CN110862629A - Preparation method of novel high-temperature-resistant and flame-retardant polymer nanocomposite - Google Patents
Preparation method of novel high-temperature-resistant and flame-retardant polymer nanocomposite Download PDFInfo
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- CN110862629A CN110862629A CN201911215376.3A CN201911215376A CN110862629A CN 110862629 A CN110862629 A CN 110862629A CN 201911215376 A CN201911215376 A CN 201911215376A CN 110862629 A CN110862629 A CN 110862629A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
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- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2003/387—Borates
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/02—Flame or fire retardant/resistant
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention relates to the technical field of preparation of polymer nanocomposites, in particular to a preparation method of a novel high-temperature-resistant and flame-retardant polymer nanocomposite, which comprises the following steps of 1: mixing and fully stirring the dissolved solutions of the polyvinyl chloride, the polyethylene and the polyethylene block copolymer; step 2: sequentially adding a coupling agent and a flame retardant into the mixed solution in the stirring process; and step 3: carrying out ultrasonic treatment on the solution obtained in the step 2; step 4; and (3) carrying out vacuum evaporation on the solution after ultrasonic treatment, thereby preparing the high-temperature-resistant and flame-retardant polymer nano composite material. The method is simple and effective, and the prepared high-molecular nano composite material has extremely high limit oxygen index by adopting the special flame retardant, thereby realizing good flame-retardant and high-temperature resistant effects, reducing the use limit of products and increasing the practicability.
Description
Technical Field
The invention relates to the technical field of preparation of polymer nanocomposites, in particular to a preparation method of a novel high-temperature-resistant and flame-retardant polymer nanocomposite.
Background
The nano composite material is a composite material with the particle size of a disperse phase between 1nm and 10nm, fully exerts the structural characteristics of a molecular level, has the functions of high strength, high rigidity, heat resistance and the like, and is a material with new performance macroscopically formed by a physical or chemical method.
However, the flame retardant and high temperature resistance of the existing nano polymer composite material are poor, so that the use is limited, and the practical effect is poor. Therefore, the skilled in the art provides a method for preparing a novel high temperature resistant and flame retardant polymer nanocomposite, so as to solve the problems in the background art.
Disclosure of Invention
The invention aims to provide a preparation method of a novel high-temperature-resistant and flame-retardant polymer nano composite material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a novel high-temperature-resistant and flame-retardant polymer nano composite material comprises the following steps:
step 1: mixing and fully stirring the dissolved solutions of the polyvinyl chloride, the polyethylene and the polyethylene block copolymer;
step 2: sequentially adding a coupling agent and a flame retardant into the mixed solution in the stirring process;
and step 3: carrying out ultrasonic treatment on the solution obtained in the step 2;
step 4; and (3) carrying out vacuum evaporation on the solution after ultrasonic treatment, thereby preparing the high-temperature-resistant and flame-retardant polymer nano composite material.
As a still further scheme of the invention: and (2) respectively dissolving the polyvinyl chloride and the polyethylene block copolymer in the step (1) into two different tetrahydrofuran solutions, wherein the ratio of the polyvinyl chloride to the polyethylene block copolymer to the tetrahydrofuran solutions is 1: 2.5, the polyethylene is dissolved in the benzene solution, and the ratio of the polyethylene to the benzene solution is 1: 2.5.
as a still further scheme of the invention: the polyvinyl chloride and the tetrahydrofuran are dissolved at normal temperature, the dissolution temperature of the polyethylene and the benzene solution is kept between 55 and 80 ℃, and the dissolution temperature of the polyethylene block copolymer and the tetrahydrofuran solution is kept between 75 and 100 ℃.
As a still further scheme of the invention: and (3) adopting a titanate coupling agent as the coupling agent in the step (2).
As a still further scheme of the invention: the flame retardant in the step 2 is prepared from the following raw materials in parts by weight: 15-20 parts of antimony trioxide, 3-6 parts of montmorillonite, 3-9 parts of paraffin oil, 10-17 parts of magnesium borate, 4-8 parts of ammonium polyphosphate and 12-17 parts of phosphate.
As a still further scheme of the invention: the preparation of the flame retardant comprises the following steps:
s1, grinding montmorillonite into powder with the particle size of 15-30 nm;
s2, mixing the ground montmorillonite, magnesium borate, ammonium polyphosphate and phosphate, and performing ultrasonic treatment for 1.5h at 45 ℃;
and S3, sequentially adding paraffin oil and antimony trioxide into the raw materials subjected to ultrasonic mixing treatment, and fully stirring to obtain the finished flame retardant.
As a still further scheme of the invention: in the S2, the ultrasonic frequency is 30kHz, and the ultrasonic power is 450W.
Compared with the prior art, the invention has the beneficial effects that: the method is simple and effective, the prepared high-molecular nano composite material has extremely high limit oxygen index by adopting the special flame retardant, thereby realizing good flame-retardant and high-temperature resistant effects, reducing the use limit of products and increasing the practicability, and the titanate coupling agent can react with various functional groups on the surfaces of the products to form strong chemical bonding, thereby improving the quality of the products.
Drawings
FIG. 1 is a flow chart of the steps of a method for preparing a novel high temperature resistant and flame retardant polymer nanocomposite;
FIG. 2 is a diagram of comparative example test data of a method for preparing a novel high temperature resistant, flame retardant polymeric nanocomposite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in 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:
referring to fig. 1-2, in an embodiment of the present invention, a method for preparing a novel high temperature resistant and flame retardant polymer nanocomposite includes the following steps:
step 1: mixing and fully stirring the dissolved solutions of the polyvinyl chloride, the polyethylene and the polyethylene block copolymer;
step 2: sequentially adding a coupling agent and a flame retardant into the mixed solution in the stirring process;
and step 3: carrying out ultrasonic treatment on the solution obtained in the step 2;
step 4; and (3) carrying out vacuum evaporation on the solution after ultrasonic treatment, thereby preparing the high-temperature-resistant and flame-retardant polymer nano composite material.
Further, the polyvinyl chloride and the polyethylene block copolymer in the step 1 are respectively dissolved in two different tetrahydrofuran solutions, and the ratio of the polyvinyl chloride to the tetrahydrofuran solution to the polyethylene block copolymer to the tetrahydrofuran solution is 1: 2.5, the polyethylene is dissolved in the benzene solution, and the ratio of the polyethylene to the benzene solution is 1: 2.5.
further, the polyvinyl chloride and the tetrahydrofuran are dissolved at normal temperature, the dissolution temperature of the polyethylene and the benzene solution is kept between 55 and 80 ℃, and the dissolution temperature of the polyethylene block copolymer and the tetrahydrofuran solution is kept between 75 and 100 ℃.
Further, the coupling agent in the step 2 is a titanate coupling agent.
Further, in the step 2, the flame retardant is prepared from the following raw materials in parts by weight: 15-20 parts of antimony trioxide, 3-6 parts of montmorillonite, 3-9 parts of paraffin oil, 10-17 parts of magnesium borate, 4-8 parts of ammonium polyphosphate and 12-17 parts of phosphate.
Further, the preparation of the flame retardant comprises the following steps:
s1, grinding montmorillonite into powder with the particle size of 15-30 nm;
s2, mixing the ground montmorillonite, magnesium borate, ammonium polyphosphate and phosphate, and performing ultrasonic treatment for 1.5h at 45 ℃;
and S3, sequentially adding paraffin oil and antimony trioxide into the raw materials subjected to ultrasonic mixing treatment, and fully stirring to obtain the finished flame retardant.
Further, in S2, the ultrasonic frequency is 30kHz and the ultrasonic power is 450W.
Example 2:
the procedure of example 1 was followed, except that in example 1: further, in the step 2, the flame retardant is prepared from the following raw materials in parts by weight: 17 parts of antimony trioxide, 5 parts of montmorillonite, 5 parts of paraffin oil, 13 parts of magnesium borate, 6 parts of ammonium polyphosphate and 14 parts of phosphate.
Comparative example:
selecting the finished high-temperature-resistant and flame-retardant polymer nanocomposite with the same gram number from the embodiment 1 and the embodiment 2 as a test material, and selecting a common polymer nanocomposite material on the market as a comparative test material;
the test contents are as follows: the comparative test material, the test materials of example 1 and example 2 were tested for heat shrinkage, tensile strength, and limiting oxygen index in that order, yielding the following data:
| heat shrinkage (%) | Tensile Strength (MPA) | Limiting oxygen index (%) | |
| Example 1 |
38 | 45 | 34 |
| Example 2 |
36 | 48 | 36 |
| |
43 | 42 | 27 |
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A preparation method of a novel high-temperature-resistant and flame-retardant polymer nano composite material is characterized by comprising the following steps:
step 1: mixing and fully stirring the dissolved solutions of the polyvinyl chloride, the polyethylene and the polyethylene block copolymer;
step 2: sequentially adding a coupling agent and a flame retardant into the mixed solution in the stirring process;
and step 3: carrying out ultrasonic treatment on the solution obtained in the step 2;
step 4; and (3) carrying out vacuum evaporation on the solution after ultrasonic treatment, thereby preparing the high-temperature-resistant and flame-retardant polymer nano composite material.
2. The method according to claim 1, wherein the polyvinyl chloride and the polyethylene block copolymer in step 1 are respectively dissolved in two different tetrahydrofuran solutions, and the ratio of the polyvinyl chloride to the polyethylene block copolymer to the tetrahydrofuran solution is 1: 2.5, the polyethylene is dissolved in the benzene solution, and the ratio of the polyethylene to the benzene solution is 1: 2.5.
3. the method for preparing the novel high temperature resistant and flame retardant polymer nanocomposite material according to claim 2, wherein the polyvinyl chloride and the tetrahydrofuran are dissolved at normal temperature, the dissolution temperature of the solution of the polyethylene and the benzene is maintained at 55-80 ℃, and the dissolution temperature of the solution of the polyethylene block copolymer and the tetrahydrofuran is maintained at 75-100 ℃.
4. The method for preparing the novel high-temperature-resistant flame-retardant polymer nanocomposite material according to claim 1, wherein the coupling agent in the step 2 is a titanate coupling agent.
5. The preparation method of the novel high-temperature-resistant flame-retardant polymer nanocomposite material according to claim 1, wherein the flame retardant in the step 2 is prepared from the following raw materials in parts by weight: 15-20 parts of antimony trioxide, 3-6 parts of montmorillonite, 3-9 parts of paraffin oil, 10-17 parts of magnesium borate, 4-8 parts of ammonium polyphosphate and 12-17 parts of phosphate.
6. The preparation method of the novel high-temperature-resistant flame-retardant polymer nanocomposite material according to claim 5, wherein the preparation of the flame retardant comprises the following steps:
s1, grinding montmorillonite into powder with the particle size of 15-30 nm;
s2, mixing the ground montmorillonite, magnesium borate, ammonium polyphosphate and phosphate, and performing ultrasonic treatment for 1.5h at 45 ℃;
and S3, sequentially adding paraffin oil and antimony trioxide into the raw materials subjected to ultrasonic mixing treatment, and fully stirring to obtain the finished flame retardant.
7. The preparation method of the novel high-temperature-resistant flame-retardant polymer nanocomposite material as claimed in claim 6, wherein the ultrasonic frequency in S2 is 30kHz, and the ultrasonic power is 450W.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280212A (en) * | 2020-10-23 | 2021-01-29 | 无锡市锡山新材料科技有限公司 | Preparation method of flame-retardant PVC (polyvinyl chloride) flexible board |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898737A (en) * | 2012-09-27 | 2013-01-30 | 惠州市怡佳电线电缆材料有限公司 | Macromolecular flame-retardant elastomer environment-friendly material and preparation method thereof |
| CN109695151A (en) * | 2017-10-20 | 2019-04-30 | 贵州省新材料研究开发基地 | A kind of fire retardant and preparation method thereof |
| CN109721887A (en) * | 2018-12-29 | 2019-05-07 | 武汉华星光电技术有限公司 | The preparation method of high molecule nano composite material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102898737A (en) * | 2012-09-27 | 2013-01-30 | 惠州市怡佳电线电缆材料有限公司 | Macromolecular flame-retardant elastomer environment-friendly material and preparation method thereof |
| CN109695151A (en) * | 2017-10-20 | 2019-04-30 | 贵州省新材料研究开发基地 | A kind of fire retardant and preparation method thereof |
| CN109721887A (en) * | 2018-12-29 | 2019-05-07 | 武汉华星光电技术有限公司 | The preparation method of high molecule nano composite material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280212A (en) * | 2020-10-23 | 2021-01-29 | 无锡市锡山新材料科技有限公司 | Preparation method of flame-retardant PVC (polyvinyl chloride) flexible board |
| CN112280212B (en) * | 2020-10-23 | 2022-10-28 | 无锡市锡山新材料科技有限公司 | Preparation method of flame-retardant PVC (polyvinyl chloride) flexible board |
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Application publication date: 20200306 |