CN112876820A - Polyethylene terephthalate composite material - Google Patents
Polyethylene terephthalate composite material Download PDFInfo
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- CN112876820A CN112876820A CN202110068375.1A CN202110068375A CN112876820A CN 112876820 A CN112876820 A CN 112876820A CN 202110068375 A CN202110068375 A CN 202110068375A CN 112876820 A CN112876820 A CN 112876820A
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
本发明公开了一种聚对苯二甲酸乙二醇酯复合材料。由聚对苯二甲酸乙二醇酯、木质素磺酸钠和苯并噁嗪三种材料制成；聚对苯二甲酸乙二醇酯的质量份数为70～99，木质素磺酸钠的质量份数为1～30，苯并噁嗪的质量份数为1～30；将三种材料干燥处理；将干燥处理后的聚对苯二甲酸乙二醇酯、苯并噁嗪与木质素磺酸钠进行熔融共混，得到共混复合材料；将共混复合材料进行注塑成型，得到复合材料样条；将复合材料样条进行加热固化；冷却至常温。本发明的聚对苯二甲酸乙二醇酯复合材料的热稳定性能和阻燃性能高，在薄膜片材、包装瓶、电子电器、汽车配件和机械设备等领域具有广泛的应用前景。The invention discloses a polyethylene terephthalate composite material. It is made of polyethylene terephthalate, sodium lignosulfonate and benzoxazine; the mass fraction of polyethylene terephthalate is 70-99, sodium lignosulfonate The parts by mass of benzoxazine are 1-30, and the parts by mass of benzoxazine are 1-30; the three materials are dried; the dried polyethylene terephthalate, benzoxazine and wood Sodium sulfonate is melted and blended to obtain a blended composite material; the blended composite material is injection-molded to obtain a composite material spline; the composite material spline is heated and solidified; and cooled to normal temperature. The polyethylene terephthalate composite material of the invention has high thermal stability and flame retardancy, and has wide application prospects in the fields of film sheets, packaging bottles, electronic appliances, auto parts, mechanical equipment and the like.
Description
Technical Field
The invention relates to a composite material, in particular to a polyethylene glycol terephthalate composite material with high thermal stability and flame retardant property.
Background
Polyethylene terephthalate is an important engineering plastic, and is widely applied to the fields of film sheets, packaging bottles, electronic and electric appliances, automobile accessories, mechanical equipment and the like due to excellent physical and mechanical properties. However, polyethylene terephthalate is highly flammable, which exhibits severe dripping behavior when burned, and thus the flame is rapidly spread. This high risk of fire poses a serious threat to the safety of people's lives and property. In order to improve the flame retardant property of polyethylene terephthalate, adding a flame retardant is an effective method. However, since the charring performance of polyethylene terephthalate is not high, the thermal stability and charring performance of common flame retardants cannot be improved significantly, and thus the problems of melt dripping and low flame retardant performance cannot be solved effectively. Therefore, how to effectively improve the char-forming performance of polyethylene terephthalate is still one of the difficulties faced in improving the flame retardant performance. The effective solution of the problem is valuable for improving the flame retardant property of the polyethylene terephthalate and expanding the application field of the polyethylene terephthalate.
Disclosure of Invention
In order to overcome the problems in the prior art, the invention provides a polyethylene terephthalate composite material.
In order to achieve the above purpose, the invention adopts a technical scheme for solving the technical problems that:
the composite material is mainly prepared from polyethylene glycol terephthalate, sodium lignosulfonate and benzoxazine.
The composite material comprises, by mass, 70-99 parts of polyethylene glycol terephthalate, 1-30 parts of sodium lignosulfonate and 1-30 parts of benzoxazine.
The composite material comprises, by mass, 80-90 parts of polyethylene glycol terephthalate, 10-20 parts of sodium lignosulfonate and 10-20 parts of benzoxazine.
The mass ratio of benzoxazine to sodium lignosulfonate in the composite material is 0.5-2.
The benzoxazine is a compound with a six-membered oxazine ring structure containing nitrogen and oxygen in the molecule.
The composite material is prepared by adopting the following steps:
1) drying polyethylene glycol terephthalate, benzoxazine and sodium lignosulfonate;
2) carrying out melt blending on the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate which are dried in the step 1) to obtain a blended composite material;
3) performing injection molding on the blended composite material obtained in the step 2) to obtain a composite material sample strip;
4) heating and curing the composite material sample strip obtained in the step 3) to obtain the polyethylene terephthalate composite material.
The drying treatment temperature in the step 1) is 80 ℃, and the drying treatment time is 8 hours.
The mass parts of the polyethylene glycol terephthalate, the sodium lignosulfonate and the benzoxazine in the blending composite material obtained in the step 2) are 70-99, 1-30 and 1-30 respectively.
The blending composite material obtained in the step 2) comprises, by mass, 80-90 parts of polyethylene glycol terephthalate, 10-20 parts of sodium lignosulfonate and 10-20 parts of benzoxazine.
The melt blending in the step 2) adopts a torque rheometer, the temperature is 270 ℃, the rotor speed is 60 r/min, and the time is 2 min.
The injection molding in the step 3) adopts an injection molding machine, the temperature of an injection zone is 255 ℃, the temperature of a template zone is 45 ℃, and the pressure maintaining time is 2 minutes.
The heating and curing process in the step 4) comprises the following steps: and step temperature control is arranged for processing, and specifically, the heat treatment is carried out for 1-3 hours at 120-140 ℃, for 1-3 hours at 150-170 ℃, for 1-3 hours at 180-200 ℃, for 0.5-2 hours at 210-230 ℃ and for 10-60 minutes at 240-260 ℃ in sequence, and then the mixture is cooled to the normal temperature.
Preferably, the heating and curing process in step 4) is as follows: the treatment is carried out by setting a step temperature control, specifically, the heat treatment is carried out at 130 ℃ for 2 hours, at 160 ℃ for 2 hours, at 190 ℃ for 2 hours, at 220 ℃ for 1 hour, at 250 ℃ for 0.5 hour, and then the mixture is cooled to the normal temperature.
The invention has the following beneficial effects:
the raw materials of benzoxazine and sodium lignosulfonate used in the invention can effectively improve the char forming capability of the polyethylene glycol terephthalate, thereby improving the combustion dripping behavior and the flame retardant property of the polyethylene glycol terephthalate, and the preparation method is simple and has wide application prospects in the fields of film sheets, packaging bottles, electronic and electric appliances, automobile accessories, mechanical equipment and the like.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
In the examples of the present invention, polyethylene terephthalate, benzoxazine (6,6' - (propane-2,2-diyl) bis (3-phenyl-3,4-dihydro-2H-benzo [ e ] [1,3] oxazine)) and sodium lignosulfonate were commercially available materials.
The thermal stability performance test method comprises the following steps: using a thermogravimetric analyzer (NETZSCH, TG 209F1), temperature range: room temperature-650 ℃, heating rate: 10 ℃/min, nitrogen atmosphere.
The flame retardant property test method comprises the following steps: testing with oxygen index analyzer (PX-01-005, Phoenix, Suzhou) according to national standard GB/T2406.2-2009; the test was carried out using a UL94 vertical horizontal burning tester (PX-03-001, Phoenix, Suzhou) according to the national standard GB/T2408-2008.
Example 1
1) 27g of polyethylene terephthalate and 3g of benzoxazine were weighed and dried in a drying oven at 80 ℃ for 8 hours to obtain dried benzoxazine and polyethylene terephthalate.
2) Adding the dried polyethylene glycol terephthalate and benzoxazine obtained in the step 1) into a torque rheometer to perform melt blending, wherein the temperature is 270 ℃, the rotor speed is 60 r/min, and the time is 2 min; taking out the blending composite material, and cooling to normal temperature to obtain the blending composite material of the polyethylene terephthalate and the benzoxazine.
3) Adding the blending composite material of the polyethylene glycol terephthalate and the benzoxazine obtained in the step 2) into a micro injection molding machine for injection molding, wherein the temperature of an injection zone is 255 ℃, the temperature of a template zone is 45 ℃, and the pressure maintaining time is 2 minutes, so as to obtain the composite material sample strip of the polyethylene glycol terephthalate and the benzoxazine.
4) Heating and curing the sample strips of the blending composite material of the polyethylene terephthalate and the benzoxazine obtained in the step 3), sequentially carrying out heat treatment at 130 ℃ for 2 hours, 160 ℃ for 2 hours, 190 ℃ for 2 hours, 220 ℃ for 1 hour and 250 ℃ for 0.5 hour, and cooling to the normal temperature.
The results of the thermal stability testing are shown in table 1.
The results of the flame retardant property test are shown in table 2.
Example 2
1) 27g of polyethylene terephthalate, 2g of benzoxazine and 1g of sodium lignosulfonate were weighed and dried in a drying oven at 80 ℃ for 8 hours to obtain dried polyethylene terephthalate, benzoxazine and sodium lignosulfonate.
2) Adding the dried polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 1) into a torque rheometer to perform melt blending, wherein the temperature is 270 ℃, the rotor speed is 60 revolutions per minute, and the time is 2 minutes; taking out the blended composite material, and cooling to normal temperature to obtain the blended composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate.
3) Adding the blending composite material of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 2) into a micro injection molding machine for injection molding, wherein the temperature of an injection area is 255 ℃, the temperature of a template area is 45 ℃, and the pressure maintaining time is 2 minutes, so as to obtain the composite material sample strip of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate.
4) Heating and curing the sample strips of the composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 3), sequentially carrying out heat treatment at 130 ℃ for 2 hours, 160 ℃ for 2 hours, 190 ℃ for 2 hours, 220 ℃ for 1 hour and 250 ℃ for 0.5 hour, and cooling to the normal temperature.
The results of the thermal stability test are shown in Table 1
The results of the flame retardant property test are shown in table 2.
Example 3
1) 27g of polyethylene terephthalate, 1.5g of benzoxazine and 1.5g of sodium lignosulfonate were weighed and dried in a drying oven at 80 ℃ for 8 hours to obtain dried polyethylene terephthalate, benzoxazine and sodium lignosulfonate.
2) Adding the dried polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 1) into a torque rheometer to perform melt blending, wherein the temperature is 270 ℃, the rotor speed is 60 revolutions per minute, and the time is 2 minutes; taking out the blended composite material, and cooling to normal temperature to obtain the blended composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate.
3) Adding the blending composite material of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 2) into a micro injection molding machine for injection molding, wherein the temperature of an injection area is 255 ℃, the temperature of a template area is 45 ℃, and the pressure maintaining time is 2 minutes, so as to obtain the composite material sample strip of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate.
4) Heating and curing the sample strips of the composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 3), sequentially carrying out heat treatment at 130 ℃ for 2 hours, 160 ℃ for 2 hours, 190 ℃ for 2 hours, 220 ℃ for 1 hour and 250 ℃ for 0.5 hour, and cooling to the normal temperature.
The results of the thermal stability testing are shown in table 1.
The results of the flame retardant property test are shown in table 2.
Example 4
1) 27g of polyethylene terephthalate, 1g of benzoxazine and 2g of sodium lignosulfonate were weighed and dried in a drying oven at 80 ℃ for 8 hours to obtain dried polyethylene terephthalate, benzoxazine and sodium lignosulfonate.
2) Adding the dried polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 1) into a torque rheometer to perform melt blending, wherein the temperature is 270 ℃, the rotor speed is 60 revolutions per minute, and the time is 2 minutes; taking out the blended composite material, and cooling to normal temperature to obtain the blended composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate.
3) Adding the blending composite material of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 2) into a micro injection molding machine for injection molding, wherein the temperature of an injection area is 255 ℃, the temperature of a template area is 45 ℃, and the pressure maintaining time is 2 minutes, so as to obtain the composite material sample strip of the polyethylene glycol terephthalate, the benzoxazine and the sodium lignosulfonate.
4) Heating and curing the sample strips of the composite material of the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate obtained in the step 3), sequentially carrying out heat treatment at 130 ℃ for 2 hours, 160 ℃ for 2 hours, 190 ℃ for 2 hours, 220 ℃ for 1 hour and 250 ℃ for 0.5 hour, and cooling to the normal temperature.
The results of the thermal stability testing are shown in table 1.
The results of the flame retardant property test are shown in table 2.
Example 5
1) 27g of polyethylene terephthalate and 3g of sodium lignin sulfonate are weighed and dried in a drying oven at 80 ℃ for 8 hours to obtain dried polyethylene terephthalate and sodium lignin sulfonate.
2) Adding the dried polyethylene terephthalate obtained in the step 1) and sodium lignin sulfonate into a torque rheometer to perform melt blending, wherein the temperature is 270 ℃, the rotor speed is 60 r/min, and the time is 2 min; taking out the blended composite material, and cooling to normal temperature to obtain the blended composite material of the polyethylene terephthalate and the sodium lignosulfonate.
3) Adding the blending composite material of the polyethylene terephthalate and the sodium lignin sulfonate obtained in the step 2) into a micro injection molding machine for injection molding, wherein the temperature of an injection area is 255 ℃, the temperature of a template area is 45 ℃, and the pressure maintaining time is 2 minutes, so as to obtain the composite material sample strip of the polyethylene terephthalate and the sodium lignin sulfonate.
4) Heating and curing the sample strip of the composite material of the polyethylene terephthalate and the sodium lignosulfonate obtained in the step 3), sequentially carrying out heat treatment at 130 ℃ for 2 hours, 160 ℃ for 2 hours, 190 ℃ for 2 hours, 220 ℃ for 1 hour and 250 ℃ for 0.5 hour, and cooling to the normal temperature.
The results of the thermal stability testing are shown in table 1.
The results of the flame retardant property test are shown in table 2.
TABLE 1
Note: the control was pure polyethylene terephthalate.
As can be seen from table 1:
compared with pure polyethylene terephthalate, the residual carbon content of the polyethylene terephthalate composite material added with benzoxazine and sodium lignosulfonate is obviously improved at 650 ℃. The highest carbon residue at 650 ℃ in example 2 is higher than the carbon residues at 650 ℃ in examples 1 and 5 and also higher than the carbon residues at 650 ℃ in examples 3 and 4, indicating that the two materials sodium lignosulfonate and benzoxazine are synergistic and related to the formulation ratio.
TABLE 2
| Sample (I) | Limiting oxygen index (%) | Vertical burning class UL-94 |
| Example 1 | 25.5 | V-2 |
| Example 2 | 26.4 | V-1 |
| Example 3 | 24.8 | V-2 |
| Example 4 | 24.6 | V-2 |
| Example 5 | 23.1 | V-2 |
| Control | 21.8 | NR |
Note: the control was pure polyethylene terephthalate.
As can be seen from table 2:
the limiting oxygen index of example 2 is the highest, higher than that of examples 1 and 5, and also higher than that of examples 3 and 4. Example 2 the vertical burn rating reached a V-1 rating better than the other examples. The two materials of sodium lignosulfonate and benzoxazine have synergistic effect on flame retardance and are related to the mixture ratio.
The above examples are only for explaining the present invention, and do not limit the scope of protection of the present invention. Any equivalent changes or modifications made within the spirit of the present invention and the scope of the claims are to be considered as within the scope of the present invention.
Claims (10)
1. A polyethylene terephthalate composite material is characterized in that: the composite material is mainly prepared from polyethylene glycol terephthalate, sodium lignosulfonate and benzoxazine.
2. The polyethylene terephthalate composite material according to claim 1, wherein: the composite material comprises, by mass, 70-99 parts of polyethylene glycol terephthalate, 1-30 parts of sodium lignosulfonate and 1-30 parts of benzoxazine.
3. The polyethylene terephthalate composite material according to claim 2, wherein: the composite material comprises, by mass, 80-90 parts of polyethylene glycol terephthalate, 10-20 parts of sodium lignosulfonate and 10-20 parts of benzoxazine.
4. The polyethylene terephthalate composite material according to claim 1, wherein: the mass ratio of benzoxazine to sodium lignosulfonate in the composite material is 0.5-2.
5. The polyethylene terephthalate composite material according to claim 1, wherein: the benzoxazine is a compound with a six-membered oxazine ring structure containing nitrogen and oxygen in the molecule.
6. The polyethylene terephthalate composite material according to claim 1, wherein: the composite material is prepared by adopting the following steps:
1) drying polyethylene glycol terephthalate, benzoxazine and sodium lignosulfonate;
2) carrying out melt blending on the polyethylene terephthalate, the benzoxazine and the sodium lignosulfonate which are dried in the step 1) to obtain a blended composite material;
3) performing injection molding on the blended composite material obtained in the step 2) to obtain a composite material sample strip;
4) heating and curing the composite material sample strip obtained in the step 3).
7. The polyethylene terephthalate composite material according to claim 6, wherein: the drying treatment temperature in the step 1) is 80 ℃, and the drying treatment time is 8 hours.
8. The polyethylene terephthalate composite material according to claim 6, wherein: the mass parts of the polyethylene glycol terephthalate, the sodium lignosulfonate and the benzoxazine in the blending composite material obtained in the step 2) are 70-99, 1-30 and 1-30 respectively.
9. The polyethylene terephthalate composite material according to claim 6, wherein: the blending composite material obtained in the step 2) comprises, by mass, 80-90 parts of polyethylene glycol terephthalate, 10-20 parts of sodium lignosulfonate and 10-20 parts of benzoxazine.
10. The polyethylene terephthalate composite material according to claim 6, wherein: the heating and curing process in the step 4) comprises the following steps: and step temperature control is arranged for processing, and specifically, the heat treatment is carried out for 1-3 hours at 120-140 ℃, for 1-3 hours at 150-170 ℃, for 1-3 hours at 180-200 ℃, for 0.5-2 hours at 210-230 ℃ and for 10-60 minutes at 240-260 ℃ in sequence, and then the mixture is cooled to the normal temperature.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161762A (en) * | 2011-01-19 | 2011-08-24 | 华东理工大学 | Method for modifying benzoxazine resin |
| CN102250383A (en) * | 2011-06-28 | 2011-11-23 | 华南理工大学 | Halogen-free fire retardant containing benzoxazine and polymer material comprising same |
| CN109942894A (en) * | 2019-02-23 | 2019-06-28 | 河南大学 | A halogen-free intumescent flame retardant system containing benzoxazine char-forming agent and its flame retardant thermoplastic resin |
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- 2021-01-19 CN CN202110068375.1A patent/CN112876820B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161762A (en) * | 2011-01-19 | 2011-08-24 | 华东理工大学 | Method for modifying benzoxazine resin |
| CN102250383A (en) * | 2011-06-28 | 2011-11-23 | 华南理工大学 | Halogen-free fire retardant containing benzoxazine and polymer material comprising same |
| CN109942894A (en) * | 2019-02-23 | 2019-06-28 | 河南大学 | A halogen-free intumescent flame retardant system containing benzoxazine char-forming agent and its flame retardant thermoplastic resin |
Non-Patent Citations (1)
| Title |
|---|
| AKSHAY ET AL: "Sodium lignin sulfonate: a bio-macromolecule for making fire retardant cotton fabric", 《CELLULOSE》 * |
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