CN110903516A - High-strength high-toughness flame-retardant polypropylene composite material and preparation method thereof - Google Patents
High-strength high-toughness flame-retardant polypropylene composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: 20-38 parts of wood fiber, 30-55 parts of fibrilia, 17-26 parts of polypropylene, 3-9 parts of a shape-stabilized phase change material, 2-8 parts of an ethylene-octene block copolymer, 6-13 parts of an antioxidant, 3-8 parts of a sodium octaborate flame retardant and the balance of a dispersant, and the invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, wherein S1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate the residual meat on the wood fibers and the fibrilia from the fibers, and then airing the wood fibers and the fibrilia without the meat for later use. The invention enhances the interaction between the matrix and the filler; the dispersion effect of the micro-nano particles is improved, and the formation of a high-efficiency heat-conducting network of multi-component fillers with different scales under a low filling condition is realized; the formula design is optimized, and the prepared composite material has better performance.
Description
Technical Field
The invention relates to the technical field of polypropylene composite materials, in particular to a high-strength high-toughness flame-retardant polypropylene composite material and a preparation method thereof.
Background
The polypropylene (PP) has the characteristics of good mechanical property, processability, chemical corrosion resistance, electrical insulation, no toxicity, light weight and the like, is a general plastic with excellent comprehensive performance, and can be widely applied to the fields of household appliances, electronics, building materials, automobile industry, textile, decoration and the like; because polypropylene is easy to burn, if the oxygen index of the polypropylene is only 17-18, a large amount of molten drops are generated during burning, if the polypropylene is not burnt sufficiently, toxic gases such as CO and the like are released, the hazard of fire is large, and the like, so that the application range of the polypropylene is limited; with the wide application of polypropylene in some fields such as building and automobile industries which have certain requirements on the flame retardant property of products, how to improve the flame retardant property of polypropylene on the premise of ensuring that the mechanical property of polypropylene meets the requirements of products is a very important subject.
The Intumescent Flame Retardant (IFR) is considered as the most potential environment-friendly flame retardant and generally comprises three parts, namely an acid source, a gas source and a carbon source. Ammonium polyphosphate (APP) is the most common acid source and gas source, and pentaerythritol polyols are the most common carbon source; the IFR has the flame retardant mechanism that an acid source is heated to a certain temperature to release inorganic acid and polyol for esterification and dehydration to form charcoal, a viscous carbonized product expands under the action of inert gas released by the gas source to form a piny charcoal layer, and the charcoal layer has the effects of heat insulation, oxygen isolation, smoke suppression, molten drop prevention and the like; chinese patent CN102134352A discloses that 30% of intumescent flame retardant is added into polypropylene to greatly improve the flame retardant property of the material, and the composite material has the advantages of no toxicity, low smoke, environmental protection, etc., but the mechanical property is also greatly reduced.
The adoption of filler reinforced expanded flame-retardant polypropylene is the focus of research at present, and the Haohuamei reports the chopped glass fiber reinforced expanded flame-retardant polypropylene composite material in the literature (the research of halogen-free expanded flame retardant ANTI-610 flame-retardant glass fiber reinforced polypropylene, the national collection of annual meeting of flame-retardant academia, 2008, 74-77), but the adoption of chopped glass fiber reinforcement can increase the density of the material and reduce the impact strength. Therefore, it is urgent to prepare a compound with high strength, high toughness and good flame retardant property to solve the above problems.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a high-strength high-toughness flame-retardant polypropylene composite material and a preparation method thereof, wherein the high-strength high-toughness flame-retardant polypropylene composite material not only has the high strength and high elasticity of wood fibers, but also has the high toughness and fatigue resistance of a polymer matrix, and a sodium octaborate flame retardant is added to greatly improve the flame retardant property of the polymer matrix; the polypropylene is used as a matrix material, and ceramic materials with different scales, such as alumina, zinc oxide, boron nitride and other insulating materials, are used as fillers, so that the filler interface is regulated and controlled, and the interaction between the matrix and the fillers is enhanced; the acrylic acid grafted ethylene-octene segmented copolymer is used as an auxiliary dispersant, so that the dispersion effect of micro-nano particles is improved, and the formation of a high-efficiency heat-conducting network of multi-component fillers with different scales under a low filling condition is realized; the ethylene-octene segmented copolymer is used as a toughening material, the formula design is optimized, and the prepared composite material has better performance.
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: 20-38 parts of wood fiber, 30-55 parts of fibrilia, 17-26 parts of polypropylene, 3-9 parts of a shape-stabilized phase change material, 2-8 parts of an ethylene-octene block copolymer, 6-13 parts of an antioxidant, 3-8 parts of a sodium octaborate flame retardant and the balance of a dispersant.
Preferably, the feed comprises the following raw materials in parts by weight: 28-30 parts of wood fiber, 41-43 parts of fibrilia, 20-22 parts of polypropylene, 5-7 parts of a shape-stabilized phase change material, 4-6 parts of an ethylene-octene block copolymer, 6-8 parts of an antioxidant, 4-6 parts of a sodium octaborate flame retardant and the balance of a dispersant.
Preferably, the feed comprises the following raw materials in parts by weight: the composite material comprises wood fibers 29, fibrilia 42, polypropylene 21, a shaped phase change material 6, an ethylene-octene block copolymer 5, an antioxidant 7, a sodium octaborate flame retardant 5 and the balance of a dispersant.
Preferably, the weight ratio of the wood fiber, the hemp fiber and the polypropylene is 20-38: 30-55: 17-26.
Preferably, the polypropylene, the shape-stabilized phase change material, the ethylene-octene block copolymer 17-26: 3-9: 2-8.
Preferably, the shape-stabilized phase change material is prepared and molded by taking a series of high polymer materials such as different types of high-pressure polyethylene, low-pressure polyethylene, polypropylene and the like as supporting and micro-packaging materials and taking paraffin with different melting points and different types as phase change materials.
Preferably, the dispersant is an acrylic acid grafted ethylene-octene block copolymer.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for later use;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 20-30 minutes, and uniformly mixing the rest polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 25-85 ℃, and then starting vacuumizing operation to set the pressure in the preheating tank to 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) melting and blending the semi-finished product B prepared in the step S4 for 5-10 minutes at the temperature of 150-250 ℃ and the rotating speed of 50-200 r/min in an internal mixer after being uniform, and taking out to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
Preferably, in S1, the wood fiber and the hemp fiber are soaked in the lime water for 3 days.
Preferably, the semi-finished product B prepared in the step S4 is melted and blended for 7 minutes at the temperature of 200 ℃ of an internal mixer and the rotating speed of 150 r/min after being homogenized.
The invention has the following beneficial effects;
1. the composite material prepared by the invention not only has high strength and high elasticity of wood fiber, but also has high toughness and fatigue resistance of a polymer matrix, and simultaneously, the sodium octaborate flame retardant is added, so that the flame retardant property of the composite material is also greatly improved;
2. the invention takes polypropylene as a matrix material and takes ceramic materials with different scales, such as alumina, zinc oxide, boron nitride and other insulating materials as fillers, regulates and controls the filler interface, and enhances the interaction between the matrix and the fillers;
3. the acrylic acid grafted ethylene-octene segmented copolymer is used as an auxiliary dispersant, so that the dispersion effect of micro-nano particles is improved, and the formation of a high-efficiency heat-conducting network of multi-component fillers with different scales under a low filling condition is realized;
4. the ethylene-octene segmented copolymer is used as a toughening material, the formula design is optimized, and the prepared composite material has better performance.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples.
Example one
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 20, fibrilia 30, polypropylene 17, a shape-stabilized phase change material 3, an ethylene-octene block copolymer 2, an antioxidant 6, a sodium octaborate flame retardant 3 and the balance of a dispersant.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for standby;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 20 minutes, and uniformly mixing the rest of polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 25 ℃, then starting vacuumizing operation, and setting the pressure in the preheating tank to be 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) melting and blending the semi-finished product B prepared in the step S4 for 5 minutes at the temperature of 150 ℃ and the rotating speed of 50 r/min in an internal mixer, and taking out the mixture to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
Example two
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 28, fibrilia 41, polypropylene 20, a shaped phase change material 5, an ethylene-octene block copolymer 4, an antioxidant 6, a sodium octaborate flame retardant 4 and the balance of a dispersant.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for later use;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 22 minutes, and uniformly mixing the rest of polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 45 ℃, then starting vacuumizing operation, and setting the pressure in the preheating tank to be 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) melting and blending the semi-finished product B prepared in the step S4 for 7 minutes at 125 ℃ and 80 rpm of an internal mixer after homogenizing, and taking out to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
EXAMPLE III
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 29, fibrilia 42, polypropylene 21, a shaped phase change material 6, an ethylene-octene block copolymer 5, an antioxidant 7, a sodium octaborate flame retardant 5 and the balance of a dispersant.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for later use;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 25 minutes, and uniformly mixing the rest of polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 50 ℃, then starting vacuumizing operation, and setting the pressure in the preheating tank to be 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) melting and blending the semi-finished product B prepared in the step S4 for 6 minutes at the temperature of 200 ℃ of an internal mixer and at the rotating speed of 125 rpm, and taking out the mixture to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
Example four
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 30, fibrilia 43, polypropylene 22, a shaped phase change material 7, an ethylene-octene block copolymer 6, an antioxidant 8, a sodium octaborate flame retardant 6 and the balance of a dispersant.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for later use;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 28 minutes, and uniformly mixing the rest of polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 60 ℃, then starting vacuumizing operation, and setting the pressure in the preheating tank to be 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) uniformly melting and blending the semi-finished product B prepared in the step S4 for 8 minutes at the temperature of 220 ℃ of an internal mixer and at the rotating speed of 160 r/min, and taking out the mixture to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
EXAMPLE five
The invention provides a high-strength high-toughness flame-retardant polypropylene composite material which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 38, fibrilia 55, polypropylene 26, a shaped phase change material 9, an ethylene-octene block copolymer 8, an antioxidant 13, a sodium octaborate flame retardant 8 and the balance of a dispersant.
The invention also provides a preparation method of the high-strength high-toughness flame-retardant polypropylene composite material, which comprises the following steps:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for standby;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 30 minutes, and uniformly mixing the rest of polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 85 ℃, then starting vacuumizing operation, and setting the pressure in the preheating tank to be 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) uniformly melting and blending the semi-finished product B prepared in the step S4 for 10 minutes at the temperature of 250 ℃ of an internal mixer and at the rotating speed of 200 r/min, and taking out the mixture to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
The flame retardant disclosed by the invention not only has high strength and high elasticity of wood fiber, but also has high toughness and fatigue resistance of a polymer matrix, and the flame retardant performance of the flame retardant is greatly improved by adding the sodium octaborate flame retardant; the polypropylene is used as a matrix material, and ceramic materials with different scales, such as alumina, zinc oxide, boron nitride and other insulating materials, are used as fillers, so that the filler interface is regulated and controlled, and the interaction between the matrix and the fillers is enhanced; the acrylic acid grafted ethylene-octene segmented copolymer is used as an auxiliary dispersant, so that the dispersion effect of micro-nano particles is improved, and the formation of a high-efficiency heat-conducting network of multi-component fillers with different scales under a low filling condition is realized; the ethylene-octene segmented copolymer is used as a toughening material, the formula design is optimized, and the prepared composite material has better performance.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The high-strength high-toughness flame-retardant polypropylene composite material is characterized by comprising the following raw materials in parts by weight: 20-38 parts of wood fiber, 30-55 parts of fibrilia, 17-26 parts of polypropylene, 3-9 parts of a shape-stabilized phase change material, 2-8 parts of an ethylene-octene block copolymer, 6-13 parts of an antioxidant, 3-8 parts of a sodium octaborate flame retardant and the balance of a dispersant.
2. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, which comprises the following raw materials in parts by weight: 28-30 parts of wood fiber, 41-43 parts of fibrilia, 20-22 parts of polypropylene, 5-7 parts of a shape-stabilized phase change material, 4-6 parts of an ethylene-octene block copolymer, 6-8 parts of an antioxidant, 4-6 parts of a sodium octaborate flame retardant and the balance of a dispersant.
3. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, which comprises the following raw materials in parts by weight: the composite material comprises wood fibers 29, fibrilia 42, polypropylene 21, a shaped phase change material 6, an ethylene-octene block copolymer 5, an antioxidant 7, a sodium octaborate flame retardant 5 and the balance of a dispersant.
4. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, wherein the weight ratio of the wood fibers to the hemp fibers to the polypropylene is 20-38: 30-55: 17-26.
5. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, wherein the weight ratio of the polypropylene, the shape-stabilized phase change material, the ethylene-octene block copolymer 17-26: 3-9: 2-8.
6. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, wherein the shape-stabilized phase change material is prepared by using a series of high-pressure polyethylene, low-pressure polyethylene, polypropylene and other polymer materials with different types as supporting and micro-packaging materials, and paraffin with different melting points and different types as phase change materials.
7. The high-strength high-toughness flame-retardant polypropylene composite material as claimed in claim 1, wherein the dispersant is acrylic acid grafted ethylene-octene block copolymer.
8. The preparation method of the high-strength high-toughness flame-retardant polypropylene composite material is characterized by comprising the following steps of:
s1: pretreating wood fibers and fibrilia, soaking the wood fibers and the fibrilia in lime water for 2-5 days to completely separate meat from the fibers, and then airing the wood fibers and the fibrilia without meat for later use;
s2: adding a certain amount of polypropylene and a shaping phase change material into a stainless steel mixing tank with a stirring function, adding an ethylene-octene block copolymer and an antioxidant, quickly stirring, uniformly mixing, then adding the dried wood fiber fibrilia, stirring for 20-30 minutes, and uniformly mixing the rest polypropylene and the shaping phase change material to obtain a fiber mixture A;
s3: adding a sodium octaborate flame retardant into a preheating tank, adjusting the preheating temperature to 25-85 ℃, and then starting vacuumizing operation to set the pressure in the preheating tank to 0.35 Mpa;
s4: when the temperature of the sodium octaborate flame retardant in the step S3 reaches the preheating temperature, adding the fiber mixture A prepared in the step S2 into a preheating tank, adding a proper amount of antioxidant, dispersant, aluminum oxide, zinc oxide and boron nitride, and naturally cooling to obtain a semi-finished product B;
s5: and (4) melting and blending the semi-finished product B prepared in the step S4 for 5-10 minutes at the temperature of 150-250 ℃ and the rotating speed of 50-200 r/min in an internal mixer after being uniform, and taking out to obtain the high-strength high-toughness flame-retardant polypropylene composite material.
9. The method for preparing a high-strength high-toughness flame-retardant polypropylene composite according to claim 8, wherein in the step S1, the wood fibers and the hemp fibers need to be soaked in lime water for 3 days.
10. The method for preparing the high-strength high-toughness flame-retardant polypropylene composite material according to claim 8, wherein the semi-finished product B prepared in the step S4 is melt-blended for 7 minutes at 200 ℃ of an internal mixer at a rotating speed of 150 rpm after being homogenized.
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