CN111333960A - Antimony-free flame-retardant polypropylene composition and preparation method thereof - Google Patents
Antimony-free flame-retardant polypropylene composition and preparation method thereof Download PDFInfo
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- CN111333960A CN111333960A CN202010104224.2A CN202010104224A CN111333960A CN 111333960 A CN111333960 A CN 111333960A CN 202010104224 A CN202010104224 A CN 202010104224A CN 111333960 A CN111333960 A CN 111333960A
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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
- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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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
- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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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
- C08K2003/325—Calcium, strontium or barium phosphate
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
Abstract
The invention discloses an antimony-free flame-retardant polypropylene composition and a preparation method thereof, wherein the composition comprises the following components: 40-70 parts of polypropylene resin; 15-25 parts of brominated flame retardant; 1-10 parts of an inorganic barium compound; 0.1-3 parts of silicon flame-retardant lubricant. The flame-retardant polypropylene composition prepared by synergistic combination of the inorganic barium compound, the silicon flame-retardant lubricant and the bromine flame retardant can obtain excellent flame-retardant performance and toughness under the condition of synergistic effect without adding antimony element, has higher oxygen index and lower smoke density, can be prepared into products according to different purposes, is particularly suitable for electronic and electric products, and has excellent industrial application prospect.
Description
Technical Field
The invention belongs to the field of high polymer materials, and particularly relates to an antimony-free flame-retardant polypropylene composition and a preparation method thereof.
Background
Polypropylene is one of the most widely used general plastics due to its excellent comprehensive properties, good cost performance and wider processing and forming conditions. The polypropylene is a typical flammable material, the limiting oxygen index of the polypropylene is 17-18%, the polypropylene is extremely easy to burn and cannot be self-extinguished after being ignited, and the polypropylene material needs to be subjected to flame retardant modification along with the gradual increase of the safety requirement of the material.
The flame retardant for polypropylene is mainly divided into an environment-friendly brominated flame retardant and a halogen-free flame retardant, in order to meet the requirement of non-halogenation, the flame retardant containing phosphorus, nitrogen or a compound system of phosphorus and nitrogen is required to be added in the existing flame-retardant modified polypropylene material, but the halogen-free flame retardant system has the defects of large addition amount, low flame-retardant efficiency, poor physical properties (especially insufficient toughness), high water absorption and the like, and has great limitation in wide application. The environment-friendly bromine-containing flame retardant is still the main flame retardant of polypropylene resin, and has the advantages of high flame retardant efficiency, excellent heat resistance, small influence on physical properties and the like, but the bromine-containing flame retardant is generally required to be used together with antimony compounds (mainly antimony trioxide), and has the defects of high smoke density, high toxicity and the like during combustion. In addition, antimony brings some risks of environmental protection and carcinogenesis, and causes environmental pollution and harm to the safety of workers in the production and processing processes, so that the application limit is more limited. With the increasing demand of downstream industry applications, more and more products and safety regulations are expected to achieve V-0 flame retardant rating and minimum smoke emission, and antimony used as a rare element for flame retardant brings about reduction of mineral resources, and is limited to be used in part of the regulations (such as the U.S. California No. 65 act). Therefore, the research on the antimony-free flame-retardant polypropylene composition has excellent industrial application prospect.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide an antimony-free flame-retardant polypropylene composition which has excellent flame-retardant performance and toughness, higher oxygen index and lower smoke density.
Another object of the present invention is to provide a method for preparing the antimony-free flame retardant polypropylene composition.
The invention is realized by the following technical scheme:
an antimony-free flame-retardant polypropylene composition comprises the following components in parts by weight:
40-70 parts of polypropylene resin;
15-25 parts of brominated flame retardant;
1-10 parts of an inorganic barium compound;
0.1-3 parts of silicon flame-retardant lubricant.
Preferably, the polypropylene is selected from one or a mixture of two of homo-polypropylene and co-polypropylene.
Preferably, the bromine-based flame retardant is an organic bromine-based flame retardant, specifically selected from decabromodiphenylethane and tris (tribromoneopentyl)
A group) phosphate, tris (2, 3-dibromopropyl) isocyanurate, tetrabromobisphenol A bis (2, 3-dibromopropyl) ether, tetrabromobisphenol S bis (2, 3-dibromopropyl) ether or ethyl-bis (tetrabromophthalimide), and decabromodiphenylethane or ethyl-bis (tetrabromophthalimide) is preferable from the viewpoint of heat resistance and flame retardant efficiency of the material.
From the viewpoint of rationalization of performance, based on the total weight of the whole antimony-free flame-retardant polypropylene composition, the addition amount of the brominated flame retardant is 15-25 parts, preferably 18-22 parts, when the addition amount is too small, the flame-retardant effect is relatively poor, and when the addition amount is less than 15 parts, the flame-retardant stability is reduced; when the addition amount is too high, the flame retardant performance is not obviously different, but the toughness of the material is reduced and the smoke density is increased.
Preferably, the inorganic barium compound is one or more selected from precipitated barium sulfate, barite, barium titanate or barium phosphate, and is preferably precipitated barium sulfate or barium phosphate.
From the viewpoint of rationalization of performance, based on the total weight of the whole antimony-free flame-retardant polypropylene composition, the addition amount of the inorganic barium compound is 1-10 parts, and when the addition amount is too small, the flame-retardant efficiency is insufficient, and the flame-retardant grade is low; when the addition amount is too high, the flame retardant property has no obvious difference.
Preferably, the silicon-based flame-retardant lubricant is one or a mixture of more of SFR-100, dimethyl silicone oil and vinyl silicone oil, and more preferably SFR-100 or vinyl silicone oil.
According to actual performance requirements, the antimony-free flame-retardant polypropylene composition further comprises 0-25 parts of talcum powder, 0-1 part of antioxidant and 0-1 part of processing aid in parts by weight.
Preferably, the antioxidant is selected from one or a mixture of several of phenols, phosphites, bivalent sulfur antioxidants or hindered amine antioxidants, wherein the phenol antioxidants comprise antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant SP, antioxidant 2246, antioxidant CA, antioxidant 330, Irganox1890 or antioxidant 3114, the phosphites comprise antioxidant TNP, antioxidant ODP, antioxidant 168, Irganox1093 or Irganox1222, the bivalent sulfur antioxidants comprise dilaurate thiodipropionate (DLTP) and distearate thiodipropionate (DSTP), and the hindered amine antioxidants comprise LS-744, LS-770, GW-540 or Flamstab NOR 116.
Preferably, the processing aid is one or more of low molecular weight lipid, metal soap, stearic acid complex ester and amide, wherein the low molecular weight lipid is solid paraffin, liquid paraffin or low molecular weight polyolefin wax, the metal soap is calcium stearate, magnesium stearate, zinc stearate or barium stearate, the stearic acid complex ester is ethylene glycol stearate, glyceryl stearate or pentaerythritol stearate, and the amide is erucyl amide, methylene bis stearamide or N, N-ethylene bis stearamide.
The invention also provides a preparation method of the antimony-free flame-retardant polypropylene composition, which comprises the following steps:
after weighing the components in proportion, uniformly mixing the components through a high-speed mixer, then performing melt extrusion and granulation at the temperature of 180-200 ℃ through a double-screw extruder, and drying to obtain the antimony-free flame-retardant polypropylene composition.
Compared with the prior art, the invention has the following beneficial effects:
1) the invention adopts inorganic barium compound, silicon flame-retardant lubricant and bromine flame retardant for synergistic effect, the inorganic barium compound is used as Lewis acid and bromine flame retardant for synergistic effect, the silicon flame-retardant lubricant promotes the compatibility of the two, the flame-retardant polypropylene can pass the vertical combustion V-0 test by adding a small amount of bromine flame retardant (15-25 parts), the oxygen index is more than 25 percent and the smoke density is less than 70, the flame-retardant polypropylene composition has very high-efficiency flame-retardant effect, the prepared flame-retardant polypropylene composition has excellent flame-retardant property and toughness, higher oxygen index and lower smoke density, can be prepared into products according to different purposes, is especially suitable for electronic and electric products, and has excellent industrial application prospect;
2) the flame-retardant polypropylene composition utilizes the synergistic effect of the inorganic barium compound and the silicon flame-retardant lubricant on the bromine flame retardant, thereby replacing the traditional bromine-antimony flame-retardant mechanism, having excellent flame-retardant performance, and simultaneously, as antimony halide gas is not generated any more, the toxic and harmful gas generated in the combustion process of the material can be effectively reduced, and the smoke release in the product combustion is reduced;
3) in the flame-retardant polypropylene composition provided by the invention, the raw materials are common materials sold in the market, no special chemicals are used, the preparation process is simple and easy, the requirement on equipment is low, the comprehensive cost performance of the product is higher, various flame-retardant products can be prepared according to different purposes, and the flame-retardant polypropylene composition has an excellent industrial application prospect.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention and are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw materials used in the examples and comparative examples are now described below, but are not limited to these materials:
polypropylene resin: homo-polypropylene: PP HP500N, zhonghai shell brand;
polypropylene resin: copolymerized polypropylene: PP K9010, taihua group;
brominated flame retardants: decabromodiphenylethane, israel chemical group;
brominated flame retardants: ethyl-bis (tetrabromophthalimide), israel chemical group;
antioxidant 1010, Tianjin Lianlong New Material Ltd;
antioxidant 168, Tianjin Lianlong New Material Ltd;
processing aid: calcium stearate, zhongshan huamingtai chemical corporation;
inorganic barium compound: precipitating barium sulfate and barium phosphate, which are sold in markets;
silicon-based flame-retardant lubricant: vinyl silicone oil, SFR-100, commercially available;
talc, commercially available;
halogen-free flame retardant: ammonium polyphosphate, Budenheim, germany;
antimony trioxide: it is commercially available.
The relevant performance test criteria or methods are as follows:
test method of vertical burning: according to the UL94 standard, the test sample strips have the thickness of 1.6mm and 3.2 mm;
smoke density rating test (SDR): according to the test method of GB/T8627, the thickness of a test sample strip is 6.0 mm;
and (3) oxygen index test: according to the test method of GB/T2406.2, the thickness of the test sample strip is 4.0 mm;
notched izod impact strength: the test was carried out according to ISO 180 standard.
Examples 1-10 and comparative examples 1-6:
weighing the components according to the proportion shown in the table 1, uniformly mixing the components through a high-speed mixer, then carrying out melt extrusion at 200 ℃ through a double-screw extruder, granulating, and drying to obtain the flame-retardant polypropylene composition; the flame retardant polypropylene compositions prepared in examples and comparative examples were tested for vertical flame retardancy, oxygen index, and smoke density, and the results are shown in Table 1.
TABLE 1 examples and comparative examples the specific proportions of the components and the performance results (in parts by weight)
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | Example 7 | Example 8 | Example 9 | Example 10 | |
| Polypropylene copolymer | 68.5 | 68.5 | 68.5 | 64.5 | 60.5 | 64.5 | 60.5 | 64.5 | 60.5 | |
| Homo-polypropylene | 64.5 | |||||||||
| Decabromodiphenylethane | 15 | 18 | 21 | 18 | 21 | 18 | 21 | 18 | ||
| Ethyl-bis (tetrabromophthalimide) | 18 | 21 | ||||||||
| Precipitated barium sulfate | 5 | 5 | 5 | 6 | 7 | 6 | 7 | 6 | ||
| Barium phosphate | 6 | 7 | ||||||||
| Vinyl silicone oil | 1 | 1 | ||||||||
| SFR-100 | 1 | 1 | 1 | 1 | 1 | 1 | 2 | 1 | ||
| Talcum powder | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 | 10 |
| Antimony trioxide | ||||||||||
| Commercially available halogen-free flame retardant | ||||||||||
| Antioxidant 1010 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Antioxidant 168 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Calcium stearate | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| UL-94,3.2mm | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| UL-94,1.6mm | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
| Smoke density rating | 57 | 62 | 68 | 60 | 67 | 63 | 69 | 60 | 67 | 62 |
| Oxygen index (%) | 25.2 | 26.3 | 28.4 | 27.3 | 29.2 | 25.9 | 27.8 | 26.1 | 28.5 | 26.5 |
| Cantilever beam notch impact (kJ/m 2) | 32 | 25 | 20 | 23 | 17 | 25 | 21 | 24 | 19 | 4 |
Continuing with Table 1:
| comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
| Polypropylene copolymer | 68.5 | 68.5 | 68.5 | 68.5 | 68.5 | 59.5 |
| Homo-polypropylene | ||||||
| Decabromodiphenylethane | 18 | 18 | 18 | 18 | 18 | |
| Ethyl-bis (tetrabromophthalimide) | ||||||
| Precipitated barium sulfate | 5 | |||||
| Barium phosphate | ||||||
| Vinyl silicone oil | ||||||
| SFR-100 | 1 | 1 | ||||
| Talcum powder | 10 | 10 | 10 | 10 | ||
| Antimony trioxide | 5 | 5 | ||||
| Commercially available halogen-free flame retardant | 30 | |||||
| Antioxidant 1010 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Antioxidant 168 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Calcium stearate | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| UL-94,3.2mm | NR | NR | NR | V-0 | V-0 | V-0 |
| UL-94,1.6mm | NR | NR | NR | V-1 | V-0 | V-1 |
| Smoke density rating | 75 | 73 | 74 | 85 | 88 | 46 |
| Oxygen index (%) | 19.2 | 21.2 | 20.5 | 23.2 | 24.9 | 31 |
| Cantilever beam notch impact (kJ/m 2) | 32 | 25 | 30 | 24 | 20 | 4 |
From a comparison of the examples and comparative examples of table 1, it can be seen that: the bromine-containing flame retardant, the inorganic barium compound and the silicon-containing flame retardant lubricant are used together to generate a synergistic effect, and a good flame retardant effect on the polypropylene resin can be realized by adding a small amount of flame retardant (15-25 parts), so that the vertical combustion V-0 grade, the oxygen index of more than 25 percent and the smoke density of less than 70 are achieved. Compared with the comparative example 1, the bromine flame retardant is used independently, so that the flame retardant effect is poor, the oxygen index is low, and the smoke density grade is high; in comparative examples 2 to 3, the bromine-based flame retardant and the inorganic barium compound, the bromine-based flame retardant and the silicon-based flame retardant lubricant were used in combination, respectively, and the oxygen index was slightly increased, but the increase range was small, and the vertical burning performance was not significantly increased. In comparative examples 4-5, the brominated flame retardant was used in combination with antimony trioxide, the oxygen index was lower and the smoke density rating was not greater. Compared with the prior art, the toughness of the material is obviously reduced by adding a large amount of halogen-free flame retardant in the comparative example 6.
Claims (9)
1. The antimony-free flame-retardant polypropylene composition is characterized by comprising the following components in parts by weight:
40-70 parts of polypropylene resin;
15-25 parts of brominated flame retardant;
1-10 parts of an inorganic barium compound;
0.1-3 parts of silicon flame-retardant lubricant.
2. An antimony-free flame retardant polypropylene composition according to claim 1, wherein the polypropylene is selected from one or a mixture of homo polypropylene and co polypropylene.
3. The antimony-free flame-retardant polypropylene composition as claimed in claim 1, wherein the brominated flame retardant is a brominated flame retardant
The organic bromine flame retardant is specifically selected from one or a mixture of more of decabromodiphenylethane, tris (tribromoneopentyl) phosphate, tris (2, 3-dibromopropyl) isocyanurate, tetrabromobisphenol A bis (2, 3-dibromopropyl) ether, tetrabromobisphenol S bis (2, 3-dibromopropyl) ether or ethyl-bis (tetrabromophthalimide), and is preferably decabromodiphenylethane or ethyl-bis (tetrabromophthalimide).
4. The antimony-free flame retardant polypropylene composition according to claim 3, wherein the brominated flame retardant is added in an amount of 18 to 22 parts based on the total weight of the entire antimony-free flame retardant polypropylene composition.
5. The antimony-free flame-retardant polypropylene composition as claimed in claim 1, wherein the inorganic barium compound is
The compound is one or more of precipitated barium sulfate, barite, barium titanate or barium phosphate, preferably precipitated barium sulfate or barium phosphate.
6. The antimony-free flame-retardant polypropylene composition according to claim 1, wherein the silicon-based flame-retardant lubricant is selected from one or more of SFR-100, dimethicone or vinyl silicone oil, preferably SFR-100 or vinyl silicone oil.
7. The antimony-free flame-retardant polypropylene composition according to any one of claims 1 to 6, further comprising 0 to 25 parts by weight of talc, 0 to 1 part by weight of antioxidant and 0 to 1 part by weight of processing aid.
8. The antimony-free flame retardant polypropylene composition according to claim 7, wherein the antioxidant is selected from one or a mixture of several of phenol, phosphite, divalent sulfur or hindered amine antioxidants; the processing aid is selected from one or more of low molecular lipid, metal soap, stearic acid composite ester or amide.
9. The method for preparing an antimony-free flame retardant polypropylene composition according to any of claims 1-8, comprising the steps of:
after weighing the components in proportion, uniformly mixing the components through a high-speed mixer, then performing melt extrusion and granulation at the temperature of 180-200 ℃ through a double-screw extruder, and drying to obtain the antimony-free flame-retardant polypropylene composition.
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| CN202010104224.2A CN111333960A (en) | 2020-02-20 | 2020-02-20 | Antimony-free flame-retardant polypropylene composition and preparation method thereof |
| PCT/CN2020/130127 WO2021164353A1 (en) | 2020-02-20 | 2020-11-19 | Antimony-free flame-retardant polypropylene composition and preparation method therefor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112194845A (en) * | 2020-09-09 | 2021-01-08 | 武汉金发科技有限公司 | Halogen flame-retardant reinforced polypropylene composite material and preparation method thereof |
| CN112745571A (en) * | 2020-12-16 | 2021-05-04 | 金发科技股份有限公司 | Antimony-free flame-retardant ceramic polyolefin composition and preparation method and application thereof |
| WO2021164353A1 (en) * | 2020-02-20 | 2021-08-26 | 金发科技股份有限公司 | Antimony-free flame-retardant polypropylene composition and preparation method therefor |
| CN114163725A (en) * | 2021-12-07 | 2022-03-11 | 广东安拓普聚合物科技有限公司 | Polypropylene resin composition and preparation method and application thereof |
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| CN113956572B (en) * | 2021-11-24 | 2023-01-17 | 湖南省新基源新材料科技有限公司 | Flame-retardant polyolefin composition and preparation method thereof |
| CN114989513A (en) * | 2022-04-20 | 2022-09-02 | 李平 | Halogen-free environment-friendly flame-retardant polyethylene material and preparation method thereof |
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- 2020-11-19 WO PCT/CN2020/130127 patent/WO2021164353A1/en active Application Filing
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| CN106832566A (en) * | 2016-12-18 | 2017-06-13 | 合肥会通新材料有限公司 | A kind of low smell polypropylene flame redardant compound material of antibacterial and preparation method thereof |
| CN109265822A (en) * | 2018-08-30 | 2019-01-25 | 江苏金发科技新材料有限公司 | Without white point thermoplastic flame-proof process for producing composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2021164353A1 (en) * | 2020-02-20 | 2021-08-26 | 金发科技股份有限公司 | Antimony-free flame-retardant polypropylene composition and preparation method therefor |
| CN112194845A (en) * | 2020-09-09 | 2021-01-08 | 武汉金发科技有限公司 | Halogen flame-retardant reinforced polypropylene composite material and preparation method thereof |
| CN112745571A (en) * | 2020-12-16 | 2021-05-04 | 金发科技股份有限公司 | Antimony-free flame-retardant ceramic polyolefin composition and preparation method and application thereof |
| CN114163725A (en) * | 2021-12-07 | 2022-03-11 | 广东安拓普聚合物科技有限公司 | Polypropylene resin composition and preparation method and application thereof |
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Application publication date: 20200626 |