CN116253861B - Spraying airtight plugging polyurethane foam and preparation method thereof - Google Patents
Spraying airtight plugging polyurethane foam and preparation method thereof Download PDFInfo
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Abstract
The invention provides a spray-coating airtight sealing polyurethane foam and a preparation method thereof, wherein the spray-coating airtight sealing polyurethane foam comprises A, B double components, and the A component comprises the following raw materials: polymer polyol, foaming agent, micromolecular polyol, fluorine-containing dihydric alcohol compound, catalyst and foam stabilizer; the fluorine-containing dihydric alcohol compound is prepared by reacting fluorine-containing ester with an amino diol compound; the component B comprises the following raw materials: polymeric MDI, naphthalene 1, 5-diisocyanate. The polyurethane foam prepared by the invention has good ultraviolet resistance, stability of mechanical property and working safety.
Description
Technical Field
The invention belongs to the technical field of polyurethane foam, and particularly relates to spray-coating airtight plugging polyurethane foam and a preparation method thereof.
Background
The polyurethane rigid foam is a low-density microporous polymer foam plastic with a closed-cell structure, and is widely applied to the fields of construction, electronic and electrical, chemical coating and the like due to the advantages of excellent chemical resistance, low toxicity, good mechanical property, good electrical insulation and the like.
In the electrical field, people often use polyurethane rigid foam as an anti-condensation airtight blocking material, such as anti-condensation airtight blocking materials of terminal box transformer substation, wind box transformer substation, photovoltaic box transformer substation, high-speed rail special box transformer substation and other power equipment, and the like, and the anti-condensation airtight blocking material has the advantages of good sealing effect, convenience in operation and low cost. The concrete anti-condensation blocking principle is as follows: the plane is sealed by using flowable liquid polyurethane material, foaming and solidification reaction are carried out after liquid is immersed in various gaps and holes, extrusion force generated by foaming is formed in the longitudinal direction, and a sealing system is formed, so that airtight sealing is realized.
The bio-based polyurethane spray foam with high content of bio-based material disclosed in patent CN106317365B is produced by mixing, foaming and polymerizing a polyurethane spray composition white material component prepared by using at least one bio-based polyether polyol as a raw material and an isocyanate component. The product has high content of biological base material and good waterproof and heat-insulating functions. Patent CN113667088A discloses a condensation-preventing high-flame-retardant polyurethane foaming material and a preparation method thereof, the condensation-preventing high-flame-retardant polyurethane foaming material comprises a first component and a second component, and the first component comprises the following raw materials in parts by weight: 30-130 parts of polyether polyol, 30-60 parts of flame retardant, 0.1-0.5 part of foaming agent, 1-2 parts of foam stabilizer and 1-5 parts of chain extender; the second component comprises the following raw materials: 30-90 parts of polyisocyanate and 10-30 parts of polyether polyol, the condensation-preventing high-flame-retardance polyurethane foaming material is a double-component foaming hard foam material, has the characteristics of high closing porosity, high flame retardance and high strength, and can effectively seal wiring holes, so that condensation is prevented from occurring in an electric ring main unit, an outdoor switch cabinet, an outdoor tapping box and the like, and the safety is improved. However, the blocked power equipment is often exposed to sunlight, and the polyurethane rigid foam is easy to be aged under the influence of ultraviolet rays, so that the mechanical performance is reduced, the surface is easy to embrittle, the airtight blocking effect is reduced, and great potential safety hazards exist for the operation of the power equipment. Therefore, there is a need to develop a uv aging resistant, airtight blocked polyurethane foam.
Disclosure of Invention
In order to solve the technical problems, the invention provides a spray-coating airtight plugging polyurethane foam and a preparation method thereof, wherein a fluorine-containing dihydric alcohol compound is introduced into a raw material for preparing A components of polyurethane to serve as a chain extender, so that amide bonds are generated in a hard segment of the polyurethane, the amide bonds are easy to form hydrogen bonds with urethane bonds, the hard segment of the urethane is better in orientation, orderly crystallized, more perfect in crystallization and improved in crystallinity, the ultraviolet resistance is further improved, and meanwhile, the stability of the mechanical property and the working safety of the polyurethane foam are also improved; by introducing 1, 5-naphthalene diisocyanate into the raw material of the component B as isocyanate, the hard segment of the polyurethane contains naphthalene rings, and the ultraviolet resistance of the polyurethane is further improved.
In order to realize the technical scheme, the invention adopts the following specific technical scheme:
the spray-coated airtight plugging polyurethane foam comprises A, B two components, wherein the component A comprises the following raw materials: polymer polyol, foaming agent, micromolecular polyol, fluorine-containing dihydric alcohol compound, catalyst and foam stabilizer; the fluorine-containing dihydric alcohol compound is prepared by reacting fluorine-containing ester with an amino diol compound;
the component B comprises the following raw materials: polymeric MDI, naphthalene 1, 5-diisocyanate.
The spray airtight sealing polyurethane foam comprises A, B two components, wherein the mass ratio of the two components is 1:1-2, wherein the component A comprises the following raw materials in parts by weight: 100 parts of polymer polyol, 1-5 parts of water, 1-3 parts of micromolecular polyol, 3-5 parts of fluorine-containing dihydric alcohol compound, 2-6 parts of catalyst and 1-3 parts of foam stabilizer;
the dosage of the 1, 5-naphthalene diisocyanate in the component B is 14-18wt% of that of the polymeric MDI; the polymeric MDI has an NCO content of 30 to 35% by weight.
Preferably, the mass ratio of the component A to the component B is 1:1.2-1.5.
The molar ratio of the fluorine-containing ester to the amino diol compound is 1:1.1-1.25.
The fluorine-containing ester is selected from one or a combination of two or more of methyl trifluoroacetate, ethyl trifluoroacetate, methyl 2, 3-tetrafluoropropionate, ethyl 2, 3-tetrafluoropropionate, methyl pentafluoropropionate, ethyl pentafluoropropionate, methyl 4, 4-trifluorobutyrate and ethyl 4, 4-trifluorobutyrate; the amino diol compound is selected from one or more of 3-amino-1, 2-propanediol, 2- (aminomethyl) -1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol and serinol.
Specifically, the fluorine-containing dihydric alcohol compound is prepared by a method comprising the following steps:
adding fluorine-containing ester, amino diol compound, solvent and catalyst into a reaction kettle, stirring until the mixture is uniform, heating to a reflux state, reacting at constant temperature, and distilling under reduced pressure after the reaction is finished to obtain the fluorine-containing dihydric alcohol compound.
The solvent is selected from one or more of diethyl ether, acetone, methanol and ethanol; the reaction time is 5-8h. The catalyst is selected from one of sodium methoxide and sodium ethoxide, and the dosage of the catalyst is 0.5-1.0wt% of the total weight of fluorine-containing ester and amino diol compounds.
The hydroxyl value of the polymer polyol is 300-800mgKOH/g, the functionality is 2-6, and the polymer polyol is one or the combination of two of polyether polyol and polyester polyol.
The small molecular polyol is selected from one or a combination of two or more of 1, 4-butanediol, ethylene glycol, diethylene glycol, propylene glycol and trimethylolpropane.
The catalyst is selected from one or two of tertiary amine compounds and organic tin compounds. The tertiary amine compound is not particularly limited, and may be one or a combination of two or more selected from the group consisting of triethylene diamine, N, N-dimethylcyclohexylamine, N, N, N ', N ' -tetramethyl-1, 6-hexamethylenediamine, N, N, N ', N ' ', N ' ' -pentamethylene divinyl triamine, which are commonly used in the art. The organotin compound is not particularly limited, and may be one or a combination of two or more selected from dibutyltin dilaurate, stannous octoate and stannous oleate, which are commonly used in the art. Preferably, the catalyst is a tertiary amine compound and an organotin compound according to the mass ratio of 4-6:1.
The foam stabilizer is not particularly limited, and includes, but is not limited to, silicone-based foam stabilizers.
The foaming agent comprises one or a combination of two of a physical foaming agent and a chemical foaming agent. The chemical foaming agent is water. The physical foaming agent is not particularly limited, and may be one or a combination of two or more selected from the group consisting of monofluorodichloroethane, trichlorofluoromethane and trichlorofluoroethane, which are commonly used in the art.
The invention also provides a preparation method of the spray-coated airtight plugging polyurethane foam, which comprises the following steps:
weighing the raw materials of the component A: uniformly mixing polymer polyol, a foaming agent, micromolecular polyol, a fluorine-containing dihydric alcohol compound, a catalyst and a foam stabilizer to obtain a component A; weighing the raw materials of the component B, namely polymeric MDI and 1, 5-naphthalene diisocyanate, heating and uniformly stirring at a constant temperature, and discharging to obtain the component B.
The temperature is raised to 60-80 ℃.
According to the invention, the fluorine-containing dihydric alcohol compound is introduced into the raw material for preparing the component A of the polyurethane to serve as a chain extender, so that the ultraviolet resistance is better, the applicant considers that possible reasons are that amide bonds are generated in a hard segment of the polyurethane, and the amide bonds are easy to form hydrogen bonds with urethane bonds, so that the orientation of the hard segment of the urethane is better, the urethane is crystallized orderly, the crystallization is more perfect, the crystallinity is improved, the ultraviolet resistance is further improved, and meanwhile, the stability of the mechanical property and the working safety of the polyurethane foam are also improved; by introducing 1, 5-naphthalene diisocyanate into the raw material of the component B as isocyanate, the hard segment of the polyurethane contains naphthalene rings, and the ultraviolet resistance of the polyurethane is further improved.
Detailed Description
The invention is further illustrated below in connection with specific examples, but is not limited to the disclosure. If no special description exists, the parts are parts by weight in the embodiment of the invention. All reagents used are those commercially available in the art.
Polyester polyol: the sol vay company CAPA3041, hydroxyl value 395mgKOH/g, initiator is trimethylolpropane.
Polyether polyol: red Baoli group Co., ltd.H 8404, hydroxyl value 460mgKOH/g, and pentaerythritol as initiator.
Foam stabilizer: demeishichuang silicone oil AK8803.
Polymeric MDI: PM-300 of Vanhua polyurethane Co., ltd, average functionality 2.8, -NCO content 32% by weight.
Preparation example 1
1mol of methyl trifluoroacetate, 1.25mol of 3-amino-1, 2-propylene glycol, 160g of diethyl ether and 1.2g of sodium methoxide are added into a reaction kettle, stirred until the mixture is uniform, heated to a reflux state and reacted at a constant temperature for 7.5 hours, no methanol is distilled out, the reaction is stopped, and the fluorine-containing dihydric alcohol compound is obtained through reduced pressure distillation.
Preparation example 2
The remainder was the same as in preparation example 1 except that 1mol of ethyl 4, 4-trifluorobutyrate was used instead of 1mol of methyl trifluoroacetate.
Preparation example 3
The remainder was the same as in preparation example 1 except that 3-amino-1, 2-propanediol was replaced with an equimolar amount of 2-amino-2-ethyl-1, 3-propanediol.
Comparative preparation example 1
The remainder was the same as in preparation example 1 except that 1mol of methyl acetate was used instead of 1mol of methyl trifluoroacetate.
Preparation of spray-coated air-tight sealing polyurethane foam
Example 1
Weighing the raw materials of the component A: 50 parts of polyester polyol (CAPA 3041), 50 parts of polyether polyol (H8404), 3.5 parts of water, 1 part of trimethylolpropane, 5 parts of fluorine-containing dihydric alcohol compound prepared in preparation example 1, 2.5 parts of catalyst formed by mixing triethylene diamine, N, N ', N ' ', N ' ' -pentamethylene divinyl triamine and dibutyltin dilaurate according to the mass ratio of 2:2.5:1, and 2 parts of Demeishi silicone oil AK8803 are uniformly mixed to obtain a component A;
the component B is 100 parts of MDI and 18 parts of 1, 5-naphthalene diisocyanate mixture, the temperature is raised to 70 ℃, the mixture is stirred uniformly at constant temperature, and the component B is obtained after discharging.
When in use, the component A and the component B are mixed according to the mass ratio of 1:1.2.
examples 2 to 3
The other matters were the same as in example 1 except that fluorine-containing diol compounds were prepared in accordance with preparation examples 2 to 3, respectively.
Example 4
The other components were the same as in example 1 except that the fluorine-containing diol compound of preparation example 1 was used in an amount of 3 parts.
Example 5
The remainder was the same as in example 1 except that in the B component, 14 parts of 1, 5-naphthalene diisocyanate was used.
Comparative example 1
The other components were the same as in example 1 except that trimethylolpropane was used in an amount of 6 parts by weight in the starting material of component A, and the fluorine-containing diol compound was not contained.
Comparative example 2
The remainder is the same as in example 1 except that in the raw material for the A-component, the fluorine-containing diol compound is replaced with the diol produced in comparative preparation example 1.
The spray air-tight plugging polyurethane foams prepared in the above examples 1 to 5 and comparative examples 1 to 2 were sprayed on a board by a spray coater to prepare foams, and the prepared foams were subjected to the following performance tests:
water vapor transmission rate: measurement of the Water vapor Transmission Properties of QB/T2411-1998, g/m 2· 24h。
Ultraviolet aging resistance: ultraviolet ageing oven with temperature of 50 ℃ and irradiation intensity of 400 mu w/cm 2 The time is 500h.
Compressive strength: with reference to standard GB/T8813-2008, the materials are tested for compressive strength before and after ultraviolet aging, KPa.
Table 1 spray air tight shutoff polyurethane performance test
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It can be seen from table 1 that the polyurethane foam prepared by the invention has good mechanical properties and ultraviolet aging resistance, and the mechanical properties after ultraviolet aging are stable, so that the working safety of power equipment can be greatly improved.
The foregoing detailed description is directed to one of the possible embodiments of the present invention, which is not intended to limit the scope of the invention, but is to be accorded the full scope of all such equivalents and modifications so as not to depart from the scope of the invention.
Claims (5)
1. The spray airtight plugging polyurethane foam comprises A, B two components, and is characterized in that the mass ratio of A, B two components is 1:1-2, wherein the component A comprises the following raw materials in parts by weight: 100 parts of polymer polyol, 1-5 parts of foaming agent, 1-3 parts of micromolecular polyol, 3-5 parts of fluorine-containing dihydric alcohol compound, 2-6 parts of catalyst and 1-3 parts of foam stabilizer; the foaming agent is water;
the fluorine-containing dihydric alcohol compound is prepared by a method comprising the following steps: adding fluorine-containing ester, amino diol compound, solvent and catalyst into a reaction kettle, stirring until the mixture is uniform, heating to a reflux state, reacting at constant temperature, and distilling under reduced pressure after the reaction is finished to obtain fluorine-containing dihydric alcohol compound;
the solvent is selected from one or more of diethyl ether, acetone, methanol and ethanol; the reaction is carried out at constant temperature for 5-8h; the catalyst is selected from one of sodium methoxide and sodium ethoxide, and the dosage of the catalyst is 0.5-1.0wt% of the total weight of fluorine-containing ester and amino diol compounds;
the molar ratio of the fluorine-containing ester to the amino diol compound is 1:1.1-1.25; the fluorine-containing ester is selected from methyl trifluoroacetate, ethyl trifluoroacetate, methyl 2, 3-tetrafluoropropionate, ethyl 2, 3-tetrafluoropropionate methyl pentafluoropropionate, ethyl pentafluoropropionate, methyl 4, 4-trifluorobutyrate, ethyl 4, 4-trifluorobutyrate, or a combination of two or more thereof; the amino diol compound is selected from one or more than two of 3-amino-1, 2-propanediol, 2- (aminomethyl) -1, 3-propanediol, 2-amino-2-ethyl-1, 3-propanediol and serinol;
the component B comprises the following raw materials: the content of the polymeric MDI and the 1, 5-naphthalene diisocyanate is 14-18wt% of the polymeric MDI.
2. The spray gas-tight shutoff polyurethane foam of claim 1, wherein the polymeric MDI has an NCO content of 30 to 35 weight percent.
3. The spray gas-tight shutoff polyurethane foam of claim 1, wherein the polymer polyol has a hydroxyl value of 300 to 800mgKOH/g and a functionality of 2 to 6, and the polymer polyol is one or a combination of two of a polyether polyol or a polyester polyol.
4. The spray gas-tight shutoff polyurethane foam of claim 1, wherein the small molecule polyol is selected from one or more of 1, 4-butanediol, ethylene glycol, diethylene glycol, propylene glycol, and trimethylolpropane.
5. The method for preparing the spray-coated airtight sealed polyurethane foam according to any one of claims 1 to 4, comprising the steps of:
weighing the raw materials of the component A: uniformly mixing polymer polyol, a foaming agent, micromolecular polyol, a fluorine-containing dihydric alcohol compound, a catalyst and a foam stabilizer to obtain a component A; weighing the raw materials of the component B, namely polymeric MDI and 1, 5-naphthalene diisocyanate, heating and uniformly stirring at a constant temperature, and discharging to obtain the component B.
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Citations (9)
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