CN112679788A - Nano composite foaming agent for preparing polyurethane and preparation method thereof - Google Patents
Nano composite foaming agent for preparing polyurethane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nano composite foaming agent for preparing polyurethane, and particularly relates to the technical field of foaming agents, wherein the nano composite foaming agent comprises the following raw materials: 4, 4-oxo-bis-benzenesulfonyl hydrazide, modified nano-silica and layered montmorillonite. According to the invention, after pore-expanding treatment, polymer grafting reaction is carried out on mesoporous silica, so that the mesoporous silica has an oversized mesoporous channel, the mesoporous silica has excellent dispersibility and good interface compatibility, and then n-octanol is added to carry out modification treatment on the mesoporous silica and acetone, so that a nano composite foaming agent can be more uniformly dispersed into polyurethane, and the local foaming agent amount is reduced.
Description
Technical Field
The invention relates to the technical field of foaming agents, in particular to a nano composite foaming agent for preparing polyurethane and a preparation method thereof.
Background
In the field of polymer technology, polyurethane foam is the most commonly used polymer heat insulation material at present, has the advantages of light weight, high strength, heat conductivity and the like, and is widely applied to the specific fields of building energy-saving materials, automobile interiors, cold storage and heat preservation materials, refrigerators and the like. An important parameter for determining whether polyurethane foam has excellent thermal insulation properties is the thermal conductivity. While polyurethane foam's heat transfer relies primarily on three approaches: gas phase conduction in the foam cells, solid phase conduction of the foam body, and thermal radiation. At lower temperatures, thermal radiation heat transfer is minimal, so that gas phase conduction within the cells, which accounts for about 90% of the foam volume, has the greatest effect on thermal conductivity, i.e., the magnitude of the foam thermal conductivity depends primarily on the type and amount of blowing agent used. At present, most of these blowing agents are chlorofluorocarbon substances except cyclopentane, and because of their ability to destroy the atmospheric ozone layer, the governments have signed the international convention of "montreal protocol" to limit and phase out, banning the production and use of such products.
The prior art uses water as a polyurethane blowing agent. However, the solubility of water molecules in polyester polyols and/or polyether polyols is not good due to the very strong hydrogen bonding in water molecules, which leads to the water molecules usually being present in the polyether polyol component in the form of droplets, often causing local excessive foaming, which in turn affects the strength and thermal insulation properties of the final material. Halogenated olefins, represented by the class of hexafluorobutenes, such as 1, 1, 1, 4,4, 4-hexafluoro-2-butene, in addition to carbon dioxide and water, belong to the class of liquid blowing agents, having the following advantages: ODP is close to 0, GWP value is less than 7, toxicity is small, the foaming agent is not flammable under normal temperature and normal pressure, and the foaming agent is a better fourth-generation foaming agent with small thermal conductivity coefficient (10.2 mW/(m.K)) at 25 ℃ and is increasingly applied to the foaming agent.
The existing foaming agent for polyurethane has large particle size and is not uniform enough to cause local overheating, the size of a foam hole is not easy to control, and the foaming efficiency and the quality are greatly reduced, so that the application of the foaming agent in microporous foam plastic is limited.
Disclosure of Invention
In order to overcome the above defects in the prior art, embodiments of the present invention provide a nanocomposite blowing agent for preparing polyurethane and a preparation method thereof, and the problems to be solved by the present invention are: how to ensure that the foaming agent is dispersed uniformly and improve the quality of the foaming agent.
In order to achieve the purpose, the invention provides the following technical scheme: a nano composite foaming agent for preparing polyurethane comprises the following raw materials in parts by weight: 80-120 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 30-50 parts of modified nano-silica and 20-30 parts of layered montmorillonite.
In a preferred embodiment, the feed comprises the following raw materials in parts by weight: 90-110 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 35-45 parts of modified nano-silica and 23-27 parts of layered montmorillonite.
In a preferred embodiment, the feed comprises the following raw materials in parts by weight: 100 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 40 parts of modified nano-silica and 25 parts of layered montmorillonite.
In a preferred embodiment, the layered montmorillonite is calcium-based montmorillonite, and the particle size of the layered montmorillonite is 20-70 um.
The invention also provides a preparation method of the nano composite foaming agent for preparing polyurethane, which comprises the following specific preparation steps:
the method comprises the following steps: preparation of modified nano-silica
Weighing a certain amount of mesoporous silica, reaming by using a salt soaking method, adding a copolymer for grafting reaction after reaming treatment, adding n-octanol into a grafted product, heating and refluxing for 3-6h, extracting for 8-10h by using acetone after heating and refluxing are finished, and drying for 10-12h at 60-70 ℃ after extraction is finished to obtain modified nano-silica;
step two: treatment of layered montmorillonite
Adding hydrochloric acid into the weighed layered montmorillonite for modification to obtain hydrogenated montmorillonite, dispersing the hydrogenated montmorillonite into water, stirring, carrying out ultrasonic treatment, adding dimethylformamide, and carrying out ultrasonic treatment to obtain stripped montmorillonite for later use;
step three: preparation of nano composite foaming agent
Adding a solvent into the weighed 4, 4-oxo-bis-benzenesulfonylhydrazide, mixing, adding the modified nano-silica and the peeled montmorillonite into the mixed solution, slowly stirring for 5-10 minutes under the assistance of ultrasonic waves, washing, drying, and drying to constant weight to obtain the nano-composite foaming agent.
In a preferred embodiment, the salt used in the step-one salt leaching method comprises a mixture of one or more than two alkali metal salts, wherein the mass concentration of the salt is 30-60%, and the alkali metal salt is a double salt consisting of one or more than two of sodium chloride, lithium chloride or potassium nitrate.
In a preferred embodiment, the pore-expanding treatment in the first step is performed by adding mesoporous silica into a salt solution and then calcining the mesoporous silica by a temperature programming method, wherein the temperature programming method comprises the following steps: (1) raising the temperature from room temperature to a first calcining temperature, and keeping the temperature for 30-60 minutes; (2) raising the temperature from a first calcining temperature to a second calcining temperature, and keeping the temperature for 3-5h, wherein the first calcining temperature is 200-300 ℃, and the second calcining temperature is 400-600 ℃.
In a preferred embodiment, the temperature of the heated reflux in step one is 60 to 68 ℃.
In a preferred embodiment, the ultrasonic treatment time of the hydrogenated montmorillonite in water in the second step is 10-40 minutes, the ultrasonic treatment time of the hydrogenated montmorillonite in a dimethylformamide solution is 20-60 minutes, and the particle size of the exfoliated montmorillonite in the second step is 10-20 um.
In a preferred embodiment, the solvent in step three is dimethyl sulfoxide, the slow stirring rate in step three is 100-150 rpm, and the washing in step three is performed by a mixed solution of methanol, 4 '-oxybis-benzenesulfonylhydrazide and N, N' -dimethylformamide, and then by a methanol solution.
The invention has the technical effects and advantages that:
1. according to the nano composite foaming agent for preparing polyurethane, which is prepared by adopting the raw material formula, modified nano silicon dioxide is added, and polymer grafting reaction is carried out on the mesoporous silicon dioxide after reaming treatment, so that the mesoporous silicon dioxide has an oversized mesoporous channel, the mesoporous silicon dioxide has excellent dispersibility and good interface compatibility, and then n-octanol is added to carry out modification treatment on the mesoporous silicon dioxide and acetone, so that the nano composite foaming agent can be more uniformly dispersed into polyurethane to reduce the local foaming dose;
2. the layered montmorillonite is added to treat the layered montmorillonite to obtain the stripped montmorillonite, the organic foaming agent is embedded between the nano-scale montmorillonite layers and has weak interaction with the laminates, and the laminates of the inorganic clay provide a large number of nucleation points for the organic foaming agent between the layers, so that the formed bubbles are uniform, the foam holes are small, the decomposition is avoided in the compounding process, the dosage of the foaming agent is effectively controlled, the purpose of refining the foaming agent is achieved, and the local overheating in the foaming process is avoided.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the invention provides a nano composite foaming agent for preparing polyurethane, which comprises the following raw materials in parts by weight: 80 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 30 parts of modified nano-silica and 20 parts of layered montmorillonite.
In a preferred embodiment, the layered montmorillonite is calcium-based montmorillonite, and the particle size of the layered montmorillonite is 20-70 um.
The invention also provides a preparation method of the nano composite foaming agent for preparing polyurethane, which comprises the following specific preparation steps:
the method comprises the following steps: preparation of modified nano-silica
Weighing a certain amount of mesoporous silica, reaming by using a salt soaking method, adding a copolymer after reaming treatment for grafting reaction, adding n-octanol into a grafted product, heating and refluxing for 4 hours, extracting for 9 hours by using acetone after heating and refluxing are finished, and drying for 12 hours at 65 ℃ after extraction is finished to obtain modified nano-silica;
step two: treatment of layered montmorillonite
Adding hydrochloric acid into the weighed layered montmorillonite for modification to obtain hydrogenated montmorillonite, dispersing the hydrogenated montmorillonite into water, stirring, carrying out ultrasonic treatment, adding dimethylformamide, and carrying out ultrasonic treatment to obtain stripped montmorillonite for later use;
step three: preparation of nano composite foaming agent
Adding a solvent into the weighed 4, 4-oxo-bis-benzenesulfonylhydrazide, mixing, adding the modified nano-silica and the peeled montmorillonite into the mixed solution, slowly stirring for 8 minutes under the assistance of ultrasonic waves, washing, drying, and drying to constant weight to obtain the nano-composite foaming agent.
In a preferred embodiment, the salt used in the step-one salt leaching method comprises a mixture of one or more than two alkali metal salts, the mass concentration of the salt is 45%, and the alkali metal salt is a double salt composed of one or more than two of sodium chloride, lithium chloride or potassium nitrate.
In a preferred embodiment, the pore-expanding treatment in the first step is performed by adding mesoporous silica into a salt solution and then calcining the mesoporous silica by a temperature programming method, wherein the temperature programming method comprises the following steps: (1) raising the temperature from room temperature to the first calcining temperature, and keeping the temperature for 45 minutes; (2) and (3) raising the temperature from a first calcining temperature to a second calcining temperature, keeping the temperature for 4 hours, wherein the first calcining temperature is 250 ℃, and the second calcining temperature is 500 ℃.
In a preferred embodiment, the temperature of the heated reflux in step one is 64 ℃.
In a preferred embodiment, the ultrasonic treatment time of the hydrogenated montmorillonite in water in the second step is 25 minutes, the ultrasonic treatment time of the hydrogenated montmorillonite in a dimethylformamide solution is 40 minutes, and the particle size of the exfoliated montmorillonite in the second step is 10-20 um.
In a preferred embodiment, the solvent in step three is dimethyl sulfoxide, the slow stirring rate in step three is 130 rpm, and the washing in step three is performed by a mixed solution of methanol, 4 '-oxybis-benzenesulfonylhydrazide and N, N' -dimethylformamide, and then by a methanol solution.
Example 2:
different from the embodiment 1, the material comprises the following raw materials in parts by weight: 100 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 40 parts of modified nano-silica and 25 parts of layered montmorillonite.
Example 3:
different from the examples 1-2, the material comprises the following raw materials in parts by weight: 120 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 50 parts of modified nano-silica and 30 parts of layered montmorillonite.
Example 4:
a nano composite foaming agent for preparing polyurethane comprises the following raw materials in parts by weight: 100 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 40 parts of modified nano-silica and 25 parts of layered montmorillonite.
In a preferred embodiment, the layered montmorillonite is calcium-based montmorillonite, and the particle size of the layered montmorillonite is 20-70 um.
The invention also provides a preparation method of the nano composite foaming agent for preparing polyurethane, which comprises the following specific preparation steps:
the method comprises the following steps: preparation of modified nano-silica
Weighing a certain amount of mesoporous silica, reaming by using a salt soaking method, adding a copolymer after reaming treatment, and carrying out grafting reaction to obtain modified nano-silica;
step two: treatment of layered montmorillonite
Adding hydrochloric acid into the weighed layered montmorillonite for modification to obtain hydrogenated montmorillonite, dispersing the hydrogenated montmorillonite into water, stirring, carrying out ultrasonic treatment, adding dimethylformamide, and carrying out ultrasonic treatment to obtain stripped montmorillonite for later use;
step three: preparation of nano composite foaming agent
Adding a solvent into the weighed 4, 4-oxo-bis-benzenesulfonylhydrazide, mixing, adding the modified nano-silica and the peeled montmorillonite into the mixed solution, slowly stirring for 8 minutes under the assistance of ultrasonic waves, washing, drying, and drying to constant weight to obtain the nano-composite foaming agent.
In a preferred embodiment, the salt used in the step-one salt leaching method comprises a mixture of one or more than two alkali metal salts, the mass concentration of the salt is 45%, and the alkali metal salt is a double salt composed of one or more than two of sodium chloride, lithium chloride or potassium nitrate.
In a preferred embodiment, the pore-expanding treatment in the first step is performed by adding mesoporous silica into a salt solution and then calcining the mesoporous silica by a temperature programming method, wherein the temperature programming method comprises the following steps: (1) raising the temperature from room temperature to the first calcining temperature, and keeping the temperature for 45 minutes; (2) and (3) raising the temperature from a first calcining temperature to a second calcining temperature, keeping the temperature for 4 hours, wherein the first calcining temperature is 250 ℃, and the second calcining temperature is 500 ℃.
In a preferred embodiment, the ultrasonic treatment time of the hydrogenated montmorillonite in water in the second step is 25 minutes, the ultrasonic treatment time of the hydrogenated montmorillonite in a dimethylformamide solution is 40 minutes, and the particle size of the exfoliated montmorillonite in the second step is 10-20 um.
In a preferred embodiment, the solvent in step three is dimethyl sulfoxide, the slow stirring rate in step three is 130 rpm, and the washing in step three is performed by a mixed solution of methanol, 4 '-oxybis-benzenesulfonylhydrazide and N, N' -dimethylformamide, and then by a methanol solution.
Example 5:
a nano composite foaming agent for preparing polyurethane comprises the following raw materials in parts by weight: 100 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 40 parts of modified nano-silica and 25 parts of layered montmorillonite.
In a preferred embodiment, the layered montmorillonite is calcium-based montmorillonite, and the particle size of the layered montmorillonite is 20-70 um.
The invention also provides a preparation method of the nano composite foaming agent for preparing polyurethane, which comprises the following specific preparation steps:
the method comprises the following steps: preparation of modified nano-silica
Weighing a certain amount of mesoporous silica, adding n-octanol, heating and refluxing for 4h, extracting with acetone for 9h after heating and refluxing, and drying at 65 ℃ for 12h after extraction to obtain modified nano-silica;
step two: treatment of layered montmorillonite
Adding hydrochloric acid into the weighed layered montmorillonite for modification to obtain hydrogenated montmorillonite, dispersing the hydrogenated montmorillonite into water, stirring, carrying out ultrasonic treatment, adding dimethylformamide, and carrying out ultrasonic treatment to obtain stripped montmorillonite for later use;
step three: preparation of nano composite foaming agent
Adding a solvent into the weighed 4, 4-oxo-bis-benzenesulfonylhydrazide, mixing, adding the modified nano-silica and the peeled montmorillonite into the mixed solution, slowly stirring for 8 minutes under the assistance of ultrasonic waves, washing, drying, and drying to constant weight to obtain the nano-composite foaming agent.
In a preferred embodiment, the temperature of the heated reflux in step one is 64 ℃.
In a preferred embodiment, the ultrasonic treatment time of the hydrogenated montmorillonite in water in the second step is 25 minutes, the ultrasonic treatment time of the hydrogenated montmorillonite in a dimethylformamide solution is 40 minutes, and the particle size of the exfoliated montmorillonite in the second step is 10-20 um.
In a preferred embodiment, the solvent in step three is dimethyl sulfoxide, the slow stirring rate in step three is 130 rpm, and the washing in step three is performed by a mixed solution of methanol, 4 '-oxybis-benzenesulfonylhydrazide and N, N' -dimethylformamide, and then by a methanol solution.
The nano composite foaming agents for preparing polyurethane prepared in the embodiments 1 to 3 are respectively taken as an experimental group 1, an experimental group 2 and an experimental group 3, the embodiments 4 and 5 are taken as a control group 1 and a control group 2, the traditional composite foaming agents for polyurethane are used as a control group 3 for testing, an electron microscope is used for scanning and analyzing the foaming agents produced by the experimental group 1, the experimental group 2, the experimental group 3, the control group 1, the control group 2 and the control group 3, and the NanoMeasure software is used for carrying out statistical analysis on the electron microscope images to obtain the percentage of the pore diameter of the foaming agent smaller than 50um, the diameter of the foaming agent cells and the density of the cells. The measurement results are shown in the table I:
| pore size less than 50um (%) | Average cell diameter (um) | Cell density (pieces/cm)-3） | |
| Experimental group 1 | 75.0 | 40.9 | 1.0×106 |
| Experimental group 2 | 79.4 | 32.6 | 1.5×106 |
| Experimental group 3 | 78.2 | 36.5 | 1.2×106 |
| Control group 1 | 49.6 | 50.3 | 9.9×105 |
| Control group 2 | 46.7 | 54.8 | 7.9×105 |
| Control group 3 | 35.7 | 64.4 | 2.9×105 |
Watch 1
As can be seen from the table I, compared with the traditional composite foaming agent, the nano composite foaming agent for preparing polyurethane produced by the invention has smaller average cell diameter, higher cell density and higher percentage of the cell diameter less than 50um, and in examples 4 and 5, n-octanol is not added and hole expanding treatment is not carried out in the production process, respectively, the foaming agents produced in examples 4 and 5 have larger average cell diameter and lower cell density, through adding modified nano-silica, the mesoporous silica is subjected to polymer grafting reaction after hole expanding treatment, so that the mesoporous silica has oversized mesoporous channels, thereby the mesoporous silica has excellent dispersibility and good interface compatibility, then n-octanol is added to carry out modification treatment on the mesoporous silica and acetone, so that the nano composite foaming agent can be more uniformly dispersed into polyurethane, the nano composite foaming agent provided by the invention has small particle size and high loading amount of a chemical foaming agent, so that microporous foam plastic with better foaming quality can be obtained, the layered montmorillonite is added and treated to obtain the exfoliated montmorillonite, the organic foaming agent is embedded between the nano-scale montmorillonite layers and has weak interaction with the laminates, the laminates of the inorganic clay provide a large amount of nucleation points for the organic foaming agent between the layers, so that the formed bubbles are more uniform, the cells are smaller, the decomposition is not generated in the compounding process, the dosage of the foaming agent is effectively controlled, the purpose of refining the foaming agent is achieved, and the local overheating in the foaming process is avoided.
And finally: the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (10)
1. A nanometer composite foaming agent for preparing polyurethane is characterized in that: the feed comprises the following raw materials in parts by weight: 80-120 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 30-50 parts of modified nano-silica and 20-30 parts of layered montmorillonite.
2. The nanocomposite blowing agent for preparing polyurethane according to claim 1, wherein: the feed comprises the following raw materials in parts by weight: 90-110 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 35-45 parts of modified nano-silica and 23-27 parts of layered montmorillonite.
3. The nanocomposite blowing agent for preparing polyurethane according to claim 1, wherein: the feed comprises the following raw materials in parts by weight: 100 parts of 4, 4-oxo-bis-benzenesulfonyl hydrazide, 40 parts of modified nano-silica and 25 parts of layered montmorillonite.
4. The nanocomposite blowing agent for preparing polyurethane according to claim 1, wherein: the layered montmorillonite is calcium-based montmorillonite, and the particle size of the layered montmorillonite is 20-70 um.
5. The method for preparing a nanocomposite blowing agent for polyurethane according to any one of claims 1 to 4, wherein: the preparation method comprises the following specific steps:
the method comprises the following steps: preparation of modified nano-silica
Weighing a certain amount of mesoporous silica, reaming by using a salt soaking method, adding a copolymer for grafting reaction after reaming treatment, adding n-octanol into a grafted product, heating and refluxing for 3-6h, extracting for 8-10h by using acetone after heating and refluxing are finished, and drying for 10-12h at 60-70 ℃ after extraction is finished to obtain modified nano-silica;
step two: treatment of layered montmorillonite
Adding hydrochloric acid into the weighed layered montmorillonite for modification to obtain hydrogenated montmorillonite, dispersing the hydrogenated montmorillonite into water, stirring, carrying out ultrasonic treatment, adding dimethylformamide, and carrying out ultrasonic treatment to obtain stripped montmorillonite for later use;
step three: preparation of nano composite foaming agent
Adding a solvent into the weighed 4, 4-oxo-bis-benzenesulfonylhydrazide, mixing, adding the modified nano-silica and the peeled montmorillonite into the mixed solution, slowly stirring for 5-10 minutes under the assistance of ultrasonic waves, washing, drying, and drying to constant weight to obtain the nano-composite foaming agent.
6. The method of claim 5, wherein the blowing agent is selected from the group consisting of: the salt used in the step one salt impregnation method comprises a mixture of one or more than two alkali metal salts, the mass concentration of the salt is 30-60%, and the alkali metal salt is a complex salt consisting of one or more than two of sodium chloride, lithium chloride or potassium nitrate.
7. The method of claim 6, wherein the blowing agent is selected from the group consisting of: the pore-expanding treatment in the first step is to add mesoporous silica into a salt solution and then calcine the mesoporous silica by a programmed heating method, wherein the programmed heating process comprises the following steps: (1) raising the temperature from room temperature to a first calcining temperature, and keeping the temperature for 30-60 minutes; (2) raising the temperature from a first calcining temperature to a second calcining temperature, and keeping the temperature for 3-5h, wherein the first calcining temperature is 200-300 ℃, and the second calcining temperature is 400-600 ℃.
8. The method of claim 7, wherein the blowing agent is selected from the group consisting of: the temperature of heating reflux in the first step is 60-68 ℃.
9. The method of claim 5, wherein the blowing agent is selected from the group consisting of: the ultrasonic treatment time of the hydrogenated montmorillonite in the water in the second step is 10-40 minutes, the ultrasonic treatment time of the hydrogenated montmorillonite in the dimethylformamide solution is 20-60 minutes, and the particle size of the peeled montmorillonite in the second step is 10-20 um.
10. The method of claim 5, wherein the blowing agent is selected from the group consisting of: the solvent in the third step is dimethyl sulfoxide, the slow stirring speed in the third step is 100-150 rpm, and the third step is washing by using a mixed solution of methanol, 4 '-oxybis-benzenesulfonyl hydrazide and N, N' -dimethylformamide and then washing by using a methanol solution.
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Application publication date: 20210420 |