CN115975468B - Durable hot-melt marking paint and preparation method thereof - Google Patents
Durable hot-melt marking paint and preparation method thereof Download PDFInfo
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- CN115975468B CN115975468B CN202211580267.3A CN202211580267A CN115975468B CN 115975468 B CN115975468 B CN 115975468B CN 202211580267 A CN202211580267 A CN 202211580267A CN 115975468 B CN115975468 B CN 115975468B
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- 239000003973 paint Substances 0.000 title claims abstract description 41
- 239000012943 hotmelt Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims description 13
- 239000011324 bead Substances 0.000 claims abstract description 97
- 239000011521 glass Substances 0.000 claims abstract description 97
- 239000011347 resin Substances 0.000 claims abstract description 45
- 229920005989 resin Polymers 0.000 claims abstract description 45
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000003208 petroleum Substances 0.000 claims abstract description 31
- 239000004611 light stabiliser Substances 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 24
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 14
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 14
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000006004 Quartz sand Substances 0.000 claims abstract description 12
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 12
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 12
- 239000007822 coupling agent Substances 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 64
- 238000005406 washing Methods 0.000 claims description 30
- 238000001035 drying Methods 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 16
- 239000011248 coating agent Substances 0.000 claims description 13
- 238000000576 coating method Methods 0.000 claims description 13
- 150000001875 compounds Chemical class 0.000 claims description 12
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 11
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 11
- KZMGYPLQYOPHEL-UHFFFAOYSA-N Boron trifluoride etherate Chemical group FB(F)F.CCOCC KZMGYPLQYOPHEL-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000010025 steaming Methods 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 4
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
- 238000005303 weighing Methods 0.000 description 7
- 238000010276 construction Methods 0.000 description 4
- 238000012669 compression test Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 229920005992 thermoplastic resin Polymers 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007757 hot melt coating Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011325 microbead Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000036316 preload Effects 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention discloses a durable hot-melt marking paint which comprises the following raw materials in parts by weight: 50-150 parts of C5 petroleum resin, 10-50 parts of heavy calcium carbonate, 50-80 parts of glass beads, 5-30 parts of EVA resin, 10-30 parts of quartz sand, 10-20 parts of talcum powder, 1-10 parts of titanium dioxide, 10-30 parts of nano silicon dioxide, 1-3 parts of dioctyl phthalate, 1-5 parts of KH550 coupling agent, 1-2 parts of sodium carbonate, 1-3 parts of PE wax, 0.1-1 part of catalyst, 1-2 parts of light stabilizer, 100-200 parts of sodium hydroxide solution, 50-100 parts of ethanol solution, 20-60 parts of dimethylbenzene and 5-15 parts of water. The invention can effectively improve the compressive strength of the glass beads in the marked lines, and can effectively prevent the glass beads from sinking in the marked lines after the marked lines are rolled by automobiles on roads at high frequency, thereby improving the continuous high-reverse reaction of the glass beads.
Description
Technical Field
The invention relates to the technical field of marking paint, in particular to durable hot-melt marking paint and a preparation method thereof.
Background
The road construction in China rapidly develops, the consumption of the coating for road marking construction is more than 20 ten thousand tons each year, the road marking coating already forms a very large industry, and the road marking coating gradually develops from low grade to high grade and from single function to multiple functions in order to meet the use requirements of different areas, different climates and different construction environments.
Road markings are classified according to the type of paint used: normal temperature solvent type marking, heating solvent type marking, hot melt type marking. The hot-melt road marking paint is developed successfully in Europe in the middle of the 50 th century, and is used after the 90 th century in China, and the largest characteristic of the hot-melt road marking paint is that the coating thickness is about 1.5-2.5mm and 10 times of that of a normal-temperature solvent marking, so that the hot-melt road marking paint is more suitable for urban arterial roads, high-grade highways and the like with large vehicle flow, and the construction of newly-built highway road markings in China basically adopts the hot-melt paint at present.
The hot melt coating generally consists of thermoplastic resin, pigment, filler, auxiliary agent and the like. The thermoplastic resin can be rosin resin, petroleum resin, polyamide resin, polyester resin and the like, and the existing road marking paint contains glass beads and is used for reflecting light rays emitted by the vehicle lamp back to eyes of a driver, so that the road marking is brighter and the driving is safer.
However, in actual use, along with the high-frequency application of pressure and friction force to the marking by the automobile, the curing mode of the hot-melt marking coating is physical drying and film forming, the resin in the coating is simply changed from a molten state to a solid state after cooling, the compatibility between the glass beads in the marking and the thermoplastic resin is poor, and after the rolling of the wheels, the glass beads sink and fall off, so that the service life of the glass beads is seriously influenced.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a durable hot-melt marking paint and a preparation method thereof.
A durable hot-melt marking paint comprises the following raw materials in parts by weight: 50-150 parts of C5 petroleum resin, 10-50 parts of heavy calcium carbonate, 50-80 parts of glass beads, 5-30 parts of EVA resin, 10-30 parts of quartz sand, 10-20 parts of talcum powder, 1-10 parts of titanium dioxide, 10-30 parts of nano silicon dioxide, 1-3 parts of dioctyl phthalate, 1-5 parts of KH550 coupling agent, 1-2 parts of sodium carbonate, 1-3 parts of PE wax, 0.1-1 part of catalyst, 1-2 parts of light stabilizer, 100-200 parts of sodium hydroxide solution, 50-100 parts of ethanol solution, 20-60 parts of dimethylbenzene and 5-15 parts of water.
Preferably, the glass beads comprise glass beads with the particle size of 0.1-0.4mm, glass beads with the particle size of 0.5-0.65mm and glass beads with the particle size of 1-1.2mm, and the weight ratio of the three is 10:1-5:1-5.
Preferably, the catalyst is boron trifluoride diethyl etherate.
Preferably, the sodium hydroxide solution has a concentration of 1-2mol/L.
Preferably, the ethanol solution has a concentration of 40-60wt%.
Preferably, the light stabilizer comprises at least one of light stabilizer UV-P, light stabilizer UV-326, light stabilizer UV-327, light stabilizer UV-5411, light stabilizer LS-744, light stabilizer LS-770, light stabilizer GW-540, light stabilizer PDS.
The preparation method of the durable hot-melt marking paint comprises the following steps:
s1, mixing heavy calcium carbonate, quartz sand, talcum powder and titanium dioxide according to a proportion, and stirring at a speed of 500-1500r/min for 1-2h to obtain a premix;
s2, adding the glass beads into a sodium hydroxide solution, stirring for 1-2h, filtering, washing, drying at 70-80 ℃, adding an ethanol solution and a KH550 coupling agent, stirring for 5-10h at 50-80 ℃, filtering, washing, and drying to obtain the amino glass beads;
s3, adding dimethylbenzene into the C5 petroleum resin, refluxing and stirring for 5-15min at the temperature of 100-150 ℃, cooling to 80-90 ℃, adding nano silicon dioxide, performing ultrasonic dispersion by adopting ultraviolet irradiation treatment, adding a catalyst, continuing ultrasonic treatment for 1-2h, adding sodium carbonate, stirring for 10-20min at the speed of 1000-3000r/min, adding the amino glass beads, stirring for 5-15min at the temperature of 100-120 ℃, sequentially performing alkaline washing and water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain the C5 petroleum resin compound glass beads;
s4, mixing the light stabilizer, EVA resin, dioctylphthalate, PE wax and C5 petroleum resin compounded glass beads, stirring at the speed of 1000-2000r/min for 10-30min, adding premix, and continuously stirring for 1-2h to obtain the durable hot melt marking paint.
Preferably, in S3, the ultraviolet light is irradiated for 5-15S at a wavelength of 200-400 nm.
Preferably, in S3, nano silicon dioxide and water are added for ultrasonic dispersion, wherein the ultrasonic dispersion time is 10-30min, the ultrasonic frequency is 10-20kHz, and the ultrasonic power is 300-500W.
The technical effects of the invention are as follows:
according to the invention, the C5 petroleum resin is compounded with the nano silicon dioxide, the C-H bond and the C-C bond in the molecular chain of the C5 petroleum resin are subjected to ultraviolet irradiation treatment to generate free radicals, and react with oxygen in the air to generate ROO-, H is continuously extracted on the molecular chain to generate carboxyl, and the carboxyl is further combined with hydroxyl on the surface of the nano silicon dioxide, so that the compatibility of the C5 petroleum resin and the premix is improved, the system flowability is excellent, the C5 petroleum resin can enter into pores of a pavement, the bonding strength of a marking coating film and the pavement is enhanced, the falling of the road marking coating is prevented, meanwhile, perfect combination of strength and toughness can be well realized, the compressive strength of a surface marking is improved, in addition, the bonding fastness of the glass bead between systems can be further improved due to the combination with the amino glass bead, and the falling of the glass bead and the marking is obviously reduced.
The invention can effectively improve the compressive strength of the glass beads in the marked lines, and can effectively prevent the glass beads from sinking in the marked lines after the marked lines are rolled by automobiles on roads at high frequency, thereby improving the continuous high-reverse reaction of the glass beads.
Drawings
FIG. 1 is a graph comparing the compression test results of the road marking paints of example 5 and comparative examples 1-2.
Detailed Description
The invention is further illustrated below in connection with specific embodiments.
Example 1
A preparation method of durable hot-melt marking paint comprises the following steps:
s1, weighing 10kg of heavy calcium carbonate, 10kg of quartz sand, 10kg of talcum powder and 1kg of titanium dioxide, mixing, and stirring at a speed of 500r/min for 1h to obtain a premix;
s2, adding 50kg of glass beads into 100kg of 1mol/L sodium hydroxide solution, stirring for 1h, filtering, washing, drying at 70 ℃, adding 50kg of 40wt% ethanol solution and 1kg of KH550 coupling agent, stirring for 5h at 50 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:1:1, a step of;
s3, adding 20kg of dimethylbenzene into 50kg of C5 petroleum resin, refluxing and stirring at 100 ℃ for 5min, cooling to 80 ℃, adding 10kg of nano silicon dioxide and 5kg of water, performing ultrasonic dispersion for 10min, wherein the ultrasonic frequency is 10kHz, the ultrasonic power is 300W, performing ultrasonic irradiation treatment for 5S by adopting ultraviolet rays with the wavelength of 200nm, adding 0.1kg of boron trifluoride diethyl ether complex, continuing ultrasonic treatment for 1h, adding 1kg of sodium carbonate, stirring at 1000r/min for 10min, adding the aminated glass beads, stirring at 100 ℃ for 5min, sequentially performing alkaline washing, water washing until the pH value of the system is neutral, performing rotary evaporation and vacuum drying to obtain the C5 petroleum resin compound glass beads;
s4, mixing 1kg of stabilizer UV-P, 5kg of EVA resin, 1kg of dioctyl phthalate, 1-3kg of PE wax and C5 petroleum resin compound glass beads, stirring at the speed of 1000r/min for 10min, adding the premix, and continuously stirring for 1h to obtain the durable hot-melt marking paint.
Example 2
A preparation method of durable hot-melt marking paint comprises the following steps:
s1, weighing 50kg of heavy calcium carbonate, 30kg of quartz sand, 20kg of talcum powder and 10kg of titanium dioxide, mixing, and stirring at a speed of 1500r/min for 2 hours to obtain a premix;
s2, adding 80kg of glass beads into 200kg of sodium hydroxide solution with the concentration of 2mol/L, stirring for 2 hours, filtering, washing, drying at the temperature of 80 ℃, adding 100kg of ethanol solution with the concentration of 60wt% and 5kg of KH550 coupling agent, stirring for 10 hours at the temperature of 80 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:5:5, a step of;
s3, adding 60kg of dimethylbenzene into 150kg of C5 petroleum resin, refluxing and stirring at 150 ℃ for 15min, cooling to 90 ℃, adding 30kg of nano silicon dioxide and 15kg of water, performing ultrasonic dispersion for 30min, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 500W, performing ultrasonic irradiation treatment for 15S by adopting ultraviolet rays with the wavelength of 400nm, adding 1kg of boron trifluoride diethyl ether complex, continuing ultrasonic treatment for 2h, adding 2kg of sodium carbonate, stirring at a speed of 3000r/min for 20min, adding the aminated glass beads, stirring at 120 ℃ for 15min, sequentially performing alkaline washing, water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain the C5 petroleum resin compound glass beads;
s4, mixing 2kg of light stabilizer UV-326, 30kg of EVA resin, 3kg of dioctyl phthalate, 3kg of PE wax and C5 petroleum resin compound glass beads, stirring at the speed of 2000r/min for 30min, adding premix, and continuously stirring for 2h to obtain the durable hot-melt marking paint.
Example 3
A preparation method of durable hot-melt marking paint comprises the following steps:
s1, weighing 20kg of heavy calcium carbonate, 15kg of quartz sand, 12kg of talcum powder and 3kg of titanium dioxide, mixing, and stirring at the speed of 700r/min for 1.2 hours to obtain a premix;
s2, adding 55kg of glass beads into 120kg of 1.2 mol/L sodium hydroxide solution, stirring for 1.5 hours, filtering, washing, drying at 72 ℃, adding 60kg of 42wt% ethanol solution and 2kg of KH550 coupling agent, stirring for 5-10 hours at 55 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:2:2;
s3, adding 30kg of dimethylbenzene into 80kg of C5 petroleum resin, refluxing and stirring at 110 ℃ for 6min, cooling to 81 ℃, adding 13kg of nano silicon dioxide and 7kg of water, performing ultrasonic dispersion for 11min, wherein the ultrasonic frequency is 12kHz, the ultrasonic power is 320W, performing irradiation treatment for 6S by adopting ultraviolet rays with the wavelength of 250nm, adding 0.14kg of boron trifluoride diethyl ether complex, continuing ultrasonic treatment for 1.2h, adding 1.04kg of sodium carbonate, stirring at 1500r/min for 13min, adding the aminated glass beads, stirring at 105 ℃ for 8min, sequentially performing alkali washing and water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain C5 petroleum resin compound glass beads;
s4, mixing 1.2kg of light stabilizer LS-744, 10kg of EVA resin, 1.2kg of dioctyl phthalate, 1.5kg of PE wax and C5 petroleum resin compound glass beads, stirring at the speed of 1200r/min for 12min, adding premix, and continuously stirring for 1.2h to obtain the durable hot-melt marking paint.
Example 4
A preparation method of durable hot-melt marking paint comprises the following steps:
s1, weighing 41kg of heavy calcium carbonate, 25kg of quartz sand, 14kg of talcum powder and 8kg of titanium dioxide, mixing, and stirring at 1350r/min for 1.8h to obtain a premix;
s2, adding 72kg of glass beads into 180kg of 1.6mol/L sodium hydroxide solution, stirring for 1.5 hours, filtering, washing, drying at the temperature of 76 ℃, adding 85kg of 52wt% ethanol solution and 3kg of KH550 coupling agent, stirring for 8 hours at the temperature of 72 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:2:3, a step of;
s3, adding 55kg of dimethylbenzene into 125kg of C5 petroleum resin, refluxing and stirring at a temperature of 135 ℃ for 12min, cooling to 88 ℃, adding 26kg of nano silicon dioxide and 12kg of water, performing ultrasonic dispersion for 24min, wherein the ultrasonic frequency is 15kHz, the ultrasonic power is 400W, performing ultrasonic irradiation treatment for 10S by adopting ultraviolet rays with a wavelength of 350nm, adding 0.2kg of boron trifluoride diethyl ether complex, continuing ultrasonic treatment for 1.5h, adding 1.6kg of sodium carbonate, stirring at a speed of 2600r/min for 15min, adding the aminated glass beads, stirring at a temperature of 118 ℃ for 12min, sequentially performing alkali washing and water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain the C5 petroleum resin compound glass beads;
s4, mixing 1.8kg of light stabilizer LS-744, 25kg of EVA resin, 2.1kg of dioctyl phthalate, 2.5kg of PE wax and C5 petroleum resin compound glass beads, stirring for 24min at the speed of 1800r/min, adding premix, and continuously stirring for 1.8h to obtain the durable hot-melt marking paint.
Example 5
A preparation method of durable hot-melt marking paint comprises the following steps:
s1, weighing 35kg of heavy calcium carbonate, 20kg of quartz sand, 15kg of talcum powder and 5kg of titanium dioxide, mixing, and stirring at a speed of 1000r/min for 1.5 hours to obtain a premix;
s2, adding 70kg of glass beads into 160kg of sodium hydroxide solution with the concentration of 1.5mol/L, stirring for 1.5 hours, filtering, washing, drying at the temperature of 76 ℃, adding 80kg of ethanol solution with the concentration of 55wt% and 2kg of KH550 coupling agent, stirring for 6 hours at the temperature of 75 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:2.5:2.5;
s3, adding 30kg of dimethylbenzene into 100kg of C5 petroleum resin, refluxing and stirring at 120 ℃ for 10min, cooling to 85 ℃, adding 20kg of nano silicon dioxide and 12kg of water, performing ultrasonic dispersion for 28min, wherein the ultrasonic frequency is 12kHz, the ultrasonic power is 450W, performing ultrasonic irradiation treatment for 10S by adopting ultraviolet rays with the wavelength of 250nm, adding 0.4kg of boron trifluoride diethyl ether complex, continuing ultrasonic treatment for 1.5h, adding 1.5kg of sodium carbonate, stirring at 2000r/min for 15min, adding the aminated glass beads, stirring at 110 ℃ for 10min, sequentially performing alkali washing and water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain C5 petroleum resin compound glass beads;
s4, mixing 1.2kg of light stabilizer UV-326, 20kg of EVA resin, 2kg of dioctyl phthalate, 2kg of PE wax and C5 petroleum resin compound glass beads, stirring at a speed of 1500r/min for 20min, adding premix, and continuously stirring for 1.5h to obtain the durable hot-melt marking paint.
Comparative example 1
A preparation method of a hot melt marking paint comprises the following steps:
weighing 35kg of heavy calcium carbonate, 20kg of quartz sand, 15kg of talcum powder and 5kg of titanium dioxide, mixing, and stirring at the speed of 1000r/min for 1.5h to obtain a premix;
1.2kg of light stabilizer UV-326, 20kg of EVA resin, 2kg of dioctyl phthalate, 2kg of PE wax, 100kg of C5 petroleum resin, 70kg of glass beads and 20kg of nano silica are mixed, stirred at the speed of 1500r/min for 20min, and the premix is added for continuous stirring for 1.5h, so that the hot-melt marking paint is obtained.
Wherein the glass beads comprise glass beads with the particle size of 0.1-0.4mm, glass beads with the particle size of 0.5-0.65mm and glass beads with the particle size of 1-1.2mm, and the weight ratio of the three is 10:2.5:2.5;
comparative example 2
A preparation method of a hot melt marking paint comprises the following steps:
s1, weighing 35kg of heavy calcium carbonate, 20kg of quartz sand, 15kg of talcum powder and 5kg of titanium dioxide, mixing, and stirring at a speed of 1000r/min for 1.5 hours to obtain a premix;
s2, adding 70kg of glass beads into 160kg of sodium hydroxide solution with the concentration of 1.5mol/L, stirring for 1.5 hours, filtering, washing, drying at the temperature of 76 ℃, adding 80kg of ethanol solution with the concentration of 55wt% and 2kg of KH550 coupling agent, stirring for 6 hours at the temperature of 75 ℃, filtering, washing, and drying to obtain the amino glass beads;
the glass beads comprise 0.1-0.4mm glass beads, 0.5-0.65mm glass beads and 1-1.2mm glass beads, and the weight ratio of the three is 10:2.5:2.5;
s3, mixing 1.2kg of light stabilizer UV-326, 20kg of EVA resin, 2kg of dioctyl phthalate, 2kg of PE wax, 100kg of C5 petroleum resin, amino glass beads and 20kg of nano silicon dioxide, stirring at a speed of 1500r/min for 20min, adding premix, and continuously stirring for 1.5h to obtain the hot-melt marking paint.
1. Appearance and fastness detection
Putting the marking paint of the example 5 and the marking paint of the comparative examples 1-2 into a hot melting kettle, uniformly stirring at 180-200 ℃, then putting into a small kettle of an engineering vehicle, putting into a hopper through the small kettle, uniformly scraping the paint on a road surface according to a lofting line, and naturally curing to obtain a road marking sample to be detected.
(1) Appearance conditions: testing the color and brightness factors of the marked line sample to be tested according to JT/T280-2004 industry standard, and observing the surface quality of the marked line to be tested by naked eyes;
(2) Fastness of glass beads to road markings: and (3) using the empty load of the automobile with the weight of about 1.5t to sequentially press each road marking sample, circulating for 100 times, and observing the falling condition of the glass beads on the surface of the sample and the sinking condition of the glass beads.
The test results are shown in the following table:
| test item | Apparent condition | Glass bead firmness |
| Example 5 | White, 0.77 | No falling off and no sinking down |
| Comparative example 1 | White, 0.86 | A small amount of microbeads drop off and sink |
| Comparative example 2 | White, 0.75 | Does not fall off and sinks |
As can be seen from the table, the road marking has good surface quality, higher whiteness and high bonding fastness of the glass beads in the marking, the brightness factor reaches more than 0.75, and the situation that the glass beads fall off and sink after being continuously rolled by an automobile is not seen, so that the continuous high-reverse reaction of the road marking is improved.
2. Mechanical property test
According to the JT/T280-2004 test standard, the hot melt paint is heated to 190 ℃, the paint forms a uniform fluid and is placed in a sample vessel of each index, and the sample vessel is placed for 24 hours under a standard environment, wherein:
the wear resistance test condition is weight reduction after 200rad/1000 load;
the low-temperature anti-cracking test is carried out under the conditions of 20-4 h, 25-4 h as one cycle, 200 times of microscope observation is carried out to obtain cracks (national standard requirements of 10-4 h, 10-4 h as one cycle, 5 times of magnifier observation is carried out to obtain no cracks as cycle times), and when micro cracks are observed under 200 times of microscope, the low-temperature test is ended;
when the drawing strength is tested, the thickness of a paint film is 2mm, and the base material is a cement asbestos plate.
The test results are shown in the following table:
from the above table, the invention can effectively improve abrasion performance and low-temperature cracking resistance, effectively enhance drawing strength and has excellent mechanical properties.
3. Compressive Strength test
The marked line paint to be detected is cast into a compression test block with the size of 20mm multiplied by 20mm, and the compression test block is carried out after being placed for 24 hours at the standard test temperature, wherein the preload of an electronic universal tester is 10N, the loading speed is 30mm/min, and the test result is shown in figure 1.
As can be seen from FIG. 1, comparative example 1 is extremely susceptible to brittle fracture and no plastic deformation. In contrast to comparative example 2, example 5 not only had a plastic deformation plateau, i.e., a first high point occurred and a set variable was maintained and then increased, but also a large deformation amount, a high initial compression resistance value and excellent compression resistance.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The durable hot-melt marking paint is characterized by comprising the following raw materials in parts by weight: 50-150 parts of C5 petroleum resin, 10-50 parts of heavy calcium carbonate, 50-80 parts of glass beads, 5-30 parts of EVA resin, 10-30 parts of quartz sand, 10-20 parts of talcum powder, 1-10 parts of titanium dioxide, 10-30 parts of nano silicon dioxide, 1-3 parts of dioctyl phthalate, 1-5 parts of KH550 coupling agent, 1-2 parts of sodium carbonate, 1-3 parts of PE wax, 0.1-1 part of catalyst, 1-2 parts of light stabilizer, 100-200 parts of sodium hydroxide solution, 50-100 parts of ethanol solution, 20-60 parts of dimethylbenzene and 5-15 parts of water;
the preparation method of the marking paint comprises the following steps:
s1, mixing heavy calcium carbonate, quartz sand, talcum powder and titanium dioxide according to a proportion, and stirring at a speed of 500-1500r/min for 1-2h to obtain a premix;
s2, adding the glass beads into a sodium hydroxide solution, stirring for 1-2h, filtering, washing, drying at 70-80 ℃, adding an ethanol solution and a KH550 coupling agent, stirring for 5-10h at 50-80 ℃, filtering, washing, and drying to obtain the amino glass beads;
s3, adding dimethylbenzene into the C5 petroleum resin, refluxing and stirring for 5-15min at the temperature of 100-150 ℃, cooling to 80-90 ℃, adding nano silicon dioxide, performing ultrasonic dispersion on the mixture, performing ultraviolet irradiation treatment, wherein the ultraviolet wavelength is 200-400nm, the irradiation time is 5-15S, adding a catalyst, continuing ultrasonic treatment for 1-2h, adding sodium carbonate, stirring for 10-20min at the speed of 1000-3000r/min, adding the aminated glass beads, stirring for 5-15min at the temperature of 100-120 ℃, sequentially performing alkali washing and water washing until the pH value of the system is neutral, performing rotary steaming and vacuum drying to obtain the C5 petroleum resin compound glass beads;
s4, mixing the light stabilizer, EVA resin, dioctylphthalate, PE wax and C5 petroleum resin compounded glass beads, stirring at the speed of 1000-2000r/min for 10-30min, adding premix, and continuously stirring for 1-2h to obtain the durable hot melt marking paint.
2. The durable hot-melt marking paint according to claim 1, wherein the glass beads comprise glass beads with a particle size of 0.1-0.4mm, glass beads with a particle size of 0.5-0.65mm and glass beads with a particle size of 1-1.2mm, and the weight ratio of the three is 10:1-5:1-5.
3. The durable hot melt striping coating of claim 1, wherein the catalyst is boron trifluoride etherate.
4. The durable hot melt striping coating of claim 1, wherein the sodium hydroxide solution has a concentration of 1-2mol/L.
5. The durable hot melt striping coating of claim 1, wherein the ethanol solution has a concentration of 40-60% by weight.
6. The durable hot melt striping coating of claim 1, wherein the light stabilizer comprises at least one of light stabilizer UV-P, light stabilizer UV-326, light stabilizer UV-327, light stabilizer UV-5411, light stabilizer LS-744, light stabilizer LS-770, light stabilizer GW-540, and light stabilizer PDS.
7. The durable hot-melt striping coating of claim 1, wherein in S3, nano silica is added, water is added for ultrasonic dispersion, wherein the ultrasonic dispersion time is 10-30min, the ultrasonic frequency is 10-20kHz, and the ultrasonic power is 300-500W.
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