane chain extender molecule contains a group urethane bond with larger cohesive force, and is decomposed into two secondary amine chain extenders after water is added, the chain extenders react with isocyanate to form carbamido groups, and the cohesive force strength of the chain extenders is higher than that of the urethane bond formed by the reaction of 1, 4-butanediol and isocyanate. The reactivity of isocyanate and secondary amine group is much higher than that of isocyanate, hydroxyl and water, so the molecular weight can be formed by using the self-made chain extender, and the molecular weight formed by using 1, 4-butanediol for chain extension is small. Therefore, the performance of the modified asphalt coating prepared from the self-made polyurethane chain extender is superior to that of the modified asphalt coating prepared from the conventional polyurethane chain extender 1, 4-butanediol. Compared with examples 4-7, the comparison of comparative example 4 and examples 4-7 shows that the modified asphalt coating prepared by using the conventional castor oil polyol has higher gel fraction, and the tensile strength, adhesion and elongation at break of the modified asphalt coating prepared by using the conventional castor oil polyol are obviously lower than those of the modified asphalt coating prepared by using the hydrophilic castor oil polyol. Because the conventional castor oil polyalcohol does not contain salt-forming groups, the prepared urethane-acrylate interpenetrating network emulsion is difficult to form stable emulsion particles, is easy to break emulsion and gel, and reduces the content of bio-based polyurethane-acrylate film-forming substances in the modified asphalt coating, so that the tensile strength, the adhesive force and the elongation at break are obviously reduced.
Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art may still make modifications to the technical solutions described in the foregoing embodiments, or may substitute some technical features of the embodiments; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating is characterized by being prepared from the following raw materials in parts by weight:
2. the bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 1, wherein the bio-based polyurethane-acrylate interpenetrating network emulsion is prepared from the following raw materials:
3. the bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 2, wherein the bio-based polyurethane-acrylate interpenetrating network emulsion is prepared by the following method:
adding hydrophilic castor oil polyester polyol and diphenylmethane diisocyanate into a reaction container, reacting for 2-3h at a set temperature of 80-85 ℃ under the protection of nitrogen, stopping heating after the content of isocyanato reaches a theoretical value is determined, adding butyl acrylate, propyl acrylate, trimethylolpropane triacrylate, a polyurethane chain extender, an emulsifier CO-436 and triethylamine after the temperature is reduced to 45-50 ℃, continuously stirring for 25-30min, adding deionized water at a set stirring speed of 800 ℃ for 1000r/min, stirring for 10-15min, adding ammonium persulfate and sodium bicarbonate, reacting for 2-2.5h at a set temperature of 80-85 ℃, reacting for 1-1.5h at a set temperature of 85-90 ℃, and stopping heating to obtain the bio-based modified acrylate interpenetrating network emulsion.
4. The bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating as claimed in claim 1, wherein the urethane chain extender is oxazolidine chain extender, and the oxazolidine chain extender is prepared from the following raw materials:
33-39 parts of diethanolamine;
22-28 parts of isobutyraldehyde;
36-42 parts of isophorone diisocyanate.
5. The bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 4, wherein the preparation method of the oxazolidine chain extender is as follows:
adding diethanolamine into a reaction vessel, adding isobutyraldehyde, cooling to 40-45 ℃, keeping for 2-2.5h, heating to react for 3h at a set temperature of 90-95 ℃, cooling to 50-60 ℃, removing water under reduced pressure, heating to 100-.
6. The bio-based modified low-temperature-resistant quick-setting asphalt emulsion coating as claimed in claim 2, wherein the hydrophilic castor oil polyester polyol is prepared from the following raw materials:
7. the bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 6, wherein the modified castor oil polyester polyol is prepared by the following steps:
adding castor oil and glycerol into a reaction vessel, setting the temperature at 220-.
8. The bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 1, wherein said defoamer is selected from FOAMEX 825.
9. The bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in claim 1, wherein said flame retardant is selected from ZH-8024, and said anti-settling auxiliary is selected from ECO-6000.
10. The preparation method of the bio-based modified low temperature resistant quick-setting asphalt emulsion coating as claimed in any one of claims 1 to 9, which is characterized by comprising the following steps:
adding the bio-based polyurethane-acrylate interpenetrating network emulsion and the asphalt emulsion into a stirring device according to the formula ratio, stirring for 20-35 minutes at the speed of 300-.
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