CN113502055B - High-flame-retardance high-damping organic silicon foam material as well as preparation method and application thereof - Google Patents
High-flame-retardance high-damping organic silicon foam material as well as preparation method and application thereof Download PDFInfo
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- CN113502055B CN113502055B CN202110765611.5A CN202110765611A CN113502055B CN 113502055 B CN113502055 B CN 113502055B CN 202110765611 A CN202110765611 A CN 202110765611A CN 113502055 B CN113502055 B CN 113502055B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a high-flame-retardance high-damping organic silicon foam material as well as a preparation method and application thereof, wherein the organic silicon foam material comprises the following components in parts by mass: 5-20 parts of hydroxyl silicone oil; 15-65 parts of vinyl silicone oil; 5-20 parts of hydrogen-containing silicone oil; 10-40 parts of phosphorus-nitrogen-containing mesoporous silica; 1-3 parts of a catalyst; 0.1-0.5 part of inhibitor; the particle size of the phosphorus-nitrogen containing mesoporous silica is 30-400 nm. The invention adopts hydroxyl silicone oil, vinyl silicone oil, hydrogen-containing silicone oil and phosphorus-nitrogen-containing mesoporous silicon dioxide with the particle size of 30-400 nm to compound, realizes rigidity-toughness balance of the organic silicon foam material, improves the damping performance and the flame retardant performance of the organic silicon foam material, and can be widely applied to the preparation of various fireproof materials.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high-flame-retardance high-damping organic silicon foam material and a preparation method and application thereof.
Background
The organic silicon foam is a universal elastic material, combines the characteristics of the silicon rubber and the foam material, and has the advantages of no toxicity, good chemical stability and good electrical insulation. As a high-performance material, the organic silicon foam is applied to the fields of aerospace, national defense, medicine, transportation, electricity, construction and the like. Compared with the traditional high polymer material, the organic silicon foam material has a special organic-inorganic hybrid structure, the main chain of the inorganic siloxane is an incombustible part, and a certain flame retardant property is endowed to the organic silicon foam material, but the side chain of the organic silicon foam material is rich in hydrocarbon groups, so that the organic silicon foam material is combustible. Once ignited, silicone foams can burn and release suffocating fumes, and silicone foams have an extremely rich cell structure, exhibiting greater airflow and greater specific surface area, making them more conducive to combustion. Therefore, flame retardancy achieved solely by non-flammable ingredients of the inorganic silicone backbone has not been satisfactory for use.
The Chinese invention patent CN111500071A discloses an organosilicon foam material which is prepared by taking an organosilicon polymer as a matrix and adding a reinforcing material and a flame-retardant filler, and the organosilicon foam material has higher rigidity and better flame-retardant property, but has the problems of insufficient toughness (elongation at break is less than 150%) and low damping (sound absorption coefficient is less than 0.5). Accordingly, there is a need to provide silicone foams having an excellent combination of properties.
Disclosure of Invention
The invention aims to solve the problems that the prior art cannot combine high toughness (elongation at break > 150%), high rigidity (tensile strength >1 MPa), high damping (sound absorption coefficient > 0.5) and excellent flame retardant property, and provides a high-flame-retardant high-damping silicone foam material.
The invention also aims to provide a preparation method of the high-flame-retardant high-damping organic silicon foam material.
It is a further object of the present invention to provide the use of the above high flame retardant, high damping silicone foam.
The above object of the present invention is achieved by the following technical solutions:
a high-flame-retardance high-damping organic silicon foam material comprises the following components in parts by mass:
the particle size of the phosphorus-nitrogen containing mesoporous silica is 30-400 nm.
In the invention, hydroxyl silicone oil and hydrogen-containing silicone oil are subjected to dehydrogenation reaction to generate hydrogen as an internal foaming agent, and are simultaneously crosslinked with vinyl silicone oil, so that the foam strength and porosity of the organic silicon foam are controlled, the organic silicon foam has sufficient mechanical properties, the rigidity strength and the crack growth prevention capability of the phosphorus-nitrogen-containing mesoporous silicon dioxide with the particle size of 30-400 nm can endow the material with high rigidity, high toughness and excellent flame retardant property, and the mesoporous structure of the organic silicon foam has excellent energy absorption and shock absorption effects, so that the organic silicon foam material can give consideration to high toughness (elongation at break > 150%), high rigidity (tensile strength >1 MPa), high damping (sound absorption coefficient > 0.5) and excellent flame retardant property.
Preferably, the high-flame-retardant high-damping organosilicon foam material is prepared from the following raw materials in parts by mass:
preferably, the particle size of the phosphorus-nitrogen containing mesoporous silica is 200 to 300nm.
The hydroxyl silicone oil is hydroxyl-terminated polymethylsiloxane and/or hydroxyl-terminated polymethylphenylsiloxane.
The vinyl silicone oil of the invention has a vinyl mass fraction of 1-5% and a viscosity of 5000-10000 mPas.
The hydrogen-containing silicone oil is selected from one or more of trimethylsiloxy end-capped polyhydrocarbon hydrogen siloxane, phenyl hydrogen-containing polysiloxane and ethylene hydrogen-containing polysiloxane.
The hydrogen content in the hydrogen-containing silicone oil is 0.5mol% -0.7 mol%.
The inhibitor is selected from one or more of methylbutynol, ethynl cyclohexanol and methyl maleate.
The preparation method of the phosphorus-nitrogen-containing mesoporous silica comprises the following steps:
s1, adding mesoporous silica with the particle size of 30-400 nm prepared by a sol-gel method into a zinc sulfate aqueous solution, and performing ultrasonic dispersion to obtain a mesoporous silica-zinc solution;
s2, preparing an amino trimethylene phosphonic acid or ammonium polyphosphate and zinc sulfate aqueous solution, and uniformly dispersing by ultrasonic;
and S3, adding the amino trimethylene phosphonic acid or ammonium polyphosphate obtained by the preparation of the S2 and a zinc sulfate aqueous solution into a mesoporous silica-zinc solution, and carrying out post-treatment to obtain the mesoporous silica containing phosphorus and nitrogen.
The invention also provides a preparation method of the high-flame-retardant high-damping organosilicon foam material, which comprises the following steps:
mixing and stirring hydroxyl silicone oil, vinyl silicone oil, a catalyst, phosphorus-nitrogen-containing mesoporous silicon dioxide and an inhibitor according to a proportion, adding hydrogen-containing silicone oil, stirring uniformly, and curing and foaming to obtain the organic silicon foam material.
The invention also protects the application of the high-flame-retardant high-damping organic silicon foam material in a fireproof material.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a high-flame-retardant high-damping organic silicon foam material, which is prepared by compounding hydroxyl silicone oil, vinyl silicone oil, hydrogen-containing silicone oil and phosphorus-nitrogen-containing mesoporous silicon dioxide, realizes rigidity-toughness balance of the organic silicon foam material, improves the damping performance and the flame-retardant performance of the organic silicon foam material, and can be widely applied to various fireproof materials.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, but the embodiments of the present invention are not limited thereto.
The reagents, methods and equipment adopted by the invention are conventional in the technical field if no special description is given.
The high-flame-retardant high-damping organic silicon foam material of each embodiment and the comparative example is prepared by the following steps:
mixing and stirring hydroxyl silicone oil, vinyl silicone oil, a catalyst, phosphorus-nitrogen-containing mesoporous silicon dioxide and an inhibitor according to a proportion, adding hydrogen-containing silicone oil, stirring uniformly, curing, foaming and drying to obtain the organic silicon foam material. The curing time is 3-5 min, and the drying temperature is 80 ℃.
Example 1
A preparation method of a phosphorus-nitrogen-containing mesoporous silicon dioxide flame retardant comprises the following steps:
s1, dissolving 4.8g of hexadecyl trimethyl ammonium bromide in 192ml of deionized water, continuously stirring at 30 ℃, then adding 102ml of ethanol and 19.2ml of alkaline catalyst into the mixed solution, keeping for 10 minutes under stirring, then adding 7ml of tetraethyl orthosilicate into the previous solution, pouring the reaction mixed solution into 300ml of deionized water after 35 seconds, and keeping stirring by magnetic force; after dilution, 2mol/L HCl solution is dripped to neutralize the system for 180s until the pH value of the system is reduced to 9.5 from 11, so as to obtain silicon dioxide suspension, the silicon dioxide suspension is placed into a muffle furnace at 550-600 ℃ to be calcined for 6h after high-speed centrifugation and suction filtration, and the template agent is removed, so as to obtain mesoporous silicon dioxide powder with the particle size of 200-300 nm;
s2, pouring the mesoporous silica powder with the particle size of 200-300 nm prepared in the step S1 into a zinc sulfate aqueous solution with the concentration of 0.3%, and performing ultrasonic dispersion for 2 hours to obtain a mesoporous silica-zinc solution; and preparing aminotrimethylene phosphonic acid (or ammonium polyphosphate) and 50% zinc sulfate aqueous solution, uniformly dispersing by ultrasonic, then dropwise adding the mixture into the mesoporous silica solution, stirring for 24 hours, centrifugally dispersing, washing for several times by using deionized water, and drying in vacuum at 80 ℃ for 48 hours to obtain the phosphorus and nitrogen containing mesoporous silica flame retardant with the particle size of 200-300 nm, which is marked as phosphorus and nitrogen containing mesoporous silica A.
Example 2
The difference between this example and example 1 is that, in step S1, the stirring temperature of the solution of cetyltrimethylammonium bromide in deionized water is 35 ℃, and the phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 150 to 200nm is obtained, and is labeled as phosphorus-nitrogen-containing mesoporous silica B.
Example 3
The difference between this example and example 1 is that, in step S1, the stirring temperature of the solution of cetyltrimethylammonium bromide in deionized water is 40 ℃, so as to obtain a phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 100-200 nm, which is labeled as phosphorus-nitrogen-containing mesoporous silica C.
Example 4
The difference between this embodiment and embodiment 1 is that, in step S1, the stirring temperature of the solution of cetyltrimethylammonium bromide in deionized water is 42 ℃, so as to obtain the phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 130-150 nm, which is labeled as phosphorus-nitrogen-containing mesoporous silica D.
Example 5
The difference between this embodiment and embodiment 1 is that, in step S1, the stirring temperature of hexadecyl trimethyl ammonium bromide dissolved in deionized water is 45 ℃, so as to obtain the phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 50-150 nm, which is denoted as phosphorus-nitrogen-containing mesoporous silica E.
Example 6
The difference between this example and example 1 is that, in step S1, the stirring temperature of the solution of cetyltrimethylammonium bromide in deionized water is 50 ℃, and the phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 30-100 nm is obtained, and is labeled as phosphorus-nitrogen-containing mesoporous silica F.
Example 7
The difference between this example and example 1 is that, in step S1, the stirring temperature of the solution of cetyltrimethylammonium bromide in deionized water is 25 ℃, and the phosphorus-nitrogen-containing mesoporous silica flame retardant with a particle size of 300 to 400nm is obtained, and is labeled as phosphorus-nitrogen-containing mesoporous silica G.
Examples 8 to 11
The embodiment provides a series of high-flame-retardant high-damping silicone foam materials, the content of the selected hydroxyl silicone oil in different embodiments is different, and the specific formula is shown in table 1, so as to explore the influence of different hydroxyl silicone oil contents on the performance of the silicone foam materials.
TABLE 1 examples 8-11 formulations of Silicone foams
Examples 12 to 14
The embodiment provides a series of high flame retardant and high damping silicone foams, different embodiments have different vinyl silicone oil contents, and the specific formula is shown in table 2, so as to explore the influence of different vinyl silicone oil contents on the performance of the silicone foams.
TABLE 2 examples 12-14 formulations of Silicone foams
| Example 12 | Example 13 | Example 14 | |
| Hydroxyl silicone oil | 10 | 10 | 10 |
| Vinyl silicone oil | 15 | 45 | 65 |
| Hydrogen-containing silicone oil | 10 | 10 | 10 |
| Mesoporous silica A containing phosphorus and nitrogen | 20 | 20 | 20 |
| Platinum catalyst | 2 | 2 | 2 |
| Inhibitors | 0.2 | 0.2 | 0.2 |
Examples 15 to 17
The embodiment provides a series of high flame retardant and high damping silicone foam materials, different hydrogen-containing silicone oil contents selected in different embodiments are different, and the specific formula is shown in table 3 to explore the influence of different hydrogen-containing silicone oil contents on the performance of the silicone foam materials.
TABLE 3 examples 15-17 formulation of silicone foams
| Example 15 | Example 16 | Example 17 | |
| Hydroxy silicone oil | 10 | 10 | 10 |
| Vinyl silicone oil | 30 | 30 | 30 |
| Hydrogen-containing silicone oil | 5 | 15 | 20 |
| Mesoporous silica A containing phosphorus and nitrogen | 20 | 20 | 20 |
| Platinum catalyst | 2 | 2 | 2 |
| Inhibitors | 0.2 | 0.2 | 0.2 |
Examples 18 to 20
This example provides a series of high flame retardant and high damping silicone foams, different examples have different contents of the mesoporous silica a containing phosphorus and nitrogen, and the specific formulation is shown in table 4, so as to explore the influence of the different contents of the mesoporous silica a containing phosphorus and nitrogen on the performance of the silicone foams.
TABLE 4 examples 18-20 formulations of Silicone foams
| Example 18 | Example 19 | Example 20 | |
| Hydroxy silicone oil | 10 | 10 | 10 |
| Vinyl silicone oil | 30 | 30 | 30 |
| Hydrogen-containing silicone oil | 10 | 10 | 10 |
| Mesoporous silica A containing phosphorus and nitrogen | 10 | 30 | 40 |
| Platinum catalyst | 2 | 2 | 2 |
| Inhibitors | 0.2 | 0.2 | 0.2 |
Examples 21 to 26
This example provides a series of high flame retardant, high damping silicone foams having the formulations shown in table 5.
TABLE 5 formulations (parts) of examples 21 to 26
Comparative examples 1 to 5
The comparative example provides a series of silicone foams, wherein the mesoporous silica is common mesoporous silica with the particle size of 200-300 nm, and the specific formula of the silicone foam is shown in table 6.
TABLE 6 formulations of comparative examples 1 to 5 (parts)
The performance of the silicone foam materials prepared in the above examples and comparative examples is tested, the limit oxygen index LOI and UL-94 test methods refer to GB/T10707-2008, the tensile strength and elongation at break test methods refer to GB/T528-2009, the average sound absorption coefficient test method refers to GB/T20247-2006, and the test results are shown in Table 7 below.
Table 7 results of performance tests of examples and comparative examples.
From examples 8 to 11, it is seen that the overall properties of the silicone foams generally tend to increase and then decrease with increasing content of the hydroxysilicone oil.
From examples 9 and 12 to 14, it is seen that the tensile strength and flame retardant property of the foam are improved by increasing the amount of the vinyl silicone oil.
From examples 9 and 15 to 17, it is seen that the tensile strength of the foam is improved by increasing the amount of the hydrogen-containing silicone oil.
From examples 9 and 18 to 20, it is seen that the flame retardant property of the foam is greatly improved by increasing the amount of the phosphorus and nitrogen containing mesoporous silica A.
From the embodiment 9 and the embodiments 21 to 26, when the particle size of the silicon dioxide containing phosphorus and nitrogen mesoporous is 200 to 300nm, the rigidity loss of the material is not large, the toughness is improved well, and the comprehensive performance is more excellent.
From comparative examples 1 to 4, the foam material has poor comprehensive properties without adding the hydroxyl silicone oil; vinyl silicone oil is not added, so that the comprehensive mechanical property of the foam material is poor; the flame retardant property and the mechanical property of the material are poor because no hydrogen-containing silicone oil is added; the flame retardant property of the material is poor because the phosphorus-nitrogen-containing mesoporous silica is not added.
From example 9 and comparative example 5, it can be seen that the flame retardant property of the foam is poor when the conventional mesoporous silica is added.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (9)
1. The high-flame-retardance high-damping organosilicon foam material is characterized by being prepared from the following raw materials in parts by mass:
the particle size of the phosphorus-nitrogen-containing mesoporous silica is 30-400 nm;
the preparation method of the phosphorus-nitrogen-containing mesoporous silica comprises the following steps:
s1, adding mesoporous silica with the particle size of 30-400 nm prepared by a sol-gel method into a zinc sulfate aqueous solution, and performing ultrasonic dispersion to obtain a mesoporous silica-zinc solution;
s2, preparing an amino trimethylene phosphonic acid or ammonium polyphosphate and zinc sulfate aqueous solution, and uniformly dispersing by ultrasonic;
and S3, adding the amino trimethylene phosphonic acid or ammonium polyphosphate obtained by the preparation of the S2 and a zinc sulfate aqueous solution into a mesoporous silica-zinc solution, and carrying out post-treatment to obtain the mesoporous silica containing phosphorus and nitrogen.
2. The high-flame-retardance high-damping organosilicon foam material as claimed in claim 1, is prepared from the following raw materials in parts by weight:
3. the high flame-retardant high-damping silicone foam material as claimed in any one of claims 1 to 2, wherein the particle size of the phosphorus-nitrogen-containing mesoporous silica is 200 to 300nm.
4. The high flame-retardant high-damping silicone foam material according to any one of claims 1 to 2, wherein the hydroxyl silicone oil is hydroxyl-terminated polymethylsiloxane and/or hydroxyl-terminated polymethylphenylsiloxane.
5. The high flame retardant high damping silicone foam material according to any of claims 1-2, wherein the catalyst is a platinum catalyst.
6. The high flame-retardant high-damping silicone foam material according to any one of claims 1 to 2, wherein the hydrogen-containing silicone oil is selected from one or more of trimethylsiloxy terminated polyhydrocarbylhydrosiloxane, phenyl-hydrosiloxane and vinyl-hydrosiloxane.
7. The high flame retardant high damping silicone foam material according to any of claims 1-2, wherein the inhibitor is selected from one or more of methyl butynol, ethynl cyclohexanol, methyl maleate.
8. The preparation method of the high flame-retardant high damping organosilicon foam material according to any of claims 1-7, characterized by comprising the following steps:
mixing and stirring hydroxyl silicone oil, vinyl silicone oil, a catalyst, phosphorus-nitrogen-containing mesoporous silicon dioxide and an inhibitor according to a proportion, adding hydrogen-containing silicone oil, stirring uniformly, and curing and foaming to obtain the organic silicon foam material.
9. Use of the high flame-retardant high damping silicone foam material according to any one of claims 1 to 7 in fire-retardant materials.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4189545A (en) * | 1978-03-13 | 1980-02-19 | General Electric Company | Silicone foam composition which has burn resistant properties |
| CN102643655A (en) * | 2012-04-16 | 2012-08-22 | 中南林业科技大学 | Method for preparing mesoporous silica/ammonium polyphosphate compound fire retardant |
| CN109438992A (en) * | 2018-10-23 | 2019-03-08 | 株洲时代新材料科技股份有限公司 | A kind of flame-proof organosilicon foamed material and preparation method thereof |
| CN111500071A (en) * | 2020-04-30 | 2020-08-07 | 新纳奇材料科技江苏有限公司 | Single-component flame-retardant silica gel foam material and preparation method thereof |
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- 2021-07-06 CN CN202110765611.5A patent/CN113502055B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4189545A (en) * | 1978-03-13 | 1980-02-19 | General Electric Company | Silicone foam composition which has burn resistant properties |
| CN102643655A (en) * | 2012-04-16 | 2012-08-22 | 中南林业科技大学 | Method for preparing mesoporous silica/ammonium polyphosphate compound fire retardant |
| CN109438992A (en) * | 2018-10-23 | 2019-03-08 | 株洲时代新材料科技股份有限公司 | A kind of flame-proof organosilicon foamed material and preparation method thereof |
| CN111500071A (en) * | 2020-04-30 | 2020-08-07 | 新纳奇材料科技江苏有限公司 | Single-component flame-retardant silica gel foam material and preparation method thereof |
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