CN114591557B - Flame-retardant low-density polyethylene composite material and preparation method thereof - Google Patents
Flame-retardant low-density polyethylene composite material and preparation method thereof Download PDFInfo
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- CN114591557B CN114591557B CN202210421751.5A CN202210421751A CN114591557B CN 114591557 B CN114591557 B CN 114591557B CN 202210421751 A CN202210421751 A CN 202210421751A CN 114591557 B CN114591557 B CN 114591557B
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/36—Silica
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- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
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- C08K9/00—Use of pretreated ingredients
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- C08K3/32—Phosphorus-containing compounds
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- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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Abstract
The invention relates to a flame-retardant low-density polyethylene composite material, which comprises, by mass, 50-60% of low-density polyethylene, 15-30% of silicon dioxide coated ammonium polyphosphate, 5-20% of dipentaerythritol and 1-5% of silicon dioxide coated melamine cyanurate. The invention uses silicon dioxide coated ammonium polyphosphate as acid source and a small amount of air source, dipentaerythritol as carbon source, and silicon dioxide coated melamine urate as main air source to form an intumescent flame-retardant system, and prepares the modified intumescent flame-retardant low-density polyethylene composite material through melt blending. The oxygen index of the product can meet the fire-retardant requirement and reduce the release amount of smoke, and meanwhile, the mechanical property of the product is far better than that of the similar product.
Description
Technical Field
The invention relates to the field of materials, in particular to a flame-retardant low-density polyethylene composite material and a preparation method thereof.
The background technology is as follows:
low Density Polyethylene (LDPE) is a resin material and is also an important component of composite materials. Because LDPE has the characteristics of low price, good mechanical and processing properties, good physical and chemical properties, less harm to human beings and environment and easy reuse, the LDPE is widely applied to industry, agriculture and daily life. However, polyethylene severely limits its use, particularly in products with high flame retardant requirements, such as cables, because it is flammable at lower temperatures and can produce large amounts of flammable droplets. Therefore, flame retardant modification thereof has become a research hotspot for many scholars.
One of the simplest methods to improve the flame retardancy of LDPE is to add a flame retardant. While the most common flame retardants are halogen-based, inorganic or intumescent flame retardants. Halogen-based flame retardants have excellent flame retardant properties, but when burned, produce gases that are relatively toxic and are now not acceptable to the environment. The inorganic flame retardant has the characteristics of good stability, low toxicity, no corrosive gas, long-term flame retardant effect and the like, however, in order to enable LDPE to have higher flame retardance, the addition amount of the inorganic flame retardant needs to be increased. Because of the incompatibility of the inorganic filler and the organic material, the mechanical properties of the LDPE are greatly reduced, although the flame retardancy of the LDPE can be ensured by adding a large amount of inorganic flame retardant. The traditional intumescent flame retardant (Intumescent Flame Retardant, IFR) takes P, N, C as a core component, can form an intumescent porous protective carbon layer on the surface of a polymer after being heated and decomposed, inhibits heat and oxygen transfer, reduces combustible product quantity, can inhibit polymer melt drops, realizes effective flame retardance of the polymer, and reduces mechanical properties of the polymer after being added.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide a modified intumescent flame-retardant low-density polyethylene composite material and a preparation method thereof, which can improve the flame retardant property of low-density polyethylene on the premise of not sacrificing the tensile strength of low-density polyethylene as much as possible and solve the problem of serious dripping of molten drops during combustion.
In order to achieve the above purpose, the invention provides a flame-retardant low-density polyethylene composite material, which comprises 50-60% of low-density polyethylene, 15-30% of silicon dioxide coated ammonium polyphosphate, 5-20% of dipentaerythritol and 1-5% of silicon dioxide coated melamine cyanurate by mass percent.
Preferably or alternatively, the silica coated ammonium polyphosphate in the feedstock is prepared by the steps of:
mixing ammonium polyphosphate, ethanol and deionized water, regulating pH to be alkaline by ammonia solution, adding OP-10, carrying out heat preservation and stirring at 40 ℃, adding silicate, continuing heat preservation and stirring reaction, adding a silane coupling agent with vinyl, heating to 60 ℃, carrying out heat preservation and stirring reaction for 1h, filtering to obtain a solid product, and washing with ethanol to obtain the product.
Preferably or alternatively, the silicate is any one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
Preferably or alternatively, the silane coupling agent with vinyl is any one of vinyl triethoxysilane, KH570, vinyl trimethoxysilane and vinyl trimethylsilane.
Preferably or alternatively, the silica coated melamine cyanurate in the feed is prepared by:
mixing melamine cyanurate, ethanol and deionized water, regulating pH to be alkaline by ammonia solution, adding OP-10, carrying out heat preservation and stirring at 40 ℃, adding silicate, continuing heat preservation and stirring reaction, adding a silane coupling agent with vinyl, heating to 60 ℃, carrying out heat preservation and stirring reaction for 1h, filtering to obtain a solid product, and washing with ethanol to obtain the polyurethane emulsion.
Preferably or alternatively, the silicate is any one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
Preferably or alternatively, the silane coupling agent with vinyl is any one of vinyl triethoxysilane, KH570, vinyl trimethoxysilane and vinyl trimethylsilane.
On the other hand, the invention provides a preparation method of the flame-retardant low-density polyethylene composite material, which comprises the following steps:
s1, preheating an internal mixer, and adding low-density polyethylene;
s2, adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine cyanurate;
s3, mixing for 10-15min to obtain the product.
Preferably or alternatively, the internal mixer has a preheating temperature of 155-165 ℃.
The invention uses silicon dioxide coated ammonium polyphosphate as acid source and a small amount of air source dipentaerythritol as carbon source, uses silicon dioxide coated melamine urate as main air source to form an intumescent flame-retardant system, and prepares the modified intumescent flame-retardant low-density polyethylene composite material through melt blending. The oxygen index of the product can meet the flame-retardant requirement and reduce the release amount of smoke, and simultaneously solves the problem that the mechanical property of the material can be greatly reduced when the flame retardant is added in the prior art. The mechanical property of the modified intumescent flame retardant low density polyethylene composite material product prepared by the invention is far superior to that of similar products with similar flame retardant property to the product.
Drawings
FIG. 1 is a Fourier infrared (FTIR) diagram of ammonium polyphosphate and silica coated ammonium polyphosphate;
FIG. 2 is an X-ray diffraction (XRD) pattern of ammonium polyphosphate and silica coated ammonium polyphosphate;
FIG. 3 is a FTIR plot of melamine cyanurate and silica coated melamine cyanurate;
fig. 4 is an XRD pattern of melamine cyanurate and silica coated melamine cyanurate.
Detailed Description
The following describes specific embodiments of the present invention in detail. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
The experimental methods used in the following examples are conventional methods unless otherwise specified.
Materials, reagents and the like used in the examples described below are commercially available unless otherwise specified.
The Low Density Polyethylene (LDPE) of the invention is a type with a density of 0.91-0.93g/cm 3 Is a polyethylene resin material of (a).
Example 1
The embodiment of the invention provides a flame-retardant low-density polyethylene composite material.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 58% of low-density polyethylene, 30% of silicon dioxide coated ammonium polyphosphate, 10% of dipentaerythritol and 2% of silicon dioxide coated melamine cyanurate in percentage by weight.
The silica coated ammonium polyphosphate in the raw materials is prepared in the following manner:
50g of ammonium polyphosphate, 100mL of ethanol and 50mL of deionized water were added to a 500mL three-necked round bottom flask. The pH of the solution was adjusted to 10.0 with an ammonia solution, and 1g of OP-10 was added. The solution in the flask was mechanically stirred in a water bath at 500r/min to 40 ℃. After stirring for a further 10min, 10g of TEOS was added, and stirring was continued for 4 hours at 40 ℃. 1g of YDH-151 was added while the temperature was raised to 60℃and the reaction was continued with stirring for 1 hour. Filtering to obtain a solid product, washing the solid product with ethanol, and vacuum drying to obtain the silicon dioxide coated ammonium polyphosphate.
The raw materials are prepared by the following steps of:
50g of melamine cyanurate, 100mL of ethanol, and 50mL of deionized water were added to a 500mL three-necked round bottom flask. The pH of the solution was adjusted to 10.0 with an ammonia solution, and 1g of OP-10 was added. The solution in the flask was mechanically stirred in a water bath at 500r/min to 40 ℃. After stirring for a further 10min, 10g of TEOS was added, and stirring was continued for 4h at 40 ℃. 1g of YDH-151 was added while the temperature was raised to 60℃and the reaction was continued with stirring for 1 hour. Filtering to obtain a solid product, washing the solid product with ethanol, and vacuum drying to obtain the silica coated melamine cyanurate.
The flame-retardant low-density polyethylene composite material is prepared by the following method:
placing low-density polyethylene, silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine urate serving as raw materials in an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine cyanurate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Example 2
The embodiment of the invention provides a flame-retardant low-density polyethylene composite material.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 50% of low-density polyethylene, 30% of silicon dioxide coated ammonium polyphosphate, 10% of dipentaerythritol and 10% of silicon dioxide coated melamine cyanurate in percentage by weight.
The preparation method of the silica coated ammonium polyphosphate in the raw material was the same as in example 1.
The preparation method of the silica coated melamine cyanurate in the raw material is the same as in example 1.
The flame-retardant low-density polyethylene composite material is prepared by the following method:
placing low-density polyethylene, silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine urate serving as raw materials in an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine cyanurate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Example 3
The embodiment of the invention provides a flame-retardant low-density polyethylene composite material.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 55% of low-density polyethylene, 30% of silicon dioxide coated ammonium polyphosphate, 10% of dipentaerythritol and 5% of silicon dioxide coated melamine cyanurate in percentage by weight.
The preparation method of the silica coated ammonium polyphosphate in the raw material was the same as in example 1.
The preparation method of the silica coated melamine cyanurate in the raw material is the same as in example 1.
The flame-retardant low-density polyethylene composite material is prepared by the following method:
placing low-density polyethylene, silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine urate serving as raw materials in an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine cyanurate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Comparative example 1
This comparative example provides a flame retardant low density polyethylene composite.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 60% of low-density polyethylene, 30% of ammonium polyphosphate and 10% of dipentaerythritol in percentage by weight.
Placing low-density polyethylene, ammonium polyphosphate and dipentaerythritol serving as raw materials in an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of ammonium polyphosphate and dipentaerythritol after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Comparative example 2
This comparative example provides a flame retardant low density polyethylene composite.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 58% of low-density polyethylene, 30% of silicon dioxide coated ammonium polyphosphate, 10% of dipentaerythritol and 2% of melamine cyanurate in percentage by weight.
Wherein the silica-coated ammonium polyphosphate in the raw material was prepared in the same manner as in example 2.
The flame-retardant low-density polyethylene composite material is prepared by the following method:
placing low-density polyethylene, silicon dioxide coated ammonium polyphosphate, dipentaerythritol and melamine urate serving as raw materials in an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and melamine cyanurate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Comparative example 3
This comparative example provides a flame retardant low density polyethylene composite.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 60% of low-density polyethylene and 40% of ammonium polyphosphate in percentage by weight.
Placing low-density polyethylene and ammonium polyphosphate serving as raw materials into an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding ammonium polyphosphate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Comparative example 4
This comparative example provides a flame retardant low density polyethylene composite.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 60% of low-density polyethylene and 40% of silicon dioxide coated ammonium polyphosphate in percentage by weight.
Wherein the silica-coated ammonium polyphosphate in the raw material was prepared in the same manner as in example 1.
Placing low-density polyethylene and silicon dioxide coated ammonium polyphosphate serving as raw materials into an oven at 60 ℃ for 12 hours, and drying to remove water;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding silicon dioxide coated ammonium polyphosphate after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Comparative example 5
The embodiment of the invention provides a flame-retardant low-density polyethylene composite material.
The raw materials of the flame-retardant low-density polyethylene composite material comprise 60% of low-density polyethylene, 30% of silicon dioxide coated ammonium polyphosphate and 10% of dipentaerythritol in percentage by weight.
The silica coated ammonium polyphosphate in the raw materials is prepared in the following manner:
the preparation method of the silica coated ammonium polyphosphate in the raw material was the same as in example 1.
The flame-retardant low-density polyethylene composite material is prepared by the following method:
putting the low-density polyethylene, the silicon dioxide coated ammonium polyphosphate and the dipentaerythritol which are taken as raw materials into an oven at 60 ℃ for 12 hours, and drying and dewatering;
preheating an internal mixer to 155 ℃, slowly adding low-density polyethylene after the temperature is stable, and slowly adding a mixture of silicon dioxide coated ammonium polyphosphate and dipentaerythritol after the low-density polyethylene is added, so that all raw materials are fully extruded, sheared and uniformly mixed in the internal mixer. And mixing for 10min to obtain the flame-retardant low-density polyethylene composite material product.
Effect example 1
The silica coated ammonium polyphosphate, silica coated melamine cyanurate prepared in example 2 was subjected to FTIR and XRD measurements with ammonium polyphosphate and melamine cyanurate, respectively, and the results are shown in fig. 1-4.
FIG. 1 is a FTIR graph of ammonium polyphosphate and silica coated ammonium polyphosphate, from which it can be seen that the typical characteristic peak of ammonium polyphosphate has a value of 3431cm -1 N-H characteristic peak at 1020cm -1 PO at 2 And PO (PO) 3 Symmetrical vibration peak, 1253cm -1 P=o bond at and 1079cm -1 Symmetrical stretching vibration peak of P-O bond at 886cm -1 P-O bond at and 802cm -1 Asymmetric stretching vibration peak of P-O-P bond. The absorption peak of the silica-coated ammonium polyphosphate is 1440cm in addition to the typical characteristic peak of ammonium polyphosphate -1 Characteristic peaks of c=c are also shown. At the same time at 1106cm -1 And 1250cm -1 Characteristic peaks of Si-O-Si and Si-O-C appear at the position and are 1079cm -1 And 1253cm -1 Is covered by strong absorption peaks which are characteristic peaks of ammonium polyphosphate. This shows that example 2 successfully produced a silica gel-coated ammonium polyphosphate having vinyl groups in the shell.
Figure 2 is an XRD pattern of ammonium polyphosphate and silica coated ammonium polyphosphate. From the graph, the characteristic absorption peak of ammonium polyphosphate is shown at the diffraction angle 2 theta of 14.57 degrees, 15.42 degrees, 20.06 degrees and 22.8 degrees. With the introduction of TEOS and YDH-15, the peak value of the silicon dioxide coated ammonium polyphosphate has no obvious change, which indicates that the crystal structure of the ammonium polyphosphate is stable. Whereas the peak of the silica coated ammonium polyphosphate was enhanced at 22.8 deg. due to the silicon element contained in TEOS and YDH-151. The XRD results demonstrate that example 2 successfully produced a vinyl-containing silica gel-coated ammonium polyphosphate in its shell, consistent with the FTIR pattern results.
FIG. 3 is a FTIR image of melamine cyanurate and silica coated melamine cyanurate, from which 3389cm of the image can be seen -1 ，3230cm -1 ，1780cm -1 ，1736cm -1 ，1662cm -1 ，1536cm -1 ，1450cm -1 And 1203cm -1 There appears a characteristic peak of melamine cyanurate. Absorption peak of silica-coated melamine cyanurate is 1087cm apart from typical melamine urate characteristic peak -1 Si-O-Si asymmetric telescopic vibration absorption peak appears nearby 970cm -1 Bending vibration absorption peak at Si-OHDisappeared, indicating that there may be a portion of Si-OH reacted with melamine urate at the same time at 804cm -1 The Si-O telescopic vibration absorption peak appears at the position, which indicates SiO 2 The sol may be attached to the MCA. This shows that example 2 successfully produced a silicone gel-encapsulated melamine cyanurate with vinyl groups in the shell.
Fig. 4 is an XRD pattern of melamine cyanurate and silica coated melamine cyanurate, from which it can be seen that the characteristic absorption peaks for melamine cyanurate are at diffraction angles 2θ of 11.03 °,11.96 °,21.95 °,28.05 ° and 33.18 °. With the introduction of TEOS and YDH-15, the peak value of the silicon dioxide coated melamine cyanurate is shifted, but the change is not obvious, which indicates that the crystal structure of the melamine cyanurate is stable. Whereas silica coats SiO in melamine cyanurate 2 The peak of (2) is similar to the peak of 22.08 DEG of melamine cyanurate, thus SiO 2 The peak at 22.8 ° was not shown, whereas the peak of the silica coated melamine cyanurate at 28.05 ° was enhanced due to the silicon element contained in TEOS and YDH-151. The XRD results demonstrate that example 2 successfully produced a silica gel encapsulated melamine cyanurate with vinyl-containing shell, consistent with the FTIR pattern results.
Effect example 2
The flame retardant low density polyethylene composite materials prepared in examples 1 to 3 and comparative examples 1 to 5 were subjected to related tests of vertical combustion, limiting oxygen index, tensile strength and elongation at break, and the test results are shown in Table 1.
Table 1 results of flame retardant property tests for examples and comparative examples
| Test item | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Vertical combustion | V-0 | V-0 | V-0 | V-2 | V-0 | NR | NR | V-0 |
| Limiting oxygen index (%) | 30.3 | 29.2 | 29.8 | 22.6 | 27.2 | 17.2 | 19.3 | 25.9 |
The vertical burning test was performed according to the American national Standard UL-94 (ANSI/ASTMD 635-77), and the size of each sample was 125X 12.5X 3.2mm. In the evaluation scale, V-0 indicates that the vertical sample stops burning within 10 seconds and no droplet is allowed; v-1 indicates that the vertical sample stopped burning within 30 seconds and was not allowed to have droplets; v-2 indicates that the vertical sample stopped burning within 30 seconds and that there was allowed to be a burn drop.
Limiting oxygen index was measured using an oxygen index instrument and according to the national standard LOI (ASTM D2863-97) for each sample size of 120X 6.5X 3.2mm. The project tests that the lowest oxygen concentration for a material just maintains equilibrium combustion, the higher the index, the better for a flame retardant material.
As can be seen from Table 1, the invention adopts the silicon dioxide coated ammonium polyphosphate as an acid source and a small amount of dipentaerythritol as a carbon source, adopts the silicon dioxide coated melamine urate as a main air source to form an intumescent flame retardant system, and prepares the modified intumescent flame retardant low density polyethylene composite material through melt blending. The prepared modified intumescent flame retardant low density polyethylene composite material has good flame retardant property and solves the problem of molten drops. For the flame retardant material, the flame retardant material can be called when the limiting oxygen index is more than 27%, so that the modified intumescent flame retardant low density polyethylene composite material prepared in the embodiment 1-3 of the application can be called as the flame retardant material, and the flame retardant performance is far better than that of other similar products.
Effect example 3
The flame retardant low density polyethylene composite materials prepared in example 1 and comparative examples 1 to 5 were subjected to related tests of tensile strength and elongation at break, and the test results are shown in table 2.
The tensile strength and elongation at break are measured by a universal material tester with reference to national standard GB/T1040.2-2006, the tensile rate at room temperature is 20+ -2 mm/min, each sample is dumbbell-shaped with a size of 2X 4mm, and each sample is measured 5 times to obtain an average value. The higher the tensile strength and the greater the elongation at break of the test specimen, the better the mechanical strength of the test specimen.
Table 2 results of mechanical property test of examples and comparative examples
| Test item | Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
| Tensile Strength (MPa) | 13.52 | 10.56 | 12.92 | 12.51 | 12.62 | 12.45 |
| Elongation at break (%) | 14.65 | 12.50 | 13.33 | 13.20 | 13.60 | 13.60 |
As can be seen from Table 2, the invention improves the components, so that the mechanical properties of the prepared modified intumescent flame retardant low density polyethylene composite material product are better than those of similar products, and the technical problem that the mechanical properties of the product are greatly reduced when the flame retardant is added into the low density polyethylene material in the prior art is solved.
In summary, the invention uses the silicon dioxide coated ammonium polyphosphate as an acid source and a small amount of air source dipentaerythritol as a carbon source, uses the silicon dioxide coated melamine urate as a main air source to form an intumescent flame retardant system, and prepares the modified intumescent flame retardant low density polyethylene composite material through melt blending. The oxygen index of the product can meet the flame-retardant requirement and reduce the release amount of smoke, and simultaneously solves the problem that the mechanical property of the material can be greatly reduced when the flame retardant is added in the prior art. The mechanical property of the modified intumescent flame retardant low density polyethylene composite material product prepared by the invention is far superior to that of similar products with similar flame retardant property to the product.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
Moreover, any combination of the various embodiments of the invention can be made without departing from the spirit of the invention, which should also be considered as disclosed herein.
Claims (4)
1. The flame-retardant low-density polyethylene composite material is characterized in that the raw materials of the flame-retardant low-density polyethylene composite material consist of 50-60% of low-density polyethylene, 15-30% of silicon dioxide coated ammonium polyphosphate, 5-20% of dipentaerythritol and 1-5% of silicon dioxide coated melamine urate in percentage by mass;
the silicon dioxide coated ammonium polyphosphate in the raw materials is prepared by the following steps:
mixing 30-50g of ammonium polyphosphate, 50.0-100mL of ethanol and 10-50mL of deionized water, regulating pH to be alkaline by using an ammonia solution, adding 1-3g of OP-10, carrying out heat preservation and stirring at 25-40 ℃, adding 10-13g of silicate, continuing heat preservation and stirring for reaction, adding 1-3g of silane coupling agent with vinyl, heating to 40-60 ℃, carrying out heat preservation and stirring for reaction for 1-1.5h, filtering to obtain a solid product, and washing with ethanol to obtain the product;
the silicon dioxide coated melamine cyanurate in the raw materials is prepared by the following steps:
mixing 30-50g of melamine cyanurate, 50-100mL of ethanol and 10-50mL of deionized water, regulating the pH to be alkaline by using an ammonia solution, adding 1-3g of OP-10, carrying out heat preservation and stirring at 25-40 ℃, adding 10-13g of silicate, continuing heat preservation and stirring for reaction, adding 1-3g of silane coupling agent with vinyl, heating to 40-60 ℃, carrying out heat preservation and stirring for reaction for 1-1.5h, filtering to obtain a solid product, and washing with ethanol to obtain the product;
the silicate is any one of methyl orthosilicate, ethyl orthosilicate, propyl orthosilicate and butyl orthosilicate.
2. The low-density polyethylene composite material according to claim 1, wherein said silane coupling agent having vinyl group is any one of vinyltriethoxysilane, KH570, vinyltrimethoxysilane, vinyltrimethylsilane.
3. A method of preparing a flame retardant low density polyethylene composite material according to any one of claims 1-2, characterized in that the preparation method is carried out by the steps of:
s1, preheating an internal mixer, and adding low-density polyethylene;
s2, adding a mixture of silicon dioxide coated ammonium polyphosphate, dipentaerythritol and silicon dioxide coated melamine cyanurate;
s3, mixing for 10-15min to obtain the product.
4. A method of preparing a flame retardant low density polyethylene composite material according to claim 3, wherein the internal mixer has a preheating temperature of 155-165 ℃.
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