CN113105617A - Preparation method of polyether polyol for high-performance waterproof coating - Google Patents
Preparation method of polyether polyol for high-performance waterproof coating Download PDFInfo
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- CN113105617A CN113105617A CN202110388487.5A CN202110388487A CN113105617A CN 113105617 A CN113105617 A CN 113105617A CN 202110388487 A CN202110388487 A CN 202110388487A CN 113105617 A CN113105617 A CN 113105617A
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- polyether polyol
- initiator
- waterproof coating
- ethylene oxide
- oxide
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- 229920000570 polyether Polymers 0.000 title claims abstract description 58
- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 53
- 238000000576 coating method Methods 0.000 title claims abstract description 51
- 239000011248 coating agent Substances 0.000 title claims abstract description 50
- 229920005862 polyol Polymers 0.000 title claims abstract description 45
- 150000003077 polyols Chemical class 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 35
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 10
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 238000007670 refining Methods 0.000 claims abstract description 7
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 5
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 5
- 230000001588 bifunctional effect Effects 0.000 claims abstract description 4
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 claims description 36
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 35
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical compound [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 239000003973 paint Substances 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 3
- BDAWXSQJJCIFIK-UHFFFAOYSA-N potassium methoxide Chemical compound [K+].[O-]C BDAWXSQJJCIFIK-UHFFFAOYSA-N 0.000 claims description 3
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 7
- 229920002635 polyurethane Polymers 0.000 abstract description 13
- 239000004814 polyurethane Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000013461 design Methods 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 238000012360 testing method Methods 0.000 description 6
- 239000002253 acid Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229920005749 polyurethane resin Polymers 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 229910001220 stainless steel Inorganic materials 0.000 description 5
- 239000010935 stainless steel Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000001276 controlling effect Effects 0.000 description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 3
- 239000008199 coating composition Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000012948 isocyanate Substances 0.000 description 3
- 150000002513 isocyanates Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000003472 neutralizing effect Effects 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 239000002313 adhesive film Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000013022 formulation composition Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000004078 waterproofing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Polyurethanes Or Polyureas (AREA)
- Polyethers (AREA)
Abstract
The invention relates to a preparation method of polyether polyol for a high-performance waterproof coating, belonging to the technical field of polyether polyol preparation. The method takes a mixture of a bifunctional compound and a trifunctional compound as an initiator, takes alkali metal or DMC as a catalyst, and carries out polymerization reaction with alkylene oxide to prepare a polyether polyol crude polymer; and then refining the crude polymer to obtain the polyether polyol for the high-performance waterproof coating. The invention has scientific and reasonable design, and when the prepared polyether polyol is applied to the formula of the polyurethane waterproof coating, one polyether polyol is used for replacing the traditional mixture of multiple polyethers, the viscosity of the coating is reduced, and the performance of the polyurethane waterproof coating after film formation is improved.
Description
Technical Field
The invention relates to a preparation method of polyether polyol for a high-performance waterproof coating, belonging to the technical field of polyether polyol preparation.
Background
Polyurethane waterproof coatings are widely used for waterproofing work in the fields of airports, railways, municipal works, civil buildings and the like because of their excellent water resistance, adhesion, abrasion resistance, chemical stability and cold resistance.
Currently, with the continuous improvement of people's environmental awareness and the stricter and stricter relevant legal regulations, the market demand for high-performance environment-friendly polyurethane waterproof paint in the market is larger and larger. In a traditional polyurethane waterproof coating formula system, multiple polyether polyols (mainly polyether polyols with 2000g/mol of bifunctionality and 5000g/mol of trifunctional degree) are required to be compounded for use, so that the required mechanical properties can be achieved. The coating prepared from the traditional polyether has high viscosity, a large amount of organic solvent is needed to reduce the viscosity of the coating for facilitating the construction of downstream customers, and the organic solvent is completely volatilized into the air in the curing process of the coating, so that the air pollution is caused.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the preparation method of the polyether polyol for the high-performance waterproof coating overcomes the defects of the prior art, is scientific and reasonable in design, and when the prepared polyether polyol is applied to a formula of the polyurethane waterproof coating, not only is one polyether polyol substituted for traditional mixing of multiple polyethers, but also the viscosity of the coating is reduced, and the performance of the polyurethane waterproof coating after film forming is improved.
The preparation method of the polyether polyol for the high-performance waterproof coating takes a mixture of a bifunctional compound and a trifunctional compound as an initiator, takes alkali metal or DMC as a catalyst, and carries out polymerization reaction with alkylene oxide to prepare a polyether polyol crude polymer; then refining the crude polymer to obtain the polyether polyol for the high-performance waterproof coating;
the difunctional compound is one or more of bisphenol A, ethylene glycol, diethylene glycol, butanediol, diethylene glycol, propylene glycol or dipropylene glycol;
the tri-functional compound is one or more of trimethylolpropane, glycerol, triethanolamine or triethylene glycol.
Preferably, the pressure is-0.1-0.4 MPa and the temperature is 80-180 ℃ during the polymerization reaction.
Preferably, the alkylene oxide is one or a mixture of two of propylene oxide and ethylene oxide according to any proportion.
Preferably, the mass ratio of the initiator to the alkylene oxide is 0.01-0.2: 1.
Preferably, the alkali metal catalyst is potassium hydroxide, sodium hydroxide, cesium hydroxide, potassium methoxide or sodium methoxide.
Preferably, the polymerization mode of the initiator and the alkylene oxide is one of the following modes:
the mode (1) is initiator + propylene oxide + ethylene oxide;
the mode (2) is that the initiator, the mixture of ethylene oxide and propylene oxide are added;
the mode (3) is initiator + ethylene oxide + propylene oxide + ethylene oxide;
the mode (4) is a mixture of an initiator + propylene oxide and ethylene oxide;
the mode (5) is a mixture of an initiator, ethylene oxide and propylene oxide;
the mode (6) is initiator + propylene oxide;
mode (7) is initiator + ethylene oxide;
the way (8) is to polymerize the initiator with a mixture of ethylene oxide and propylene oxide.
The concrete description is as follows:
the method (1) is to polymerize an initiator with propylene oxide and then with ethylene oxide.
The way (2) is that the initiator is polymerized with the mixture of ethylene oxide and propylene oxide first and then with propylene oxide.
The mode (3) is that the initiator is polymerized with ethylene oxide, then with propylene oxide, and finally with ethylene oxide.
The way (4) is that the initiator is polymerized with propylene oxide first and then with a mixture of propylene oxide and ethylene oxide.
The way (5) is that the initiator is polymerized with ethylene oxide first and then with a mixture of ethylene oxide and propylene oxide.
The mode (6) is polymerization of the initiator with propylene oxide.
The mode (7) is a polymerization of the initiator with ethylene oxide.
The way (8) is to polymerize the initiator with a mixture of ethylene oxide and propylene oxide.
Preferably, when the alkylene oxide is ethylene oxide, the amount of ethylene oxide is 0 to 100% by mass of the final product.
Preferably, the purification treatment comprises neutralization, adsorption, crystallization and filtration in this order.
The polyether polyol for the high-performance waterproof coating prepared by the invention has the number average molecular weight of 1000-5000g/mol, the functionality of 2.1-2.6 and the hydroxyl value of 23-145 mgKOH/g.
The invention uses a plurality of initiator coupling technologies to obtain polyether polyol with a specific molecular structure by optimizing and controlling the functionality and molecular weight of the initiator. The crosslinking density of the polyurethane resin is regulated and controlled through regulating and controlling the functionality, so that the molecular weight of the polyurethane resin is controlled, the molecular weight of the polyurethane resin is related to the viscosity of the polyurethane resin, and the viscosity of the polyurethane resin in the coating can be reduced through optimization in a reasonable range. Therefore, downstream paint manufacturers can add no or little organic solvent, and the produced paint is more green and environment-friendly. The product uses a composite initiator, and initiators with different functionalities react with a polymerization monomer in a reaction kettle simultaneously to grow together. The degree of homogeneity of the composite polyether is incomparable with the traditional polyether through physical mixing.
In addition, the addition of isocyanate is regulated and controlled by regulating and controlling the molecular weight of the polyether, the addition of the isocyanate is related to the mechanical property of the cured coating, and the requirement on the mechanical property of the polyurethane waterproof coating can be met by optimizing the molecular weight without matching the polyether with other polyethers. Therefore, one polyether can replace two or even more conventional polyethers for preparing the polyurethane waterproof coating, and the prepared waterproof coating is superior to the conventional product in the aspects of mechanical property, acid resistance, alkali resistance and heat aging resistance after film formation. The product can reduce the conveying cost of downstream customers, reduce the storage and processing difficulty of the downstream customers and improve the quality stability of the downstream customers.
Compared with the prior art, the invention achieves the following beneficial effects:
(1) when the polyether polyol prepared by the invention is applied to a polyurethane waterproof coating formula, one polyether polyol is used for replacing the traditional mixing of various polyethers, so that the conveying cost of downstream customers can be effectively reduced, the storage of the downstream customers is facilitated, the processing difficulty of the downstream customers is reduced, and the stability of coating products of the downstream customers is improved;
(2) the viscosity of the waterproof coating prepared by using the polyether polyol is reduced, and downstream customers can add less organic solvent, so that the produced waterproof coating is more environment-friendly; the prepared waterproof coating is superior to the traditional coating product in the aspects of mechanical property, acid resistance, alkali resistance and heat aging resistance.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
160g of diethylene glycol, 92.68g of glycerol and 11.39g of solid potassium hydroxide catalyst were charged into a 5L stainless steel reactor, and the oxygen content in the reactor was measured to be less than 80ppm by nitrogen substitution. The temperature of the reaction kettle is raised to 105 ℃, and nitrogen bubbling and reduced pressure dehydration are carried out. 2975.68g of propylene oxide was continuously added while maintaining the temperature in the vessel at 110. + -. 2 ℃ and the pressure at 0.2. + -. 0.2MPa, followed by internal pressure reaction for 30 minutes to remove unreacted propylene oxide. Then adding 569.71g of ethylene oxide, carrying out end-capping polymerization at 130 ℃, carrying out internal pressure reaction, cooling and discharging to obtain the polyether polyol crude polymer for the high-performance waterproof coating.
And neutralizing, adsorbing, crystallizing, filtering and refining the polyether polyol crude polymer to obtain the polyether polyol for the high-performance waterproof coating.
The number average molecular weight of the product is 3000g/mol, the functionality is 2.4, and the hydroxyl value is 48 mgKOH/g.
Example 2
200g of propylene glycol, 151.14g of trimethylolpropane and 7.0g of potassium methoxide catalyst were charged into a 5L stainless steel reactor, and the oxygen content in the reactor was measured to be less than 80ppm by nitrogen substitution. The temperature of the reaction kettle is raised to 105 ℃, and nitrogen bubbling and reduced pressure dehydration are carried out. 1984.82g of propylene oxide was continuously added while maintaining the temperature in the vessel at 110. + -. 2 ℃ and the pressure at 0.2. + -. 0.2MPa, and the internal pressure reaction was carried out to remove unreacted propylene oxide. And then neutralizing, adsorbing, crystallizing, filtering and refining the polyether polyol crude polymer to prepare the oligomer.
And adding 810g of the oligomer into a 5L stainless steel reaction kettle, adding 0.024g of sulfuric acid and 0.12g of DMC catalyst, performing reduced pressure dehydration at 120 ℃ for 2h, continuously adding a mixture of 2390g of propylene oxide and 300g of ethylene oxide at 140 ℃, performing internal pressure reaction, and removing unreacted propylene oxide and ethylene oxide to obtain the polyether polyol for the high-performance waterproof coating.
The number average molecular weight of the product was 2800g/mol, the functionality was 2.3, and the hydroxyl value was 48 mgKOH/g.
Example 3
320g of diethylene glycol, 185.36g of glycerol, 60g of bisphenol A and 10.37g of solid sodium methoxide catalyst were placed in a 5L stainless steel reaction kettle, and nitrogen gas was used for replacement, and the oxygen content in the reaction kettle was measured to be less than 80 ppm. The temperature of the reaction kettle is raised to 105 ℃, and nitrogen bubbling and reduced pressure dehydration are carried out. Keeping the temperature in the kettle at 110 +/-2 ℃ and the pressure at 0.2 +/-0.2 MPa, continuously adding a mixture of 2692.44g of propylene oxide and 200g of ethylene oxide, carrying out internal pressure reaction, and removing unreacted propylene oxide. And then neutralizing, adsorbing, crystallizing, filtering and refining the polyether polyol crude polymer to prepare the oligomer.
Adding 800g of the oligomer into a 5L stainless steel reaction kettle, adding 0.024g of sulfuric acid and 0.12g of DMC catalyst, carrying out vacuum dehydration at 120 ℃ for 2h, continuously adding a mixture of 2400g of propylene oxide and 300g of ethylene oxide at 140 ℃, carrying out internal pressure reaction, and removing unreacted propylene oxide to obtain the polyether polyol for the high-performance waterproof coating.
The number average molecular weight of the product was 2800g/mol, the functionality was 2.38, and the hydroxyl value was 48 mgKOH/g.
Testing the performance of the prepared coating:
two polyether polyols (high-resilience polyether polyol with a trifunctional degree of 5000g/mol, EP-330N (G) and polyether polyol DL-2000D with a bifunctional degree of 2000g/mol CASE, which are produced by Shandong Lanxingdong GmbH) which are most commonly used for the current polyurethane waterproof coating are selected as comparative examples, and the same resin content and the similar functionality are set for comparison. The above materials were compared with conventional polyether polyols and the coating formulations are shown in table 1.
Table 1 verification of the formulation composition
Note: calculated as 25% of the same resin content.
The specific verification method comprises the following steps:
(1) dehydrating polyether, powder and plasticizer at high temperature for 2 hours;
(2) cooling to 50 ℃, adding isocyanate, and reacting for 2 hours;
(3) adding a small amount of environment-friendly solvent and catalyst, and reacting for 0.5 hour;
(4) cooling to about 30 ℃, and removing bubbles by regulating and controlling the stirring rotating speed and the vacuum degree;
(5) measuring the viscosity at a constant temperature of 23 ℃;
(6) coating the coating on a coating device by scraping;
(7) aging for 7 days at constant temperature (23 + -2 deg.C) and constant humidity (relative humidity 50 + -10);
(8) cutting the coating film into dumbbell shapes by using a slicer;
(9) and testing the mechanical property of the adhesive film by using a universal testing machine.
The acid resistance, alkali resistance and heat aging resistance tests are carried out according to GB/T19250-2013.
As can be seen from tables 2 and 3, compared with the polyurethane waterproof coating prepared from the traditional polyether, the polyurethane waterproof coating prepared from the polyether polyol obtained by the invention has lower viscosity, and the mechanical property, acid resistance, alkali resistance and heat aging resistance of the coating film are more excellent.
TABLE 2 test of the Water-repellent paint Properties
TABLE 3 acid, alkali, thermal aging resistance test after film formation of the coating
Of course, the foregoing is only a preferred embodiment of the invention and should not be taken as limiting the scope of the embodiments of the invention. The present invention is not limited to the above examples, and equivalent changes and modifications made by those skilled in the art within the spirit and scope of the present invention should be construed as being included in the scope of the present invention.
Claims (8)
1. A preparation method of polyether polyol for high-performance waterproof paint is characterized by comprising the following steps: taking a mixture of a bifunctional compound and a trifunctional compound as an initiator, taking alkali metal or DMC as a catalyst, and carrying out polymerization reaction with alkylene oxide to obtain a polyether polyol crude polymer; then refining the crude polymer to obtain the polyether polyol for the high-performance waterproof coating;
the difunctional compound is one or more of bisphenol A, ethylene glycol, diethylene glycol, butanediol, diethylene glycol, propylene glycol or dipropylene glycol;
the tri-functional compound is one or more of trimethylolpropane, glycerol, triethanolamine or triethylene glycol.
2. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: during polymerization, the pressure is-0.1-0.4 MPa and the temperature is 80-180 ℃.
3. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: the alkylene oxide is one or a mixture of two of propylene oxide and ethylene oxide according to any proportion.
4. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: the mass ratio of the initiator to the alkylene oxide is 0.01-0.2: 1.
5. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: the alkali metal catalyst is potassium hydroxide, sodium hydroxide, cesium hydroxide, potassium methoxide or sodium methoxide.
6. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: the polymerization mode of the initiator and the alkylene oxide is one of the following modes:
the mode (1) is initiator + propylene oxide + ethylene oxide;
the mode (2) is that the initiator, the mixture of ethylene oxide and propylene oxide are added;
the mode (3) is initiator + ethylene oxide + propylene oxide + ethylene oxide;
the mode (4) is a mixture of an initiator + propylene oxide and ethylene oxide;
the mode (5) is a mixture of an initiator, ethylene oxide and propylene oxide;
the mode (6) is initiator + propylene oxide;
mode (7) is initiator + ethylene oxide;
the way (8) is to polymerize the initiator with a mixture of ethylene oxide and propylene oxide.
7. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: when the alkylene oxide is ethylene oxide, the mass consumption of the ethylene oxide is 0-100% of the mass of the final product.
8. The method for producing a polyether polyol for high-performance waterproof coating material according to claim 1, characterized in that: the refining treatment sequentially comprises neutralization, adsorption, crystallization and filtration.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110388487.5A CN113105617A (en) | 2021-04-12 | 2021-04-12 | Preparation method of polyether polyol for high-performance waterproof coating |
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| CN202110388487.5A CN113105617A (en) | 2021-04-12 | 2021-04-12 | Preparation method of polyether polyol for high-performance waterproof coating |
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| CN202110388487.5A Pending CN113105617A (en) | 2021-04-12 | 2021-04-12 | Preparation method of polyether polyol for high-performance waterproof coating |
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| CN115304761A (en) * | 2022-08-11 | 2022-11-08 | 山东一诺威新材料有限公司 | Polyester ether polyol for high-performance polyurethane waterproof coating and preparation method thereof |
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| CN115304761B (en) * | 2022-08-11 | 2023-12-12 | 山东一诺威新材料有限公司 | Polyester ether polyol for high-performance polyurethane waterproof coating and preparation method thereof |
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