CN114957826A - Extrusion-grade halogen-free flame-retardant wood-plastic composite material and preparation method and application thereof - Google Patents
Extrusion-grade halogen-free flame-retardant wood-plastic composite material and preparation method and application thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C08L23/12—Polypropene
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08L2205/00—Polymer mixtures characterised by other features
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- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses an extrusion-grade halogen-free flame-retardant wood-plastic composite material, and a preparation method and application thereof, wherein the material is prepared from the following components in parts by weight: 5-45 parts of polypropylene, 15-25 parts of polyethylene, 20-30 parts of halogen-free intumescent flame retardant, 3-7 parts of silicon nitride, 1-5 parts of cubic boron nitride, 2-6 parts of compatilizer, 10-20 parts of plant fiber powder, 0.2-0.6 part of antioxidant, 0.2-0.4 part of dispersant and 0.1-0.3 part of lubricant. According to the invention, silicon nitride and cubic boron nitride are added into the material, and when the material is combusted at a high temperature, a layer of compact ceramic shell is formed on the surface of the material, so that the effects of heat insulation, oxygen isolation and smoke suppression are achieved, and the material has a good flame retardant effect. The extrusion-grade halogen-free flame-retardant wood-plastic composite material prepared by the invention can be widely applied to products of home decoration plates.
Description
Technical Field
The invention belongs to the technical field of polymer composite materials, and particularly relates to an extrusion-grade halogen-free flame-retardant wood-plastic composite material and a preparation method and application thereof.
Background
With the wide application of plastic products in various industries and the enhancement of national requirements on environmental protection and environment, the traditional wood home decoration materials are gradually replaced by wood-plastic composite materials. The wood-plastic composite material is a novel composite material which is briskly developed in recent years at home and abroad, and is a new material which is prepared by replacing a common resin adhesive with polyethylene, polypropylene, polyvinyl chloride and the like and mixing the wood-plastic composite material with waste plant fibers such as wood flour, rice hulls, straws and the like. The composition of the wood-plastic composite material determines that the wood-plastic composite material has certain characteristics of plastics and wood, has excellent application prospect in the field of home materials, and has the defects of poor flame retardance and potential safety hazard.
To improve the flame retardancy of such materials, flame retardants have been gradually introduced into such product applications. The commonly used halogen-free flame retardant mainly comprises an inorganic flame retardant and a phosphorus-nitrogen intumescent flame retardant. The compatibility of the inorganic flame retardant and the polyolefin resin is slightly poor, the flame retardant efficiency is low, a certain flame retardant effect is achieved only when a large amount of the inorganic flame retardant is filled, and the mechanical property of the polyolefin is seriously damaged by the large amount of the flame retardant, so that the processing property is influenced.
Silicon nitride is an important component for manufacturing precise ceramic devices, has excellent characteristics of high temperature resistance, wear resistance, corrosion resistance and the like, and is widely applied to the fields of chemical industry, machinery, aerospace, energy and the like. The cubic boron nitride micro powder is produced by cubic boron nitride single crystal abrasive grains through crushing and shaping treatment by adopting a special process method, has good thermal stability and good self-sharpening property, can obtain a precise and high-finish working surface by using the cubic boron nitride micro powder, and ensures that the product has higher quality. Based on the properties of silicon nitride and cubic boron nitride, the silicon nitride and cubic boron nitride serving as modified materials are introduced into the wood-plastic composite material, and the comprehensive performance of the wood-plastic composite material is expected to be improved.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide an extrusion-grade halogen-free flame-retardant wood-plastic composite material and a preparation method and application thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme:
an extrusion-grade halogen-free flame-retardant wood-plastic composite material is prepared from the following components in parts by weight: 5-45 parts of polypropylene, 15-25 parts of polyethylene, 20-30 parts of intumescent flame retardant, 3-7 parts of silicon nitride, 1-5 parts of cubic boron nitride, 2-6 parts of compatilizer, 10-20 parts of plant fiber powder, 0.2-0.6 part of antioxidant, 0.2-0.4 part of dispersant and 0.1-0.3 part of lubricant.
In a further scheme, the polypropylene is extrusion grade polypropylene with a melt index less than 3 at 230 ℃ and under the test condition of 2.16 KG; the polyethylene is extrusion grade high density polyethylene with a melt index less than 3 under the test conditions of 190 ℃ and 2.16 KG.
In a further scheme, the silicon nitride is powder with the average particle size of 1000-2000 meshes, and the cubic boron nitride is powder with the average particle size of 1000-2000 meshes.
In a further scheme, the compatilizer is maleic anhydride grafted polypropylene.
In a further scheme, the plant fiber powder is powder with the mesh number of 200-350 meshes, which is prepared by crushing plant fibers, and the plant fibers are wood fiber powder, rice hulls or straws.
In a further scheme, the antioxidant is at least one of antioxidant 1010, antioxidant DSTDP and antioxidant 168.
In a further scheme, the dispersing agent is a silicone high-efficiency dispersing agent, and the lubricating agent is at least one of calcium stearate, stearic acid and pentaerythritol stearate.
The invention also provides a preparation method of the extrusion-grade halogen-free flame-retardant wood-plastic composite material, which comprises the following steps: uniformly mixing polypropylene, polyethylene, an intumescent flame retardant, silicon nitride, cubic boron nitride, a compatilizer, plant fiber powder, an antioxidant, a dispersant and a lubricant according to a ratio to obtain a mixed material; and melting and extruding the mixed material by a co-rotating double-screw extruder, and granulating to obtain the final product. Further, the length-diameter ratio of the co-rotating double-screw extruder is 32-40, the rotating speed is 180-400 rpm, and the extrusion temperature is 170-205 ℃. The extrusion-grade halogen-free flame-retardant wood-plastic composite material prepared by the invention has good application prospect in home decoration plates.
Compared with the prior art, the invention has the beneficial effects that:
the extrusion-grade halogen-free flame-retardant wood-plastic composite material is prepared by utilizing the excellent hardness, high temperature resistance and good self-sharpening of silicon nitride and cubic boron nitride. The extrusion-grade halogen-free flame-retardant wood-plastic composite material has high surface hardness and good wear resistance. In the high-temperature combustion process, a smooth and closed surface layer can be formed on the surface of the wood-plastic polypropylene composite material, so that the wood-plastic polypropylene composite material has the effects of heat insulation, oxygen isolation, smoke suppression and molten drop prevention, has a good flame retardant effect, and improves the flame retardant property of the wood-plastic polypropylene composite material. At the same time, NH released by the intumescent flame retardant 3 The gas is in the composite material, and can dilute the oxygen concentration, thereby achieving the effect of rapid flame retardance. And the flame retardant process of the material has no halogen, no corrosive gas and low toxicity, and belongs to an environment-friendly flame retardant system.
In addition, the silicon nitride and the cubic boron nitride can also correspondingly improve the mechanical property, the wear resistance and the high temperature resistance of the material.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The types and manufacturers of raw materials related to the preparation process of the extrusion-grade halogen-free flame-retardant wood-plastic composite material in the following examples are as follows:
wherein the polypropylene is BA212E (northern Europe chemical industry), B4901 (Yanshan petrochemical industry);
polyethylene is 5502FA (shanghai seideae), 4902T (winnowing chemical);
silicon nitride powder H1500 (hebei high nitrogen-rich silicon material ltd);
the cubic boron nitride powder is DK-BN-0019 (Beijing Deke island gold science and technology Co., Ltd.);
the compatilizer is maleic anhydride graft GPM128 (light of Ningbo energy);
the plant fiber powder is wood fiber powder with the mesh number of 200-325 meshes (far from the mining industry in the Lingshu county);
the halogen-free intumescent flame retardant is HP-2500S (Addick Shanghai trade Co., Ltd.);
the antioxidant is antioxidant 1010, antioxidant DSTDP and antioxidant 168;
the dispersant used is E525;
the lubricant is calcium stearate, stearic acid, pentaerythritol stearate.
The reagents are provided only for illustrating the sources and components of the reagents used in the experiments of the present invention, so as to be fully disclosed, and do not indicate that the present invention cannot be realized by using other reagents of the same type or other reagents supplied by other suppliers.
The present invention will be further described with reference to the following examples.
Example 1
(1) Weighing 45 parts by weight of polypropylene BA212E, 15 parts by weight of polyethylene 5502FA, 20 parts by weight of halogen-free intumescent flame retardant HP-2500S, 3 parts by weight of silicon nitride, 1 part by weight of cubic boron nitride, 2 parts by weight of compatilizer GPM128, 10 parts by weight of wood fiber powder, 0.1 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.2 part by weight of dispersant E525 and 0.1 part by weight of calcium stearate, putting the components into a high-speed mixer, mixing for 5 minutes, and uniformly mixing to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder for melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of the extruder barrel is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
Example 2
(1) Putting 5 parts of polypropylene B4901, 25 parts of polyethylene 4902T, 30 parts of halogen-free intumescent flame retardant 110DM, 7 parts of silicon nitride, 5 parts of cubic boron nitride, 6 parts of compatilizer GPM128, 20 parts of wood fiber powder, 0.2 part of antioxidant 1010, 0.4 part of antioxidant 168, 0.4 part of dispersant E525 and 0.3 part of calcium stearate into a high-speed mixer, mixing for 5 minutes, and uniformly mixing to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder for melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of the extruder barrel is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
Example 3
(1) Weighing 25 parts by weight of polypropylene BA212E, 20 parts by weight of polyethylene 5502FA, 25 parts by weight of halogen-free intumescent flame retardant HP-2500S, 5 parts by weight of silicon nitride, 3 parts by weight of cubic boron nitride, 4 parts by weight of compatilizer GPM128, 15 parts by weight of wood fiber powder, 0.2 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.3 part by weight of dispersant E525 and 0.2 part by weight of calcium stearate, putting the components into a high-speed mixer, mixing for 5 minutes, and uniformly mixing to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder to perform melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of the extruder barrel is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
Comparative example 1
(1) Weighing 30 parts by weight of polypropylene BA212E, 23 parts by weight of polyethylene 5502FA, 25 parts by weight of halogen-free intumescent flame retardant HP-2500S, 4 parts by weight of compatilizer GPM128, 15 parts by weight of wood fiber powder, 0.2 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.3 part by weight of dispersant E525 and 0.2 part by weight of calcium stearate, putting the components into a high-speed mixer, mixing for 5 minutes, and uniformly mixing to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder for melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of a material cylinder of the extruder is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
Comparative example 2
(1) Weighing 25 parts by weight of polypropylene BA212E, 23 parts by weight of polyethylene 5502FA, 25 parts by weight of halogen-free intumescent flame retardant HP-2500S, 5 parts by weight of silicon nitride, 4 parts by weight of compatilizer GPM128, 0.2 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.3 part by weight of dispersant E525 and 0.2 part by weight of calcium stearate, putting the components into a high-speed mixer, and uniformly mixing for 5 minutes to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder for melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of the extruder barrel is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
Comparative example 3
(1) Weighing 30 parts by weight of polypropylene BA212E, 20 parts by weight of polyethylene 5502FA, 25 parts by weight of halogen-free intumescent flame retardant HP-2500S, 3 parts by weight of cubic boron nitride, 4 parts by weight of compatilizer GPM128, 0.2 part by weight of antioxidant 1010, 0.2 part by weight of antioxidant 168, 0.3 part by weight of dispersant E525 and 0.2 part by weight of calcium stearate, putting the components into a high-speed mixer, mixing for 5 minutes, and uniformly mixing to obtain a mixture;
(2) and adding the mixture into a co-rotating double-screw extruder for melt blending extrusion, traction and granulation to obtain the extrusion-grade halogen-free flame-retardant wood-plastic polyolefin composite material. Wherein the length-diameter ratio of the extruder is 40, the temperature of the extruder barrel is 170 ℃, 180 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, and the rotating speed of the fixed main screw is 180 r/min.
The extrusion-grade halogen-free flame-retardant wood-plastic composite material prepared in the above examples and comparative examples is subjected to performance test, and the performance test results are shown in table 1 below.
Table 1: results of performance test of products prepared in each example and comparative example
Remarking: the mechanical properties are tensile bending notch impact sample strips according to GB standard, wherein the tensile strength test is carried out according to GB1040, the tensile sample strips are 1A type dumbbell sample strips specified in the national standard 1040.2, and the tensile test speed is 50 mm/min; the flexural modulus test was performed according to GB9341 with flexural spline dimensions 80 x 10 x 4mm, test speed 2 mm/min; IZOD notched impact strength was measured according to GB1843, IZOD notched impact spline 80 x 10 x 4mm, with notch depth of 2mm, impact pendulum energy of 2.75J; flame retardant performance was according to UL94, flame retardant spline size 127 × 13 × 1.6mm and 127 × 13 × 3.2 mm.
As can be seen from the data in the table 1, compared with the comparative example, the extrusion-grade halogen-free flame-retardant wood-plastic composite material prepared according to the formula and the process in the embodiment has excellent mechanical properties, and the flame retardant property of the material is higher and more stable due to the application of silicon nitride and cubic boron nitride. Therefore, the invention can produce more efficient extrusion-grade halogen-free flame-retardant wood-plastic composite material according to the requirements of customers.
It should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The extrusion-grade halogen-free flame-retardant wood-plastic composite material is characterized in that: the composition is prepared from the following components in parts by weight: 5-45 parts of polypropylene, 15-25 parts of polyethylene, 20-30 parts of halogen-free intumescent flame retardant, 3-7 parts of silicon nitride, 1-5 parts of cubic boron nitride, 2-6 parts of compatilizer, 10-20 parts of plant fiber powder, 0.2-0.6 part of antioxidant, 0.2-0.4 part of dispersant and 0.1-0.3 part of lubricant.
2. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the polypropylene is extrusion grade polypropylene with a melt index less than 3 under the test conditions of 230 ℃ and 2.16 KG; the polyethylene is extrusion grade high density polyethylene with a melt index less than 3 under the test conditions of 190 ℃ and 2.16 KG.
3. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the silicon nitride is powder with the average grain diameter of 1000-2000 meshes, and the cubic boron nitride is powder with the average grain diameter of 1000-2000 meshes.
4. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the compatilizer is maleic anhydride grafted polypropylene.
5. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the plant fiber powder is powder with the mesh number of 200-350 meshes, which is prepared by crushing plant fibers, and the plant fibers are wood fiber powder, rice hulls or straws.
6. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the antioxidant is at least one of antioxidant 1010, antioxidant DSTDP and antioxidant 168.
7. The extrusion-grade halogen-free flame-retardant wood-plastic composite material of claim 1, characterized in that: the dispersing agent is a silicone high-efficiency dispersing agent, and the lubricating agent is at least one of calcium stearate, stearic acid and pentaerythritol stearate.
8. The preparation method of the extrusion-grade halogen-free flame-retardant wood-plastic composite material as claimed in any one of claims 1 to 7, characterized in that: the method comprises the following steps: uniformly mixing polypropylene, polyethylene, an intumescent flame retardant, silicon nitride, cubic boron nitride, a compatilizer, plant fiber powder, an antioxidant, a dispersant and a lubricant according to a ratio to obtain a mixed material; and melting and extruding the mixed material by a co-rotating double-screw extruder, and granulating to obtain the final product.
9. The method of claim 8, wherein: the length-diameter ratio of the co-rotating double-screw extruder is 32-40, the rotating speed is 180-400 rpm, and the extrusion temperature is 170-205 ℃.
10. Use of the extruded grade halogen free flame retardant wood plastic composite according to any of claims 1 to 7 in a home furnishing panel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831112A (en) * | 2010-05-14 | 2010-09-15 | 金发科技股份有限公司 | Halogen-free flame-retardant type injection molding-class polyolefin wood plastic composite material and preparation method thereof |
| CN102964860A (en) * | 2012-11-12 | 2013-03-13 | 沈阳化工大学 | Halogen-free flame retardant wood-plastic composite material made by expansive type fire retardant and preparation method thereof |
| CN108948476A (en) * | 2017-05-23 | 2018-12-07 | 宁波帕斯卡新材料有限公司 | A kind of halogen-free fire-retardant polyethylene material and preparation method thereof |
| CN111621087A (en) * | 2019-02-27 | 2020-09-04 | 合肥杰事杰新材料股份有限公司 | Halogen-free flame-retardant master batch and preparation method and application thereof |
-
2021
- 2021-02-26 CN CN202110214366.9A patent/CN114957826A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831112A (en) * | 2010-05-14 | 2010-09-15 | 金发科技股份有限公司 | Halogen-free flame-retardant type injection molding-class polyolefin wood plastic composite material and preparation method thereof |
| CN102964860A (en) * | 2012-11-12 | 2013-03-13 | 沈阳化工大学 | Halogen-free flame retardant wood-plastic composite material made by expansive type fire retardant and preparation method thereof |
| CN108948476A (en) * | 2017-05-23 | 2018-12-07 | 宁波帕斯卡新材料有限公司 | A kind of halogen-free fire-retardant polyethylene material and preparation method thereof |
| CN111621087A (en) * | 2019-02-27 | 2020-09-04 | 合肥杰事杰新材料股份有限公司 | Halogen-free flame-retardant master batch and preparation method and application thereof |
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