CN117510963A - Polyether polyol microemulsion, preparation method and application thereof - Google Patents
Polyether polyol microemulsion, preparation method and application thereof Download PDFInfo
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- CN117510963A CN117510963A CN202311539001.9A CN202311539001A CN117510963A CN 117510963 A CN117510963 A CN 117510963A CN 202311539001 A CN202311539001 A CN 202311539001A CN 117510963 A CN117510963 A CN 117510963A
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- polyether polyol
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- 239000004721 Polyphenylene oxide Substances 0.000 title claims abstract description 108
- 229920000570 polyether Polymers 0.000 title claims abstract description 108
- 150000003077 polyols Chemical class 0.000 title claims abstract description 108
- 229920005862 polyol Polymers 0.000 title claims abstract description 106
- 239000004530 micro-emulsion Substances 0.000 title claims abstract description 100
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000011737 fluorine Substances 0.000 claims abstract description 77
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 77
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 76
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 45
- 239000004094 surface-active agent Substances 0.000 claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000839 emulsion Substances 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 230000001804 emulsifying effect Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 45
- -1 perfluoro-2-methyl-3, 6-dioxaheptanoic acid Chemical compound 0.000 claims description 31
- RGSFGYAAUTVSQA-UHFFFAOYSA-N Cyclopentane Chemical compound C1CCCC1 RGSFGYAAUTVSQA-UHFFFAOYSA-N 0.000 claims description 19
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 claims description 18
- AQYSYJUIMQTRMV-UHFFFAOYSA-N hypofluorous acid Chemical compound FO AQYSYJUIMQTRMV-UHFFFAOYSA-N 0.000 claims description 11
- XGWSFQONMCFRNK-UHFFFAOYSA-N 2,3,4,5-tetrafluoro-6-(1,1,2,2,3,3,4,4,5,5,6,6,7,7,8,8,9,9,9-nonadecafluorononyl)benzenesulfonic acid Chemical compound C1(=C(C(=C(C(=C1S(=O)(=O)O)F)F)F)F)C(C(C(C(C(C(C(C(C(F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F)(F)F XGWSFQONMCFRNK-UHFFFAOYSA-N 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 10
- DMEGYFMYUHOHGS-UHFFFAOYSA-N heptamethylene Natural products C1CCCCCC1 DMEGYFMYUHOHGS-UHFFFAOYSA-N 0.000 claims description 10
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- 229920005830 Polyurethane Foam Polymers 0.000 claims description 7
- 239000011496 polyurethane foam Substances 0.000 claims description 7
- COWKRCCNQSQUGJ-UHFFFAOYSA-N 1,1,2,2,3-pentafluoropropan-1-ol Chemical compound OC(F)(F)C(F)(F)CF COWKRCCNQSQUGJ-UHFFFAOYSA-N 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- SAPOZTRFWJZUFT-UHFFFAOYSA-N 1,1,1,2,3,4,5,5,5-nonafluoro-4-(trifluoromethyl)pent-2-ene Chemical compound FC(F)(F)C(F)=C(F)C(F)(C(F)(F)F)C(F)(F)F SAPOZTRFWJZUFT-UHFFFAOYSA-N 0.000 claims description 5
- FFTOUVYEKNGDCM-OWOJBTEDSA-N (e)-1,3,3-trifluoroprop-1-ene Chemical compound F\C=C\C(F)F FFTOUVYEKNGDCM-OWOJBTEDSA-N 0.000 claims description 3
- YIHRGKXNJGKSOT-UHFFFAOYSA-N 1,1,2,2,3,3-hexafluorobutan-1-ol Chemical compound CC(F)(F)C(F)(F)C(O)(F)F YIHRGKXNJGKSOT-UHFFFAOYSA-N 0.000 claims description 3
- CSUFEOXMCRPQBB-UHFFFAOYSA-N 1,1,2,2-tetrafluoropropan-1-ol Chemical compound CC(F)(F)C(O)(F)F CSUFEOXMCRPQBB-UHFFFAOYSA-N 0.000 claims description 3
- VUYQBMXVCZBVHP-UHFFFAOYSA-N 1,1-difluoroethanol Chemical compound CC(O)(F)F VUYQBMXVCZBVHP-UHFFFAOYSA-N 0.000 claims description 3
- CSEBNABAWMZWIF-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-(heptafluoropropoxy)propanoic acid Chemical compound OC(=O)C(F)(C(F)(F)F)OC(F)(F)C(F)(F)C(F)(F)F CSEBNABAWMZWIF-UHFFFAOYSA-N 0.000 claims description 3
- RHQDFWAXVIIEBN-UHFFFAOYSA-N Trifluoroethanol Chemical compound OCC(F)(F)F RHQDFWAXVIIEBN-UHFFFAOYSA-N 0.000 claims description 3
- KQNSPSCVNXCGHK-UHFFFAOYSA-N [3-(4-tert-butylphenoxy)phenyl]methanamine Chemical compound C1=CC(C(C)(C)C)=CC=C1OC1=CC=CC(CN)=C1 KQNSPSCVNXCGHK-UHFFFAOYSA-N 0.000 claims description 3
- PGFXOWRDDHCDTE-UHFFFAOYSA-N hexafluoropropylene oxide Chemical class FC(F)(F)C1(F)OC1(F)F PGFXOWRDDHCDTE-UHFFFAOYSA-N 0.000 claims description 3
- BYEAHWXPCBROCE-UHFFFAOYSA-N 1,1,1,3,3,3-hexafluoropropan-2-ol Chemical compound FC(F)(F)C(O)C(F)(F)F BYEAHWXPCBROCE-UHFFFAOYSA-N 0.000 claims description 2
- KUGBQWBWWNPMIT-UHFFFAOYSA-N 1,1,2,2,3,3,4,4-octafluoropentan-1-ol Chemical compound CC(F)(F)C(F)(F)C(F)(F)C(O)(F)F KUGBQWBWWNPMIT-UHFFFAOYSA-N 0.000 claims description 2
- NPNPZTNLOVBDOC-UHFFFAOYSA-N 1,1-difluoroethane Chemical compound CC(F)F NPNPZTNLOVBDOC-UHFFFAOYSA-N 0.000 claims 1
- 229940051271 1,1-difluoroethane Drugs 0.000 claims 1
- JEDHLIXWSMGAEZ-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-(1,1,2,2,3,3,4,4,5,5,5-undecafluoropentoxy)propanoic acid Chemical compound OC(=O)C(F)(C(F)(F)F)OC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F JEDHLIXWSMGAEZ-UHFFFAOYSA-N 0.000 claims 1
- 238000005187 foaming Methods 0.000 abstract description 13
- 238000002156 mixing Methods 0.000 abstract description 3
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000013329 compounding Methods 0.000 description 6
- 239000004215 Carbon black (E152) Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 229920002545 silicone oil Polymers 0.000 description 5
- 238000004945 emulsification Methods 0.000 description 4
- 239000012948 isocyanate Substances 0.000 description 4
- 150000002513 isocyanates Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- GGDYAKVUZMZKRV-UHFFFAOYSA-N 2-fluoroethanol Chemical compound OCCF GGDYAKVUZMZKRV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 239000003995 emulsifying agent Substances 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 230000000149 penetrating effect Effects 0.000 description 2
- 238000013112 stability test Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LDTMPQQAWUMPKS-OWOJBTEDSA-N (e)-1-chloro-3,3,3-trifluoroprop-1-ene Chemical compound FC(F)(F)\C=C\Cl LDTMPQQAWUMPKS-OWOJBTEDSA-N 0.000 description 1
- FRCHKSNAZZFGCA-UHFFFAOYSA-N 1,1-dichloro-1-fluoroethane Chemical compound CC(F)(Cl)Cl FRCHKSNAZZFGCA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- OWCNWICUDXNCTI-UHFFFAOYSA-N azanium;2,2,3,3,4,4,5,5,6,6,6-undecafluorohexanoate Chemical compound N.OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F OWCNWICUDXNCTI-UHFFFAOYSA-N 0.000 description 1
- RJWVKMAIYPNUSL-UHFFFAOYSA-N azanium;2,3,3,3-tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)propanoate Chemical compound [NH4+].[O-]C(=O)C(F)(C(F)(F)F)OC(F)(F)C(F)(F)C(F)(F)F RJWVKMAIYPNUSL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000005337 ground glass Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- MSSNHSVIGIHOJA-UHFFFAOYSA-N pentafluoropropane Chemical compound FC(F)CC(F)(F)F MSSNHSVIGIHOJA-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- BKXMWPWFFZIYID-UHFFFAOYSA-M sodium;2,3,3,3-tetrafluoro-2-(1,1,2,2,3,3,3-heptafluoropropoxy)propanoate Chemical compound [Na+].[O-]C(=O)C(F)(C(F)(F)F)OC(F)(F)C(F)(F)C(F)(F)F BKXMWPWFFZIYID-UHFFFAOYSA-M 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Abstract
The application relates to the field of foaming microemulsion, and particularly discloses a polyether polyol microemulsion, a preparation method and application thereof. The microemulsion is prepared from the following raw materials: polyether polyol, fluorine-containing hydrocarbon compound, pentane and emulsifying solution; the emulsifying solution consists of a fluorine-containing surfactant, fluocinol and water, wherein the weight ratio of the fluorine-containing surfactant to the fluocinol to the water is 0.01-0.1:0-0.01:100; the preparation method comprises the following steps: firstly preparing an emulsion solution, then premixing polyether polyol and a fluorine-containing hydrocarbon compound, and finally mixing to prepare the microemulsion. It has the advantage of being uniform and stable.
Description
Technical Field
The application relates to the technical field of foaming microemulsions, in particular to a polyether polyol microemulsion, a preparation method and application thereof.
Background
The common foaming system is generally formed by mixing white materials (polyether polyol system) and black materials (isocyanate system) in a certain proportion, wherein different types of foaming agents are used, and the common foaming agents are monofluorodichloroethane (HFC-141 b), and the foaming agents are gradually eliminated due to environmental protection; in addition, there are 1.1.1.3.3-pentafluoropropane (HFC-245 fa) systems, 1.1.1.3.3-pentafluorobutane (HFC-365) systems and pentane systems. If HFC-245fa or HFC365 systems are used alone, the overall cost is high and it is difficult to achieve the level of HFC-141b systems used in polyurethane foam systems. Thus, pentane + fluoro nucleator systems are commonly employed in the european union and asian countries. Wherein the nucleating agent is a fluorine-containing hydrocarbon compound such as (trans) -1-chloro-3.3.3-trifluoropropene (LBA), perfluoro-4-methyl-2-pentene, PF-5056 or the like. Because the fluorine-containing hydrocarbon compound has a large number of F-C bonds, the problem that the polyether polyol and a pentane foaming system are not mutually dissolved exists, so that polyurethane foaming is uneven, the fluidity is poor and the like, the comprehensive cost is still high, the problem of mutual dissolution of the polyether polyol white material system and pentane (cyclopentane, n-pentane, isopentane or a mixed system) +fluorine-containing nucleating agent is solved, and it is very important to form uniform and stable microemulsion. It is difficult to obtain a stable polyurethane foaming emulsion system by using a traditional hydrocarbon surfactant or silicone oil surfactant as an emulsifier. Therefore, the simple, efficient and stable polyurethane foaming microemulsion system and the preparation method thereof are found to have important significance for preparing the polyurethane hard foam with good heat preservation performance and higher cost performance.
Disclosure of Invention
In order to obtain a uniform and stable polyether polyol microemulsion, a foam material with good heat insulation performance and higher cost performance can be prepared, and the application provides a polyether polyol microemulsion, a preparation method and application.
In a first aspect, the present application provides a polyether polyol microemulsion, which adopts the following technical scheme:
a polyether polyol microemulsion is prepared from the following raw materials: polyether polyol, fluorine-containing hydrocarbon compound, pentane and emulsifying solution; the emulsified solution consists of a fluorine-containing surfactant, fluocinol and water, wherein the weight ratio of the fluorine-containing surfactant to the fluocinol to the water is 0.01-0.1:0-0.01:100.
By adopting the technical scheme, the fluorine-containing hydrocarbon compound has low surface tension, so that the interfacial tension can be reduced, and the permeability of the microemulsion can be improved; the polyether polyol has better water solubility and temperature resistance, and can improve the stability of the microemulsion; pentane has lower viscosity and better solubility, and is helpful for improving the fluidity of the microemulsion; the microemulsion is prepared by compounding polyether polyol, fluorine-containing hydrocarbon compound and pentane, firstly, the stability and the temperature resistance of the microemulsion can be improved by compounding the polyether polyol with the pentane, and the fluorine-containing hydrocarbon compound and the polyether polyol have the effect of further reducing the surface tension, so that the wetting and the penetrating capacity of the microemulsion can be improved; the emulsification solution prepared by adding a small amount of fluorine-containing surfactant, fluorine alcohol and a water system into the system plays an obvious role in emulsification and wetting, the fluorine-containing surfactant is used for improving the intersolubility of fluorine-containing hydrocarbon compounds and polyether polyol in the microemulsion, the polyether polyol forms a uniform microemulsion system when the fluorine-containing hydrocarbon compounds and pentane are intersoluble, the disadvantage that the polyether polyol and the fluorine-containing hydrocarbon compounds are difficult to intersoluble is solved, and finally uniform and stable microemulsion is obtained; polyether polyol, pentane and fluorine-containing hydrocarbon compounds are all environment-friendly components, have good biodegradability, are environment-friendly, and improve the environment-friendly performance of the microemulsion.
Preferably, the emulsified solution: fluorine-containing hydrocarbon compound: pentane: the weight ratio of the polyether polyol is 1-10:1-10:6-20:100.
By adopting the technical scheme, the stability of the microemulsion is further improved by adopting the proportion to prepare the polyether polyol microemulsion.
Preferably, the weight ratio of the fluorine-containing surfactant to the fluorine alcohol to the water is 0.05-0.1:0.05-0.01:1000.
By adopting the technical scheme, the emulsified solution prepared according to the proportion has better emulsification effect compared with the traditional hydrocarbon surfactant or water-soluble silicone oil surfactant serving as an emulsifier, and forms stable polyether polyol/cyclopentane/fluorine-containing hydrocarbon microemulsion, the system still has the possibility of layering when the traditional hydrocarbon surfactant or silicone oil surfactant is adopted, and the emulsified solution prepared according to the proportion cannot have poor raw material flowability, so that the problem of high cost is caused by uneven density of foaming materials.
The molecular weight of the polyether polyol is 2000-20000;
preferably, the polyether polyol has a molecular weight of 2000 to 8000.
By adopting the technical scheme, the polyether polyols with high molecular weight can provide better foaming stability and mechanical properties, because the polyether polyols have higher functional group density and higher viscosity, and the higher the molecular weight is, the higher the viscosity is, which helps to improve the stability of the microemulsion; however, the molecular weight of the polyether polyol must not be too high either, which may lead to reduced solubility and compatibility problems. Therefore, when the molecular weight of the polyether polyol in the above range is selected, the stability of the microemulsion can be further improved while the problem of compatibility can be effectively ensured.
Preferably, the pentane is one or a mixed system of cyclopentane, n-pentane and isopentane.
By adopting the technical scheme, the solubility of polyether polyol can be increased by using cyclopentane, n-pentane or isopentane, so that the stability of the microemulsion is improved. These alkane compounds can form stable emulsion system with polyether polyol and other components, reduce layering and precipitation phenomena; cyclopentane, n-pentane and isopentane have lower viscosity and higher fluidity, and when polyurethane foam is prepared, the alkane compounds are helpful to form a uniform and fine foam structure, so that the foaming efficiency and the product quality are improved; and cyclopentane, n-pentane and isopentane are easy to degrade in nature, are environment-friendly, and the use of these compounds for preparing polyether polyol microemulsions helps to reduce the influence on the environment.
The fluorocarbon compound is 1, 3-pentafluoropropane 1, 3-pentafluorobutane (trans) -1-chloro-3, 3-trifluoropropene, 1-difluoroethane one or more of 2, 3-tetrafluoropropene, 1, 3-tetrafluoropropene and perfluoro-4-methyl-2-pentene.
Preferably, the fluorocarbon compound is 1, 3-pentafluoropropane, 1, 3-pentafluorobutane, 1, 3-tetrafluoropropene, perfluoro-4-methyl-2-pentene.
By adopting the technical scheme, the fluorine-containing hydrocarbon compound has lower surface energy, and can form a compact waterproof and oil-proof layer. Therefore, the incorporation of these compounds into microemulsions can enhance the weatherability of the microemulsions, improving its storage stability and its service properties. The fluorine-containing hydrocarbon compound has higher chemical stability and weather resistance, can improve the acid and alkali resistance, oxidation resistance and other properties of the microemulsion, can prolong the service life of the microemulsion, and reduces the influence on the environment.
The fluorine-containing surfactant is selected from perfluorononylbenzenesulfonic acid, sodium perfluorononylbenzenesulfonate, ammonium perfluorononylbenzenesulfonate, perfluorohexanoic acid, ammonium perfluorohexanoate, perfluoro-2-methyl-3, 6-dioxaheptanoic acid, sodium perfluoro-2-methyl-3, 6-dioxaheptanoic acid, perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid ammonium, perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid sodium, perfluoro-2, 5-dimethyl-3, 6-dioxaoctanoic acid ammonium, perfluoro-2, 5-dimethyl-3, 6-dioxaoctanoic acid sodium perfluoro-2-methyl-3-oxahexanoic acid, perfluoro-2-methyl-3-oxaammonium perfluoro-3, perfluoro-methyl-3-oxahexanoic acid sodium perfluoro-3-methyl-hexanoic acid.
Preferably, the fluorine-containing surfactant is one of perfluorononylbenzenesulfonic acid, sodium perfluorononylbenzenesulfonate and perfluorohexanoic acid.
By adopting the technical scheme, the fluorine-containing surfactant has good compatibility with polyether polyol, pentane and fluorine-containing hydrocarbon compounds, so that the stability and compatibility of the microemulsion can be effectively promoted.
The fluoroalcohol is one or more of difluoroethanol, trifluoroethanol, tetrafluoropropanol, pentafluoropropanol, hexafluoroisopropanol, hexafluorobutanol, octafluoropentanol and hexafluoropropylene oxide dimer alcohol.
Preferably, the fluoroalcohol is tetrafluoropropanol, pentafluoropropanol, hexafluorobutanol, hexafluoropropylene oxide dimer alcohol.
By adopting the technical scheme, the fluorine-containing alcohol compound has higher thermal stability and can still keep stable in a high-temperature environment. They can maintain an effective emulsifying effect over a wider temperature range. Has stronger resistance and can be kept stable under stronger chemical environment. The fluorine-containing surfactant and the fluorine-containing alcohol compound have lower surface tension, so that the interfacial tension can be effectively reduced, and the emulsifying effect can be improved. This helps to form fine, uniform emulsion particles, improving the application properties of the microemulsion. Fluorosurfactants and fluoroalcohol compounds generally have low toxicity and good biocompatibility, and have relatively little influence on the human body and environment. The fluorine-containing alcohol compounds have good compatibility with polyether polyol, pentane and fluorine-containing hydrocarbon compounds, and can further promote the stability and compatibility of the microemulsion.
In a second aspect, the present application provides a method for preparing a polyether polyol microemulsion, which adopts the following technical scheme: a preparation method of polyether polyol microemulsion comprises the following preparation steps:
preparation of the emulsion: adding a fluorine-containing surfactant and fluoroalcohol into water, and uniformly stirring at a stirring rate of 100-800rpm at a temperature of 20-40 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding polyether polyol and a fluorocarbon compound into a reaction kettle, and stirring for 3-120min at the stirring speed of 200-1500rpm at the temperature of 20-40 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: adding the emulsified solution and pentane into the uniformly mixed system, and stirring for 3-60min at the stirring speed of 20-2000rpm at the temperature of 20-40 ℃ to obtain the polyether polyol microemulsion.
By adopting the technical scheme, the polyether polyol microemulsion prepared by adopting the process is simple and efficient, low in cost and good in uniform stability.
In a third aspect, the present application provides an application of a polyether polyol microemulsion, which adopts the following technical scheme:
the application of the polyether polyol microemulsion is applied to the preparation of polyurethane foam materials;
slowly adding isocyanate to the polyether polyol microemulsion, and continuously stirring the mixture to ensure that all components are fully mixed; subsequently, the mixture is poured into a mold and foamed; and after the foam is solidified, taking out the foam from the mold to obtain the polyurethane hard foam product.
By adopting the technical scheme, the polyether polyol microemulsion has good stability, can be transported, can be directly reacted with isocyanate for use in the polyurethane foaming process, ensures the stability of the polyurethane foaming performance in the later period, and has mild reaction process and safe discharging process in the process of preparing the polyurethane foam material by the polyether polyol microemulsion.
In summary, the present application has the following beneficial effects:
1. because the microemulsion is prepared by compounding polyether polyol, fluorine-containing hydrocarbon compound, pentane and emulsion solution, the stability and the temperature resistance of the microemulsion can be improved by compounding the polyether polyol, the fluorine-containing hydrocarbon compound and the pentane, and the effect of further reducing the surface tension is achieved by compounding the fluorine-containing hydrocarbon compound and the polyether polyol, so that the wetting and penetrating capacity of the microemulsion can be improved, and the microemulsion with uniform stability can be obtained.
2. The preparation method of the polyether polyol microemulsion comprises the steps of firstly preparing an emulsion solution, then premixing polyether polyol and a fluorine-containing hydrocarbon compound, and finally mixing to prepare the microemulsion, wherein the microemulsion is simple and efficient, has low cost, and has good uniform stability.
3. The polyether polyol microemulsion is applied to the preparation of polyurethane foam materials, can be directly used by reacting with isocyanate, ensures the stability of the foaming performance of polyurethane in the later period, and has mild reaction process and safe discharging process in the process of preparing the polyurethane foam materials by the polyether polyol microemulsion.
Detailed Description
The present application is described in further detail below with reference to examples.
The sources of raw materials used in this application are all from common commercial products.
Examples
Example 1
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.01g of a fluorine-containing surfactant into 1000g of water, and uniformly stirring at a stirring rate of 100rpm at a temperature of 20 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 1g of fluorocarbon compound into a reaction kettle, and stirring for 5min at a stirring speed of 800rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 2g of the emulsified solution and 6g of pentane were added to the above uniformly mixed system, and stirred at 20℃and a stirring rate of 200rpm for 60 minutes to obtain a polyether polyol microemulsion.
In the embodiment, the fluorine-containing surfactant adopts perfluoro nonylbenzenesulfonic acid; the fluorine-containing hydrocarbon compound adopts 1, 3-pentafluoropropane; the molecular weight of the polyether polyol is 2000; the pentane is cyclopentane.
Example 2
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.1g of a fluorine-containing surfactant into 1000g of water, adding 0.01g of fluocinol, and uniformly stirring at a stirring speed of 500rpm at a temperature of 20 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 1g of fluorocarbon compound into a reaction kettle, and stirring for 3min at a stirring speed of 200rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 20g of the emulsified solution and 20g of pentane were added to the above uniformly mixed system, and stirred at 40℃and a stirring rate of 800rpm for 3 minutes to obtain a polyether polyol microemulsion.
In the embodiment, the fluorine-containing surfactant adopts ammonium perfluoro nonylbenzenesulfonate; the fluorine-containing hydrocarbon compound adopts (trans) -1-chloro-3, 3-trifluoropropene; the molecular weight of the polyether polyol is 8000; the pentane adopts a mixed system of cyclopentane and isopentane (mass ratio 1:1); the fluoroethanol is trifluoroethanol.
Example 3
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.05g of fluorine-containing surfactant into 1000g of water, adding 0.005g of fluorine alcohol, and uniformly stirring at 40 ℃ and stirring speed of 800rpm to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 2g of fluorocarbon compound into a reaction kettle, and stirring for 3min at a stirring speed of 1500rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 6g of the emulsified solution and 12g of pentane were added to the above uniformly mixed system, and stirred at 30℃and 800rpm for 5 minutes to obtain a polyether polyol microemulsion.
In the embodiment, the fluorine-containing surfactant adopts sodium perfluoro nonylbenzenesulfonate; the fluorine-containing hydrocarbon compound adopts perfluoro-4 methyl-2 pentene; the molecular weight of the polyether polyol is 8000; the pentane adopts n-pentane; the fluoroethanol is difluoroethanol.
Example 4
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.01g of a fluorine-containing surfactant into 1000g of water, adding 0.01g of fluocinol, and uniformly stirring at a stirring speed of 200rpm at a temperature of 30 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 8g of fluorocarbon compound into a reaction kettle, and stirring for 20min at a stirring speed of 700rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 2g of the emulsified solution and 8g of pentane were added to the above uniformly mixed system, and stirred at 40℃for 30 minutes at a stirring rate of 200rpm, to obtain a polyether polyol microemulsion.
In this example, perfluoro-2-methyl-3-oxahexanoic acid was used as the fluorosurfactant; the fluorine-containing hydrocarbon compound adopts 1, 3-pentafluoropropane; the molecular weight of the polyether polyol is 7000; the pentane adopts n-pentane; the fluoroalcohol is pentafluoropropanol.
Example 5
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.08g of fluorine-containing surfactant into 1000g of water, adding 0.01g of fluorine alcohol, and uniformly stirring at a stirring speed of 200rpm at a temperature of 30 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 4g of fluorocarbon compound into a reaction kettle, and stirring for 4min at a stirring speed of 1000rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 5g of the emulsified solution and 12g of pentane were added to the above uniformly mixed system, and stirred at a stirring rate of 1200rpm for 3 minutes at 20℃to obtain a polyether polyol microemulsion.
In this example, sodium perfluoro-2-methyl-3-oxahexanoate was used as the fluorosurfactant; the fluorine-containing hydrocarbon compound adopts 1, 3-tetrafluoropropene; the molecular weight of the polyether polyol is 6000; the pentane adopts a mixed system of n-pentane and isopentane (mass ratio 1:1); the fluoroalcohol is pentafluoropropanol.
Example 6
A polyether polyol microemulsion is prepared by the following steps:
preparation of the emulsion: adding 0.04g of a fluorine-containing surfactant into 1000g of water, adding 0.01g of fluocinol, and uniformly stirring at a stirring speed of 200rpm at a temperature of 30 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding 100g of polyether polyol and 3g of fluorocarbon compound into a reaction kettle, and stirring for 120min at a stirring speed of 200rpm at a temperature of 20 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: 5g of the emulsified solution and 15g of pentane were added to the above uniformly mixed system, and stirred at a stirring rate of 800rpm for 3 minutes at 20℃to obtain a polyether polyol microemulsion.
In this example, ammonium perfluoro-2-methyl-3-oxahexanoate was used as the fluorosurfactant; 2, 3-tetrafluoropropene is used as the fluorine-containing hydrocarbon compound; the molecular weight of the polyether polyol is 3000; the pentane adopts n-pentane; the fluoroalcohol is pentafluoropropanol.
Examples 7 to 18
A polyether polyol microemulsion differs from example 6 in that the raw material components and their corresponding parameters are shown in Table 1.
TABLE 1 raw materials and parameters thereof in examples 7-18
Comparative example
Comparative example 1
The polyether polyol microemulsion differs from example 1 in that the preparation step emulsion solution is prepared: 0.01g of sodium dodecyl benzene sulfonate was added to 1000g of water, and stirred uniformly at a stirring rate of 100rpm at 20℃to obtain an emulsified solution.
Comparative example 2
The polyether polyol microemulsion differs from example 1 in that the preparation step emulsion solution is prepared: 0.01g of silicone oil surfactant is added into 1000g of water, and the mixture is stirred uniformly at a stirring rate of 100rpm at a temperature of 20 ℃ to obtain an emulsified solution.
Comparative example 3
The polyether polyol microemulsion differs from example 3 in that the preparation step emulsion solution is prepared: 0.05g of sodium perfluorononylbenzenesulfonate was added to 1000g of water, and then 0.005g of fluoroalcohol was added thereto, and the mixture was stirred uniformly at a stirring rate of 800rpm at a temperature of 40℃to obtain an emulsified solution.
Performance test
1. Storage stability test
The microemulsions prepared in examples 1 to 18 and comparative examples 1 to 3 were placed in stopper-equipped ground glass bottles, respectively, and left to stand at constant temperature (23.+ -. 2 ℃ C.) for recording time; and the appearance of the microemulsion in the glass bottle with stopper was observed with eye force at 4h intervals under intense illumination until the occurrence of the layering phenomenon recording duration, which is recorded in table 2.
2. Centrifugal stability test
The microemulsions prepared in examples 1 to 18 and comparative examples 1 to 3 were each poured into a 10mL centrifuge tube, centrifuged at 4000r/min for 15min, and the appearance of the microemulsion in a glass bottle with a stopper was observed with a visual force under intense illumination, and visually evaluated and recorded in Table 2.
TABLE 2
As can be seen from the combination of examples 1 to 18 and comparative examples 1 to 3 and the combination of Table 2, the emulsified solution prepared under certain conditions by compounding the fluorine-containing surfactant and the fluoroalcohol has better emulsification effect than the conventional hydrocarbon surfactant or water-soluble silicone oil surfactant in the polyether polyol microemulsion system, and forms stable polyether polyol microemulsion.
As can be seen from the combination of examples 1-18 and Table 2, the polyether polyol forms a uniform microemulsion system when being mutually dissolved with the fluorine-containing hydrocarbon compound and the cyclopentane/n-pentane/isopentane, the disadvantage that the polyether polyol and the fluorine-containing hydrocarbon compound are difficult to be mutually dissolved is solved, and the microemulsion system can be stabilized for more than 2 months, the effect is unchanged, and the storage and transportation performances are good.
The present embodiment is merely illustrative of the present application and is not intended to be limiting, and those skilled in the art, after having read the present specification, may make modifications to the present embodiment without creative contribution as required, but is protected by patent laws within the scope of the claims of the present application.
Claims (10)
1. The polyether polyol microemulsion is characterized by comprising the following raw materials: polyether polyol, fluorine-containing hydrocarbon compound, pentane and emulsifying solution; the emulsified solution consists of a fluorine-containing surfactant, fluocinol and water, wherein the weight ratio of the fluorine-containing surfactant to the fluocinol to the water is 0.01-0.1:0-0.01:100.
2. A polyether polyol microemulsion according to claim 1, wherein: the emulsion solution: fluorine-containing hydrocarbon compound: pentane: the weight ratio of the polyether polyol is 1-10:1-10:6-20:100.
3. A polyether polyol microemulsion according to claim 1, wherein: the weight ratio of the fluorine-containing surfactant to the fluorine alcohol to the water is 0.05-0.1:0.05-0.01:1000.
4. A polyether polyol microemulsion according to claim 1, wherein: the molecular weight of the polyether polyol is 2000-20000.
5. A polyether polyol microemulsion according to claim 4, wherein: the pentane is one or a mixed system of cyclopentane, n-pentane and isopentane.
6. A polyether polyol microemulsion according to claim 1, wherein: the fluorine-containing hydrocarbon compound is 1, 3-pentafluoropropane 1, 3-pentafluorobutane, (trans) -1-chloro-3, 3-trifluoropropene 1, 1-difluoroethane, 2, 3-tetrafluoropropene, 1, 3-tetrafluoropropene, perfluoro-4-methyl-2-pentene.
7. A polyether polyol microemulsion according to claim 1, wherein: the fluorine-containing surfactant is one of perfluorononyl benzenesulfonic acid, sodium perfluorononyl benzenesulfonic acid, ammonium perfluorononyl benzenesulfonic acid, perfluorohexanoic acid, ammonium perfluoro-2-methyl-3, 6-dioxaheptanoic acid, sodium perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid, ammonium perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid, sodium perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid, perfluoro-2, 5-dimethyl-3, 6-dioxaoctanoic acid, ammonium perfluoro-2, 5-dimethyl-3, 6-dioxasodium perfluoro-2-methyl-3-oxahexanoic acid, perfluoro-2-methyl-3-oxaoctanoic acid, perfluoro-2-methyl-3, 6, 8-trioxanonanoic acid, perfluoro-2-methyl-3, 6-dioxaoctanoic acid.
8. A polyether polyol microemulsion according to claim 1, wherein: the fluoroalcohol is one or a combination of more of difluoroethanol, trifluoroethanol, tetrafluoropropanol, pentafluoropropanol, hexafluoroisopropanol, hexafluorobutanol, octafluoropentanol and hexafluoropropylene oxide dimer alcohol.
9. A process for the preparation of a polyether polyol microemulsion according to any one of claims 1 to 9, wherein: the preparation method comprises the following steps:
preparation of the emulsion: adding a fluorine-containing surfactant and fluoroalcohol into water, and uniformly stirring at a stirring rate of 100-800rpm at a temperature of 20-40 ℃ to obtain an emulsified solution;
premixing the polyether polyol with the fluorine-containing hydrocarbon compound: adding polyether polyol and a fluorocarbon compound into a reaction kettle, and stirring for 3-120min at the stirring speed of 200-1500rpm at the temperature of 20-40 ℃ to obtain a uniformly mixed system;
preparing a microemulsion: adding the emulsified solution and pentane into the uniformly mixed system, and stirring for 3-60min at the stirring speed of 20-2000rpm at the temperature of 20-40 ℃ to obtain the polyether polyol microemulsion.
10. Use of a polyether polyol microemulsion according to any one of claims 1 to 8, wherein: the microemulsion is applied to the preparation of polyurethane foam materials.
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