CN109679203B - Halogen-free glass fiber reinforced polypropylene composite material and preparation method thereof - Google Patents
Halogen-free glass fiber reinforced polypropylene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a halogen-free glass fiber reinforced polypropylene composite material and a preparation method thereof, wherein the material is prepared by adsorbing a carbon forming agent on the surface of glass fiber by utilizing the hydrogen bond action between the glass fiber treated by a coupling agent and the carbon forming agent to obtain a surface modified glass fiber reinforcement; the polypropylene resin, the modified glass fiber reinforcement, the intumescent flame retardant, the compatilizer and the antioxidant are compounded by a melt blending method to prepare the polypropylene composite material. Because the surface of the glass fiber is coated with the carbon forming agent, the carbon forming agent on the interface and the intumescent flame retardant in the matrix generate a synergistic effect, in the combustion process, the wettability of polymer melt to the glass fiber is reduced, and the heat backflow is slowed down so as to slow down the decomposition and combustion of the polymer, so that the 'wick effect' is effectively eliminated. The polypropylene composite material has the advantages of good flame retardant property, high flame retardant efficiency and excellent mechanical property.
Description
Technical Field
The invention belongs to the field of composite materials, relates to a preparation method of a halogen-free flame-retardant glass fiber reinforced polypropylene composite material, and more particularly relates to a glass fiber reinforcement loaded with a charring agent and a polypropylene composite material with good flame retardant property, high flame retardant efficiency and excellent mechanical property, which are prepared through hydrogen bonding.
Background
The polypropylene has the advantages of good mechanical property, easy forming and processing, low cost and the like, and is one of four general materials. In practical engineering applications, in order to make the mechanical properties meet engineering requirements, glass fibers are usually added into a polypropylene matrix for reinforcement treatment, so as to obtain a glass fiber reinforced polypropylene composite material.
The polypropylene only contains C and H as constituent elements, has an oxygen index of about 17.5, is extremely easy to burn, and has a great fire hazard, so that the polypropylene is often subjected to flame retardant modification by adding a flame retardant into a polypropylene matrix. Flame retardants for flame retarding polypropylene can be broadly classified into three categories: inorganic flame retardant, halogen flame retardant and intumescent flame retardant. The intumescent flame retardant is a composite flame retardant mainly composed of nitrogen and phosphorus, does not contain halogen, does not adopt antimony oxide as a synergist, foams and expands when being heated, is called as the intumescent flame retardant and is an environment-friendly flame retardant with high efficiency and low toxicity. The flame retardant has the advantages of no toxicity, low smoke, is the best environment-friendly flame retardant, and also conforms to the current development trend of environmental protection.
The glass fiber can be used as a reinforcing body to effectively improve the mechanical property of the polypropylene, although the glass fiber is not flammable, the burning process of the glass fiber reinforced polypropylene composite material is more violent due to the wick effect in the burning process, and therefore, the flame retardance of the glass fiber reinforced polypropylene composite material is more difficult than that of the polypropylene.
Patent CN104693604A reports a halogen-free flame-retardant glass fiber reinforced polypropylene composite material and a preparation method thereof, wherein a main flame retardant used is a phosphorus-nitrogen flame retardant, a secondary flame retardant is a phosphate flame retardant, the flame retardant is high in cost, and the introduction of flame retardant particles in a matrix can destroy interface combination, so that the mechanical property is greatly influenced L iu L and the like (2015, compositions Science and Technology 121, volume: 9-15) in an Interfacealcarring method to over-working in glass fiber-reinforford polypropylene composite, an interface flame-retardant mechanism is proposed, a phosphorus-containing flame retardant micromolecule DOPO is grafted on the surface of a glass fiber, the modified glass fiber is added into the polypropylene matrix, so that the 'wick effect' in the combustion process can be effectively overcome, but the interface flame-retardant mechanism can not enable the polypropylene composite material to reach the usable flame-retardant grade, the addition of the flame-retardant glass fiber reinforced polypropylene composite material and the preparation method thereof is better than that of a traditional expanded polypropylene flame retardant and an ammonium polyphosphate flame retardant is added to the polypropylene matrix, and the flame retardant is tested by the traditional flame retardant Technology.
Disclosure of Invention
The invention aims to provide a halogen-free flame-retardant glass fiber reinforced polypropylene composite material with good flame-retardant property, high flame-retardant efficiency and excellent mechanical property and a preparation method thereof.
The specific technical scheme of the invention is as follows: a halogen-free glass fiber reinforced polypropylene composite material is characterized in that a carbon forming agent is adsorbed on the surface of glass fiber under the action of hydrogen bonds between the glass fiber treated by a coupling agent and the carbon forming agent to obtain a surface modified glass fiber reinforcement; the polypropylene resin, the modified glass fiber reinforcement, the intumescent flame retardant, the compatilizer and the antioxidant are compounded by a melt blending method to prepare the polypropylene composite material.
Because the surface of the glass fiber is coated with the carbon forming agent, the carbon forming agent on the interface and the intumescent flame retardant in the matrix generate a synergistic effect, in the combustion process, the wettability of polymer melt to the glass fiber is reduced, and the heat backflow is slowed down so as to slow down the decomposition and combustion of the polymer, so that the 'wick effect' is effectively eliminated.
The invention also provides a preparation method of the halogen-free flame-retardant glass fiber reinforced composite material, which comprises the following steps:
(1) weighing 20-40 parts by weight of commercial glass fiber, soaking the glass fiber in nitric acid solution with the molar concentration of 0.5-1.5 mol/L for 4-6 hours, and repeatedly cleaning with deionized water to remove sizing agent on the surface of the glass fiber.
(2) And (2) soaking the glass fiber obtained in the step (1) in 1-3 wt% of hydrolyzed silane coupling agent, treating for 1-2 hours, and repeatedly cleaning with deionized water.
(3) And (3) soaking the glass fiber obtained in the step (2) in 3-5 wt% of a carbon forming agent, treating for 4-6 hours, repeatedly cleaning with deionized water, and drying to obtain the glass fiber reinforcement with the surface coated with the carbon forming agent.
(4) And (3) mixing an acid source, a gas source and a carbon source of the intumescent flame retardant according to the ratio of 7-10: 3-5: and 2-4, adding the mixture into a high-speed mixer, and uniformly mixing to obtain the intumescent flame retardant.
(5) And (3) melting and blending polypropylene resin, an intumescent flame retardant, a compatilizer and an antioxidant with the glass fiber obtained in the step (3), and extruding and granulating by using a double-screw extruder to obtain the halogen-free flame-retardant glass fiber reinforced polypropylene composite material.
Wherein, the polypropylene resin, the intumescent flame retardant, the compatilizer and the antioxidant are added from a main feed, the glass fiber is fed from a glass fiber feeding hole of a double-screw extruder, the double-screw extruder is divided into five temperature control intervals from a feeding port to a machine head, and the processing conditions are as follows:
temperature in the first zone: 180-200 ℃ and the temperature of the second zone: 200-220 ℃, and three-zone temperature: 200-220 ℃ and four-zone temperature: 180-200 ℃ and the temperature of the five zones: 180-200 ℃. Head temperature: 180-200 ℃; screw rotation speed: 150 to 180 r/min.
The halogen-free flame-retardant glass fiber reinforced polypropylene composite material comprises the following components in percentage by weight: (a) 40-60 parts of polypropylene resin, (b) 20-40 parts of intumescent flame retardant, (c) 20-40 parts of glass fiber coated with carbon forming agent, (d) 2-6 parts of compatilizer, and (e) 0.4-0.6 part of antioxidant.
The polypropylene resin is a polypropylene resin with a melt flow rate of 2-4 g/10 min.
The glass fiber is alkali-free high-strength glass fiber, and the charring agent is coated through the action of hydrogen bonds.
The compatilizer is polypropylene grafted maleic anhydride.
The coupling agent is (3-aminopropyl) triethoxysilane.
The antioxidant is one or a combination of several of antioxidant 168, antioxidant 1010 and antioxidant 628.
The acid source in the intumescent flame retardant is any one of ammonium phosphate, ammonium polyphosphate and melamine phosphate.
The gas source in the intumescent flame retardant is any one of melamine, melamine cyanurate and polyamide.
The carbon source in the intumescent flame retardant is any one of pentaerythritol, dipentaerythritol, tripentaerythritol and pentaerythritol phosphate.
The carbon forming agent is any one of pentaerythritol, dipentaerythritol, tripentaerythritol and pentaerythritol phosphate.
According to the invention, the coupling agent is used for carrying out surface modification on the glass fiber, then the hydrogen bond effect between the coupling agent and the char forming agent is utilized to prepare the glass fiber reinforcement loaded with the char forming agent, and the interfacial phase flame retardant mechanism and the matrix phase flame retardant mechanism have synergistic effect, so that the flame retardant property of the polymer can be improved, the interfacial bonding between the reinforcement and the matrix is improved, and the mechanical property is further improved.
Drawings
FIG. 1 is a scanning electron microscope image of a carbon layer of a glass fiber reinforced polypropylene composite material of comparative example 1 after a cone calorimetry test;
FIG. 2 is a scanning electron microscope image of a carbon layer of the glass fiber reinforced polypropylene composite material of comparative example 2 after a cone calorimetry test;
FIG. 3 is a scanning electron microscope image of a glass fiber reinforcement obtained by treating a glass fiber reinforcement with 1 mol/L nitric acid for 5 hours, treating the glass fiber reinforcement with 3 wt% hydrolyzed (3-aminopropyl) triethoxysilane for 1 hour, and treating the glass fiber reinforcement with 3-5 wt% char-forming agent for 4 hours;
FIG. 4 is a scanning electron microscope image of the carbon layer of the glass fiber reinforced polypropylene composite material after cone calorimetry test.
Detailed Description
The following examples are presented to enhance understanding of the present invention, but the scope of the present invention is not limited to the examples. Other variations and modifications to the present invention may occur to those skilled in the art without departing from the spirit and scope of the present invention.
Comparative example 1
20 parts by weight of untreated glass fiber, 3 parts by weight of compatilizer, 0.5 part by weight of antioxidant 168 and 76.5 parts by weight of polypropylene are compounded through an extrusion molding process to obtain the polypropylene composite material in the example.
FIG. 1 is a scanning electron microscope image of a carbon layer of a glass fiber reinforced polypropylene composite material of comparative example 1 after a cone calorimetry test.
Comparative example 2
Mixing ammonium polyphosphate, melamine cyanuric acid and dipentaerythritol according to the ratio of 8:4:3 to obtain an intumescent flame retardant; 20 parts by weight of untreated glass fiber, 30 parts by weight of intumescent flame retardant, 3 parts by weight of compatilizer, 0.5 part by weight of antioxidant 168 and 46.5 parts by weight of polypropylene are compounded through an extrusion molding process to obtain the glass fiber reinforced polypropylene composite material in the embodiment.
FIG. 2 is a scanning electron microscope image of a carbon layer of the glass fiber reinforced polypropylene composite material of comparative example 2 after a cone calorimetry test.
Example 1
Weighing 20 parts by weight of commercial glass fiber, soaking the glass fiber in 1 mol/L nitric acid solution for 5 hours, treating the glass fiber in 3 wt% hydrolyzed (3-aminopropyl) triethoxysilane for 1 hour, treating the glass fiber in 5 wt% charring agent for 4 hours to obtain a glass fiber reinforcement body with the charring agent coated on the surface, mixing ammonium polyphosphate, melamine cyanuric acid and dipentaerythritol according to the ratio of 8:4:3 to obtain an intumescent flame retardant, and compounding the 20 parts by weight of glass fiber, 30 parts by weight of intumescent flame retardant, 3 parts by weight of compatilizer, 0.5 part by weight of antioxidant 168 and 46.5 parts by weight of polypropylene through an extrusion molding process to obtain the glass fiber reinforced polypropylene composite material in the embodiment.
FIG. 3 is a scanning electron microscope image of a glass fiber reinforcement obtained by treating a glass fiber reinforcement with 1 mol/L nitric acid for 5 hours, treating the glass fiber reinforcement with 3 wt% hydrolyzed (3-aminopropyl) triethoxysilane for 1 hour, and treating the glass fiber reinforcement with 3-5 wt% char-forming agent for 4 hours;
FIG. 4 is a scanning electron microscope image of the carbon layer of the glass fiber reinforced polypropylene composite material after cone calorimetry test.
Example 2
Weighing 20 parts by weight of commercial glass fiber, soaking the glass fiber in 1 mol/L nitric acid solution for 5 hours, treating the glass fiber in 3 wt% hydrolyzed silane coupling agent for 1 hour, treating the glass fiber in 5 wt% charring agent for 5 hours to obtain a glass fiber reinforcement body coated with the charring agent on the surface, mixing ammonium polyphosphate, melamine cyanuric acid and dipentaerythritol according to the ratio of 7:4:3 to obtain an intumescent flame retardant, and compounding the 20 parts by weight of glass fiber, 30 parts by weight of intumescent flame retardant, 3 parts by weight of compatilizer, 0.5 part by weight of antioxidant 168 and 46.5 parts by weight of polypropylene through an extrusion molding process to obtain the polypropylene composite material in the embodiment.
Example 3
Weighing 20 parts by weight of commercial glass fiber, soaking the glass fiber in 1 mol/L nitric acid solution for 5 hours, treating the glass fiber in 3 wt% hydrolyzed silane coupling agent for 1 hour, treating the glass fiber in 3 wt% charring agent for 4 hours to obtain a glass fiber reinforcement body coated with the charring agent on the surface, mixing ammonium polyphosphate, melamine cyanuric acid and dipentaerythritol according to the ratio of 8:4:3 to obtain an intumescent flame retardant, and compounding the 20 parts by weight of glass fiber, 28 parts by weight of intumescent flame retardant, 3 parts by weight of compatilizer, 0.5 part by weight of antioxidant 168 and 46.5 parts by weight of polypropylene through an extrusion molding process to obtain the polypropylene composite material in the embodiment.
The glass fiber reinforced polypropylene composites prepared in comparative examples 1-2 and examples 1-3 each contained 20% glass fibers. The test results of the mechanical properties, the horizontal and vertical combustion, the oxygen index test and the cone calorimetry test of the sample strips of comparative examples 1-2 and examples 1-3 are shown in Table 1.
The test results of comparative examples 1-2 and examples 1-3 show that the L OI and U L-94 burning grades of each example and the relevant data of the cone calorimetry test are superior to those of the comparative examples, and the glass fiber loaded with the char-forming agent can improve the wick effect generated in the burning process of the polypropylene, so that the synergistic effect of the interface flame-retardant mechanism and the matrix phase flame-retardant mechanism is achieved, and the flame-retardant property of the polypropylene composite material is improved.
Mechanical property and flame retardant property of glass fiber reinforced polypropylene composite material with content of 120% in table
Claims (9)
1. A preparation method of a halogen-free flame-retardant glass fiber reinforced polypropylene composite material is characterized in that a carbon forming agent is adsorbed on the surface of glass fiber under the action of hydrogen bonds between the glass fiber treated by a coupling agent and the carbon forming agent to obtain a surface modified glass fiber reinforcement; the preparation method comprises the following steps of compounding polypropylene resin, a modified glass fiber reinforcement, an intumescent flame retardant, a compatilizer and an antioxidant by a melt blending method:
(1) weighing 20-40 parts by weight of commercial glass fiber, soaking the glass fiber in a nitric acid solution with the molar concentration of 0.5-1.5 mol/L for 4-6 hours, and repeatedly cleaning with deionized water to remove a sizing agent on the surface of the glass fiber;
(2) soaking the glass fiber obtained in the step (1) in 1-3 wt% of hydrolyzed silane coupling agent, treating for 1-2 hours, and repeatedly cleaning with deionized water;
(3) soaking the glass fiber obtained in the step (2) in 3-5 wt% of a carbon forming agent, treating for 4-6 hours, repeatedly cleaning with deionized water, and drying to obtain a glass fiber reinforcement body with the surface coated with the carbon forming agent;
(4) and (3) mixing an acid source, a gas source and a carbon source of the intumescent flame retardant according to the ratio of 7-10: 3-5: 2-4, adding the mixture into a high-speed mixer, and uniformly mixing to obtain the intumescent flame retardant;
(5) melting and blending polypropylene resin, an intumescent flame retardant, a compatilizer and an antioxidant with the glass fiber obtained in the step (3), and extruding and granulating by using a double-screw extruder to obtain the halogen-free flame-retardant glass fiber reinforced polypropylene composite material;
wherein, the polypropylene resin, the intumescent flame retardant, the compatilizer and the antioxidant are added from a main feed, the glass fiber is fed from a glass fiber feeding hole of a double-screw extruder, the double-screw extruder is divided into five temperature control intervals from a feeding port to a machine head, and the processing conditions are as follows:
temperature in the first zone: 180-200 ℃ and the temperature of the second zone: 200-220 ℃, and three-zone temperature: 200-220 ℃ and four-zone temperature: 180-200 ℃ and the temperature of the five zones: 180-200 ℃; head temperature: 180-200 ℃; screw rotation speed: 150-180 r/min;
the halogen-free flame-retardant glass fiber reinforced polypropylene composite material comprises the following components in percentage by weight: (a) 40-60 parts of polypropylene resin, (b) 20-40 parts of intumescent flame retardant, (c) 20-40 parts of glass fiber coated with carbon forming agent, (d) 2-6 parts of compatilizer, and (e) 0.4-0.6 part of antioxidant.
2. The method according to claim 1, wherein the polypropylene resin has a melt flow rate of 2 to 4g/10 min.
3. The method according to claim 1, wherein the glass fiber is an alkali-free high-strength glass fiber, and the char-forming agent is coated by hydrogen bonding.
4. The method according to claim 1, wherein the compatibilizer is polypropylene-grafted maleic anhydride.
5. The method according to claim 1, wherein the coupling agent is (3-aminopropyl) triethoxysilane.
6. The method for preparing the antioxidant of claim 1, wherein the antioxidant is one or a combination of antioxidant 168, antioxidant 1010 and antioxidant 628.
7. The preparation method according to claim 1, wherein the acid source in the intumescent flame retardant is any one of ammonium phosphate, ammonium polyphosphate and melamine phosphate.
8. The preparation method according to claim 1, wherein the gas source in the intumescent flame retardant is any one of melamine, melamine cyanurate and polyamide.
9. The preparation method according to claim 1, wherein the char source and char forming agent in the intumescent flame retardant are any one of pentaerythritol, dipentaerythritol, tripentaerythritol, and pentaerythritol phosphate.
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| CN115246966A (en) * | 2022-07-08 | 2022-10-28 | 湖北合聚新材料有限公司 | Expansion flame-retardant polypropylene composition, polypropylene composite material and preparation method thereof |
| CN115011041B (en) * | 2022-07-15 | 2023-07-21 | 中广核俊尔(浙江)新材料有限公司 | Environment-friendly high-gloss low-fiber-floating continuous-reinforced long glass fiber polypropylene composite material |
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| CN101343392B (en) * | 2008-08-27 | 2011-04-27 | 蔡增坤 | Halogen-free flame-proof reinforced polypropylene composite material and preparation thereof |
| CN102372907B (en) * | 2010-08-23 | 2013-03-13 | 上海锦湖日丽塑料有限公司 | Halogen-free flame retarding and glass fiber reinforced resin and its preparation method |
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