CN113150671B - Non-ionic water-based polyurethane-based expansion type steel structure fireproof coating and preparation method thereof - Google Patents
Non-ionic water-based polyurethane-based expansion type steel structure fireproof coating and preparation method thereof Download PDFInfo
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- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention relates to the field of constructional steel structure coatings, and particularly discloses a non-ionic waterborne polyurethane-based intumescent steel structure fireproof coating and a preparation method thereof. Specifically, the non-ionic aqueous polyurethane emulsion and the triethanolamine acetate aqueous solution are prepared, and then the non-ionic aqueous polyurethane emulsion, the triethanolamine acetate aqueous solution and the thickening agent are mixed and dispersed according to a required proportion to prepare the non-ionic aqueous polyurethane-based intumescent steel structure fireproof coating. The fireproof coating has the advantages of high fireproof performance, long service life, good physical properties and high water resistance.
Description
Technical Field
The invention relates to the field of constructional steel structure coatings, in particular to a non-ionic waterborne polyurethane-based intumescent steel structure fireproof coating and a preparation method thereof.
Background
In recent years, steel materials have been favored in the construction industry, but steel materials have some inevitable drawbacks in fire protection as a construction material, and their mechanical properties are rapidly reduced by an increase in temperature. The steel structure usually loses the bearing capacity at the temperature of 450-650 ℃, and the fire resistance limit of the steel structure without protection is about 15 minutes.
The expansion type steel structure fireproof coating has a good decorative effect, slowly expands and foams to form a compact and hard fireproof heat-insulating layer when being subjected to fire, and the fireproof layer has strong fireproof impact property, so that the temperature rise of steel is delayed, and a steel member is effectively protected. Various light steel structures, net racks and the like are protected against fire by adopting the fireproof coating. Because the coating of the fireproof coating is thin, the using amount of the fireproof coating is greatly reduced compared with that of the non-expansion type steel structure fireproof coating, so that the total engineering cost is reduced, the steel structure is effectively protected from fire, and the fireproof effect is good.
The steel structure fireproof paint consists of matrix resin, catalyst, carbon forming agent and foaming agent. The fire-proof and heat-insulating principle of the ultra-thin or thin steel structure fire-proof coating coated on a steel structure is that a fire-proof coating layer expands and foams when being fired to form foam, and the foam layer not only isolates oxygen, but also has good heat-insulating property because of loose texture and can delay the speed of heat transferring to a protected substrate; according to the analysis of the physical and chemical principles, the process of the foam layer generated by the expansion and foaming of the coating presents endothermic reaction due to the expansion of the volume, the heat during combustion is also consumed, the temperature of the system is favorably reduced, and the fireproof coating produces obvious fireproof and heat insulation effects.
Disclosure of Invention
The invention provides a non-ionic water-based polyurethane-based expanded steel structure fireproof coating and a preparation method thereof, aiming at the problems, the prepared non-ionic water-based polyurethane-based expanded steel structure fireproof coating can play a good role in heat insulation when being used for a steel structure, and meanwhile, a coating film formed by the non-ionic water-based polyurethane-based expanded steel structure fireproof coating has high fire resistance, long service life and good physical properties.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a non-ionic water-based polyurethane-based intumescent fire-retardant coating for a steel structure, which comprises the following components in parts by weight: 10-40 parts of deionized water, 0.1-0.5 part of defoaming agent, 0.5-2 parts of dispersing agent, 0.1-0.5 part of pH value regulator, 5-15 parts of rutile titanium dioxide, 5-15 parts of pentaerythritol, 5-15 parts of melamine, 20-30 parts of ammonium polyphosphate, 0.5-5 parts of aerogel slurry, 15-40 parts of nonionic aqueous polyurethane emulsion, 1-10 parts of vinegar tertiary emulsion, 0.5-5 parts of triethanolamine acetate water solution and 0.3-1 part of thickening agent.
Further, the non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure specifically comprises the following components in parts by weight: 16-25 parts of deionized water, 0.2-0.4 part of defoaming agent, 0.5-1 part of dispersing agent, 0.2-0.4 part of pH value regulator, 6-10 parts of rutile titanium dioxide, 5-12 parts of pentaerythritol, 6-10 parts of melamine, 20-25 parts of ammonium polyphosphate, 0.5-2 parts of aerogel slurry, 20-35 parts of nonionic aqueous polyurethane emulsion, 3-6 parts of vinegar tertiary emulsion, 1-2 parts of triethanolamine acetate aqueous solution and 0.5-1 part of thickening agent.
The invention also provides a preparation method of the non-ionic water-based polyurethane-based intumescent fire retardant coating for the steel structure, which comprises the following steps:
step 1, mixing amino-terminated polytetrahydrofuran, isophorone diisocyanate, a nonionic diol hydrophilic chain extender and dibutyltin dilaurate and reacting;
step 2, adding a diethylenetriamine aqueous solution into the product obtained in the step 1, and stirring for reaction to obtain a non-ionic aqueous polyurethane emulsion;
step 3, slowly dropwise adding glacial acetic acid into a mixture of deionized water and triethanolamine at the temperature of 0-10 ℃ to react to obtain a triethanolamine acetate aqueous solution;
and 4, mixing and dispersing deionized water, a defoaming agent, a dispersing agent, a pH value regulator, rutile titanium dioxide, melamine, pentaerythritol, ammonium polyphosphate, aerogel slurry, the nonionic aqueous polyurethane emulsion obtained in the step 2, the acetate emulsion, the triethanolamine acetate aqueous solution obtained in the step 3 and a thickening agent to obtain the nonionic aqueous polyurethane-based intumescent steel structure fireproof coating.
Further, the molar ratio of isophorone diisocyanate to amino-terminated polytetrahydrofuran in the step 1 is 1-6: 1; the molar ratio of the nonionic diol hydrophilic chain extender to the isophorone diisocyanate is 0.05-0.60: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate was 1X 10 -4 ～1×10 -2 : 1; the concentration of the aqueous solution of the diethylenetriamine in the step 2 is 1 x 10 -4 ～1×10 -1 g/L; the molar ratio of the diethylenetriamine to the isophorone diisocyanate in the step 1 is 0.01-0.5: 1; the molar ratio of the triethanolamine to the glacial acetic acid in the step 3 is 1-1.5: 1; the ratio of the weight of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is (1-1.5): 1; step 4, deionized water, a defoaming agent, a dispersing agent, a pH value regulator, rutile titanium dioxide, melamine, pentaerythritol, ammonium polyphosphate, aerogel slurryThe mass ratio of the nonionic aqueous polyurethane emulsion obtained in the step 2, the acetic acid tertiary emulsion, the aqueous solution of triethanolamine acetate obtained in the step 3 and the thickening agent is 10-40: 0.1-0.5: 0.5-2: 0.1-0.5: 5-15: 5: 15: 5-15: 20-30: 0.5-5: 15-40: 1-10: 0.5-5: 0.3 to 1.
In the step 1, the reaction temperature is 50-90 ℃, and the reaction time is 3-6 h; stirring in the step 2 is 400-3000 r/min, and the reaction time is 0.5-1 h; the reaction temperature in the step 3 is normal temperature, and the reaction time is 0.5 h; and the dispersion condition of the step 4 is that the dispersion is carried out for 0.5-2.0 h at the rotating speed of 200-500 r/min.
In the step 1, the amino-terminated polytetrahydrofuran is at least one of polytetrahydrofuran with amino functionality of 2 and number average molecular weight of 888-3238, and both ends of the polytetrahydrofuran are blocked by amino; the nonionic diol hydrophilic chain extender is an ethoxy terminated polymeric diol having a hydroxyl functionality of 2 and a number average molecular weight of 1000; in the step 4, pentaerythritol is any one of monopentaerythritol or dipentaerythritol; the defoaming agent is a compound silicone defoaming agent; the dispersant is polycarboxylate dispersant; the pH value regulator is a water solution of reactive organosilicon; the ammonium polyphosphate is II type ammonium polyphosphate with the polymerization degree n of more than or equal to 1000 and the water solubility of less than or equal to 0.5g/100 ml; the aerogel slurry is prepared by uniformly dispersing hydrophobic nano silicon dioxide aerogel in water; the vinyl acetate-ethylene emulsion is vinyl acetate-ethylene aqueous copolymer emulsion; the thickening agent is polyurethane modified polyether associative thickening agent.
Furthermore, the molar ratio of the isophorone diisocyanate to the amino terminated polytetrahydrofuran in the step 1 is preferably 1-4.5: 1; the mole ratio of the nonionic diol hydrophilic chain extender to the isophorone diisocyanate is preferably 0.1-0.60: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate is preferably 1X 10 -3 ～1×10 -2 (ii) a The concentration of the aqueous solution of diethylenetriamine in the step 2 is preferably 1 x 10 -3 ～1×10 - 1 g/L; the mol ratio of the diethylenetriamine to the isophorone diisocyanate in the step 1 is preferably 0.01-0.3: 1; the above-mentionedThe preferable molar ratio of the triethanolamine to the glacial acetic acid in the step 3 is 1-1.2: 1; the ratio of the weight of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is preferably 1-1.2: 1; the mass ratio of the deionized water, the defoaming agent, the dispersing agent, the pH value regulator, the rutile titanium dioxide, the melamine, the pentaerythritol, the ammonium polyphosphate, the aerogel slurry, the nonionic aqueous polyurethane emulsion and the acetic tertiary emulsion obtained in the step 2, the triethanolamine acetate aqueous solution obtained in the step 3 and the thickening agent in the step 4 is preferably 16-25: 0.2-0.4: 0.5-1: 0.2-0.4: 6-10: 6: 10: 5-12: 20-25: 0.5-2: 20-35: 3-6: 1-2: 0.5 to 1.
In the step 4, the aerogel slurry is prepared by mixing aerogel with the solid content of 10% and the dry density of 40kg/m 3 And nano silicon dioxide aerogel slurry with the particle size of 20 mu m and the pore diameter of 20 nm.
Still further, the molar ratio of isophorone diisocyanate to amino terminated polytetrahydrofuran in the step 1 is more preferably 1-3: 1; the mol ratio of the nonionic diol hydrophilic chain extender to the isophorone diisocyanate is more preferably 0.1-0.4: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate is more preferably 1X 10 -3 ～5×10 -3 (ii) a The concentration of the aqueous solution of diethylenetriamine in the step 2 is more preferably 1 × 10 -3 ～5×10 -2 g/L; the molar ratio of the diethylenetriamine to the isophorone diisocyanate in the step 1 is more preferably 0.01-0.2: 1; the molar ratio of triethanolamine to glacial acetic acid in the step 3 is more preferably 1-1.05: 1; the ratio of the weight of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is more preferably 1-1.1: 1.
compared with the prior art, the invention has the following advantages:
1. the non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure, prepared by the invention, has higher fire resistance.
2. The non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure, which is prepared by the invention, has better physical properties.
3. The non-ionic waterborne polyurethane-based intumescent fire retardant coating for the steel structure, prepared by the invention, has longer service life.
4. The non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure, which is prepared by the invention, has better water resistance.
Detailed Description
The present invention will be described in more detail with reference to specific examples. It should be noted that the description and examples are intended to facilitate the understanding of the invention, and are not intended to limit the invention.
Examples
In the present invention, unless otherwise indicated, all reagents used were commercially available products and were used without further purification treatment. Further, "%" mentioned is "% by weight", and "parts" mentioned is "parts by weight".
In the example, the amino-terminated polytetrahydrofuran is one or more of XYlink P-1000 and XYlink P-650 manufactured by Jiangsu Xiangyuan chemical Co., Ltd; the nonionic diol hydrophilic chain extender is nonionic diol Ymer N120 provided by Customos, Sweden; the antifoaming agents are SN-DEFOAMER 327 and SN-DEFOAMER 328 supplied by Santa Clauru, Japan; the dispersants are SN-DISPERSANT 5027 and SN-DISPERSANT 5029 provided by Santa Nordisk Co., Ltd, Japan; the pH regulator is supplied by Wake, Germany
A BS 168; rutile titanium dioxide includes rutile titanium dioxide R902 and R105, available from DuPont, USA; the ammonium polyphosphate is Exolit AP422 and Exolit AP 428 provided by Germany Clariant, or JLS-APP provided by Hangzhou Jieisi flame retardant chemical company; the aerogel slurry is an aerogel slurry AG-Paste provided by Shanxi Yang New materials Co., Ltd; the emulsion of vinegar-tert is emulsion of vinegar-tert EZ 3112 and EZ 3066 supplied by Wacker Germany; the thickeners were SN-THICKENER 612 and SN-THICKENER 623N supplied by Santa Nuo Co., Ltd, Japan.
Test method
In the following examples, the properties of the nonionic aqueous polyurethane-based intumescent steel structure fire retardant coatings obtained in examples 1 to 5 were measured and the measurement results are shown in Table 1. Specific measurement methods for relevant properties are described in GB/T14907-2018 Steel Structure fire retardant coatings.
Example 1
Step 1, adding 100 g of amino-terminated polytetrahydrofuran XYlink P-1000 with functionality of 2 and molecular weight of 1238, 40 g of isophorone diisocyanate, 35 g of nonionic diol Ymer N120 and 0.05 g of dibutyltin dilaurate into a three-neck flask provided with a stirrer, a thermometer and a reflux device, mixing, heating to 85 ℃, reacting for 4.0 hours, cooling the reaction system to 40 ℃, adding an aqueous solution formed by 2.0 g of diethylenetriamine and 268 g of deionized water into the mixture, and dispersing in a dispersion machine at the rotating speed of 1000 revolutions per minute for 1.0 hour to obtain the nonionic aqueous polyurethane emulsion, wherein the solid content is 40.0%.
Step 2, adding 60 g of glacial acetic acid and 209 g of deionized water into a three-neck flask provided with a stirrer, a thermometer and a reflux device, slowly dripping 149 g of triethanolamine into the flask under the condition of water bath cooling at 10 ℃, and stirring the mixture for 0.5 hour at normal temperature after dripping to obtain an aqueous solution of triethanolamine acetate
Step 3, 20 parts by weight of deionized water, 0.2 parts by weight of SN-DEFAOAMER 327 antifoaming agent of Santa Clara, 0.5 parts by weight of SN-DISPERSANT 5027 dispersing agent of Santa Clara, 0.3 parts by weight of
BS 168PH regulator, 8.0 weight parts of American Dupont R902 rutile type titanium dioxide, 6.0 weight parts of melamine, 12.0 weight parts of monopentaerythritol, 20 weight parts of Exolite AP 428 ammonium polyphosphate, 1.0 weight parts of AG-Pase aerogel slurry, 26 weight parts of the nonionic aqueous polyurethane emulsion obtained in step 1, 4.0 weight parts of German Wake EZ 3112 vinegar tertiary emulsion, 1.0 weight parts of the aqueous solution of triethanolamine acetate obtained in step 2 and 1.0 weight parts of SN-THICKENER 612 thickener of Japan Santa Nuo-Proco, dispersing for 1.0 hour at the rotating speed of 500R/min to obtain the nonionic aqueous polyurethaneA fire-proof paint for expansion steel structure.
Example 2
Step 1, adding 100 g of amino-terminated polytetrahydrofuran XYlink P-650 with functionality of 2 and molecular weight of 888, 40 g of isophorone diisocyanate, 40 g of nonionic diol YMer N120 and 0.03 g of dibutyltin dilaurate into a three-neck flask provided with a stirrer, a thermometer and a reflux device, mixing, heating to 75 ℃ for reaction for 6.0 hours, cooling a reaction system to 40 ℃, adding an aqueous solution formed by 1.0 g of diethylenetriamine and 336 g of deionized water into the mixture, and dispersing in a dispersion machine at the rotating speed of 1000 revolutions per minute for 1.0 hour to obtain the nonionic aqueous polyurethane emulsion, wherein the solid content is 35.0%.
And 2, adding 60 g of glacial acetic acid and 216 g of deionized water into a three-neck flask provided with a stirrer, a thermometer and a reflux device, slowly dripping 156 g of triethanolamine under the condition of water bath cooling at 20 ℃, and stirring at normal temperature for 0.5 hour after dripping to obtain the aqueous solution of the triethanolamine acetate.
20.6 parts by weight of deionized water, 0.3 parts by weight of SN-DEFAOAMER 328 antifoaming agent of Santa Clara, 0.7 parts by weight of SN-DISPERSANT 5027 dispersing agent of Santa Clara, 0.2 parts by weight of
BS 168PH value regulator, 6.0 weight parts of American DuPont R902 rutile type titanium dioxide, 8.0 weight parts of melamine, 8.0 weight parts of monopentaerythritol, 20.0 weight parts of Exolite AP 428 ammonium polyphosphate, 0.5 weight parts of AG-Pase aerogel slurry, 30.0 weight parts of the nonionic aqueous polyurethane emulsion obtained in the step 1, 3.0 weight parts of German Wake EZ 3112 vinegar tertiary emulsion, 2.0 weight parts of the aqueous solution of triethanolamine acetate obtained in the step 2 and 0.7 weight parts of Japan Senno-Proco SN-THICKENER 612 thickener are mixed and dispersed for 2.0 hours at the rotating speed of 500R/min to obtain the nonionic aqueous polyurethane-based intumescent fire-resistant coating for the steel structure.
Example 3
Step 1, 50 g of amino terminated polytetrahydrofuran XYlink P-1000 having a functionality of 2 and a molecular weight of 1238, 40 g of amino terminated polyether XYlink P-650 having a functionality of 2 and a molecular weight of 888, 45 g of isophorone diisocyanate, 35 g of nonionic diol YMR N120, and 0.04 g of dibutyltin dilaurate were mixed and heated to 80 ℃ for reaction for 5.0 hours in a three-necked flask equipped with a stirrer, a thermometer, and a reflux device, and then the reaction system was cooled to 40 ℃ and an aqueous solution of 2.0 g of diethylenetriamine and 210 g of deionized water was added to the mixture for emulsification and chain extension for 10 minutes. And then dispersing the mixture in a dispersion machine at the rotating speed of 1000 revolutions per minute for 1.0 hour to obtain the non-ionic water-based polyurethane emulsion, wherein the solid content is 45.0 percent.
And 2, adding 60 g of glacial acetic acid and 238 g of deionized water into a three-neck flask provided with a stirrer, a thermometer and a reflux device, slowly dripping 156 g of triethanolamine under the condition of water bath cooling at 20 ℃, and stirring at normal temperature for 0.5 hour after dripping to obtain the aqueous solution of the triethanolamine acetate.
Step 3, mixing 23 parts by weight of deionized water, 0.2 parts by weight of SN-DEFAOAMER 327 antifoaming agent of Nothopaceae Japan, 0.7 parts by weight of SN-DISPERSANT 5027 dispersing agent of Nothopaceae Japan, and 0.3 parts by weight of dispersant
BS 168PH value regulator, 10.0 weight parts of American Dupont R902 rutile type titanium dioxide, 9.0 weight parts of melamine, 8.0 weight parts of monopentaerythritol, 20.0 weight parts of Exolite AP422 ammonium polyphosphate, 1.5 weight parts of AG-Pase aerogel slurry, 20 weight parts of the nonionic aqueous polyurethane emulsion obtained in the step 1, 5 weight parts of German Wake EZ 3112 acetate-tert-emulsion, 1 weight part of the aqueous solution of triethanolamine acetate obtained in the step 2 and 1.3 weight parts of SN-THICKENER 623N thickener of the Nipponpoko family, and dispersing for 0.5 hours at the rotating speed of 500R/min to obtain the nonionic aqueous polyurethane-based intumescent fire-retardant coating for the steel structure.
Example 4
Step 1, 100 g of amino terminated polytetrahydrofuran XYlink P-1000 with the functionality of 2 and the molecular weight of 1238, 45 g of isophorone diisocyanate, 30 g of nonionic diol YMer N120 and 0.08 g of dibutyltin dilaurate are added into a three-neck flask provided with a stirrer, a thermometer and a reflux device, mixed and heated to 90 ℃ for reaction for 6.0 hours, then the reaction system is cooled to 40 ℃, and an aqueous solution formed by 2.0 g of diethylenetriamine and 332 g of deionized water is added into the mixture for emulsification and chain extension for 10 minutes. And then, dispersing the mixture in a dispersion machine at the rotating speed of 1000 rpm for 1.0 hour to obtain the nonionic aqueous polyurethane emulsion, wherein the solid content is 35.0 percent.
And 2, adding 60 g of glacial acetic acid and 229 g of deionized water into a three-neck flask provided with a stirrer, a thermometer and a reflux device, slowly dripping 149 g of triethanolamine under the condition of water bath cooling at 20 ℃, and stirring at normal temperature for 0.5 hour after dripping to obtain the aqueous solution of triethanolamine acetate.
Step 3, 18 parts by weight of deionized water, 0.4 part by weight of SN-DEFAOAMER 328 antifoaming agent of Nothopaceae Japan, 1.0 part by weight of SN-DISPERSANT 5029 dispersant of Nothopaceae Japan, and 0.4 part by weight of dispersant
BS 168PH value regulator, 5.0 weight parts of American DuPont R105 rutile type titanium dioxide, 10.0 weight parts of melamine, 10.0 weight parts of dipentaerythritol, 20 weight parts of Exolite AP422 ammonium polyphosphate, 2.0 weight parts of AG-Pase aerogel slurry, 25 weight parts of the nonionic aqueous polyurethane emulsion obtained in the step 1, 6.0 weight parts of German Wake EZ 3066 vinegar tertiary emulsion, 1.0 weight part of the aqueous solution of triethanolamine acetate obtained in the step 2 and 0.7 weight part of SN-THICKENER 623N thickener of Japan Santa Nuo family are mixed and dispersed for 1.5 hours at the rotating speed of 500R/min to obtain the nonionic aqueous polyurethane-based intumescent fire-retardant coating for the steel structure.
Example 5
Step 1, 100 g of an amino-terminated polyether XYlink P-650 having a functionality of 2 and a molecular weight of 888, 60 g of isophorone diisocyanate, 35 g of a nonionic diol Ymer N120, and 0.02 g of dibutyltin dilaurate were added to a three-necked flask equipped with a stirrer, a thermometer, and a reflux device, mixed and heated to 85 ℃ for reaction for 5.0 hours, then the reaction system was cooled to 40 ℃, and an aqueous solution of 4.0 g of diethylenetriamine and 460 g of deionized water was added to the mixture for emulsification and chain extension for 10 minutes. Then, the mixture was dispersed in a dispersion machine at a rotation speed of 1000 rpm for 1.0 hour to obtain a nonionic aqueous polyurethane emulsion having a solid content of 30.0%.
And 2, adding 60 g of glacial acetic acid and 218 g of deionized water into a three-neck flask provided with a stirrer, a thermometer and a reflux device, slowly dripping 152 g of triethanolamine under the condition of water bath cooling at 20 ℃, and stirring at normal temperature for 0.5 hour after dripping to obtain the aqueous solution of the triethanolamine acetate.
Step 3, 25 parts by weight of deionized water, 0.3 parts by weight of SN-DEFAOAMER 327 antifoaming agent of Santa Clara, 0.5 parts by weight of SN-DISPERSANT 5029 dispersing agent of Santa Clara, 0.2 parts by weight of
BS 168PH value regulator, 10.0 weight parts of American Dupont R105 rutile type titanium dioxide, 8.0 weight parts of melamine, 4.0 weight parts of monopentaerythritol, 10 weight parts of JLS-APP ammonium polyphosphate, 2.0 weight parts of AG-Pase aerogel slurry, 35.0 weight parts of nonionic aqueous polyurethane emulsion obtained in step 1, 3.0 weight parts of German Wake EZ 3066 vinegar tertiary emulsion, 1.5 weight parts of triethanolamine acetate aqueous solution obtained in step 2, 0.5 weight parts of SN-THICKENER 623N thickener of Nippon Santo Puke family SN-89623N, dispersing for 1.5 hours at the rotating speed of 500R/min to obtain the nonionic aqueous polyurethane-based intumescent fire-retardant coating material for steel structure
Performance testing
Table 1 shows the results of the performance tests of the non-ionic aqueous polyurethane-based intumescent fire-retardant coating for steel structures obtained in examples 1-5 of the present invention. The technical requirement refers to the technical standard which the intumescent steel structure fireproof coating needs to meet according to the related test method.
TABLE 1 Performance test results of non-ionic waterborne polyurethane-based intumescent fire-retardant coating for steel structure
The above examples 1-5 confirm that the non-ionic aqueous polyurethane-based intumescent fire-retardant coating for steel structures prepared by the method according to the invention can obtain an intumescent fire-retardant coating film for steel structures with high fire resistance, long service life and good physical properties.
The embodiment of the present invention is described only for the preferred embodiment of the present invention, and not for the purpose of limiting the spirit and scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the design concept of the present invention shall fall within the protection scope of the present invention.
Claims (9)
1. A non-ionic water-based polyurethane-based intumescent fire-retardant coating for a steel structure is characterized by comprising the following components in parts by weight: 10-40 parts of deionized water, 0.1-0.5 part of defoaming agent, 0.5-2 parts of dispersing agent, 0.1-0.5 part of pH value regulator, 5-15 parts of rutile titanium dioxide, 5-15 parts of pentaerythritol, 5-15 parts of melamine, 20-30 parts of ammonium polyphosphate, 0.5-5 parts of aerogel slurry, 15-40 parts of nonionic aqueous polyurethane emulsion, 1-10 parts of vinegar tertiary emulsion, 0.5-5 parts of triethanolamine acetate aqueous solution and 0.3-1 part of thickening agent;
the nonionic waterborne polyurethane emulsion is prepared by the following method:
step 1, mixing amino-terminated polytetrahydrofuran, isophorone diisocyanate, a nonionic diol hydrophilic chain extender and dibutyltin dilaurate and reacting;
step 2, adding a diethylenetriamine aqueous solution into the product obtained in the step 1, and stirring for reaction to obtain a non-ionic aqueous polyurethane emulsion;
the amino-terminated polytetrahydrofuran is at least one of polytetrahydrofuran with amino functionality of 2 and number average molecular weight of 888-3238, and both ends of the polytetrahydrofuran are terminated by amino; the nonionic glycol hydrophilic chain extender is an ethoxy terminated polymeric diol having a hydroxyl functionality of 2 and a number average molecular weight of 1000.
2. The non-ionic water-based polyurethane-based intumescent fire-retardant coating for steel structures according to claim 1, which is characterized by comprising the following components in parts by weight: 16-25 parts of deionized water, 0.2-0.4 part of defoaming agent, 0.5-1 part of dispersing agent, 0.2-0.4 part of pH value regulator, 6-10 parts of rutile titanium dioxide, 5-12 parts of pentaerythritol, 6-10 parts of melamine, 20-25 parts of ammonium polyphosphate, 0.5-2 parts of aerogel slurry, 20-35 parts of nonionic aqueous polyurethane emulsion, 3-6 parts of vinegar tertiary emulsion, 1-2 parts of triethanolamine acetate aqueous solution and 0.5-1 part of thickening agent.
3. A method for preparing the non-ionic aqueous polyurethane-based intumescent fire retardant coating for steel structures according to claim 1 or 2, characterized by comprising the following steps:
step 1, mixing amino-terminated polytetrahydrofuran, isophorone diisocyanate, a nonionic diol hydrophilic chain extender and dibutyltin dilaurate and reacting;
step 2, adding a diethylenetriamine aqueous solution into the product obtained in the step 1, and stirring for reaction to obtain a non-ionic aqueous polyurethane emulsion;
step 3, slowly dropwise adding glacial acetic acid into a mixture of deionized water and triethanolamine at the temperature of 0-10 ℃ for reaction to obtain an aqueous solution of triethanolamine acetate;
and 4, mixing and dispersing deionized water, a defoaming agent, a dispersing agent, a pH value regulator, rutile titanium dioxide, melamine, pentaerythritol, ammonium polyphosphate, aerogel slurry, the nonionic aqueous polyurethane emulsion obtained in the step 2, the acetic acid tertiary emulsion, the aqueous solution of triethanolamine acetate obtained in the step 3 and a thickening agent to obtain the nonionic aqueous polyurethane-based intumescent steel structure fireproof coating.
4. The method for preparing the non-ionic aqueous polyurethane-based intumescent fire-retardant coating for the steel structure according to claim 3, wherein the method is characterized in thatThe method comprises the following steps: in the step 1, the molar ratio of isophorone diisocyanate to amino-terminated polytetrahydrofuran is 1-6: 1; the molar ratio of the nonionic diol hydrophilic chain extender to the isophorone diisocyanate is 0.05-0.60: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate was 1X 10 -4 ~1×10 -2 : 1; the concentration of the aqueous solution of the diethylenetriamine in the step 2 is 1 x 10 -4 ~1×10 -1 g/L; the molar ratio of diethylenetriamine to isophorone diisocyanate in the step 1 is 0.01-0.5: 1; the molar ratio of the triethanolamine to the glacial acetic acid in the step 3 is 1-1.5: 1; the ratio of the weight of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is 1-1.5: 1; in the step 4, the mass ratio of deionized water, a defoaming agent, a dispersing agent, a pH value regulator, rutile titanium dioxide, melamine, pentaerythritol, ammonium polyphosphate, aerogel slurry, the nonionic aqueous polyurethane emulsion and the acetic tertiary emulsion obtained in the step 2, the aqueous solution of triethanolamine acetate obtained in the step 3 and a thickening agent is 10-40: 0.1-0.5: 0.5-2: 0.1-0.5: 5-15: 5-15: 5-15: 20-30: 0.5-5: 15-40: 1-10: 0.5-5: 0.3 to 1.
5. The preparation method of the non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure according to claim 4, wherein the preparation method comprises the following steps: the mole ratio of the isophorone diisocyanate to the amino-terminated polytetrahydrofuran is preferably 1-4.5: 1; the mole ratio of the nonionic diol hydrophilic chain extender to isophorone diisocyanate is preferably 0.1-0.60: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate is preferably 1X 10 -3 ~1×10 -2 (ii) a The concentration of the aqueous solution of diethylenetriamine is preferably 1 x 10 -3 ~1×10 -1 g/L; the mol ratio of the diethylenetriamine to the isophorone diisocyanate in the step 1 is preferably 0.01-0.3: 1; the preferable molar ratio of the triethanolamine to the glacial acetic acid is 1-1.2: 1; the weight ratio of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is preferably 1-1.2: 1; deionization in said step 4The mass ratio of water, a defoaming agent, a dispersing agent, a pH value regulator, rutile titanium dioxide, melamine, pentaerythritol, ammonium polyphosphate, aerogel slurry, the nonionic aqueous polyurethane emulsion obtained in the step 2, the acetic tertiary emulsion, the aqueous solution of triethanolamine acetate obtained in the step 3 and a thickening agent is preferably 16-25: 0.2-0.4: 0.5-1: 0.2-0.4: 6-10: 6-10: 5-12: 20-25: 0.5-2: 20-35: 3-6: 1-2: 0.5 to 1.
6. The method for preparing the non-ionic water-based polyurethane-based intumescent fire retardant coating for the steel structure according to claim 5 is characterized in that: the molar ratio of the isophorone diisocyanate to the amino-terminated polytetrahydrofuran is more preferably 1-3: 1; the molar ratio of the nonionic diol hydrophilic chain extender to isophorone diisocyanate is more preferably 0.1-0.4: 1; the ratio of the weight of dibutyltin dilaurate to the sum of the weights of the amino-terminated polytetrahydrofuran and isophorone diisocyanate is more preferably 1X 10 -3 -5×10 -3 (ii) a The concentration of the aqueous solution of diethylenetriamine is more preferably 1X 10 -3 -5×10 -2 g/L; the molar ratio of the diethylenetriamine to the isophorone diisocyanate in the step 1 is more preferably 0.01-0.2: 1; the molar ratio of triethanolamine to glacial acetic acid is more preferably 1-1.05: 1; the ratio of the weight of the deionized water to the sum of the weights of the triethanolamine and the glacial acetic acid is more preferably 1-1.1: 1.
7. the method for preparing the non-ionic water-based polyurethane-based intumescent fire retardant coating for the steel structure according to claim 3 is characterized in that: in the step 1, the reaction temperature is 50-90 ℃, and the reaction time is 3-6 h; stirring in the step 2 is 400-3000 r/min, and the reaction time is 0.5-1 h; the reaction temperature in the step 3 is normal temperature, and the reaction time is 0.5 h; and the dispersion condition of the step 4 is that the dispersion is carried out for 0.5-2.0 h at the rotating speed of 200-500 r/min.
8. The preparation method of the non-ionic water-based polyurethane-based intumescent fire-retardant coating for the steel structure according to claim 3, characterized by comprising the following steps: in the step 4, pentaerythritol is any one of monopentaerythritol or dipentaerythritol; the defoaming agent is a compound silicone defoaming agent; the dispersant is polycarboxylate dispersant; the pH value regulator is a water solution of reactive organosilicon; the ammonium polyphosphate is II-type ammonium polyphosphate with the polymerization degree n being more than or equal to 1000 and the water solubility being less than or equal to 0.5g/100 mL; the aerogel slurry is prepared by uniformly dispersing hydrophobic nano silicon dioxide aerogel in water; the vinyl acetate-ethylene emulsion is vinyl acetate-ethylene aqueous copolymer emulsion; the thickening agent is polyurethane modified polyether associative thickening agent.
9. The preparation method of the non-ionic water-based polyurethane-based intumescent fire retardant coating for steel structures according to claim 8, characterized by comprising the following steps: in the step 4, the aerogel slurry is prepared by mixing aerogel with the solid content of 10% and the dry density of 40kg/m 3 And nano silicon dioxide aerogel slurry with the particle size of 20 mu m and the pore diameter of 20 nm.
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