CN112852376B - Environment-friendly colored anti-skid pavement capable of melting ice and preparation method thereof - Google Patents
Environment-friendly colored anti-skid pavement capable of melting ice and preparation method thereof Download PDFInfo
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- 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
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
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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
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- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
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- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
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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
- 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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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C11/00—Details of pavings
- E01C11/005—Methods or materials for repairing pavings
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C11/00—Details of pavings
- E01C11/24—Methods or arrangements for preventing slipperiness or protecting against influences of the weather
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C11/00—Details of pavings
- E01C11/24—Methods or arrangements for preventing slipperiness or protecting against influences of the weather
- E01C11/245—Methods or arrangements for preventing slipperiness or protecting against influences of the weather for preventing ice formation or for loosening ice, e.g. special additives to the paving material, resilient coatings
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- E—FIXED CONSTRUCTIONS
- E01—CONSTRUCTION OF ROADS, RAILWAYS, OR BRIDGES
- E01C—CONSTRUCTION OF, OR SURFACES FOR, ROADS, SPORTS GROUNDS, OR THE LIKE; MACHINES OR AUXILIARY TOOLS FOR CONSTRUCTION OR REPAIR
- E01C7/00—Coherent pavings made in situ
Abstract
The invention relates to an environment-friendly colored anti-skid pavement capable of melting ice and a preparation method thereof, wherein the method comprises the following steps: firstly, repairing and cleaning a pavement; then spreading an environment-friendly colored antiskid pavement adhesive, and spreading colored ceramic particles on the adhesive; after the adhesive is solidified, spraying an environment-friendly colored anti-skid pavement surface layer protective agent, and spreading potassium acetate particles within 3-5min after spraying. The environment-friendly color anti-skid pavement adhesive is toughened and modified by polyurethane, has better matching property of elongation at break and shearing strength, and remarkably improves the crack resistance and fatigue resistance of the paved color anti-skid pavement. The use of the surface layer protective agent effectively improves the anti-stripping capability of the ceramic particles of the color anti-skid pavement and further improves the water loss resistance of the environment-friendly color anti-skid pavement. The potassium acetate particles can well sink into the transparent surface layer protective agent or partially inlay on the surface of the surface layer protective agent, and can play a role in melting ice and snow in ice and snow weather.
Description
Technical Field
The invention belongs to the technical field of pavement maintenance, and particularly relates to an environment-friendly colored anti-skid pavement capable of melting ice and a preparation method thereof.
Background
The Chinese highways are distributed in the south and north of the great river, and the different road conditions, the use environments and the requirements are different. In winter in northern China, the influence of ice and snow weather is often encountered, so that a plurality of traffics are in a paralyzed or semi-paralyzed state, the life of residents is severely restricted and influenced, and a plurality of driving safety hidden hazards are also caused.
The colored anti-slip pavement can solve the wet slippery problem of pavement caused by rainy and snowy weather to a certain extent, but when the snowy amount is large, snow is deposited in the gaps of the colored anti-slip pavement, and after the constructional depth of ceramic particles is filled, the colored anti-slip pavement also loses the functions of anti-slip and safety performance improvement. In order to solve the problems, the prior color pavement needs to be technically upgraded and modified, so that the color pavement has the functions of pavement skid resistance, function indication and environment beautifying, and has a certain capacity of melting snow and ice, so that the capacity of melting snow and ice can be achieved when the snow brightness is large, and the service performance of the color skid-proof pavement in ice and snow weather is improved. Therefore, research on the environment-friendly color anti-skid pavement which is energy-saving, environment-friendly, good in wear resistance and has the effects of melting snow and ice has important significance.
Disclosure of Invention
In order to effectively solve the problems of cracking of the color anti-skid pavement caused by the large shrinkage rate and insufficient elongation at break of the existing water-based epoxy resin and insufficient abrasion performance of the color anti-skid pavement caused by serious early particle drop, the snow melting and deicing functions of the snow melting agent are integrated, and the service capacity of the color pavement in ice and snow weather is further improved. The invention develops an environment-friendly colored anti-skid pavement capable of melting ice and a preparation method thereof.
The preparation method of the ice-melting environment-friendly colored anti-skid pavement comprises the following steps of:
1) Cleaning and purging the constructed pavement, wherein the constructed pavement is required to be cleaned, has no oil pollution, no pulverization, no clear water and no floating ash; repairing the damaged part of the basal plane by using epoxy mortar, and cleaning, drying and solidifying the surface of the concrete;
2) Mixing 100 parts by mass of an environment-friendly color anti-slip pavement adhesive A component, 150 parts by mass of an environment-friendly color anti-slip pavement adhesive B component, 100 parts by mass of tap water and 10 parts by mass of pigment, stirring for 3-5min at a rotating speed of 1000-1500rpm, pouring the mixture on a construction pavement, spreading the mixture, and spreading color ceramic particles with the particle size of 1-3mm until the color ceramic particles completely cover the environment-friendly color anti-slip pavement adhesive; curing for more than 24 hours, cleaning the colored ceramic particles with incompletely bonded surfaces by using a broom, and blowing by using a pavement blowing tool;
3) Uniformly mixing the component A of the environment-friendly color anti-skid pavement surface layer protective agent and the component B of the environment-friendly color anti-skid pavement surface layer protective agent according to the mass ratio of 1.2-1.5:2, and spraying the mixture on the surface of a pavement; uniformly spraying potassium acetate solid particles with the particle diameter of 0.5mm within 3-5min after spraying by manual spreading or a distribution sieve, wherein the spreading amount is 0.3-0.5kg/m 2 And after the road surface is dried, the environment-friendly color anti-skid road surface capable of melting ice is obtained.
The preparation method of the component A of the environment-friendly color anti-skid pavement adhesive comprises the following steps:
1) Drying oleum Ricini, polyethylene glycol 2000, dimethyl carbonate, and 4,4' -dicyclohexylmethane diisocyanate at 40deg.C in a vacuum drying oven to remove water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) A mixture of 10 parts by mole of castor oil and 10 parts by mole of polyethylene glycol 2000 was dissolved in 30 parts by mole of dimethyl carbonate, stirred uniformly at 45℃until completely dissolved, and then stirred at N 2 Under the protection, the temperature is raised to 70 ℃, and the reaction is carried out for 3h under 3000rpm mechanical stirring, N 2 The outlet is provided with a condensation recovery device at 5 ℃ for collecting the evaporated dimethyl carbonate;
3) Slowly dripping 20 parts of 4,4' -dicyclohexylmethane diisocyanate in molar weight into the reaction mixture in the step 2), keeping the reaction condition unchanged after the dripping is finished, and continuing the reaction for 3 hours to obtain a reaction product (1);
4) Weighing hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester with the molar weight of 15 parts, placing the hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester into a reactor, adding boron trifluoride diethyl ether with the addition of 0.5 weight percent of the hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester under the conditions of nitrogen protection, the reaction temperature of 70 ℃ and the stirring speed of 1500rpm, and slowly dropwise adding the reaction product (1) after uniformly stirring for 3 hours, and continuously stirring for 2 hours after dropwise adding to obtain the reaction product (2);
5) The reaction product (2) was heated to 80℃and N-flow was stopped 2 At N 2 The condensing recovery device at 5 ℃ of the outlet is connected with a vacuum pump, and the vacuum pumping treatment is carried out at a constant temperature and a constant speed under a stirring speed of 3000rpm until no bubbles are generated, and a yellowish transparent mucus substance is obtained as a reaction product (3);
6) Adding bisphenol A epoxy resin E51 with the molar quantity of 85 parts into the reaction product (3), adjusting the reaction temperature to 60 ℃, adjusting the stirring speed to 3000rpm, dismantling a vacuumizing device to ensure that the whole reaction equipment is communicated with the atmosphere, slowly dropwise adding deionized water for 30min-2h, and keeping the temperature and the stirring speed for continuous reaction for 30min after the dropwise adding is finished to obtain modified epoxy resin emulsion with the solid content of 50 wt%;
7) And (3) adding 0.5% of stabilizer and leveling agent into the modified epoxy resin emulsion obtained in the step (6), and continuously stirring for 15min to form a homogeneous milky emulsion, thus obtaining the component A of the environment-friendly color anti-skid pavement adhesive.
The preparation steps of the component B of the environment-friendly color anti-skid pavement adhesive comprise:
1) Weighing 70 parts by mole of methylcyclopentadiene diamine and 10 parts by mole of polyether amine in a reactor, heating to 60 ℃, stirring and mixing uniformly, and introducing nitrogen for protection;
2) Slowly dripping 80 parts of tetrahydrodiglycidyl phthalate into the reactor in the step 1), and continuously stirring at 60 ℃ for 12 hours until the tetrahydrodiglycidyl phthalate turns into brown yellow viscous liquid at a stirring speed of 1500rpm;
3) Slowly dripping 20 parts of hexanediol diglycidyl ether into the product in the step 2), and continuously stirring at 60 ℃ for 8 hours after the dripping is finished, wherein the stirring speed is 1500rpm;
4) Slowly dripping deionized water into the product of the step 3) while keeping the temperature and the rotating speed unchanged to prepare a brown yellow homogeneous liquid with the solid content of 50wt%, and continuously stirring until no foaming and no wiredrawing phenomenon are caused after the dripping is finished, so as to obtain the environment-friendly color anti-skid pavement adhesive B component.
The preparation steps of the component A of the environment-friendly colored anti-skid pavement surface layer protective agent comprise:
1) Drying oleum Ricini, trimethylolpropane, dimethyl carbonate, HMDI, hydroxyethyl methacrylate, and bis-hydroxymethyl butyric acid at 40deg.C in vacuum drying oven to remove water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) Placing 60 parts of HMDI in a reactor, adjusting the reaction temperature to 70-75 ℃, stirring at 1500rpm, and introducing N 2 Protection, N 2 A condensing recovery device at the temperature of 5 ℃ is arranged at the outlet, then a dimethyl carbonate solution with 3 parts of trimethylolpropane and 7 parts of castor oil in molar quantity is slowly dripped, and the reaction is continued for 1h after the dripping is completed;
3) Adjusting the reaction temperature to 60 ℃, dropwise adding 18 parts of hydroxyethyl methacrylate in molar quantity into the reactor in the step 2) for 1h, and stirring at a speed of 3000rpm;
4) Further reducing the reaction temperature to 40 ℃, then keeping the stirring speed unchanged, adding potassium persulfate into the product of the step 3), slowly dropwise adding 54 parts of MMA monomer in molar quantity for 1h, and rapidly adding phenol after the completion of dropwise adding, wherein the adding quantity of the phenol is 0.5% of the mass of MMA;
5) The stirring speed is adjusted to 3000rpm, the reaction temperature is adjusted to 60 ℃, 8 parts of dihydroxymethyl butyric acid with molar weight is dripped into the product of the step 4), the reaction is continued for 1h after the dripping is finished, then triethylamine with 8 parts of molar weight is added at one time, the mixture is stirred for 30min, and the excessive dimethyl carbonate solvent in the reactant is removed by a vacuumizing heating mode until no bubbles are generated in the viscous liquid;
6) And adding deionized water to adjust the solid content to be 50wt%, adding a defoaming agent, and uniformly stirring to obtain the component A of the environment-friendly color pavement surface layer protective agent.
The preparation steps of the component B of the environment-friendly color pavement surface layer protective agent comprise:
1) Placing 40 parts by mole of diglycidyl hexahydrophthalate in a reactor, adjusting the reaction temperature to 60 ℃, stirring at 1500rpm, introducing nitrogen for protection, and dropwise adding 15 parts by mole of polyetheramine D400 to prepare an epoxy resin prepolymer;
2) Weighing 50 parts of castor oil in molar weight, adding boron trifluoride diethyl etherate, wherein the mass of the boron trifluoride diethyl etherate is 0.5% of that of the castor oil, uniformly stirring, adjusting the reaction temperature to 60 ℃, introducing nitrogen for protection, and adjusting the stirring speed to 1500rpm;
3) Slowly dripping the epoxy resin prepolymer prepared in the step 1) into the mixture in the step 2) for 2h, keeping stirring at 60 ℃ for reaction for 6h, wherein the stirring speed is 1500rpm, and dripping DMC to adjust the viscosity of the product;
4) Dropwise adding 20 parts of HMDI grafted and modified by DMPA into the product of the step 3) in molar quantity, keeping the reaction temperature and stirring speed unchanged, and continuing to react for 1h after the dropwise adding is finished;
5) Keeping the temperature and the rotating speed unchanged, adding triethanolamine with the molar quantity of 20 parts at one time to neutralize the product of the step 4), vacuumizing to remove redundant DMC until no bubbles are generated in reactant liquid, slowly dripping deionized water to prepare a dispersion liquid with the solid content of 50wt%, and continuously stirring after dripping until no foaming and no wire drawing phenomenon occur, thus obtaining the component B of the environment-friendly color pavement surface layer protective agent.
In the synthesis of the environment-friendly color anti-skid pavement adhesive:
the feeding speed and the reaction temperature need to be strictly controlled, and particularly in the process of polyurethane prepolymerization and polyurethane modified epoxy resin, the feeding speed and the reaction temperature are key to influence the success of experiments, and gel or explosion polymerization can be initiated due to unsuitable temperature and stirring speed.
After the polyurethane modified epoxy resin is finished, the organic solvent dimethyl carbonate needs to be vacuumized and recovered, and if the recovery is not clean, the problems of layering, incomplete emulsification, overlarge emulsion viscosity and the like in the subsequent emulsification process can be caused. In the preparation process of the environment-friendly color anti-skid pavement adhesive B component, the compatibility of the B component and E51 in the A component can be improved by adopting the tetrahydrophthalic acid diglycidyl ester, the faster reaction of the two components in the adhesive curing process is facilitated, the tetrahydrophthalic acid diglycidyl ester has better space rotation capability compared with the E51, and the water loss resistance of the whole system is better than that of the linear glycidyl ester after the adhesive curing reaction is finished due to the existence of unsaturated bonds.
In the synthesis process of the environment-friendly colored anti-skid pavement surface layer protective agent, the following steps are:
the reaction temperature and the reaction speed need to be controlled, a polyurethane catalyst cannot be added in the polymerization process of polyurethane, and the problems that the storage stability of a product is insufficient due to catalyst residues, and the construction of a spraying coater is difficult due to the increase of the viscosity of a sample in the later period are solved. In the experimental process, the HMDI type isocyanate can not only prevent yellowing and chalking caused by ultraviolet aging of isocyanate with a benzene ring structure, but also has longer operation time compared with the isocyanate with a benzene ring structure, but also has higher reactivity compared with HDI, thereby avoiding the problem of overlong real drying time.
When the MMA grafting modified polyurethane prepolymer is used, the reaction temperature and the stirring speed are required to be controlled, so that the heat released by MMA free radical polymerization is timely emitted, meanwhile, the adding speed of MMA is controlled, the prepolymer is prevented from being gelled due to bursting, and a small amount of phenol is added after the reaction is finished, so that the unstable system caused by further self-polymerization of acrylic acid radical which is not completely reflected in the heavy end chain of the polyurethane prepolymer can be effectively prevented.
The prepolymerization process of the components A and B of the surface layer protective agent is mainly characterized in that the reactivity of isocyanate and castor oil is low, the molecular weight is small, the film formation is difficult to form after construction because of no prepolymerization, and the surface layer protective agent has incomplete reaction because of low polymerization degree.
Both TMP and castor oil have the effect of grafting modification, but the castor oil is mainly introduced to raise the molecular weight of the prepolymer, the too low TMP content is easy to cause the reduction of the node density of the crosslinking reaction, so that the strength is poor, the too high TMP content is easy to cause the too short molecular weight of the soft end of the prepolymer, and the toughness and the ductility of the polymer are poor, so that the molar ratio of the TMP to the castor oil is 3:7 according to the comprehensive use requirement.
The invention has the advantages that:
1. the environment-friendly color anti-skid pavement adhesive prepared by the invention is toughened and modified by polyurethane, and the waterborne epoxy resin toughened and modified by polyurethane has good toughening effect, and the elongation at break and the shearing strength are obviously improved compared with those of the waterborne epoxy resin sold in the market; the tensile strength, the elongation at break and the shearing strength are better matched, so that the anti-cracking performance and the fatigue resistance of the prepared color anti-skid pavement are obviously improved;
2. the PEG structure with large molecular weight is introduced in the process of the prepared polyurethane grafted modified epoxy resin, so that the polyurethane grafted modified epoxy resin has certain emulsifying capacity, E51 can be emulsified into stable emulsion, but compared with the existing water-based epoxy resin, the emulsifying capacity of the emulsifier is poorer, mainly because the hydrophilic groups in the polyurethane modified epoxy resin occupy relatively lower molecular weight, and the water loss resistance of the final product is obviously attenuated because more hydrophilic groups are introduced, so that hydrophilic molecular links are introduced as little as possible when the emulsifying capacity is met;
3. HMDI and refined castor oil are introduced into the polyurethane modified epoxy resin, and hydrogenated bisphenol A epoxy resin adopted by the epoxy resin has better space movement capability and rotation capability, so that the environment-friendly color pavement adhesive has better elongation at break and shear strength performance;
4. the use of the surface layer protective agent effectively improves the anti-stripping capability of the ceramic particles of the color anti-skid pavement and further improves the water loss resistance of the environment-friendly color anti-skid pavement;
5. the potassium acetate particles can well sink into the transparent surface layer protective agent or partially inlay on the surface of the surface layer protective agent, the sprinkling amount is controlled according to the construction depth of the color anti-skid pavement, most of the potassium acetate particles are ensured to be inlaid between ceramic particles and not higher than the ceramic particles, the effect of melting ice and snow can be achieved in ice and snow weather, and the potassium acetate can be synchronously scattered when the surface layer protective agent maintenance is carried out on the environment-friendly color anti-skid pavement every year, so that the problem that the ice melting capability is gradually weakened along with the lapse of the using time is avoided.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate, but are not to be construed as limiting the invention.
Example 1:
1. the preparation of the component A of the environment-friendly color anti-skid pavement adhesive comprises the following steps:
1) Drying oleum Ricini (purity 99.5%), polyethylene glycol 2000, dimethyl carbonate, and 4,4' -dicyclohexylmethane diisocyanate (HMDI) at 40deg.C in vacuum drying oven to remove water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) Dissolving a mixture of 10 parts by mole of castor oil and 10 parts by mole of polyethylene glycol (molecular weight 2000) into 30 parts by mole of dimethyl carbonate, placing the mixture in a reactor at a temperature of 45 ℃, uniformly stirring until the mixture is completely dissolved, and then providing 99.99% of N to the reactor 2 Protecting, heating the reactor by oil bath, adjusting the reaction temperature to 70 ℃, mechanically stirring at 3000rpm, and N 2 The outlet is provided with a condensation recovery device at 5 ℃ for collecting evaporated dimethyl carbonate, the reaction temperature needs to be controlled in the reaction process, the stirring speed is increased, and the phenomena of gel agglomeration caused by the fact that the exothermic heat in the reaction process cannot be timely emitted and the explosion reaction is caused are prevented;
3) Weighing 20 parts of 4,4' -dicyclohexylmethane diisocyanate (HMDI) in molar quantity, slowly dropwise adding the mixture into a reactor of the reactor 2), keeping the reaction condition unchanged after the dropwise adding is finished, and continuously reacting for 3 hours to obtain a reaction product (1);
4) Weighing 15 parts of diglycidyl hexahydrophthalate in molar quantity, placing the diglycidyl ester in a reactor, providing nitrogen protection, adjusting the reaction temperature to 70 ℃, stirring at 1500rpm, adding boron trifluoride diethyl etherate with the mass fraction of 0.5% of the diglycidyl ester of the hexahydrophthalate, uniformly stirring, slowly dropwise adding the reaction product (1) for 3 hours, and continuing stirring for 2 hours after dropwise adding to obtain the reaction product (2); in the reaction process, the stirring speed needs to be controlled to enable the reaction to be more sufficient, the reaction temperature is reduced, and the reaction degree of NH-and epoxy groups in polyurethane is prevented from being deepened due to the overhigh temperature, so that the gel of the polyurethane modified epoxy resin is prevented from being solidified;
5) The reaction product (2) was heated to 80℃and N-flow was stopped 2 At N 2 The condensation recovery device at 5 ℃ of the outlet is connected with a vacuumizing pump for vacuumizing operation, the stirring speed of the reactor is regulated to 3000rpm, the constant temperature and constant speed vacuumizing treatment is carried out for 1 hour, and a large amount of bubbles are generated in the reaction product (2) just before the reaction product (3) is obtained until no bubbles are generated, so that a yellowish transparent mucus substance is the reaction product (3);
6) Adding 85 parts of bisphenol A epoxy resin E51 into the reaction product (3), adjusting the reaction temperature to 60 ℃, adjusting the stirring speed to 3000rpm, dismantling a vacuumizing device to enable the whole reaction equipment to be communicated with the atmosphere, slowly obtaining dropwise adding deionized water, keeping the temperature and the stirring speed unchanged after the dropwise adding is completed for 30min, and continuously stirring for 30min to prepare a modified epoxy resin emulsion (4) with 50% of solid content;
7) Adding the stabilizer PVA with the mass of 0.5 percent of the total mass of (4) and the flatting agent alkyl modified organosiloxane with the mass of 0.5 percent into the (6), and continuing stirring for 15 minutes until the mixture shows a homogeneous milky emulsion, thus obtaining the component A of the environment-friendly color anti-skid pavement adhesive.
2. The preparation of the environment-friendly color anti-skid pavement adhesive B component comprises the following steps:
1) Weighing 70 parts by mole of methylcyclopentadiene diamine (TAC-900) and 10 parts by mole of polyetheramine D400, heating to 60 ℃ in a reactor, stirring and mixing uniformly, and introducing nitrogen for protection;
2) Slowly dropwise adding 80 parts of tetrahydrophthalic acid diglycidyl ester into the solution 1), keeping stirring at 60 ℃ for 12 hours at a stirring speed of 1500rpm until the solution turns into a brown yellow viscous solution, wherein the molar amount of the tetrahydrophthalic acid diglycidyl ester is 0.5 part/min;
3) Slowly dripping 20 parts of hexanediol diglycidyl ether into 2), keeping the dripping speed at 0.5 part/min, stirring at 60 ℃ for 8 hours, wherein the stirring speed is 1500rpm, the viscosity of the liquid is gradually increased, the liquid is still a brown yellow viscous liquid, and the dripping speed and the reaction temperature cannot be too fast, so that the gel phenomenon can be caused;
4) Keeping the temperature and the rotating speed unchanged, slowly dripping deionized water into the mixture 3) to prepare brown yellow homogeneous liquid with the solid content of 50%, and continuously stirring until no foaming and no wiredrawing phenomenon are caused after the dripping is finished, so that the environment-friendly color anti-skid pavement adhesive B component can be obtained.
3. The preparation of the environment-friendly colored anti-skid pavement surface layer protective agent A component:
1) Drying oleum Ricini (purity 99.5%), trimethylolpropane (TMP), dimethyl carbonate (DMC), HMDI, hydroxyethyl methacrylate and bis-hydroxymethyl butyric acid (DMBA) at 40deg.C in a vacuum oven, removing water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) Placing 60 parts of HMDI in a reactor, adjusting the reaction temperature to 70-75 ℃, stirring at 1500rpm, and introducing N 2 Protection, N 2 A condensing recovery device at the temperature of 5 ℃ is arranged at the outlet and is used for collecting evaporated dimethyl carbonate (the molecular weight of prepolymer is increased too fast due to the too high reaction temperature, the subsequent grafting modification is difficult, a catalyst is not added for controlling the reaction speed), then DMC solution dissolved with TMP and castor oil (the molar quantity of TMP is 3 parts and the molar quantity of castor oil is 7 parts) is slowly added dropwise, the dropping speed is 5 parts by mol/h, and the reaction is continued for 1h after the completion of the dropwise addition;
3) Adjusting the reaction temperature to 60 ℃, dropwise adding 18 parts of hydroxyethyl methacrylate (HEMA) into the mixture 2) for 1h, wherein the stirring speed is 3000rpm (reducing the reaction speed, improving the heat release and preventing HEMA from self-polymerization);
4) Further reducing the reaction temperature to 40 ℃, then keeping the stirring speed unchanged, adding potassium persulfate into the 3), wherein the mass of the potassium persulfate is 0.5% of that of HEMA, slowly dripping MMA monomer with the molar quantity of 54 parts for 1h, and rapidly adding phenol after dripping, wherein the adding quantity of the phenol is 0.5% of that of MMA (preventing the polyurethane prepolymer modified by MMA grafting from undergoing free radical polymerization to cause gel aggregation);
5) The stirring speed is adjusted to 3000rpm, the reaction temperature is adjusted to 60 ℃, 8 parts of DMBA with molar weight is dripped into 4), the dripping speed is 2 parts/h, the reaction is continued for 1h after the dripping is finished, then triethylamine with 8 parts of molar weight is added at one time and stirred for 30min, and then the redundant DMC solvent in the reactant is removed by a vacuumizing and heating mode until no bubbles are generated in the viscous liquid;
6) And then deionized water is added to adjust the solid content to be 50%, and a polyether modified organic silicon type defoamer accounting for 0.5wt% of the total solid content is added to be uniformly stirred, so that the component A of the environment-friendly color anti-skid pavement surface layer protective agent is prepared.
4. The preparation of the B component of the environment-friendly color anti-skid pavement surface layer protective agent comprises the following steps:
1) Placing 40 parts by mole of diglycidyl hexahydrophthalate in a reactor, adjusting the reaction temperature to 60 ℃, stirring at 1500rpm, introducing nitrogen for protection, dropwise adding 15 parts by mole of polyetheramine D400, and preparing an epoxy resin prepolymer at a dropwise adding speed of 5 parts/h;
2) Weighing 50 parts of castor oil in molar weight, adding boron trifluoride diethyl etherate accounting for 0.5% of the castor oil in mass, uniformly stirring, adjusting the reaction temperature to 60 ℃, introducing nitrogen for protection, and adjusting the stirring speed to 1500rpm;
3) Slowly dripping the epoxy resin prepolymer prepared in the step 1) into the step 2) for 2 hours, keeping the temperature of 60 ℃ and stirring for reaction for 6 hours, wherein the stirring speed is 1500rpm, and adding DMC into the mixture after the reaction is completed to adjust the viscosity of the product;
4) Dropwise adding 20 parts of HMDI grafted and modified by DMPA into the 3) at a molar amount of 5 parts per hour at a constant reaction temperature and stirring speed, and continuing to react for 1 hour after the dropwise adding is finished;
5) Keeping the temperature and the rotating speed unchanged, adding triethanolamine with the molar quantity of 20 parts at one time to neutralize the product of 4), vacuumizing to remove redundant DMC until no bubbles are generated in reactant liquid, slowly dripping deionized water to prepare a dispersion liquid with the solid content of 50%, and continuously stirring until no foaming and no wiredrawing phenomenon occur after dripping, thus obtaining the component B of the environment-friendly color anti-skid pavement surface layer protective agent.
5. Preparation of ice-melting environment-friendly colored anti-skid pavement:
1) Cleaning and purging the constructed pavement, wherein the constructed pavement is required to be cleaned, has no oil pollution, no pulverization, no clear water and no floating ash;
2) Repairing the damaged part of the basal plane by using epoxy mortar, and cleaning, drying and solidifying the surface of the concrete;
3) Mixing 100 parts by mass of an environment-friendly color anti-skid pavement adhesive A component, 150 parts by mass of an environment-friendly color anti-skid pavement adhesive B component, 100 parts by mass of tap water and 10 parts by mass of pigment; stirring uniformly by using a stirrer at a stirring speed of 1500rpm for 5min until the emulsion shows uniform pigment color;
4) Pouring the prepared environment-friendly color anti-skid pavement adhesive on a construction pavement, spreading the pavement adhesive by using a serrated rubber scraper (the width of the saw teeth is 2mm and the depth is 3 mm), and waiting for the environment-friendly color anti-skid pavement adhesive to automatically flow to be completely smooth;
5) Spreading color ceramic particles with the particle size of 1-3mm in a top-down mode until the color ceramic particles completely cover the environment-friendly color anti-skid pavement adhesive;
6) After the environment-friendly colored antiskid pavement adhesive is completely solidified (more than or equal to 24 hours), cleaning colored ceramic particles with incompletely adhered surfaces by using a broom, and uniformly blowing by using a pavement blowing tool;
7) After collecting excessive aggregate, mixing the components A and B of the environment-friendly color anti-skid pavement surface layer protective agent according to the mass ratio of 1.5:2, adding water to adjust the viscosity of the whole surface layer protective agent, and spraying the surface layer protective agent on the surface of a pavement by a spraying machine;
8) Within 5min after the finish layer protective agent is sprayed, potassium acetate solid particles with the particle size of 0.5mm are manually sprayed, and the spraying amount is 0.5kg/m 2 The size of the sprinkling amount is related to the construction depth of the color anti-skid pavement, so that all potassium acetate particles are inlaid among ceramic particles, and the environment-friendly color anti-skid pavement capable of melting ice can be prepared after the ceramic particles are dried.
The performance of the prepared environment-friendly color anti-skid pavement adhesive is evaluated:
1) And (3) preparing the prepared environment-friendly color anti-skid pavement adhesive, leaving a part of the adhesive for mechanical property test, and preparing the rest part of the adhesive into a wet wheel abrasion test piece.
2) In order to better test the service life of the color anti-skid pavement prepared from different materials, the invention adopts an accelerated loading fatigue testing machine to test, a prototype AC-13 asphalt mixture test piece is manufactured, the thickness is 5cm, then the color anti-skid pavement is paved on the surface layer of the test piece according to the construction method of the color anti-skid pavement, and redundant ceramic particles on the surface are cleaned after maintenance at room temperature. Weigh mass m of test block of non-paved color antiskid pavement 0 Paving a color anti-skid pavement and collecting excessive aggregate to obtain the mass m of the test block 1 After the surface suspended redundant ceramic particles and waste materials are cleaned after the accelerated loading fatigue test is finished, weighing the mass m of the test piece again 2 The fatigue resistance of the color anti-skid pavement is measured by the mass loss proportion.
Fatigue resistance p= (m) 1 -m 2 )/(m 1 -m 0 )*100％
3) And (3) testing environmental protection performance: evaluating the environmental protection performance of the material by testing the content of VOCs in the adhesive;
4) Emulsion storage stability test: observing the delamination condition of the test after centrifugation at 3000rpm for 30 min;
5) Viscosity test: the flowability of the adhesive after mixing is inspected and used for inspecting the actual construction performance;
6) Curing time: the method is used for examining the construction closing time and measuring the open traffic time in the actual construction process;
7) Mechanical property test: the method is used for evaluating the mechanical properties of the materials and the shrinkage rate of the materials.
Comparative example 1:
conventional waterborne epoxy adhesives: the wet wheel abrasion test piece is prepared from aqueous epoxy resin emulsion (Wuhanshi Quanxing new material science and technology Co., ltd.) and aqueous epoxy resin curing agent (Shandong Haohao new material Co., ltd.) in a mass ratio of 1:1, 5wt% of pigment is added, a part of pigment is left for mechanical property test after uniform stirring, and the rest part of pigment is prepared into a wet wheel abrasion test piece. The potassium acetate particles are not scattered. The performance test method was the same as in example 1.
Comparative example 2:
polyurethane adhesive: is prepared from 3070 resin (Henan De chemical engineering Co., ltd.) and MDI-50 curing agent (Wanhua chemical group Co., ltd.) in a ratio of 4:1, 5wt% of pigment is added, and after uniform stirring, a part of the pigment is left for mechanical property test, and the rest part of the pigment is prepared into a wet wheel abrasion test piece. The potassium acetate particles are not scattered. The performance test method was the same as in example 1.
Comparative example 3:
MMA adhesive: is prepared from MMA resin (Taiyuan Chengcheng technology Co., ltd.) and dibenzoyl peroxide initiator in a mass ratio of 100:2, 5wt% of pigment is added, a part of pigment is left for mechanical property test after uniform stirring, and the rest part of pigment is prepared into a wet wheel abrasion test piece. The potassium acetate particles are not scattered. The performance test method was the same as in example 1.
The results of the above performance tests are shown in the following table, and the test methods refer to the relevant standards.
The experiment results show that the performance of the environment-friendly color anti-skid pavement material prepared by the invention is overall superior to that of conventional waterborne epoxy resin and polyurethane, the fatigue resistance is inferior to that of MMA, but the environment-friendly performance is superior to that of MMA.
The environment-friendly color anti-skid pavement with the surface layer protective agent is remarkably improved in water loss resistance and fatigue test performance, and is mainly beneficial to forming a sandwich structure by the environment-friendly color adhesive, the ceramic particles and the surface layer protective agent, so that the ceramic particles have better embeddability and better wear resistance. The spreading of the potassium acetate needs to be adjusted according to the constructional depth of the colorful anti-skid pavement, so that the potassium acetate particles are fully embedded among the ceramic particles and are not higher than the ceramic particles, thus reducing the loss in non-ice and snow weather, and dissolving the potassium acetate out to realize the function of melting ice when the weather is ice and snow. And the potassium acetate can be synchronously spread when the surface layer protective agent is maintained on the environment-friendly color anti-skid pavement every year, so that the problem that the ice melting capacity is gradually weakened along with the use time is avoided.
Claims (1)
1. The preparation method of the ice-melting environment-friendly colored anti-skid pavement is characterized by comprising the following specific steps of:
1) Cleaning and purging the constructed pavement, wherein the constructed pavement is required to be cleaned, has no oil pollution, no pulverization, no clear water and no floating ash; repairing the damaged part of the basal plane by using epoxy mortar, and cleaning, drying and solidifying the surface of the concrete;
2) Mixing 100 parts by mass of an environment-friendly color anti-slip pavement adhesive A component, 150 parts by mass of an environment-friendly color anti-slip pavement adhesive B component, 100 parts by mass of tap water and 10 parts by mass of pigment, stirring for 3-5min at a rotating speed of 1000-1500rpm, pouring the mixture on a construction pavement, spreading the mixture, and spreading color ceramic particles with the particle size of 1-3mm until the color ceramic particles completely cover the environment-friendly color anti-slip pavement adhesive; curing for more than 24 hours, cleaning the colored ceramic particles with incompletely bonded surfaces by using a broom, and blowing by using a pavement blowing tool;
3) Uniformly mixing the component A of the environment-friendly color anti-skid pavement surface layer protective agent and the component B of the environment-friendly color anti-skid pavement surface layer protective agent according to the mass ratio of 1.2-1.5:2, and spraying the mixture on the surface of a pavement; the spraying is carried out within 3-5min, and the powder is manually scattered or distributed by a sieveUniformly throwing potassium acetate solid particles with the particle diameter of 0.5mm, wherein the distribution amount is 0.3-0.5kg/m 2 After the ice is dried, the environment-friendly colored anti-skid pavement capable of melting ice is obtained;
the preparation method of the component A of the environment-friendly color anti-skid pavement adhesive comprises the following steps:
1) Drying oleum Ricini, polyethylene glycol 2000, dimethyl carbonate, and 4,4' -dicyclohexylmethane diisocyanate at 40deg.C in a vacuum drying oven to remove water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) A mixture of 10 parts by mole of castor oil and 10 parts by mole of polyethylene glycol 2000 was dissolved in 30 parts by mole of dimethyl carbonate, stirred uniformly at 45℃until completely dissolved, and then stirred at N 2 Under the protection, the temperature is raised to 70 ℃, and the reaction is carried out for 3h under 3000rpm mechanical stirring, N 2 The outlet is provided with a condensation recovery device at 5 ℃ for collecting the evaporated dimethyl carbonate;
3) Slowly dripping 20 parts of 4,4' -dicyclohexylmethane diisocyanate in molar weight into the reaction mixture in the step 2), keeping the reaction condition unchanged after the dripping is finished, and continuing the reaction for 3 hours to obtain a reaction product (1);
4) Weighing hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester with the molar weight of 15 parts, placing the hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester into a reactor, adding boron trifluoride diethyl ether with the addition of 0.5 weight percent of the hydrogenated bisphenol A epoxy resin or hexahydrophthalic acid diglycidyl ester under the conditions of nitrogen protection, the reaction temperature of 70 ℃ and the stirring speed of 1500rpm, and slowly dropwise adding the reaction product (1) after uniformly stirring for 3 hours, and continuously stirring for 2 hours after dropwise adding to obtain the reaction product (2);
5) The reaction product (2) was heated to 80℃and N-flow was stopped 2 At N 2 The condensing recovery device at 5 ℃ of the outlet is connected with a vacuum pump, and the vacuum pumping treatment is carried out at a constant temperature and a constant speed under a stirring speed of 3000rpm until no bubbles are generated, and a yellowish transparent mucus substance is obtained as a reaction product (3);
6) Adding bisphenol A epoxy resin E51 with the molar quantity of 85 parts into the reaction product (3), adjusting the reaction temperature to 60 ℃, adjusting the stirring speed to 3000rpm, dismantling a vacuumizing device to ensure that the whole reaction equipment is communicated with the atmosphere, slowly dropwise adding deionized water for 30min-2h, and keeping the temperature and the stirring speed for continuous reaction for 30min after the dropwise adding is finished to obtain modified epoxy resin emulsion with the solid content of 50 wt%;
7) Adding 0.5% of stabilizer and leveling agent into the modified epoxy resin emulsion obtained in the step 6), and continuously stirring for 15min to form a homogeneous milky emulsion, namely the environment-friendly color anti-skid pavement adhesive A component;
the preparation steps of the component B of the environment-friendly color anti-skid pavement adhesive comprise:
1) Weighing 70 parts by mole of methylcyclopentadiene diamine and 10 parts by mole of polyether amine in a reactor, heating to 60 ℃, stirring and mixing uniformly, and introducing nitrogen for protection;
2) Slowly dripping 80 parts of tetrahydrodiglycidyl phthalate into the reactor in the step 1), and continuously stirring at 60 ℃ for 12h until the tetrahydrodiglycidyl phthalate turns into brown yellow viscous liquid at a stirring speed of 1500rpm;
3) Slowly dripping 20 parts of hexanediol diglycidyl ether into the product in the step 2), and continuously stirring at 60 ℃ for 8 hours after the dripping is finished, wherein the stirring speed is 1500rpm;
4) Slowly dripping deionized water into the product of the step 3) while keeping the temperature and the rotating speed unchanged to prepare a brown yellow homogeneous liquid with the solid content of 50wt%, and continuously stirring until no foaming and no wiredrawing phenomenon are caused after the dripping is finished, so as to obtain an environment-friendly color anti-skid pavement adhesive B component;
the preparation steps of the component A of the environment-friendly colored anti-skid pavement surface layer protective agent comprise:
1) Drying oleum Ricini, trimethylolpropane, dimethyl carbonate, HMDI, hydroxyethyl methacrylate, and bis-hydroxymethyl butyric acid at 40deg.C in vacuum drying oven to remove water, and placing in CaCl 2 In the dryer of (2) at 25 ℃ for 72 hours;
2) HMDI in 60 parts by mole was placed in a reactor and adjustedThe whole reaction temperature is 70-75 ℃, the stirring speed is 1500rpm, and N is introduced 2 Protection, N 2 A condensing recovery device at the temperature of 5 ℃ is arranged at the outlet, then a dimethyl carbonate solution with 3 parts of trimethylolpropane and 7 parts of castor oil in molar quantity is slowly dripped, and the reaction is continued for 1h after the dripping is completed;
3) Adjusting the reaction temperature to 60 ℃, dropwise adding 18 parts of hydroxyethyl methacrylate in molar quantity into the reactor in the step 2) for 1h, and stirring at a speed of 3000rpm;
4) Further reducing the reaction temperature to 40 ℃, then keeping the stirring speed unchanged, adding potassium persulfate into the product of the step 3), slowly dropwise adding 54 parts of MMA monomer in molar quantity for 1h, and rapidly adding phenol after the completion of dropwise adding, wherein the adding quantity of the phenol is 0.5% of the mass of MMA;
5) The stirring speed is adjusted to 3000rpm, the reaction temperature is adjusted to 60 ℃, 8 parts of dihydroxymethyl butyric acid with molar weight is dripped into the product of the step 4), the reaction is continued for 1h after the dripping is finished, then triethylamine with 8 parts of molar weight is added at one time, the mixture is stirred for 30min, and the excessive dimethyl carbonate solvent in the reactant is removed by a vacuumizing heating mode until no bubbles are generated in the viscous liquid;
6) Adding deionized water to adjust the solid content to 50wt%, adding a defoaming agent, and uniformly stirring to obtain an environment-friendly color anti-skid pavement surface layer protective agent A component;
the preparation steps of the component B of the environment-friendly color anti-skid pavement surface layer protective agent comprise:
1) Placing 40 parts by mole of diglycidyl hexahydrophthalate in a reactor, adjusting the reaction temperature to 60 ℃, stirring at 1500rpm, introducing nitrogen for protection, and dropwise adding 15 parts by mole of polyetheramine D400 to prepare an epoxy resin prepolymer;
2) Weighing 50 parts of castor oil in molar weight, adding boron trifluoride diethyl etherate, wherein the mass of the boron trifluoride diethyl etherate is 0.5% of that of the castor oil, uniformly stirring, adjusting the reaction temperature to 60 ℃, introducing nitrogen for protection, and adjusting the stirring speed to 1500rpm;
3) Slowly dripping the epoxy resin prepolymer prepared in the step 1) into the mixture in the step 2) for 2h, keeping stirring at 60 ℃ for reaction for 6h, wherein the stirring speed is 1500rpm, and dripping DMC to adjust the viscosity of the product;
4) Dropwise adding 20 parts of HMDI grafted and modified by DMPA into the product of the step 3) in molar quantity, keeping the reaction temperature and stirring speed unchanged, and continuing to react for 1h after the dropwise adding is finished;
5) Keeping the temperature and the rotating speed unchanged, adding triethanolamine with the molar quantity of 20 parts at one time to neutralize the product of the step 4), vacuumizing to remove redundant DMC until no bubbles are generated in reactant liquid, slowly dripping deionized water to prepare a dispersion liquid with the solid content of 50wt%, and continuously stirring until no foaming and no wire drawing phenomenon occur after the dripping is finished, thus obtaining the component B of the environment-friendly color anti-skid pavement surface layer protective agent.
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| US6437059B1 (en) * | 1999-02-11 | 2002-08-20 | Reichhold, Inc. | Composition of epoxy, urethane polyacrylate and polyamine |
| WO2005070990A1 (en) * | 2004-01-12 | 2005-08-04 | Taizhou Repow Chemical And Material Institute Co., Ltd | An epoxy resin curing agent containing elemental phosphorus and the method for preparing the same |
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