CN110894363A - Tear-resistant organic silicon foam material and preparation method thereof - Google Patents
Tear-resistant organic silicon foam material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use 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; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
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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
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/006—Additives being defined by their surface area
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
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Abstract
The invention discloses a tear-resistant organosilicon foam material which is mainly prepared from vinyl silicone oil, an auxiliary foaming agent, a tear-resistant reinforcing filler, hydrogen-containing silicone oil, a catalyst and an inhibitor, wherein the tear-resistant reinforcing filler has a pipe diameter of 10-20 nm and a specific surface area of 200-500 m2Carbon nanotubes in a ratio of/g. The invention also discloses a preparation method of the tear-resistant organosilicon foam material, which comprises the following steps of preparing the vinyl silicone oil, the auxiliary foaming agent, the tear-resistant reinforcing filler, the catalyst and the inhibitor into a component A; preparing vinyl silicone oil, hydrogen-containing silicone oil and anti-tearing reinforcing filler into a component B, and then mixing the component A and the component BAnd mixing, foaming and carrying out heat treatment on the component B to obtain the tear-resistant organic silicon foam material. The tear-resistant organosilicon foam material has good tensile property, the tensile strength is more than 150KPa, and the elongation at break is more than 80 percent; the tear strength is high, the tear strength is more than 2.5N/cm, and the polyurethane can be applied to seat core materials.
Description
Technical Field
The invention relates to the technical field of organic silicon foam materials, in particular to a high-strength tear-resistant organic silicon foam material and a preparation method thereof.
Background
The organosilicon material is a high polymer material which takes a silica part as a main body and takes an organic group as a side chain, and has excellent high and low temperature resistance, aging resistance, ozone resistance, electrical insulation and chemical reaction resistance. The organic silicon foam material has excellent performances of organic silicon materials, light weight, high elasticity and good damping and noise reduction performances, and is widely applied to the fields of aerospace, rail transit, electronic and electric appliance elements, various sealing materials and the like. Particularly in the field of rail transit, along with the further improvement of the requirements of people on comfort, environmental protection and safety, higher requirements are also put forward on the mechanical property and the environmental protection flame retardant property of the foam material for rail transit. The silicone foam replaces polyurethane foam to serve as a seat core material, has higher environment-friendly flame retardance and better environment durability, but has the defects that the general silicone foam has poorer mechanical properties, particularly tear resistance, and is easy to tear and damage in the using process compared with the polyurethane foam. For example, patent CN201811237959.1 discloses a flexible silicone foam material, which can replace polyurethane foam material as seat and/or interior material of vehicle, and can effectively solve the problem of harm of polyurethane foam material. But the silicone foam replaces polyurethane to be used as a seat core material, so that the seat core material has higher flame-retardant and environment-friendly performance, but the general silicone foam has poorer mechanical properties, particularly tear resistance, than the polyurethane foam due to the limitation of the material type.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background technology and provide a tear-resistant silicone foam material and a preparation method thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a tear-resistant organosilicon foam material is mainly prepared from the following raw materials in parts by weight:
the tear-resistant reinforcing filler has a pipe diameter of 10-20 nm and a specific surface area of 200-500 m2Carbon nanotubes in a ratio of/g.
The tear-resistant silicone foam material is preferably mainly prepared from a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
the component B comprises the following raw materials in parts by weight:
60-90 parts of vinyl silicone oil,
10-30 parts of hydrogen-containing silicone oil,
10-20 parts of a tear-resistant reinforcing filler;
the tear-resistant reinforcing filler has a pipe diameter of 10-20 nm and a specific surface area of 200-500 m2Carbon nanotubes in a ratio of/g.
In the tear-resistant silicone foam material, preferably, the vinyl silicone oil is polydimethylsiloxane containing at least two vinyl groups in each molecule; the viscosity of the vinyl silicone oil at 25 ℃ is 10-1,000,000 mPas; a viscosity of 5000 to 100,000 mPas.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.1-1.5% by mass.
Preferably, the co-blowing agent is one or more of ethanol, ethylene glycol, propanol and butanediol.
Preferably, the catalyst is chloroplatinic acid; the inhibitor is 1-alkynyl cyclohexanol.
As a general inventive concept, the present invention also provides a method for preparing the tear resistant silicone foam described above, comprising the steps of:
(1) according to the weight ratio of the raw materials, A, B components are respectively prepared and evenly mixed;
(2) and (2) foaming and heat-treating the mixture obtained in the step (1) to obtain the tear-resistant silicone foam material.
In the preparation method, preferably, in the step (2), the foaming temperature is 50-60 ℃, the foaming time is 10-30 min, the heat treatment temperature is 150-160 ℃, and the heat treatment time is 2-3 h.
Compared with the prior art, the invention has the advantages that:
(1) the tear-resistant organosilicon foam material has good tensile property, the tensile strength is more than 150KPa, and the elongation at break is more than 80 percent; the tear strength is high, the tear strength is more than 2.5N/cm, and the polyurethane can be applied to seat core materials.
(2) The tear-resistant organic silicon foam material disclosed by the invention has the advantages that the tear resistance of the organic silicon foam material is improved by utilizing the carbon nano tube for the first time, the carbon nano tube is a linear reinforcing short fiber, is large in specific surface area, and is easy to form a net-shaped physical lap joint structure after being dispersed in matrix resin and cured. The conventional granular fillers such as silica micropowder, diatomite, calcium carbonate, white carbon black and the like cannot obviously improve the tear resistance of the organic silicon foam material.
(3) According to the invention, a two-component preparation method is adopted in the process of preparing the tear-resistant organosilicon foam material, the catalyst, the reactive active substance and the filler are respectively and uniformly dispersed into the two components in advance, when the two components are mixed, the rapid and uniform mixing can be ensured, the adverse effect on the material performance caused by the local rapid reaction due to the excessive local concentration of the catalyst or the active substance is avoided, and the mechanical property and the tear-resistant property of the tear-resistant organosilicon foam material are further ensured.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the tear-resistant organosilicon foam material is mainly prepared from a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
60g of vinyl silicone oil having a viscosity of 50Pa.s and a vinyl mass fraction of 0.2%,
15g of vinyl silicone oil having a viscosity of 1000 mPas and a vinyl mass fraction of 4%,
5g of ethylene glycol,
the pipe diameter is about 15-18 nm, and the specific surface area is 250m215g of carbon nano-tubes per gram,
0.2g of chloroplatinic acid,
0.02g of 1-alkynyl cyclohexanol;
the component B is mainly prepared from the following raw materials in parts by weight:
60g of vinyl silicone oil having a viscosity of 50Pa.s and a vinyl mass fraction of 0.2%,
25g of hydrogen-containing silicone oil with a hydrogen content of 0.75%,
specific surface area of 250m215 g/g carbon nanotube.
The preparation method of the tear-resistant silicone foam material of the embodiment comprises the following steps:
(1) 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 15g of vinyl silicone oil with the viscosity of 1000mPa.s and the vinyl mass fraction of 4 percent, 5g of ethylene glycol and the specific surface area of 250m2Carbon content per gram15g of rice tube, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol are mechanically stirred and fully mixed to obtain a component A;
(2) 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2 percent, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75 percent and the specific surface area of 250m215 g/g of carbon nano tube, and fully and uniformly mixing the components through mechanical stirring to obtain a component B;
(3) a, B components are mechanically stirred uniformly according to the proportion of 1:1, and are foamed and cured for 15min at 50 ℃, and then are thermally treated for 3h at 150 ℃, so that the tear-resistant organic silicon foam is obtained, and is marked as sample 1.
The performance test result of the sample 1 comprises that the tensile strength is 195KPa, the elongation at break is 90 percent, and the tearing strength is 2.8N/cm; wherein, the test standard of tensile strength and elongation at break is GB/T6344-2008, the test standard of tear strength is GB/T10808-2006, and the other examples below are all tested according to the standard.
Example 2:
the tear-resistant organosilicon foam material is mainly prepared from a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
65g of vinyl silicone oil having a viscosity of 10Pa.s and a vinyl mass fraction of 0.5%,
15g of vinyl silicone oil having a viscosity of 1500mPa.s and a vinyl mass fraction of 3%,
8g of ethylene glycol,
the pipe diameter is about 12-15 nm, and the specific surface area is 350m212 g/g of carbon nanotubes, and,
0.2g of chloroplatinic acid,
0.02g of 1-alkynyl cyclohexanol;
the component B is mainly prepared from the following raw materials in parts by weight:
65g of vinyl silicone oil having a viscosity of 10Pa.s and a vinyl mass fraction of 0.5%,
25g of hydrogen-containing silicone oil with a hydrogen content of 0.75%,
the pipe diameter is about 12-15 nm, and the specific surface area is 350m210 g/g carbon nanotube.
The preparation method of the tear-resistant silicone foam material of the embodiment comprises the following steps:
(1) taking 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5 percent, 15g of vinyl silicone oil with the viscosity of 1500mPa.s and the vinyl mass fraction of 3 percent, 8g of ethylene glycol and 350m of specific surface area212 g/g of carbon nano tube, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol are fully and uniformly mixed by mechanical stirring to obtain a component A;
(2) taking 65g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5 percent, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75 percent and the specific surface area of 350m210 g/g of carbon nano tube, and fully and uniformly mixing the components through mechanical stirring to obtain a component B;
(3) a, B components were mechanically stirred uniformly at a ratio of 1:1, foamed and cured at 60 ℃ for 20min, and then treated at 160 ℃ for 2.5h to give a tear resistant silicone foam, which was designated sample 2.
The performance test result of the sample 2 comprises the tensile strength of 180KPa, the elongation at break of 85 percent and the tearing strength of 2.6N/cm.
Comparative example 1:
the organosilicon foam material of the comparative example is mainly prepared from a component A and a component B, wherein the component A is mainly prepared from the following raw materials in parts by weight:
60g of vinyl silicone oil having a viscosity of 50Pa.s and a vinyl mass fraction of 0.2%,
15g of vinyl silicone oil having a viscosity of 1000mPa.s and a vinyl mass fraction of 4%,
5g of ethylene glycol,
10g of white carbon black prepared by a gas phase method,
10g of silicon micro-powder,
0.2g of chloroplatinic acid,
0.02g of 1-alkynyl cyclohexanol;
the component B is mainly prepared from the following raw materials in parts by weight:
60g of vinyl silicone oil having a viscosity of 50Pa.s and a vinyl mass fraction of 0.2%,
25g of hydrogen-containing silicone oil with a hydrogen content of 0.75%,
15g of fumed silica.
The method of preparing the silicone foam of this comparative example includes the steps of:
(1) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 20g of vinyl silicone oil with the viscosity of 1500mPa.s and the vinyl mass fraction of 3%, 10g of ethylene glycol, 10g of fumed silica, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol, and fully and uniformly mixing through mechanical stirring to obtain a component A;
(2) taking 60g of vinyl silicone oil with the viscosity of 50Pa.s and the vinyl mass fraction of 0.2%, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75% and 15g of fumed silica, and fully and uniformly mixing by mechanical stirring to obtain a component B;
(3) a, B components were mechanically stirred uniformly at a ratio of 1:1, foamed and cured at 60 ℃ for 10min, and then treated at 150 ℃ for 3h to give silicone foam, which was designated as sample 3.
The result of the performance test of the sample 3 is that the tensile strength is 155KPa, the elongation at break is 75 percent, and the tearing strength is 1.7N/cm.
Comparative example 2:
a silicone foam of a comparative example, prepared by dispersing a single component raw material, wherein the single component comprises the following raw materials in parts by weight:
130g of vinyl silicone oil having a viscosity of 10Pa.s and a vinyl mass fraction of 0.5%,
15g of vinyl silicone oil having a viscosity of 1500mPa.s and a vinyl mass fraction of 3%,
25g of hydrogen-containing silicone oil with a hydrogen content of 0.75%,
8g of ethylene glycol,
the pipe diameter is about 12-15 nm, and the specific surface area is 350m222g of carbon nanotubes/g,
0.2g of chloroplatinic acid,
0.02g of 1-alkynyl cyclohexanol;
the method of preparing the silicone foam of this comparative example includes the steps of:
(1) taking 130g of vinyl silicone oil with the viscosity of 10Pa.s and the vinyl mass fraction of 0.5%, 15g of vinyl silicone oil with the viscosity of 1500mPa.s and the vinyl mass fraction of 3%, 25g of hydrogen-containing silicone oil with the hydrogen content of 0.75%, 8g of ethylene glycol and 35 of specific surface area0m222 g/g of carbon nano tube, 0.2g of chloroplatinic acid and 0.02g of 1-alkynyl cyclohexanol, and fully and uniformly mixing the components through mechanical stirring to obtain a mixture;
(3) the mixture was foamed and cured at 60 ℃ for 20min and then treated at 160 ℃ for 2.5h to give a silicone foam, which was designated sample 4.
The performance test result of the sample 4 comprises the tensile strength of 130KPa, the elongation at break of 55 percent and the tearing strength of 1.2N/cm.
As can be seen from the performance results of the samples 1 and 2, the introduction of the carbon nanotubes can enable the foam to obtain better tensile property and tearing property, the high specific surface area of the carbon nanotubes endows the filler and the resin with larger bonding force, and the carbon nanotubes with linear structures enable the material to have higher tearing resistance; the sample 3 is close to the samples 1 and 2 in tensile property by adding the reinforcing filler white carbon black, but the tearing strength is much worse than the samples 1 and 2; it can be seen from comparison of samples 4 and 2 that the basic formulation is the same, and the silicone foam prepared by the single-component process and the two-component process have a greater difference in performance, and the single-component process is inferior to the two-component process in tensile strength, elongation at break, and tear strength due to dispersion and reaction unevenness. In conclusion, the carbon nano tube is introduced into the organic silicon foam material, and the tear resistance of the organic silicon foam material can be improved by adopting a two-component process preparation method.
Claims (8)
1. The tear-resistant organosilicon foam material is characterized by being mainly prepared from the following raw materials in parts by weight:
the tear-resistant reinforcing filler has a pipe diameter of 10-20 nm and a specific surface area of 200-500 m2Carbon nanotubes in a ratio of/g.
2. The tear resistant silicone foam of claim 1 prepared from a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
the component B comprises the following raw materials in parts by weight:
60-90 parts of vinyl silicone oil,
10-30 parts of hydrogen-containing silicone oil,
10-20 parts of tear-resistant reinforcing filler.
3. The tear resistant silicone foam of claim 1 wherein the vinyl silicone oil is a polydimethylsiloxane having at least two vinyl groups per molecule; the viscosity of the vinyl silicone oil at 25 ℃ is 10 to 1,000,000 mPas.
4. The tear resistant silicone foam of claim 1 wherein the hydrogen content of the hydrogen containing silicone oil is from 0.1% to 1.5% by weight.
5. The tear resistant silicone foam of claim 1 wherein the co-blowing agent is one or more of ethanol, ethylene glycol, propanol, and butanediol.
6. The tear resistant silicone foam of claim 1 wherein the catalyst is chloroplatinic acid; the inhibitor is 1-alkynyl cyclohexanol.
7. A method of making a tear resistant silicone foam according to any of claims 1 to 6 comprising the steps of:
(1) according to the weight ratio of the raw materials, A, B components are respectively prepared and evenly mixed;
(2) and (2) foaming and heat-treating the mixture obtained in the step (1) to obtain the tear-resistant silicone foam material.
8. The preparation method according to claim 7, wherein in the step (2), the foaming temperature is 50 ℃ to 60 ℃, the foaming time is 10min to 30min, the heat treatment temperature is 150 ℃ to 160 ℃, and the heat treatment time is 2h to 3 h.
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Application publication date: 20200320 |
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| RJ01 | Rejection of invention patent application after publication |