CN112646308A - Halogen-free flame-retardant high-toughness ABS resin composition containing nano-scale flame retardant and preparation method thereof - Google Patents
Halogen-free flame-retardant high-toughness ABS resin composition containing nano-scale flame retardant and preparation method thereof Download PDFInfo
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08L55/00—Compositions of homopolymers or copolymers, obtained by polymerisation reactions only involving carbon-to-carbon unsaturated bonds, not provided for in groups C08L23/00 - C08L53/00
- C08L55/02—ABS [Acrylonitrile-Butadiene-Styrene] polymers
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The invention discloses a modified halogen-free flame-retardant high-toughness ABS resin containing a nanoscale flame retardant and a preparation method thereof, wherein the modified halogen-free flame-retardant high-toughness ABS resin is prepared from the following raw materials in percentage by weight: 45-85% of ABS resin; 10-50% of a composite flame retardant; 1-3% of a lubricant; 0.01-2% of a dispersant; 0.01-0.5% of antioxidant; the invention mainly solves the problem of halogen-free flame retardantPoor compatibility with ABS and low product performance when added in large dose. The method is characterized in that: the SAN grafted PBL latex microsphere wrapped nano-scale phosphaphenanthrene oxide graft modified aluminum hydroxide or magnesium hydroxide is used as a flame retardant, not only the flame retardant synergistic effect of metal hydroxide and phosphorus flame retardant is exerted, but also the halogen-free flame retardant is greatly promoted to be well dispersed in ABS resin, and the toughening effect is achieved. The result shows that when the effective addition amount of the flame retardant compound is as low as 5 percent, the flame retardant ABS still reaches UL 94V-0 grade, and the notch impact strength is more than 13KJ/m2。
Description
Technical Field
The invention relates to the technical field of high polymer material processing, in particular to a halogen-free flame-retardant high-toughness ABS resin composition containing a nano-scale flame retardant and a preparation method thereof.
Background
The ABS material has the characteristics of high strength, good toughness, easy processing, good gloss and the like, and is widely applied to the fields of household appliances, children toys, mechanical accessories, automobile interior and exterior decorations and the like. However, ABS is extremely easy to burn, the horizontal burning speed of ABS is about 2.5-5.1 cm/min, and a large amount of black smoke and toxic gas are generated during burning, so that great potential safety hazards are extremely easy to generate. The traditional flame retardant method is to add halogen flame retardant, and the obtained product has good flame retardant effect, but generates toxic and corrosive gas during combustion, and has great side effect on human and environment. In recent years, with the general improvement of environmental awareness of people, for example, the european union countries have issued a command on scrapped electronic and electrical equipment (WEEE) and a command on prohibition of use of certain harmful substances in electronic and electrical equipment (RoHS) in 2003 2 months, and according to the RoHS command requirements, electric and electronic products released to the european union market after 7 months and 1 days 2006 must not contain 6 kinds of harmful substances such as polybrominated biphenyls and polybrominated diphenyl ethers. Therefore, the application of halogen-containing flame retardant in ABS materials is increasingly limited, non-halogenation becomes the main trend of flame retardant development and application, and the development of environment-friendly halogen-free flame retardant ABS materials is imperative. The halogen-free flame retardant in the current market mainly comprises metal oxide, phosphorus flame retardant and the like, has poor compatibility with ABS materials, is difficult to disperse, and can cause the performance indexes such as toughness and the like to be reduced by directly adding the halogen-free flame retardant into the ABS main material.
Disclosure of Invention
Aiming at the defects in the prior art, the halogen-free flame-retardant high-toughness ABS resin composition containing the nano-scale flame retardant and the preparation method thereof are provided, so that the problems that the existing flame retardant is poor in compatibility and difficult to disperse, and ABS performance is difficult to maintain in a balanced manner are solved.
The purpose of the invention is realized by the following technical scheme.
A halogen-free flame-retardant high-toughness ABS resin containing a nanoscale flame retardant is prepared from the following raw materials in percentage by weight:
the composite flame retardant is one or two compounds of SAN grafted PBL latex microsphere wrapped nano-scale phosphaphenanthrene grafted modified aluminum hydroxide and magnesium hydroxide.
Wherein the content of the first and second substances,
the ABS resin is ABS granules or a compound of ABS powder and SAN.
In order to ensure the compatibility of the composite flame retardant and the ABS resin, the grafting efficiency of the SAN grafted PBL latex microspheres is controlled to be 45-75%, and preferably 50-65%.
The grafting rate of the phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the nano-scale flame retardant is controlled to be 45-70%, and the preferable grafting rate is 55-65%.
The effective content of the nano-level phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the flame-retardant ABS is controlled to be 3-20%, and preferably 5-13%.
Preferably, the lubricant is one or more of stearic acid, zinc stearate or calcium stearate; the dispersing agent is hexane, n-hexane or absolute ethyl alcohol; the antioxidant is one or more of 1010, 1076, DLTP, DSTP and DSTDP.
The invention also provides a preparation method of the halogen-free flame-retardant high-toughness ABS resin composition containing the nano-scale flame retardant, which comprises the following steps:
adding the ABS raw material, the composite flame retardant, the lubricant, the dispersant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Compared with the prior art, the invention has the following advantages:
according to the invention, a certain content of nano-scale phosphaphenanthrene graft modified aluminum hydroxide or magnesium hydroxide coated by SAN graft PBL latex microspheres is selected as a flame retardant, and the nano-scale composite flame retardant coated by the SAN graft PBL latex microspheres not only ensures better compatibility and dispersion of the flame retardant and ABS materials, but also enables the flame retardant to better exert flame retardant efficiency, and the obtained flame retardant ABS has better comprehensive performance. The preparation method and the technical process of the invention are simple, the cost is low, the processing process is stable, and the preparation method is very suitable for industrial production.
Detailed Description
The following examples and comparative examples use raw material information:
ABS is purchased from Qimei, the SAN grafted PBL latex microsphere wrapped nano-scale phosphaphenanthrene grafted modified aluminum hydroxide or magnesium hydroxide is self-made, the lubricant is stearic acid, and the dispersant is absolute ethyl alcohol; the antioxidant is 1010, 1076.
The conventional mechanical property and combustion property test of the flame-retardant ABS resin composition are carried out according to the following standards, and the results are shown in Table 1.
Charpy notched impact strength: according to ISO 179-1: 2010(E) standard test, impact energy 4J;
bending strength: testing according to ISO 178:2010(E) standard, wherein the testing speed is 2 mm/min;
flexural modulus: testing according to ISO 178:2010(E) standard, wherein the testing speed is 2 mm/min;
combustion performance: testing according to UL 94 standard;
the invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 10%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 and 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Example 2
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 10%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 and 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared. .
Example 3
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 10%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 and 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Example 4
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 5%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 or 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Example 5
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 18%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 and 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Comparative example 1
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 30%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 or 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Comparative example 2
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
wherein the flame retardant in the composite flame retardant is phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, the effective content of the flame retardant is controlled to be 1%, the lubricant is stearic acid, the dispersant is absolute ethyl alcohol, and the antioxidant is 1010 and 1076; putting ABS, the composite flame retardant, the lubricant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Comparative example 3
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
putting ABS, aluminum hydroxide with the particle size of 20-50 nm, microencapsulated red phosphorus with the particle size of 500-1000nm, a lubricant, an antioxidant and a dispersant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Comparative example 4
A halogen-free flame-retardant high-toughness ABS resin composition containing a nanoscale flame retardant is prepared from the following raw materials in parts by weight:
adding ABS, phosphaphenanthrene oxide graft modified aluminum hydroxide with the particle size of 20-50 nm, a lubricant, an antioxidant and a dispersant into a high-speed mixer in proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
Table 1 examples/comparative examples test performance
| Examples/comparative examples | Flexural Strength/MPa | Flexural modulus/MPa | Notched impact Strength (KJ/m)2) | Combustion characteristic |
| Example 1 | 67.6 | 2114 | 13.9 | V-0 |
| Example 2 | 67.3 | 2136 | 13.5 | V-0 |
| Example 3 | 66.4 | 2202 | 13.2 | V-0 |
| Example 4 | 66.9 | 2206 | 14.4 | V-0 |
| Example 5 | 67.3 | 2048 | 12.8 | V-0 |
| Comparative example 1 | 68.1 | 2172 | 9.3 | V-0 |
| Comparative example 2 | 68.2 | 2149 | 14.7 | HB |
| Comparative example 3 | 66.7 | 2151 | 6.6 | V-0 |
| Comparative example 4 | 67.5 | 2136 | 7.8 | V-0 |
The result shows that when the effective addition amount of the flame retardant compound is as low as 5 percent, the flame retardant ABS still reaches UL 94V-0 grade, and the notch impact strength is more than 13KJ/m2。
Claims (10)
1. A halogen-free flame-retardant high-toughness ABS resin containing a nanoscale flame retardant is characterized in that: the material is prepared from the following raw materials in percentage by weight:
the composite flame retardant is one or two compounds of SAN grafted PBL latex microsphere wrapped nano-scale phosphaphenanthrene grafted modified aluminum hydroxide and magnesium hydroxide.
2. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 1, wherein: the ABS resin is ABS granules or a compound of ABS powder and SAN.
3. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 1, wherein: in order to ensure the compatibility of the composite flame retardant and the ABS resin, the grafting efficiency of the SAN grafted PBL latex microspheres is controlled to be 45-75%.
4. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 3, wherein: the grafting efficiency of the SAN grafted PBL latex microspheres is controlled to be 50-65%.
5. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 3, wherein: the grafting rate of the phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the nano-scale flame retardant is controlled to be 45-70%.
6. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 5, wherein: the grafting rate of the phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the nano-scale flame retardant is controlled to be 55-65%.
7. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 1, wherein: the effective content of the nano-level phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the flame-retardant ABS is controlled to be 3-20%.
8. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 7, wherein: the effective content of the nano-level phosphaphenanthrene oxide grafted and modified aluminum hydroxide or magnesium hydroxide in the flame-retardant ABS is controlled to be 5-13%.
9. The halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant as claimed in claim 1, wherein: the lubricant is one or more of stearic acid, zinc stearate or calcium stearate; the dispersing agent is hexane, n-hexane or absolute ethyl alcohol; the antioxidant is one or more of 1010, 1076, DLTP, DSTP and DSTDP.
10. The preparation method of the halogen-free flame retardant high-toughness ABS resin composition containing the nanoscale flame retardant according to any one of claims 1 to 9, characterized by comprising the following steps: the method comprises the following steps:
adding the ABS raw material, the composite flame retardant, the lubricant, the dispersant and the antioxidant into a high-speed mixer together according to a proportion, and fully mixing for 1-10 minutes; the materials are sent into a double-screw extruder with the length-diameter ratio of more than or equal to 20, and extruded and granulated at the temperature of 150-250 ℃, so that the halogen-free flame-retardant high-toughness ABS resin containing the nanoscale flame retardant is prepared.
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2020
- 2020-12-09 CN CN202011426270.0A patent/CN112646308A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1810881A (en) * | 2006-03-08 | 2006-08-02 | 四川大学 | Prepn of polyformaldehyde material with polyurethane-base composite fire retardant |
| CN105440564A (en) * | 2015-12-30 | 2016-03-30 | 衢州学院 | Halogen-free and flame-retardant ABS (acrylonitrile butadiene styrene) composite and preparation method thereof |
| CN108623921A (en) * | 2017-03-15 | 2018-10-09 | 中国石油化工股份有限公司 | A kind of EPDM/PP thermoplastic elastic materials and its application |
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| Title |
|---|
| 高平强: "无机纳米硼酸盐复合阻燃材料制备技术", vol. 1, 吉林大学出版社, pages: 40 * |
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