CN112662039B - Flame-retardant EVA (ethylene-vinyl acetate copolymer) with excellent mechanical properties and preparation method thereof - Google Patents
Flame-retardant EVA (ethylene-vinyl acetate copolymer) with excellent mechanical properties and preparation method thereof Download PDFInfo
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Abstract
The invention relates to flame-retardant EVA with excellent mechanical properties, which comprises the following raw materials in parts by weight: 50-60 parts of EVA; 25-35 parts of aluminum hydroxide; 15-25 parts of magnesium hydroxide; 0.5-15 parts of calcium carbonate; 1-5 parts of stearic acid. The invention takes one or more of aluminum hydroxide, magnesium hydroxide or calcium carbonate as a flame retardant system, stearic acid as a modifier and EVA as a main body of a composite material to prepare the EVA with excellent mechanical properties and a preparation method thereof.
Description
Technical Field
The invention belongs to the field of polymer material additives, and particularly relates to flame-retardant EVA with excellent mechanical properties and a preparation method thereof.
Background
At the beginning of the 21 st century, with the advent of RoHs and WEEEs in the european union, the spread of impact, environmental protection flame retardants have gained widespread popularity. The reliable product quality enables the application range to be wider, and because the inorganic flame retardant is an indispensable important component for the environment-friendly flame retardant, more researchers begin to attach importance to the inorganic flame retardant due to the characteristics, so that the research strength is increased, and the research is hot in time. As for flame retardants, the variety of flame retardants is various, and halogen-free flame retardants are regarded as a type of flame retardants with excellent performance, and the environmental protection problem of conventional flame retardants is not well treated at that time, in which case the development of halogen-free flame retardants is carelessly advanced. In the aspect of material flame retardant technology, no halogenated key is pushed, and as one of main development directions, the research of the material is continuously carried out due to the requirements of development situations. More resources are put into the halogen-free low-toxicity flame-retardant material, and the material with better comprehensive performance is prepared.
EVA is formed by copolymerizing ethylene and acetic acid, and has the Chinese cultural name: ethylene-vinyl acetate copolymer (ethylene-vinyl acetate copolymer), EVA is widely applied, the annual market consumption is continuously increasing, and especially in the shoe industry, the EVA is applied to soles and interior materials of middle-high grade travel shoes, mountain climbing shoes, slippers and sandals, the flame retardant performance and flame retardant efficiency of the material are particularly important in application, and whether the material has low toxicity and low smoke characteristics is also considered. In the case of synthetic materials, it is necessary to add a large amount of magnesium hydroxide or aluminum hydroxide in order to satisfy the flame retardancy, but such an operation has disadvantages in that the mechanical properties of the material are lowered, particularly in that the impact strength and elongation of the material are lowered, thereby lowering the stability of the material.
Therefore, how to make the composite material have excellent mechanical properties while considering the flame retardance of the composite material, namely, not only make the material meet the flame retardant property requirement, but also do not damage the mechanical properties of the material as much as possible is a problem to be solved at present.
Disclosure of Invention
The invention aims to solve the problems and provide flame-retardant EVA with excellent mechanical properties and a preparation method thereof.
The aim of the invention is achieved by the following technical scheme:
the flame-retardant EVA with excellent mechanical properties comprises the following raw materials in parts by weight:
50-60 parts of EVA;
25-35 parts of aluminum hydroxide;
15-25 parts of magnesium hydroxide;
0.5-15 parts of calcium carbonate;
1-5 parts of stearic acid.
Preferably, the raw materials comprise the following components in parts by weight:
50 parts of EVA;
35 parts of aluminum hydroxide;
15 parts of magnesium hydroxide;
0.5 parts of calcium carbonate;
5 parts of stearic acid.
Preferably, the raw materials comprise the following components in parts by weight:
55 parts of EVA;
30 parts of aluminum hydroxide;
20 parts of magnesium hydroxide;
5 parts of calcium carbonate;
3 parts of stearic acid.
Preferably, the raw materials comprise the following components in parts by weight:
60 parts of EVA;
25 parts of aluminum hydroxide;
25 parts of magnesium hydroxide;
1 part of calcium carbonate;
15 parts of stearic acid.
Preferably, the EVA is 7470M commercially available under the trade name Taiwan chemical fiber.
A preparation method of flame-retardant EVA with excellent mechanical properties comprises the following steps: weighing according to a formula, mixing EVA by a high-speed mixer, drying by a baking oven, extruding by a double-screw extruder, granulating by a granulator, drying by the baking oven, granulating by the double-screw extruder, granulating by the granulator, drying by the baking oven, granulating by the double-screw extruder, and obtaining the finished product by an injection molding machine.
The set parameters of the twin-screw extruder should be 185 ℃ at the temperature of the machine head, 180 ℃ at the temperature of the five regions, 175 ℃ at the temperature of the four regions, 165 ℃ at the temperature of the three regions, 155 ℃ at the temperature of the two regions, 150 ℃ at the temperature of the one region and 10.4Hz of the host machine frequency.
The temperature parameters of the injection molding machine are 175 ℃ in one section, 180 ℃ in two sections and 180 ℃ in three sections.
According to the invention, one or more of aluminum hydroxide, magnesium hydroxide or calcium carbonate is used as a flame-retardant system, stearic acid is used as a modifier, EVA is used as a main body of the composite material, and the tensile strength, elongation at break and flame-retardant effect of EVA can be obviously improved.
Magnesium hydroxide, aluminum hydroxide and calcium carbonate flame retardants can exhibit a good dispersing effect in EVA compared to other flame retardants, which is difficult to achieve with other flame retardants. Not only are they readily available for flame retardant synergism with other materials, as a result of a variety of significant advantages that have led to their wider use. In the chemical experiment, the flame of the sample strip added with the flame retardant gradually reduces or even does not burn in the burning process, meanwhile, the dripping is obviously reduced, the effect on smoke suppression is outstanding, the phenomenon in the observation experiment can well indicate that the fire retardant is decomposed to emit water vapor, then the concentration of oxygen in a flame area is diluted, and meanwhile, the original high-temperature environment is broken through, so that the flame retardant has a certain cooling effect. In a great number of experimental processes, when a combustion test is carried out, dripping matters are flattened and unfolded to be a carbon-shaped substance, the phenomenon proves that the addition of the flame retardant is helpful for coking, then the dripping matters are filled into a high polymer, a certain amount of the dripping matters cannot be excessively or excessively reduced in the filling process, the purpose of the dripping matters is to facilitate forming a carbonization layer during combustion, the dripping matters are equivalent to forming a protective shell, the escaping heat of the combustible gas of small molecules can be blocked, and the entering of oxygen can be prevented, so that the flame retardant has a good flame retardant effect due to the reasons.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the preparation process is simple. The finished product can be obtained through an injection molding machine only by secondary granulation.
2. The product has excellent performance. The tensile strength, the elongation at break and the flame retardant effect are obviously improved, and the dispersion effect of the flame retardant in EVA is also good. During combustion, its flame gradually decreases or even does not burn, while dripping is significantly reduced.
3. The cost is controllable. The invention requires relatively low cost of materials and has strong practicability.
4. The method is green and environment-friendly. Because the halogen-free flame retardant is used, the secondary pollution can not be caused when the finished product is burnt.
Drawings
FIG. 1 is a graph showing the TG curve obtained by using a combined thermogravimetric-thermal differential analyzer in example 1 of the present invention.
Detailed Description
The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
Reagent: EVA (trade name: 7470M, manufacturer: taiwan chemical fiber, china), stearic acid, aluminum hydroxide, calcium carbonate, and magnesium hydroxide.
Instrument: a combined force thermogravimetry-thermal difference analyzer, an SHJ type homodromous double-screw extruder, an electrothermal constant temperature blast drying box, a plastic injection molding machine, an electronic universal testing machine and a planetary ball mill;
tensile strength test standard: GB/T1040.5-2008;
flame retardant performance test standard: UL94;
tensile strength test setup: 5mm/min.
Example 1
The raw materials and the weight parts of the raw materials are as follows: 50 parts of EVA, 35 parts of aluminum hydroxide, 15 parts of magnesium hydroxide, 5 parts of calcium carbonate and 0.5 part of stearic acid, and the specific parts are shown in Table 1.
The preparation method comprises the following steps: weighing according to a formula, mixing by a high-speed mixer (EVA mixing), drying by an oven, extruding by a double-screw extruder, granulating by a granulator, drying by an oven (primary granulating), extruding by a double-screw extruder, granulating by a granulator, drying by an oven (secondary granulating), and injecting by an injection molding machine. The set parameters of the extruder should be 185 ℃ at the temperature of the machine head, 180 ℃ at the temperature of the five regions, 175 ℃ at the temperature of the four regions, 165 ℃ at the temperature of the three regions, 155 ℃ at the temperature of the two regions, 150 ℃ at the temperature of the one region and 10.4Hz of the host machine frequency. The temperature parameters of the injection molding machine are 175 ℃ in one section, 180 ℃ in two sections and 180 ℃ in three sections.
The finished product is tested, the tensile strength is 10.743MPa, the elongation at break is 209.62%, and the flame retardant property is V-0.
The TG curve is obtained by using a combined thermal gravimetric-thermal differential analyzer, and as can be seen from fig. 1, the thermal decomposition temperature of the whole system is about 350 ℃, and at the same time, the system starts to lose weight, and when the temperature reaches about 510 ℃, the system starts to be stable. The high temperature resistance of the flame retardant system synthesized by the invention is excellent, and the high temperature resistance can reach about 350 ℃ as can be seen from the figure, which shows that the flame retardant system can be used for producing wires and cables to a certain extent, and the high temperature resistance requirement can be met. In addition, the decomposition temperature of the system added with the inorganic flame retardant is greatly improved, and the aim of flame retardance is fulfilled.
Example 2
The raw materials and the weight parts of the raw materials are as follows: 55 parts of EVA, 30 parts of aluminum hydroxide, 20 parts of magnesium hydroxide, 3 parts of stearic acid, 5 parts of calcium carbonate and the specific details are shown in table 1.
The preparation method comprises the following steps: weighing according to a formula, mixing by a high-speed mixer (EVA mixing), drying by an oven, extruding by a double-screw extruder, granulating by a granulator, drying by an oven (primary granulating), extruding by a double-screw extruder, granulating by a granulator, drying by an oven (secondary granulating), and injecting by an injection molding machine. The set parameters of the extruder should be 185 ℃ at the temperature of the machine head, 180 ℃ at the temperature of the five regions, 175 ℃ at the temperature of the four regions, 165 ℃ at the temperature of the three regions, 155 ℃ at the temperature of the two regions, 150 ℃ at the temperature of the one region and 10.4Hz of the host machine frequency. The temperature parameters of the injection molding machine are 175 ℃ in one section, 180 ℃ in two sections and 180 ℃ in three sections.
The finished product is tested, the tensile strength is 10.05MPa, the elongation at break is 218.86%, and the flame retardant property is V-0.
Example 3
The raw materials and the weight parts of the raw materials are as follows: 60 parts of EVA, 25 parts of aluminum hydroxide, 25 parts of magnesium hydroxide, 1 part of stearic acid, 15 parts of calcium carbonate and the specific details are shown in table 1.
The preparation method comprises the following steps: weighing according to a formula, mixing by a high-speed mixer (EVA mixing), drying by an oven, extruding by a double-screw extruder, granulating by a granulator, drying by an oven (primary granulating), extruding by a double-screw extruder, granulating by a granulator, drying by an oven (secondary granulating), and injecting by an injection molding machine. The set parameters of the extruder should be 185 ℃ at the temperature of the machine head, 180 ℃ at the temperature of the five regions, 175 ℃ at the temperature of the four regions, 165 ℃ at the temperature of the three regions, 155 ℃ at the temperature of the two regions, 150 ℃ at the temperature of the one region and 10.4Hz of the host machine frequency. The temperature parameters of the injection molding machine are 175 ℃ in one section, 180 ℃ in two sections and 180 ℃ in three sections.
The finished product is tested, the tensile strength is 13.011MPa, the elongation at break is 249.83%, and the flame retardant property is V-0.
Comparative example 1
Compared with the example 1, the invention has the advantages that stearic acid is not added, the rest is the same, and the finished product is tested, the tensile strength is 5.271MPa, the elongation at break is 171.62%, the flame retardant property is V-0, and the performance is greatly reduced.
Comparative example 2
Compared with the example 1, the invention has the advantages that no aluminum hydroxide is added, the rest is the same, and the finished product is tested, the tensile strength is 11.865MPa, the elongation at break is 212.47%, the flame retardant property is V-1, and the flame retardant property is reduced.
Table 1 raw material components of examples and comparative examples
From comparative example 1, it is known that stearic acid is mainly used as a dispersant, and can effectively improve the distribution of the flame retardant system; as is clear from comparative example 2, aluminum hydroxide can effectively improve flame retardant properties.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (3)
1. The preparation method of the flame-retardant EVA with excellent mechanical properties is characterized by comprising the following raw materials in parts by weight: 50 parts of EVA, 35 parts of aluminum hydroxide, 15 parts of magnesium hydroxide, 5 parts of calcium carbonate and 0.5 part of stearic acid, and the preparation method comprises the following steps: weighing according to a formula, mixing EVA by a high-speed mixer, drying by a baking oven, extruding by a double-screw extruder, granulating by a granulator, drying by the baking oven, granulating by the double-screw extruder, granulating by the granulator, drying by the baking oven, granulating by the double-screw extruder, and molding by an injection molding machine to obtain a finished product;
setting parameters of the extruder are 185 ℃ for the temperature of a machine head, 180 ℃ for the temperature of five areas, 175 ℃ for the temperature of four areas, 165 ℃ for the temperature of three areas, 155 ℃ for the temperature of two areas, 150 ℃ for the temperature of one area and 10.4Hz for the host machine frequency; the temperature parameters of the injection molding machine are 175 ℃ in the first section, 180 ℃ in the second section and 180 ℃ in the third section;
the finished product is tested, the tensile strength is 10.743MPa, the elongation at break is 209.62%, and the flame retardant property is V-0.
2. The preparation method of the flame-retardant EVA with excellent mechanical properties is characterized by comprising the following raw materials in parts by weight: 55 parts of EVA, 30 parts of aluminum hydroxide, 20 parts of magnesium hydroxide, 3 parts of stearic acid, 5 parts of calcium carbonate and the preparation method comprises the following steps: weighing according to a formula, mixing EVA by a high-speed mixer, drying by a baking oven, extruding by a double-screw extruder, granulating by a granulator, drying by the baking oven, granulating by the double-screw extruder, granulating by the granulator, drying by the baking oven, granulating by the double-screw extruder, and molding by an injection molding machine to obtain a finished product;
setting parameters of the extruder are 185 ℃ for the temperature of a machine head, 180 ℃ for the temperature of five areas, 175 ℃ for the temperature of four areas, 165 ℃ for the temperature of three areas, 155 ℃ for the temperature of two areas, 150 ℃ for the temperature of one area and 10.4Hz for the host machine frequency; the temperature parameters of the injection molding machine are 175 ℃ in the first section, 180 ℃ in the second section and 180 ℃ in the third section;
the finished product is tested, the tensile strength is 10.05MPa, the elongation at break is 218.86%, and the flame retardant property is V-0.
3. The preparation method of the flame-retardant EVA with excellent mechanical properties is characterized by comprising the following raw materials in parts by weight: 60 parts of EVA, 25 parts of aluminum hydroxide, 25 parts of magnesium hydroxide, 1 part of stearic acid and 15 parts of calcium carbonate, and the preparation method comprises the following steps: weighing according to a formula, mixing EVA by a high-speed mixer, drying by a baking oven, extruding by a double-screw extruder, granulating by a granulator, drying by the baking oven, granulating by the double-screw extruder, granulating by the granulator, drying by the baking oven, granulating by the double-screw extruder, and molding by an injection molding machine to obtain a finished product;
setting parameters of the extruder are 185 ℃ for the temperature of a machine head, 180 ℃ for the temperature of five areas, 175 ℃ for the temperature of four areas, 165 ℃ for the temperature of three areas, 155 ℃ for the temperature of two areas, 150 ℃ for the temperature of one area and 10.4Hz for the host machine frequency; the temperature parameters of the injection molding machine are 175 ℃ in the first section, 180 ℃ in the second section and 180 ℃ in the third section;
the finished product is tested, the tensile strength is 13.011MPa, the elongation at break is 249.83%, and the flame retardant property is V-0.
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