CN115850649A - Method for quickly synthesizing solvent-free polyurethane acrylate - Google Patents

Method for quickly synthesizing solvent-free polyurethane acrylate Download PDF

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CN115850649A
CN115850649A CN202211677246.3A CN202211677246A CN115850649A CN 115850649 A CN115850649 A CN 115850649A CN 202211677246 A CN202211677246 A CN 202211677246A CN 115850649 A CN115850649 A CN 115850649A
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reaction
gravity
acrylate
polyol
antioxidant
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裴小波
刘翘楚
朱建国
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Shanghai Rensu New Material Co ltd
Ige Shanghai Technologies Co ltd
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Shanghai Rensu New Material Co ltd
Ige Shanghai Technologies Co ltd
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Abstract

The invention provides a method for quickly synthesizing solvent-free polyurethane acrylate, which comprises the steps of setting the revolution speed of a gravity stirrer matched with a gravity dispersion cup to be 500-1500 rpm, setting the rotation speed to be 1000-2500 rpm, adding polymeric polyol, isocyanate and a catalyst into the gravity dispersion cup for reaction, adding a chain extender for reaction, and finally adding a polymerization inhibitor and an acrylic monomer for reaction to obtain the solvent-free polyurethane acrylate; the whole reaction process of the method is carried out in a gravity dispersion cup matched with a gravity stirrer, the revolution speed and the rotation speed of the gravity stirrer are controlled, so that materials can be fully contacted and uniformly heated in the reaction process, an additional vacuumizing step is not needed, the reaction time is greatly shortened, and the performances of raw materials and screened products can be realized in a short time.

Description

Method for quickly synthesizing solvent-free polyurethane acrylate
Technical Field
The invention belongs to the technical field of synthesis of urethane acrylate, and particularly relates to a preparation method of a polymer-coated quantum dot.
Background
Polyurethane acrylic resin is widely applied to various high-grade coatings or adhesives at present, is used as a sealing element and the like in the fields of electronic and electrical glue and the like, has different performance requirements in different application scenes, is usually subjected to various performance tests on a large amount of raw materials during the synthesis of polyurethane acrylic resin in order to meet different performance requirements, is repeatedly tested in different formulas and material proportions during the synthesis of conventional resin, and is usually subjected to one reaction for several hours, so that a large amount of time is wasted for the synthesis of resin, and the experimental process is seriously delayed.
CN104530957A discloses a method for synthesizing a urethane acrylate curing coating, which comprises the following steps: heating the polymer polyol to 110 ℃, and carrying out vacuum-pumping and water-removing for 2 hours under reduced pressure; adding diisocyanate and antioxidant into a three-necked bottle according to the formula amount, and heating for reaction for a certain time; then adding the chain extender and the catalyst into a three-necked bottle for reaction, and detecting the reaction process by using a Fourier transform after the reaction; adding monomers containing p-hydroxyanisole and hydroxyl acrylic acid into a three-necked bottle for end-capping reaction, detecting the reaction process by using Fourier infrared, and discharging the materials when the NCO peak completely disappears, namely the reaction end point, so as to obtain a polyurethane acrylate oligomer; weighing the polyurethane acrylate oligomer, the reactive diluent monomer, the coupling agent and other auxiliaries according to the formula ratio, sequentially putting the mixture into a beaker, uniformly stirring and dispersing the mixture, adding the photoinitiator under the condition of keeping out of the sun, and uniformly stirring the mixture to obtain the polyurethane acrylic curing coating/adhesive; the preparation method is complex, the reaction time is long, and the raw materials are not easy to select quickly.
Therefore, it is desired to develop a method for rapidly synthesizing a solventless urethane acrylate in which the reaction time is short and the properties of the obtained product are comparable to those of the conventional reaction.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for quickly synthesizing solvent-free polyurethane acrylate, which adopts a gravity dispersion machine as reaction equipment, utilizes a unique high-speed stirring mode, can ensure that materials are quickly turned over in the whole reaction process, further has very good contact effect of the materials and is very uniformly heated, so that the materials can be fully reacted in a short time, the reaction time is greatly shortened, the method can effectively screen the materials in a short time, the material screening time is greatly saved, and the experiment progress is effectively accelerated.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for rapidly synthesizing a solvent-free urethane acrylate, the method comprising: setting the revolution speed of a gravity stirrer matched with a gravity dispersing cup to be 500-1500 rpm (such as 500rpm, 600rpm, 700rpm, 800rpm, 900rpm, 1000rpm, 1100rpm, 1200rpm, 1300rpm or 1400rpm and the like), setting the rotation speed to be 1000-2500 rpm (such as 1200rpm, 1400rpm, 1600rpm, 1800rpm, 2000rpm, 2200rpm or 2400rpm and the like), adding polymeric polyol, isocyanate and a catalyst into the gravity dispersing cup for reaction, adding a chain extender for reaction, and finally adding a polymerization inhibitor and an acrylic monomer for blocking reaction to obtain the solvent-free polyurethane acrylate.
The whole reaction process of the method for quickly synthesizing the solvent-free polyurethane acrylate is carried out in the gravity dispersion cup matched with the gravity stirrer, the gravity stirrer has a great difference from the conventional stirrer in a stirring mode, unlike the conventional stirrer which has a stirring rod or a dispersion plate, the gravity stirrer can stir and disperse materials by depending on the rotation of the gravity dispersion cup matched with the gravity stirrer, the gravity stirrer can have a specific revolution rotating speed and a specific autorotation rotating speed, and the materials can self-heat under the specific high-speed rotation, so that the system can quickly reach the reaction temperature without additional heating in the reaction process, the materials in the whole reaction process can be quickly stirred and mixed, the whole system has sufficient heat conduction, the materials are uniformly heated, the problem of side reaction and even implosion caused by local overheating can not be caused, and meanwhile, the reaction can be carried out for effective reaction time; in addition, the gravity dispersion machine matched with the gravity dispersion cup covers the glass cover plate well during operation, and can be vacuumized, so that the vacuum degree is not higher than 2kPa, the cavity is internally positioned under a vacuum environment including the material cup, further the whole process of air isolation is realized, the polyurethane reaction (isocyanate is easy to react with water in the air, and the best air isolation is realized in the reaction process) is facilitated, the step of introducing nitrogen after extra vacuumizing is not needed, the experiment operation steps are simplified, the synthesis time is further shortened, the method can effectively screen the materials in a short time, the time for screening the materials is greatly saved, and the progress of the experiment is effectively accelerated
The method for rapidly synthesizing the solvent-free polyurethane acrylate is mainly applied to experimental synthesis of the solvent-free polyurethane acrylate in a raw material selection stage, is beneficial to rapidly selecting raw materials, proportioning and the like, and is not applied to a batch production stage of the solvent-free polyurethane acrylate.
Preferably, the blender comprises a planetary vacuum gravity blender.
Preferably, the reactions are all carried out at normal temperature, and the whole experimental process of the method provided by the invention is kept at normal temperature.
Preferably, the polymeric polyol comprises a polyether polyol and/or a polyester polyol.
Preferably, the polyether polyol comprises any one of polytetramethylene ether glycol, polypropylene glycol or hydroxyl silicone oil modified polyether polyol or a combination of at least two of the foregoing.
Preferably, the polyester polyol comprises a polycarbonate polyol and/or a polycaprolactone polyol.
Preferably, the isocyanate comprises any one of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hydrogenated MDI, hexamethylene diisocyanate or lysine diisocyanate or a combination of at least two thereof.
Preferably, the catalyst includes any one of an organic bismuth-based catalyst, an organic zinc-based catalyst, an organic titanium-based catalyst, or an organic tin-based catalyst or a combination of at least two thereof.
Preferably, the reaction time of adding the polymeric polyol, the isocyanate and the catalyst into the gravity dispersion cup for reaction is 1-10 min, such as 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min.
Preferably, an antioxidant is also added in the reaction process of adding the polymeric polyol, the isocyanate and the catalyst into the gravity dispersion cup for reaction.
Preferably, the antioxidant comprises any one of antioxidant 1010, antioxidant BHT or antioxidant 168, or a combination of at least two thereof.
Preferably, the chain extender comprises any one of ethylene glycol, propylene glycol, diethylene glycol, neopentyl glycol, pentaerythritol, 1, 6-hexanediol, trimethylolpropane, hydrogenated bisphenol a, hydroquinone dihydroxyethyl ether, 1, 4-butanediol, 1, 4-cyclohexanediol, dimethylene phenyl diol, glycerol, or an alicyclic alcohol, or a combination of at least two thereof.
Preferably, the reaction time of adding the chain extender for reaction is 1-10 min, such as 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min.
Preferably, the polymerization inhibitor comprises hydroquinone and/or p-hydroxyanisole, preferably p-hydroxyanisole.
Preferably, the acrylic monomer comprises any one of hydroxyethyl methacrylate, hydroxyethyl acrylate, hydroxybutyl acrylate, hydroxypropyl methacrylate, caprolactone acrylate, alicyclic terminal hydroxy acrylate or 2-hydroxy-3-phenoxypropyl acrylate or a combination of at least two thereof.
Preferably, the reaction time of the final addition of the polymerization inhibitor and the acrylic monomer for the end capping reaction is 1-10 min, such as 1min, 2min, 3min, 4min, 5min, 6min, 7min, 8min, 9min or 10min.
Preferably, the method comprises: setting the revolution speed of a gravity stirrer matched with a gravity dispersion cup to be 500-1500 rpm, setting the rotation speed to be 1000-2500 rpm, adding polymeric polyol, isocyanate, a catalyst and an antioxidant into the gravity dispersion cup at normal temperature to react for 1-10 min, adding a chain extender to react for 1-10 min, and finally adding a polymerization inhibitor and an acrylic monomer to react for 1-10 min to obtain the solvent-free polyurethane acrylate.
In a second aspect, the present invention provides a solvent-free urethane acrylate prepared by the method of the first aspect.
In a third aspect, the present invention provides a use of the solventless polyurethane acrylate according to the second aspect in a coating or adhesive.
Compared with the prior art, the invention has the following beneficial effects:
the method for rapidly synthesizing the solvent-free polyurethane acrylate comprises the steps of setting the revolution speed of a gravity stirrer matched with a gravity dispersion cup to be 500-1500 rpm, setting the rotation speed to be 1000-2500 rpm, adding polymeric polyol, isocyanate and a catalyst into the gravity dispersion cup for reaction, adding a chain extender for reaction, and finally adding a polymerization inhibitor and an acrylic monomer for end-capping reaction to obtain the solvent-free polyurethane acrylate; the whole reaction process of the method is carried out in a gravity dispersion cup matched with a gravity stirrer, the revolution speed and the rotation speed of the gravity stirrer are controlled, so that materials can be fully contacted and uniformly heated in the reaction process, an additional vacuumizing step is not needed, the reaction time is greatly shortened, the performances of raw materials and screened products can be screened in a short time, and the experiment progress is accelerated.
Drawings
FIG. 1 is a Fourier infrared spectrum of solvent-free urethane acrylates obtained in examples 1 to 3 and comparative example 1,
wherein, 1-example 1, 2-example 2, 3-example 3, 4-comparative example 1;
FIG. 2 is a Fourier infrared spectrum of solvent-free urethane acrylates obtained in examples 4 to 6 and comparative example 2,
among them, 5-example 4, 6-example 5, 7-example 6, 8-comparative example 2.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
Example 1
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity mixer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersing cup to be 500rpm, setting the rotation speed of the gravity dispersing cup to be 1000rpm, adding 13g of polytetramethylene ether glycol (average molecular weight is 2000), 0.051g of antioxidant 1010, 5.919g of hydrogenated MDI and 0.01g of dibutyltin dilaurate into the gravity stirring cup to react for 10min at normal temperature, adding 0.26g of 1, 4-butanediol into the gravity stirring cup to continue to react for 5min, and finally adding 0.001g of p-hydroxyanisole and 3.06g of hydroxyethyl acrylate into the gravity stirring cup to end and react for 5min to obtain the solvent-free polyurethane acrylate.
Example 2
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity mixer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersing cup to 800rpm, setting the rotation speed of the gravity dispersing cup to 2000rpm, adding 13g of polytetramethylene ether glycol (the number average molecular weight is 2000), 0.051g of antioxidant 1010, 5.92g of hydrogenated MDI and 0.01g of dibutyltin dilaurate into the gravity stirring cup at normal temperature for reaction for 3min, adding 0.26g of 1, 4-butanediol into the gravity stirring cup for continuous reaction for 3min, and finally adding 0.001g of p-hydroxyanisole and 3.06g of hydroxyethyl acrylate into the gravity stirring cup for end capping reaction for 3min to obtain the solvent-free polyurethane acrylate.
Example 3
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity mixer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersing cup to 1000rpm, setting the rotation speed of the gravity dispersing cup to 2500rpm, adding 13g of polytetramethylene ether glycol (the number average molecular weight is 2000), 0.051g of antioxidant 1010, 5.92g of hydrogenated MDI and 0.01g of dibutyltin dilaurate into the gravity stirring cup at normal temperature for reaction for 2min, adding 0.26g of 1, 4-butanediol into the gravity stirring cup for continuous reaction for 2min, and finally adding 0.001g of p-hydroxyanisole and 3.06g of hydroxyethyl acrylate into the gravity stirring cup for end-capping reaction for 2min to obtain the solvent-free polyurethane acrylate.
Example 4
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity stirrer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersion cup to be 500rpm, setting the rotation speed of the gravity dispersion cup to be 1000rpm, adding 14.9g of polybutylene adipate diol (with the average molecular weight of 5000), 0.04g of antioxidant 1010, 0.01g of antioxidant 168, 4.07g of isophorone, isocyanate and 0.01g of dibutyltin dilaurate into the gravity stirring cup at normal temperature to react for 10min, adding 0.53g of diethylene glycol into the gravity stirring cup to continue the chain extension reaction for 5min, finally adding 0.001g of p-hydroxyanisole and 2.69g of hydroxyethyl methacrylate into the gravity stirring cup to react for 5min, and obtaining the solvent-free polyurethane acrylate.
Example 5
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity mixer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersion cup to 800rpm, setting the rotation speed of the gravity dispersion cup to 2000rpm, adding 14.9g of polybutylene adipate diol (with the average molecular weight of 5000), 0.04g of antioxidant 1010, 0.01g of antioxidant 168, 4.07g of isophorone, isocyanate and 0.01g of dibutyltin dilaurate into the gravity stirring cup at normal temperature to react for 3min, adding 0.53g of diethylene glycol into the gravity stirring cup to continue to carry out chain extension reaction for 3min, finally adding 0.001g of p-hydroxyanisole and 2.69g of hydroxyethyl methacrylate into the gravity stirring cup to react for 3min, and obtaining the solvent-free polyurethane acrylate.
Example 6
A method for rapidly synthesizing a solventless urethane acrylate, the method comprising: setting the revolution speed of a planetary vacuum gravity mixer (SINOMH, model number VM300SA 2) provided with 1 gravity dispersion cup to be 1500rpm, setting the rotation speed of the gravity dispersion cup to be 2500rpm, adding 14.9g of polybutylene adipate diol (with average molecular weight of 5000), 0.04g of antioxidant 1010, 0.01g of antioxidant 168, 4.07g of isophorone, isocyanate and 0.01g of dibutyltin dilaurate into the gravity stirring cup at normal temperature to react for 2min, adding 0.53g of diethylene glycol into the gravity stirring cup to continue chain extension reaction for 2min, and finally adding 0.001g of p-hydroxyanisole and 2.69g of hydroxyethyl methacrylate into the gravity stirring cup to react for 2min to obtain the solvent-free polyurethane acrylate.
Comparative example 1
A method for synthesizing a solventless urethane acrylate, comprising the steps of:
(1) Putting 50g of polytetramethylene ether glycol (the number average molecular weight is 2000) into a three-neck flask, putting into an oil bath pan, heating to 100 ℃, vacuumizing and dehydrating for 2h for later use;
(2) Putting 13g of polytetramethylene ether glycol treated in the step (1), 0.051g of antioxidant 1010 and 5.919g of hydrogenated MDI into a 200mL three-neck flask, putting the three-neck flask into an oil bath kettle, vacuumizing and introducing nitrogen for three times of replacement, starting a stirrer, reacting for 1h at the temperature of 85 ℃ and the stirring speed of 150rpm, cooling to 65 ℃, adding 0.26g of 1, 4-butanediol and 0.001g of dibutyltin dilaurate for reacting for 30min, heating to 85 ℃ and reacting for 2h, tracking the reaction progress by adopting Fourier infrared, and carrying out the next step when the infrared display NCO peak is not changed;
(3) And (3) cooling to 50 ℃, putting 0.001g of p-hydroxyanisole and 3.06g of hydroxyethyl acrylate into a three-neck flask, heating to 70 ℃, reacting for 2 hours, sampling every 30 minutes, tracking the reaction process by adopting Fourier infrared, finishing the reaction after the NCO peak completely disappears, and discharging while the reaction is hot to obtain the solvent-free polyurethane acrylate.
Comparative example 2
A method for synthesizing a solventless urethane acrylate, comprising the steps of:
(1) 50g of poly butylene adipate glycol (with the average molecular weight of 5000) is placed in a three-neck flask, placed in an oil bath pan, heated to 100 ℃, and vacuumized and dehydrated for 2 hours for later use;
(2) Putting 14.9g of polybutylene adipate glycol treated in the step (1), 0.04g of antioxidant 1010 and 0.01g of 168 antioxidant, and 4.07g of isophorone diisocyanate into a 200mL three-neck flask, putting the three-neck flask into an oil bath pot, vacuumizing, introducing nitrogen for three times, starting a stirrer, heating to 80-85 ℃, keeping the temperature of the material at 85 ℃ for reaction for 2 hours at a stirring speed of 150rpm, tracking the reaction progress by Fourier infrared, and carrying out the next step when the infrared ray shows that the NCO peak is not changed;
(2) Cooling to 65 ℃, adding 0.53g of diethylene glycol and 0.001g of dibutyltin dilaurate to react for 30min, heating to 85 ℃ to react for 1h, tracking the reaction progress by adopting Fourier infrared, and carrying out the next step when the infrared shows that the NCO peak is not changed;
(3) And (2) cooling to 50 ℃, putting 0.001g of p-hydroxyanisole and 2.69g of hydroxyethyl methacrylate into a three-neck flask, heating to 70 ℃, reacting for 2 hours, sampling every 30 minutes, tracking the reaction process by adopting Fourier infrared, finishing the reaction after the NCO peak completely disappears, and discharging while the reaction is hot to obtain the solvent-free polyurethane acrylate.
And (3) performance testing:
(1) Viscosity: testing with CAP2000+ VISCOMETER cone-plate VISCOMETER at 20rpm for 20s at 60 deg.C, and sampling amount of 0.5mL;
(2) Refractive index: testing by using an Abbe refractometer;
(3) Shear force: the shear force with a PC substrate and a glass substrate was measured using urethane acrylate as a binder, the PC substrate had a dimensional specification of 15X 10X 5mm, the glass substrate had a dimensional specification of 40X 20X 5mm, the coating film thickness was 100 μm, and the curing conditions were 810mW/cm 2 Curing for 10s; the testing equipment is a SY-500 microcomputer tensile testing machine (Dongguan Jinton testing equipment Co., ltd.);
(5) High-temperature high-humidity shear force: testing the shearing force after the treatment under the condition of double 85;
(6) Cold and hot impact shear force: testing the shearing force after the treatment at-40 ℃ and 125 ℃;
(7) Matching rate of Fourier infrared spectrum structure: the test results are shown in fig. 1 and fig. 2 by using a fourier infrared spectrometer, wherein in fig. 1, 1 represents example 1,2 represents example 2,3 represents example 3, and 4 represents comparative example 1; in FIG. 2, 2 represents example 4,2 represents example 5,3 represents example 6,4 represents comparative example 2;
as can be seen from FIGS. 1 to 2, the urethane acrylates obtained in examples 1 to 3 and comparative example 1 had no significant difference in the peak shape, peak position, and peak intensity of the infrared peak, indicating that the molecular structures of the two are identical; the urethane acrylates obtained in examples 4 to 6 and the urethane acrylate obtained in comparative example 2 showed no difference in the peak shape and peak intensity of the infrared peak, indicating that the molecular structures of the two are the same.
The solvent-free urethane acrylates obtained in examples 1 to 6 and comparative examples 1 to 2 were tested according to the above test methods, and the test results are shown in Table 1:
TABLE 1
Figure BDA0004017491320000101
Figure BDA0004017491320000111
As can be seen from the data in table 1: the viscosity, refractive index and shearing force of the solvent-free polyurethane acrylate (examples 1 to 6) prepared by the preparation method provided by the invention are all about the same as those of the solvent-free polyurethane acrylate prepared by the existing preparation method, but the preparation time is greatly shortened.
The applicant states that the present invention is illustrated by the above examples as a method for rapidly synthesizing solvent-free urethane acrylates, but the present invention is not limited to the above process steps, i.e., it is not meant that the present invention must rely on the above process steps to be carried out. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.

Claims (10)

1. A method for rapidly synthesizing a solventless urethane acrylate, comprising: setting the revolution speed of a gravity stirrer matched with a gravity dispersion cup to be 500-1500 rpm, setting the rotation speed to be 1000-2500 rpm, adding polymeric polyol, isocyanate and a catalyst into the gravity dispersion cup for reaction, adding a chain extender for reaction, and finally adding a polymerization inhibitor and an acrylic monomer for end-capping reaction to obtain the solvent-free polyurethane acrylate.
2. The method of claim 1, wherein the gravity blender comprises a planetary vacuum gravity blender;
preferably, the reaction is carried out at normal temperature.
3. The method of claim 1 or 2, the polymeric polyol comprising a polyether polyol and/or a polyester polyol;
preferably, the polyether polyol comprises any one of polytetramethylene ether glycol, polypropylene glycol or hydroxyl silicone oil modified polyether polyol or a combination of at least two of the polytetramethylene ether glycol, the polypropylene glycol and the hydroxyl silicone oil modified polyether polyol;
preferably, the polyester polyol comprises a polycarbonate polyol and/or a polycaprolactone polyol;
preferably, the isocyanate comprises any one of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hydrogenated MDI, hexamethylene diisocyanate or lysine diisocyanate or a combination of at least two of the same;
preferably, the catalyst comprises any one or a combination of at least two of an organic bismuth-based catalyst, an organic zinc-based catalyst, an organic titanium-based catalyst or an organic tin-based catalyst;
preferably, the reaction time for adding the polymeric polyol, the isocyanate and the catalyst into the gravity dispersion cup to react is 1-10 min.
4. The method according to any one of claims 1 to 3, wherein an antioxidant is further added during the reaction process of adding the polymeric polyol, the isocyanate and the catalyst into the gravity dispersion cup for reaction;
preferably, the antioxidant comprises any one of antioxidant 1010, antioxidant BHT or antioxidant 168, or a combination of at least two thereof.
5. A method according to any one of claims 1 to 4, wherein the chain extender comprises any one of or a combination of at least two of ethylene glycol, propylene glycol, diethylene glycol, neopentyl glycol, pentaerythritol, 1, 6-hexanediol, trimethylolpropane, hydrogenated bisphenol A, hydroquinone bis hydroxyethyl ether, 1, 4-butanediol, 1, 4-cyclohexanediol, dimethylene phenyl diol, glycerol or an alicyclic alcohol;
preferably, the reaction time of adding the chain extender for reaction is 1-10 min.
6. The process according to any one of claims 1 to 5, characterized in that the polymerization inhibitor comprises hydroquinone and/or p-hydroxyanisole, preferably p-hydroxyanisole;
preferably, the acrylic monomer comprises any one of hydroxyethyl methacrylate, hydroxyethyl acrylate, hydroxybutyl acrylate, hydroxypropyl methacrylate, caprolactone acrylate, alicyclic terminal hydroxy acrylate or 2-hydroxy-3-phenoxypropyl acrylate or a combination of at least two thereof.
7. The method according to any one of claims 1 to 6, wherein the purple jade, the final addition of the polymerization inhibitor and the acrylic monomer, and the end-capping reaction are carried out for a reaction time of 1 to 10min.
8. The method according to any one of claims 1 to 7, characterized in that it comprises: setting the revolution speed of a gravity stirrer matched with a gravity dispersion cup to be 500-1500 rpm, setting the rotation speed to be 1000-2500 rpm, adding polymeric polyol, isocyanate, a catalyst and an antioxidant into the gravity dispersion cup at normal temperature to react for 1-10 min, then adding a chain extender to react for 1-10 min, and finally adding a polymerization inhibitor and an acrylic monomer to perform end capping reaction for 1-10 min to obtain the solvent-free polyurethane acrylate.
9. A solvent-free urethane acrylate prepared by the method of any one of claims 1 to 8.
10. Use of the solventless urethane acrylate according to claim 9 in coatings or adhesives.
CN202211677246.3A 2022-12-26 2022-12-26 Method for quickly synthesizing solvent-free polyurethane acrylate Pending CN115850649A (en)

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