CN111548597A - Halogen-free flame-retardant ABS composite material and preparation method thereof - Google Patents
Halogen-free flame-retardant ABS composite material and preparation method thereof Download PDFInfo
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- CN111548597A CN111548597A CN202010434860.1A CN202010434860A CN111548597A CN 111548597 A CN111548597 A CN 111548597A CN 202010434860 A CN202010434860 A CN 202010434860A CN 111548597 A CN111548597 A CN 111548597A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/17—Component parts, details or accessories; Auxiliary operations
- B29C45/76—Measuring, controlling or regulating
- B29C45/78—Measuring, controlling or regulating of temperature
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/346—Clay
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2945/00—Indexing scheme relating to injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould
- B29C2945/76—Measuring, controlling or regulating
- B29C2945/76494—Controlled parameter
- B29C2945/76531—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
Abstract
The embodiment of the invention provides a halogen-free flame-retardant ABS composite material and a preparation method thereof, the preparation raw materials of the composite material comprise ABS, halogen-free flame retardant, modified montmorillonite and antioxidant, and in the raw materials, the montmorillonite in the preparation raw materials is modified, so that the interlayer spacing of the montmorillonite is increased, and the compatibility of the montmorillonite in a high polymer is improved, thereby the dispersion of the montmorillonite in a matrix material is better, the effects of fully playing flame retardance and improving mechanical properties are achieved, and the composite material has excellent flame retardance, good mechanical properties and wide market application prospect.
Description
Technical Field
The invention belongs to the technical field of high molecular engineering plastics, and particularly relates to a halogen-free flame-retardant ABS composite material and a preparation method thereof.
Background
ABS refers to terpolymer of acrylonitrile, butadiene and styrene, and is widely applied to thermoplastic engineering plastics in the fields of automobiles, household appliances, office equipment and the like. Because ABS is copolymerized by acrylonitrile, butadiene, styrene three kinds of monomer, make ABS possess these three kinds of monomer's special properties, including acrylonitrile's high strength, chemical resistance stability, butadiene's shock resistance and the easy processing nature of styrene among them. However, ABS also has disadvantages such as flammability, a limiting oxygen index of about 19%, and the generation of smoke accompanying combustion, which greatly limits the wider range of applications of ABS resins.
In order to improve the flame retardant property of ABS resins, it is necessary to add a flame retardant to ABS resins. The flame retardant can be divided into two categories, one category is a halogen flame retardant, the dosage is small, the mechanical property is good, the flame retardant effect is obvious, but hydrogen halide gas is generated while the flame retardant is performed, and the human health is harmed. With the increasing demand for environmental protection, many halogen-based flame retardants have been banned from use. The other type is a halogen-free flame retardant which is environment-friendly, low in smoke and low in toxicity, but the mechanical property loss is large while the flame retardant property is ensured, so that the flame retardant property and the mechanical property of the material are hardly considered.
Although research on halogen-free flame retardance of ABS has been carried out for many years, the defects of large addition amount of halogen-free flame retardant, poor compatibility with matrix resin, reduction of mechanical properties of materials and the like always prevent the ABS from being widely applied in the market, so that the development of an ABS composite material with excellent mechanical properties, high-efficiency flame retardance, halogen-free property and environmental protection is still needed.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the embodiment of the invention provides a halogen-free flame-retardant ABS composite material and a preparation method thereof, and the composite material has excellent mechanical properties and high-efficiency flame retardance.
According to the embodiment of the first aspect of the invention, the halogen-free flame retardant ABS composite material comprises the following preparation raw materials in parts by weight:
ABS: 60 to 70 parts of (A) to (B),
halogen-free flame retardant: 24-30 parts of (A) a water-soluble polymer,
modified montmorillonite: 0.5 to 5 parts by weight of a stabilizer,
antioxidant: 0.5-1 part.
The halogen-free flame-retardant ABS composite material provided by the embodiment of the invention at least has the following technical effects:
according to the halogen-free flame-retardant ABS composite material disclosed by the embodiment of the invention, the montmorillonite in the preparation raw materials is modified, so that the interlayer spacing of the montmorillonite is increased, and the compatibility of the montmorillonite in a high polymer is improved, so that the montmorillonite is dispersed in a matrix material more, the effects of fully playing a role in flame retardance and improving mechanical properties are achieved, the flame retardant property of the composite material is excellent, the mechanical property is good, and the market application prospect is wide.
According to some embodiments of the invention, the halogen-free flame retardant comprises, by mass ratio (2-5): 1 and dipentaerythritol. Preferably 3: 1.
Ammonium polyphosphate is an excellent halogen-free flame retardant, and has the advantages of no toxicity, no odor, high thermal stability, no generation of corrosive gas after thermal decomposition and the like. Dipentaerythritol is flammable but is susceptible to esterification with organic acids. Generally, ammonium polyphosphate is used as an acid source and a gas source to form an expansion flame-retardant system together with dipentaerythritol so as to retard the flame of the polymer. The ammonium polyphosphate is heated and decomposed to generate ammonia gas which dilutes combustible gas generated by polymer heating and decomposition in a gas phase, and meanwhile, the polyphosphoric acid generated by the ammonium polyphosphate heating and decomposition and dipentaerythritol are dehydrated to generate esterification reaction to form carbon, and the ammonia gas enables a carbon layer to expand to prevent air from entering the surface of the polymer, so that the flame-retardant effect is achieved.
According to some embodiments of the invention, the degree of polymerization of the ammonium polyphosphate is 1000 to 2000. Preferably 1500 to 2000.
According to some embodiments of the invention, the method of preparing the modified montmorillonite comprises the steps of:
(1) dispersing sodium-based montmorillonite in a solvent to obtain a sodium-based montmorillonite dispersion liquid;
(2) dissolving ferric trichloride in a solvent to obtain a ferric trichloride solution;
(3) and (3) adding the ferric trichloride solution obtained in the step (2) into the montmorillonite dispersion liquid obtained in the step (1), and heating for reaction to obtain the modified montmorillonite.
According to some embodiments of the invention, the solvent is a mixture of deionized water and absolute ethanol in a volume ratio of 2: 1.
According to some embodiments of the invention, the Na-montmorillonite has an ion exchange capacity of 100mmol/100 g.
According to some embodiments of the invention, in step (1), the mass of the sodium montmorillonite to volume of the solvent is 1 g: (20-40) ml.
In the step (1), the dispersion of the sodium montmorillonite in the solvent is ultrasonic dispersion, and the dispersion time is more than 15 min.
According to some embodiments of the invention, in step (2), the mass to volume ratio of ferric trichloride to solvent is 1 g: (20-40) ml.
According to some embodiments of the invention, in the step (3), the temperature of the heating reaction is 40-60 ℃, and the time of the heating reaction is 12-14 h. Heating for reaction, centrifuging, washing, drying, grinding and sieving.
The preparation method of the modified montmorillonite increases the interlayer spacing of the montmorillonite and enhances the polarity, thereby improving the hydrophobicity of the montmorillonite and obtaining better modification effect by using a small amount of ferric chloride solution.
According to some embodiments of the invention, the antioxidant is a hindered phenolic antioxidant.
The hindered phenol antioxidant is at least one of antioxidant 1010 and antioxidant 1076.
The preparation method of the halogen-free flame retardant ABS composite material according to the embodiment of the second aspect of the invention comprises the following steps:
s1: uniformly mixing ABS, a halogen-free flame retardant, modified montmorillonite and an antioxidant, and then extruding and granulating to obtain halogen-free flame retardant ABS particles;
s2: and (5) injection molding the halogen-free flame-retardant ABS particles obtained in the step (S1) to obtain the halogen-free flame-retardant ABS composite material.
And S1, extruding and granulating by using an asymmetric double-screw extruder, wherein the screw rotating speed of the asymmetric double-screw extruder is 60-180 r/min, and the temperature is controlled to be 150-210 ℃.
More specifically, the temperature of each section of the asymmetric twin-screw extruder is controlled as follows: the temperature of the first section is 150-170 ℃, the temperature of the second section is 160-180 ℃, the temperature of the third section is 170-200 ℃, the temperature of the fourth section is 170-200 ℃, the temperature of the fifth section is 180-210 ℃, the temperature of the sixth section is 180-210 ℃, the temperature of the seventh section is 180-210 ℃, the temperature of the eighth section is 180-210 ℃, the temperature of the ninth section is 180-210 ℃, the temperature of the tenth section is 180-210 ℃, and the temperature of the head is 170-200 ℃.
In the step S2, injection molding is performed by injection molding, and the temperature of the injection molding machine is controlled to be 150-190 ℃.
More specifically, the temperature of the injection molding machine is controlled to be 160-190 ℃ in the first section, 160-190 ℃ in the second section and 150-190 ℃ in the third section.
Drawings
FIG. 1 shows the result of the microscopic morphology detection of Na-montmorillonite.
FIG. 2 shows the result of the microscopic morphology detection of the modified montmorillonite.
Detailed Description
The following are specific examples of the present invention, and the technical solutions of the present invention will be further described with reference to the examples, but the present invention is not limited to the examples.
Examples
The embodiment actually prepares the halogen-free flame-retardant ABS composite material, which comprises the following preparation raw materials in parts by weight:
ABS: 70 parts of halogen-free flame retardant: 24 parts of modified montmorillonite: 5 parts, antioxidant 1010: 1 part.
Wherein the halogen-free flame retardant is prepared from the following components in percentage by mass of 3:1 and dipentaerythritol.
The polymerization degree of the ammonium polyphosphate is 1000-2000.
The preparation method of the modified montmorillonite comprises the following steps:
(1) dispersing sodium-based montmorillonite in a solvent to obtain a sodium-based montmorillonite dispersion liquid;
(2) dissolving ferric trichloride in a solvent to obtain a ferric trichloride solution;
(3) and (3) adding the ferric trichloride solution obtained in the step (2) into the montmorillonite dispersion liquid obtained in the step (1), and heating for reaction to obtain the modified montmorillonite.
The solvent is the mixture of deionized water and absolute ethyl alcohol according to the volume ratio of 2: 1.
The ion exchange capacity of the sodium montmorillonite is 100mmol/100 g.
In the step (1), the mass ratio of the sodium montmorillonite to the solvent is 1 g: 30 ml. The dispersion of the sodium-based montmorillonite in the solvent is ultrasonic dispersion, and the dispersion time is more than 15 min.
In the step (2), the volume ratio of the mass of ferric trichloride to the solvent is 1 g: 30 ml.
In the step (3), the heating reaction temperature is 40 ℃, and the heating reaction time is 14 h. Heating for reaction, centrifuging, washing, drying, grinding and sieving.
The preparation method of the ABS composite material comprises the following steps:
s1: uniformly mixing ABS, a halogen-free flame retardant, modified montmorillonite and an antioxidant, and then extruding and granulating to obtain halogen-free flame retardant ABS particles;
s2: and (4) injection molding the halogen-free flame-retardant ABS particles obtained in the step (S1) to obtain the halogen-free flame-retardant ABS composite material.
And S1, extruding and granulating by using an asymmetric double-screw extruder, wherein the screw rotating speed of the asymmetric double-screw extruder is 60-180 r/min, and the temperature is controlled to be 150-210 ℃. The temperature of each section of the asymmetric twin-screw extruder is controlled as follows: the temperature of the first section is 150-170 ℃, the temperature of the second section is 160-180 ℃, the temperature of the third section is 170-200 ℃, the temperature of the fourth section is 170-200 ℃, the temperature of the fifth section is 180-210 ℃, the temperature of the sixth section is 180-210 ℃, the temperature of the seventh section is 180-210 ℃, the temperature of the eighth section is 180-210 ℃, the temperature of the ninth section is 180-210 ℃, the temperature of the tenth section is 180-210 ℃, and the temperature of the head is 170-200 ℃.
In the step S2, injection molding is performed by injection molding, and the temperature of the injection molding machine is controlled to be 150-190 ℃. Specifically, the temperature of the first section is 160-190 ℃, the temperature of the second section is 160-190 ℃, and the temperature of the third section is 150-190 ℃.
The micro-morphology of the sodium-based montmorillonite is shown in figure 1, and the micro-morphology of the modified montmorillonite is shown in figure 2.
Comparative example 1
The halogen-free flame-retardant ABS composite material is actually prepared in the embodiment, and the difference from the embodiment 3 is that the montmorillonite in the preparation raw material is sodium montmorillonite without modification.
Comparative example 2
The halogen-free flame-retardant ABS composite material is actually prepared in the embodiment, and the difference from the embodiment 3 is that montmorillonite is not contained in the preparation raw material.
Example of detection
In this example, the mechanical properties of the composite materials prepared in examples and comparative examples 1 to 2 were examined, wherein the tensile properties were tested according to the regulations of GB/T1040.2-2006, the impact strength was tested according to the regulations of GB/T1843-2008, the spline notch was an A-type oxygen index and was tested according to the regulations of GB/T2406.2-2009, and the vertical burning properties were tested according to the regulations of GB/T2408-2008. The results are shown in Table 1.
TABLE 1 halogen-free flame-retardant ABS composite Material Performance test results
Claims (10)
1. The halogen-free flame-retardant ABS composite material is characterized by comprising the following preparation raw materials in parts by weight:
ABS: 60 to 70 parts of (A) to (B),
halogen-free flame retardant: 24-30 parts of (A) a water-soluble polymer,
modified montmorillonite: 0.5 to 5 parts by weight of a stabilizer,
antioxidant: 0.5-1 part.
2. The halogen-free flame-retardant ABS composite material as claimed in claim 1, wherein the halogen-free flame retardant is prepared from the following components in mass ratio of (2-5): 1 and dipentaerythritol.
3. The halogen-free flame-retardant ABS composite material according to claim 2 characterized in that the polymerization degree of the ammonium polyphosphate is 1000-2000.
4. The halogen-free flame retardant ABS composite material according to claim 1 wherein the preparation method of the modified montmorillonite comprises the following steps:
(1) dispersing sodium-based montmorillonite in a solvent to obtain a sodium-based montmorillonite dispersion liquid;
(2) dissolving ferric trichloride in a solvent to obtain a ferric trichloride solution;
(3) and (3) adding the ferric trichloride solution obtained in the step (2) into the montmorillonite dispersion liquid obtained in the step (1), and heating for reaction to obtain the modified montmorillonite.
5. The halogen-free flame retardant ABS composite material according to claim 4 characterized in that the solvent is a mixture of deionized water and absolute ethyl alcohol in a volume ratio of 2: 1.
6. The halogen-free flame retardant ABS composite material according to claim 4 characterized in that in step (1), the mass of Na-montmorillonite to volume ratio of solvent is 1 g: (20-40) ml.
7. The halogen-free flame retardant ABS composite material according to claim 4 wherein, in step (2), the mass to volume ratio of ferric trichloride to solvent is 1 g: (20-40) ml.
8. The halogen-free flame retardant ABS composite material according to claim 4, characterized in that in step (3), the temperature of the heating reaction is 40-60 ℃ and the time of the heating reaction is 12-14 h.
9. The halogen-free flame retardant ABS composite material according to claim 1 wherein the antioxidant is a hindered phenol antioxidant.
10. The preparation method of the halogen-free flame-retardant ABS composite material according to any of claims 1-9, characterized by comprising the following steps:
s1: uniformly mixing ABS, a halogen-free flame retardant, modified montmorillonite and an antioxidant, and then extruding and granulating to obtain halogen-free flame retardant ABS particles;
s2: and (5) injection molding the halogen-free flame-retardant ABS particles obtained in the step (S1) to obtain the halogen-free flame-retardant ABS composite material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114656726A (en) * | 2021-06-11 | 2022-06-24 | 石河子大学 | Flame-retardant soft PVC composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114656726A (en) * | 2021-06-11 | 2022-06-24 | 石河子大学 | Flame-retardant soft PVC composite material and preparation method thereof |
| CN114656726B (en) * | 2021-06-11 | 2024-04-05 | 石河子大学 | Flame-retardant soft PVC composite material and preparation method thereof |
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