CN110698630A - Solvent type polyurethane resin, preparation method thereof and waterproof umbrella with lotus leaf effect - Google Patents
Solvent type polyurethane resin, preparation method thereof and waterproof umbrella with lotus leaf effect Download PDFInfo
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- CN110698630A CN110698630A CN201910956652.5A CN201910956652A CN110698630A CN 110698630 A CN110698630 A CN 110698630A CN 201910956652 A CN201910956652 A CN 201910956652A CN 110698630 A CN110698630 A CN 110698630A
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- polyurethane resin
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- type polyurethane
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- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6603—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6607—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
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- A—HUMAN NECESSITIES
- A45—HAND OR TRAVELLING ARTICLES
- A45B—WALKING STICKS; UMBRELLAS; LADIES' OR LIKE FANS
- A45B25/00—Details of umbrellas
- A45B25/18—Covers; Means for fastening same
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/32—Polyhydroxy compounds; Polyamines; Hydroxyamines
- C08G18/3203—Polyhydroxy compounds
- C08G18/3206—Polyhydroxy compounds aliphatic
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/44—Polycarbonates
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- 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
-
- 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
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a solvent type polyurethane resin and a preparation method thereof and a waterproof umbrella with a lotus leaf effect, wherein the raw material formula of the polyurethane resin comprises, by weight, 3 ~ 10% of polyester polyol, 3 ~ 10% of polyether polyol, 0.5 ~ 3% of micromolecule polyol, 5 ~ 10% of isocyanate, 55 ~ 70% of solvent, 0.001 ~ 0.1.1% of catalyst, 10 ~ 15% of fluorine-based water-repellent and oil-repellent agent, 0.05 ~ 0.2.2% of terminator and 0.01 ~ 0.15.15% of auxiliary agent.
Description
Technical Field
The invention belongs to the technical field of polyurethane resin, and particularly relates to solvent type polyurethane resin, and a preparation method and application thereof.
Background
The umbrella cloth of the existing umbrella is mainly divided into two types, namely chemical fiber cloth and sunshade cloth with a special coating at the inner layer, the umbrella cloth of the umbrella mainly takes the chemical fiber cloth as the main part and is light, but the outer surface of the umbrella cloth is not treated, so that the umbrella cloth is easy to wet in rainy days; the outer surface (namely the surface directly contacted with sunlight and rainwater) of the sunshade cloth of the sunshade is chemical fiber cloth, the inner layer is a coating (namely a resin layer), and an ultraviolet absorbent and black slurry are added in the coating, so that the effect of blocking ultraviolet rays is mainly achieved. However, the common resin coated on the inner layer of the sun-shading umbrella cloth is not high-temperature resistant and is very easy to scratch, and a surface layer polyurethane resin for the high-temperature resistant and scratch-resistant printable full sun-shading umbrella cloth and an application thereof are developed later, wherein the polyurethane resin comprises 8-17% of hydroxyl-terminated high-molecular polyol, 0.5-0.13% of a small-molecular chain extender, 0.03-0.05% of an antioxidant, 6-8% of diisocyanate, 52-58% of a urethane-grade solvent and 0.001-0.003% of an organic bismuth catalyst, although the polyurethane resin can be used on the surface layer of the sun-shading umbrella cloth to be transferred and printed, the polyurethane resin has certain high-temperature resistance and scratch resistance, but is relatively deficient in the aspect of water resistance. Therefore, the problem that the existing umbrella is wet cannot be solved, the umbrella becomes heavy when the umbrella is used in rainy days, and the umbrella needs to be unfolded and dried after the umbrella is used.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a solvent type polyurethane resin, a preparation method and application thereof.
The invention also provides an umbrella.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the solvent type polyurethane resin comprises the following raw materials in percentage by weight:
the polyether polyol is polytetrahydrofuran ether glycol with the number average molecular weight of 1000-2000; the polyester polyol is carbonate polyol with the number average molecular weight of 1000-2000.
According to some embodiments of the invention, the small molecule polyol is one or a combination of ethylene glycol and 1, 4-butanediol.
According to some embodiments of the invention, the isocyanate is 4, 4-diphenylmethane diisocyanate.
According to some embodiments of the present invention, the fluorine-based water and oil repellent agent is one or a combination of a nonionic fluorine-based water and oil repellent agent and a cationic fluorine-based water and oil repellent agent.
According to some embodiments of the invention, the solvent is one or a combination of N, N-dimethylformamide and toluene.
According to some embodiments of the invention, the auxiliary agent is an antioxidant and a wetting dispersant, wherein the antioxidant is added in an amount of 0.01 to 0.05%, and the wetting dispersant is added in an amount of 0.01 to 0.1%.
According to some example aspects of the present disclosure, the polyurethane resin may comprise the following components in weight percent:
the invention adopts another technical scheme that: a preparation method of the solvent type polyurethane resin comprises the following steps: according to the formula, stirring polyester polyol, polyether polyol, small molecular polyol and 40-60% of solvent at 50-60 ℃ for 30-60 min, then adding isocyanate, reacting at 70-80 ℃, adding a catalyst, increasing the viscosity along with the reaction, adding 10-20% of solvent for dilution when the viscosity reaches a specified value, adding a terminator and the rest of solvent when the viscosity reaches a preset end point, continuously stirring until the viscosity is stable, adding fluorine-based water-repellent agent, oil-repellent agent and auxiliary agent, continuously stirring for 30-60 min, and discharging to obtain the solvent type polyurethane resin.
According to the invention, the specified value of the viscosity is 100-140 Pa.S/60 ℃, and the preset value of the terminal point of the viscosity is 80-120 Pa.S/25 ℃.
The invention adopts another technical scheme that: the solvent type polyurethane resin is applied to umbrellas and other outdoor waterproof products.
An umbrella, including umbrella stand and umbrella face cloth, the umbrella still includes to be formed at the coating on the umbrella face cloth surface, the coating by the above-mentioned polyurethane resin with bridge agent coating after mixing the surface solidification of umbrella face cloth forms.
The addition mass of the bridging agent accounts for 11-13% of the NCO content in the polyurethane resin.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the polyurethane resin, polyether polyol and polyester polyol are combined to form a macromolecular polyol mixture, and a coating formed by the prepared polyurethane resin not only has good high-temperature resistance, hydrolysis resistance and aging resistance, but also can reduce the surface energy of the coating by matching with micromolecular polyol in a specific proportion, fluorine water-repellent agent and oil-repellent agent in a certain proportion, and the surface energy of the coating is reduced, so that the polyurethane resin is applied to the outer surface of umbrella cloth instead of the inner layer, the surface energy of the surface of the umbrella cloth can be effectively reduced, the surface energy of the coating is 15-20N/m, the surface energy of water is 60N/m, and the water cannot penetrate into the umbrella cloth, so that an umbrella used in rain can be directly folded or slightly shaken to be folded, the surface is anhydrous, and does not need to be dried.
When the polyurethane resin is used on umbrella cloth, the coating amount is small, the umbrella cloth is light, an ultraviolet absorbent and color paste can be added into the resin according to needs to play a role in blocking ultraviolet rays, and the polyurethane resin can be used as an umbrella and a sunshade.
The preparation method of the polyurethane resin has simple process, and the prepared polyurethane resin coating has adjustable surface tension.
Detailed Description
Specific embodiments of the present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited thereto.
Example 1
The formulation of the raw materials used for the solvent-based polyurethane resin provided in this example is shown in table 1, wherein,
the polycarbonate polyol had a number average molecular weight of 2000, available from Japan.
The polytetrahydrofuran ether glycol had a number average molecular weight of 2000, available from basf, germany.
The isocyanate is 4, 4-diphenylmethane diisocyanate.
The fluorine-based water and oil repellent agent is a nonionic fluorine-based water and oil repellent agent, model NF-31, and is available from Korea efforts (NURI).
The catalyst is bismuth carboxylate.
The antioxidant is CHINOX 1010.
The wetting dispersant was BYK-9565.
The solvent type polyurethane resin is prepared by the following method:
adding polytetrahydrofuran ether dihydric alcohol, polycarbonate polyol, micromolecular polyol, an antioxidant and 50% of solvent into a reaction kettle, stirring for 40min at 55 ℃, fully stirring uniformly, adding isocyanate, increasing to 80 ℃ along with reaction heat and proper auxiliary heating for reaction, adding a catalyst according to the reaction speed condition, increasing the viscosity along with the reaction, adding 15% of solvent for dilution when the viscosity reaches a specified value (the viscosity is 100-140 Pa.S/60 ℃), and adding a terminator and the residual solvent to terminate the reaction when the viscosity finally reaches a preset value of 80-120 Pa.S/25 ℃ of a terminal point. Stirring continuously until viscosity is stable, adding fluorine water-repellent oil-repellent agent and wetting dispersant, stirring continuously for 40min, discharging and packaging.
Example 2
The formulation of the raw materials used for the solvent-type polyurethane resin provided in this example is shown in Table 1, and the rest is the same as in example 1.
Example 3
The formulation of the raw materials used for the solvent-type polyurethane resin provided in this example is shown in Table 1, and the rest is the same as in example 1.
Example 4
The formulation of the raw materials used for the solvent-type polyurethane resin provided in this example is shown in Table 1, and the rest is the same as in example 1.
Example 5
This example provides a solvent-type polyurethane resin, which is prepared according to the formulation and raw materials shown in Table 1, and is otherwise the same as example 1.
Comparative example 1
This example provides a solvent-type polyurethane resin, which is prepared according to the formulation and raw materials shown in Table 1, and is otherwise the same as example 1.
The amount of the fluorine-based water-repellent and oil-repellent agent used in this comparative example was 0%.
Comparative example 2
This example provides a solvent-type polyurethane resin, which is prepared according to the formulation and raw materials shown in Table 1, and is otherwise the same as example 1.
The amount of the fluorine-based water-repellent and oil-repellent agent used in this comparative example was 20%.
TABLE 1
The polyurethane resins of examples 1 to 5 and comparative examples 1 to 2 were uniformly mixed with a bridging agent, respectively, and then coated on the outer surface of the umbrella cloth of an umbrella in an amount of 0.15mm, and cured to obtain a waterproof coating, and then tests were performed, the results of which are shown in table 2.
The bridging agent is NCO type bridging agent, the model is NX, the product of Jiangsu Hua big new material company Limited is produced by itself, and the mixing amount of the bridging agent and 100 parts of resin is 11-15%.
TABLE 2
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. The solvent type polyurethane resin is characterized in that the raw material formula of the polyurethane resin comprises the following components in percentage by weight:
3 ~ 10% of polyester polyol;
polyether polyol 3 ~ 10%;
small molecule polyol 0.5 ~ 3%;
5 ~ 10% of isocyanate;
solvent 55 ~ 70%;
catalyst 0.001 ~ 0.1.1%;
10 ~ 15% of fluorine-based water and oil repellent agent;
0.05 percent of terminator, 0.05 ~ 0.5.5 percent;
0.01 percent of auxiliary agent 0.01 ~ 0.15.15 percent.
2. The solvent-based polyurethane resin according to claim 1, wherein the polyether polyol is polytetrahydrofuran ether glycol having a number average molecular weight of 1000 ~ 2000, and the polyester polyol is polycarbonate polyol having a number average molecular weight of 1000 ~ 2000.
3. A solvent type polyurethane resin according to claim 1, wherein: the small molecular polyol is one or the combination of two of ethylene glycol and 1, 4-butanediol.
4. A solvent type polyurethane resin according to claim 1, wherein: the isocyanate is 4, 4-diphenylmethane diisocyanate.
5. A solvent type polyurethane resin according to claim 1, wherein: the fluorine-based water repellent agent and the fluorine-based oil repellent agent are one or the combination of non-ionic fluorine-based water repellent agent, non-ionic oil repellent agent and cationic fluorine-based water repellent agent and non-ionic oil repellent agent.
6. A solvent type polyurethane resin according to claim 1, wherein: the terminator is 1, 3-butanediol.
7. The solvent-based polyurethane resin as claimed in claim 1, wherein the auxiliary comprises an antioxidant and a wetting dispersant, wherein the antioxidant is added in an amount of 0.01 ~ 0.05.05%, and the wetting dispersant is added in an amount of 0.01 ~ 0.1.1%.
8. A method for preparing the solvent type polyurethane resin as claimed in claim 1 ~ 7, wherein the method comprises the steps of stirring the polyester polyol, polyether polyol, small molecular weight polyol and 40 ~ 60% solvent at 50 ~ 60 ℃ for 30 ~ 60min, adding isocyanate, reacting at 70 ~ 80 ℃ under 80 ℃, adding catalyst, increasing viscosity along with the reaction, adding 10 ~ 20% solvent for dilution when the viscosity reaches a predetermined value, adding terminator and residual solvent when the viscosity reaches a predetermined value, stirring until the viscosity is stable, adding fluorine-based water repellent, oil repellent and auxiliary agent, stirring for 30 ~ 60min, and discharging to obtain the solvent type polyurethane resin.
9. Use of the solvent borne polyurethane resin of any one of claims 1 ~ 7 in umbrellas and other outdoor waterproofing products.
10. An umbrella, comprising an umbrella frame and umbrella surface cloth, characterized in that the umbrella also comprises a coating formed on the outer surface of the umbrella surface cloth, the coating is formed by coating the polyurethane resin of any claim of claim 1 ~ 7 and the bridging agent on the outer surface of the umbrella surface cloth after mixing and curing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910956652.5A CN110698630A (en) | 2019-10-10 | 2019-10-10 | Solvent type polyurethane resin, preparation method thereof and waterproof umbrella with lotus leaf effect |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910956652.5A CN110698630A (en) | 2019-10-10 | 2019-10-10 | Solvent type polyurethane resin, preparation method thereof and waterproof umbrella with lotus leaf effect |
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