CN109206829B - High-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition and preparation method thereof - Google Patents
High-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
- C08L53/02—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 of vinyl-aromatic monomers and conjugated dienes
- C08L53/025—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 of vinyl-aromatic monomers and conjugated dienes modified
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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
- C08L23/10—Homopolymers or copolymers of propene
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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
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C08L2205/00—Polymer mixtures characterised by other features
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Abstract
The invention discloses a high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition and a preparation method thereof, and the composition comprises the following components in percentage by mass: styrenic thermoplastic elastomer: 15-30% of polyolefin resin: 10-25% of a plasticizer: 15-25% of a char-forming agent: 10-20% of phosphorus-nitrogen flame retardant: 15-30% of flame-retardant synergist: 0.5-3%, antioxidant: 0.1-1%, anti-aging agent: 0.1-1%, processing aid: 0.1 to 1 percent. According to the invention, the high charring property of the crosslinked polystyrene powder is utilized to compound the triazine charring agent instead of the traditional polyphenyl ether as the charring agent of the thermoplastic elastomer TPE, the flame retardant property and the physical property are good, the problem that the polyphenyl ether is easy to cause yellowing is solved, the UV resistance is excellent, and the high-requirement precipitation resistance test can be passed.
Description
Technical Field
The invention relates to the field of high polymer materials, and particularly relates to a high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition and a preparation method thereof.
Background
Thermoplastic elastomers (TPEs) are soft in texture, comfortable in hand feeling, wide in hardness range, good in processability, and free of halogen, and meet the trend of environmental protection, and thus are widely used in the field of consumer electronics requiring halogen-free, such as data lines. However, flame retardance is generally required for consumer electronics, and TPE has a low oxygen index and is easy to burn, so that flame retardance modification is required.
At present, halogen-free flame-retardant modification of TPE is mature, and the modification is mainly divided into the following three systems: the first one is a flame retardant system filled with inorganic fillers such as magnesium hydroxide in large quantity, although the product has better yellowing resistance, the system can reach better flame retardant grade only by filling a large quantity of inorganic fillers, has lower flame retardant efficiency and poor mechanical strength, is difficult to process and is generally used in occasions with higher requirements on smoke density; the second one is a flame retardant system mainly based on an expansion type flame retardant system, which uses micromolecular flame retardants such as APP (ammonium polyphosphate), piperazine pyrophosphate, pentaerythritol, tris (2-hydroxyethyl) isocyanurate, melamine pyrophosphate and the like, and has good flame retardant performance and good UV discoloration resistance, but the flame retardants are easily hydrolyzed or have strong hydrophilicity, so that the flame retardants are easily separated out in the use process of the product, although the flame retardants can pass a 70 ℃ x 168h boiling separation test (such as the patent No. CN102618015B) through formula adjustment, the flame retardants cannot meet the use requirements for wires with higher requirements (such as wires without separation after 80 ℃ x 168h boiling); the third one is a flame retardant system mainly comprising PPO (polyphenylene oxide) resin and hypophosphite or alkyl phosphinate, the system generates synergistic effect with flame retardants such as hypophosphite or alkyl hypophosphite, melamine cyanurate and the like by adding the PPO with high temperature resistance and high flame retardance, the flame retardant performance is good, the product has better heat resistance, good precipitation resistance and high mechanical strength, but the PPO resin has poor UV resistance, is easy to yellow, influences the appearance of the final product, and can be improved by filling a large amount of titanium dioxide, but the processing performance and the mechanical performance are sacrificed, and the flame retardant performance is also deteriorated. In conclusion, the existing flame-retardant system is difficult to reach the halogen-free flame-retardant TPE with high precipitation resistance and excellent UV yellowing resistance, so that the development of a new flame-retardant system has important significance.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides a high yellowing resistance and precipitation resistance halogen-free flame retardant thermoplastic elastomer composition and a preparation method thereof. The invention finds a new charring agent which can be used for replacing PPO (polyphenylene oxide), can realize no precipitation after being boiled in water at 80 ℃ for 168h and has UV discoloration resistance delta E of less than 0.8.
The technical means adopted by the invention for solving the technical problems is as follows:
the high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition comprises the following raw materials in percentage by mass:
styrenic thermoplastic elastomer: 15-30 percent,
Polyolefin resin: 10 to 25 percent,
Plasticizer: 15 to 25 percent,
A char-forming agent: 10 to 20 percent,
Phosphorus nitrogen flame retardant: 15-30 percent,
Flame retardant synergist: 0.5 to 3 percent,
Antioxidant: 0.1 to 1 percent,
Anti-aging agent: 0.1 to 1 percent,
Processing aid: 0.1 to 1 percent.
Preferably, the styrene thermoplastic elastomer is styrene-ethylene-butylene-styrene triblock copolymer (SEBS), and the styrene content is 10-50%, and more preferably 20-40%.
Preferably, the polyolefin resin comprises any one or more of polypropylene, propylene-ethylene copolymer and polyethylene, and is further preferably random copolymerized propylene.
Preferably, the plasticizer is white oil.
Preferably, the charring agent is a compound of styrene-divinylbenzene copolymer powder and triazine charring agent, wherein the triazine charring agent accounts for less than or equal to 10 percent of the mass of the elastomer composition;
the content of Divinylbenzene (DVB) in the styrene-divinylbenzene copolymer powder is more than or equal to 60 percent, and the average particle size is between 0.5 and 50 mu m;
the triazine charring agent is one or two of the following structures:
preferably, the phosphorus-nitrogen flame retardant is a compound of diethyl phosphinate and melamine cyanurate.
Preferably, the flame retardant synergist is any one or more of zinc borate, zirconium phosphate and organic montmorillonite.
Preferably, the antioxidant is one or two of hindered phenols and phosphites, and the anti-aging agent is one or more of benzophenones, triazoles and hindered amines.
Preferably, the processing aid comprises any one or more of silicone, EBS (N, N' -ethylene bis stearamide), polyethylene wax.
A preparation method of a high-yellowing-resistance precipitation-resistant halogen-free flame-retardant thermoplastic elastomer composition comprises the following process steps:
(1) mixing 15-30% of styrene thermoplastic elastomer and 15-25% of plasticizer according to mass percentage, and filling oil to obtain a mixture 1;
(2) putting the mixture 1 in the step (1), 10-25% of polyolefin resin, 10-20% of char forming agent, 15-30% of phosphorus-nitrogen flame retardant, 0.5-3% of flame retardant synergist, 0.1-1% of antioxidant, 0.1-1% of anti-aging agent and 0.1-1% of processing aid into a high-speed mixer according to mass percentage, and uniformly mixing to obtain a mixture 2;
(3) and (3) adding the mixture 2 obtained in the step (2) into a double-screw extruder for extrusion granulation to obtain the high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition.
Preferably, in the step (3), the process parameters of the twin-screw extruder are as follows: the rotating speed of the screw is 300-600 rpm, and the processing temperature is set between 180-220 ℃.
The basic principle of the invention is as follows:
through intensive research, the invention discovers that the carbon forming amount of the styrene-divinylbenzene polymer is increased along with the increase of the content of Divinylbenzene (DVB), the styrene-divinylbenzene polymer can be used as a carbon forming agent of TPE to replace PPO, and the carbon forming effect can be further improved after a small amount of triazine carbon forming agent is compounded; although the triazine charring agent has a large molecular weight, the triazine charring agent can be separated out when the mass percentage is more than 10%, and the mechanical property is reduced due to agglomeration caused by poor compatibility with TPE, so that when the molecular weight is controlled within 10%, the product can have excellent separation resistance.
Compared with the prior art, the technical scheme of the invention has the following advantages:
the invention provides a brand new flame retardant thought, the high char-forming performance of styrene-divinylbenzene copolymer powder is utilized to compound triazine char-forming agent to replace the traditional char-forming agent PPO resin, the problem that the halogen-free flame retardant thermoplastic elastomer cable material system is easy to yellow when PPO is added is solved, and after the material is subjected to UV aging test, Lab color difference delta E is less than 1; meanwhile, the composite material also has excellent precipitation resistance, and can be subjected to precipitation experiments of 80 ℃ multiplied by 168h at boiling and high temperature and high humidity 85 ℃ and 95% humidity multiplied by 168 h; and the good physical properties can be kept, and the high-yellowing-resistance precipitation-resistance halogen-free flame-retardant cable material with different hardness can be prepared by adjusting the composition proportion of each composition.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. Moreover, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
The triazine charring agent CFA-1 of examples 1-5 and comparative examples 1-3 has the following structural formula:
the triazine charring agent CFA-2 has the following structural formula:
the following are specific examples and comparative examples of the present invention and corresponding performance test data.
A preparation method of a high-yellowing-resistance precipitation-resistant halogen-free flame-retardant thermoplastic elastomer composition comprises the following process steps:
(1) firstly, SEBS and white oil mixed oil of examples 1-5 and comparative examples 1-3 are filled (the components and the content thereof are shown in Table 1);
(2) putting the oil-filled SEBS and other components into a high-speed mixer to be uniformly mixed (the components and the content thereof are shown in a table 1);
(3) and adding the mixed raw materials into a double-screw extruder for extrusion granulation, wherein the rotating speed of a screw is 300-600 rpm, and the processing temperature is set between 180-240 ℃.
TABLE 1 compositions of raw materials for thermoplastic elastomer compositions of examples 1 to 5 and comparative examples 1 to 3
TABLE 2 results of Performance test of thermoplastic elastomer compositions of examples 1 to 5 and comparative examples 1 to 3
Note: test conditions for UV yellowing resistance:
UVA conditions: light source: UVA-340; irradiance: 0.89W/m2(ii) nm; exposing at 60 + -3 deg.C for 8h, and exposing at 50 + -3 deg.C for 4h by non-radiation condensation; test time: and (6) 96 h.
Under UVB conditions: light source: UV-313; irradiance: 0.71W/m2(ii) nm; exposing at 60 + -3 deg.C for 4h, and exposing at 50 + -3 deg.C for 4h by non-radiation condensation; test time: and 72 h.
Through the examples and the comparative examples, the examples 1-5 have good anti-UV yellowing performance, and can reach the flame retardant level of VW-1 after the cable is manufactured through tests of 80 ℃ multiplied by 168h precipitation, high temperature, high humidity, 85 ℃ and 95% humidity multiplied by 168h precipitation; comparative example 1, the triazine charring agent used in a large amount cannot pass the precipitation test, and the flame retardant effect is poor and cannot pass the VW-1 test; comparative example 2 no char-forming agent is used, the char-forming effect by combustion is poor, and an ideal flame-retardant effect cannot be achieved; the comparative example 3 uses a styrene-divinylbenzene copolymer with DVB content less than 60%, the carbon forming effect is reduced due to low crosslinking degree, the carbon forming effect is not ideal when the flame-retardant resin is burnt, and the flame-retardant resin cannot reach the flame-retardant grade of VW-1, and the polyphenylene oxide resin used in the comparative example 4 has good flame-retardant property and precipitation resistance, but is yellowed after UV experiments, so that the requirements cannot be met.
The above description is not intended to limit the invention, nor is the invention limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the spirit of the invention.
Claims (9)
1. The high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition is characterized by comprising the following raw materials in percentage by mass:
styrenic thermoplastic elastomer: 15-30 percent,
Polyolefin resin: 10 to 25 percent,
Plasticizer: 15 to 25 percent,
A char-forming agent: 10 to 20 percent,
Phosphorus nitrogen flame retardant: 15-30 percent,
Flame retardant synergist: 0.5 to 3 percent,
Antioxidant: 0.1 to 1 percent,
Anti-aging agent: 0.1 to 1 percent,
Processing aid: 0.1-1%;
the charring agent is a compound of styrene-divinylbenzene copolymer powder and triazine charring agent, wherein the triazine charring agent accounts for less than or equal to 10% of the elastomer composition by mass;
the content of Divinylbenzene (DVB) in the styrene-divinylbenzene copolymer powder is more than or equal to 60 percent, and the average particle size is between 0.5 and 50 mu m;
the triazine charring agent is one or two of the following structures:
2. the high yellowing resistance and precipitation resistance halogen-free flame retardant thermoplastic elastomer composition according to claim 1, wherein the styrene thermoplastic elastomer is styrene-ethylene-butylene-styrene triblock copolymer (SEBS), and the styrene content is 10-50%.
3. The halogen-free flame retardant thermoplastic elastomer composition with high yellowing resistance and precipitation resistance of claim 1, wherein the polyolefin resin comprises any one or more of polypropylene, propylene-ethylene copolymer and polyethylene.
4. The high yellowing resistance, precipitation resistance, halogen-free, flame retardant thermoplastic elastomer composition according to claim 1, wherein the plasticizer is white oil.
5. The high yellowing resistance, precipitation resistance, halogen-free, flame retardant thermoplastic elastomer composition according to claim 1, wherein the phosphorus-nitrogen flame retardant is a compound of diethyl phosphinate and melamine cyanurate.
6. The high yellowing resistance and precipitation resistance halogen-free flame retardant thermoplastic elastomer composition according to claim 1, wherein the flame retardant synergist is any one or more of zinc borate, zirconium phosphate and organic montmorillonite.
7. The halogen-free flame retardant thermoplastic elastomer composition with high yellowing resistance and precipitation resistance as claimed in claim 1, wherein the antioxidant is one or two of hindered phenols and phosphites, and the anti-aging agent is one or more of benzophenones, triazoles and hindered amines.
8. The halogen-free flame retardant thermoplastic elastomer composition with high yellowing resistance and precipitation resistance of claim 1, wherein the processing aid comprises any one or more of silicone, EBS (N, N' -ethylene bis stearamide) and polyethylene wax.
9. The preparation method of the high yellowing resistance and precipitation resistance halogen-free flame retardant thermoplastic elastomer composition as claimed in any one of claims 1 to 8, characterized by comprising the following process steps:
(1) mixing 15-30% of styrene thermoplastic elastomer and 15-25% of plasticizer according to mass percentage, and filling oil to obtain a mixture 1;
(2) putting the mixture 1 in the step (1), 10-25% of polyolefin resin, 10-20% of char forming agent, 15-30% of phosphorus-nitrogen flame retardant, 0.5-3% of flame retardant synergist, 0.1-1% of antioxidant, 0.1-1% of anti-aging agent and 0.1-1% of processing aid into a high-speed mixer according to mass percentage, and uniformly mixing to obtain a mixture 2;
(3) and (3) adding the mixture 2 obtained in the step (2) into a double-screw extruder for extrusion granulation to obtain the high-yellowing-resistance precipitation-resistance halogen-free flame-retardant thermoplastic elastomer composition.
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| CN110938275A (en) * | 2019-12-17 | 2020-03-31 | 东莞市瑞能塑胶科技有限公司 | High-weather-resistance high-flame-retardant thermoplastic elastomer material and preparation method thereof |
| CN112778687B (en) * | 2021-01-29 | 2022-04-22 | 杭州捷尔思阻燃化工有限公司 | Ultraviolet yellowing resistant halogen-free flame retardant thermoplastic elastomer composition and preparation method thereof |
| CN112940435B (en) * | 2021-01-29 | 2023-03-28 | 宁波市青湖弹性体科技有限公司 | Low-compression permanent deformation thermoplastic elastomer sealing material and preparation method thereof |
| CN114350025B (en) * | 2022-01-10 | 2023-08-18 | 复旦大学 | High-char-forming halogen-free composite intumescent flame retardant and flame-retardant polystyrene resin |
| CN116515186A (en) * | 2023-04-26 | 2023-08-01 | 广东祥利特种材料科技有限公司 | Thermoplastic elastomer cable material and preparation method thereof |
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