CN113201217B - Dark flame-retardant nylon and preparation method thereof - Google Patents
Dark flame-retardant nylon and preparation method thereof Download PDFInfo
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- CN113201217B CN113201217B CN202110555299.7A CN202110555299A CN113201217B CN 113201217 B CN113201217 B CN 113201217B CN 202110555299 A CN202110555299 A CN 202110555299A CN 113201217 B CN113201217 B CN 113201217B
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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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Abstract
The invention discloses a dark flame-retardant nylon and a preparation method thereof, belonging to the field of nylon material reinforcement. According to the nylon product, the specific hyperbranched lubricant is added into the components, so that the fusion property among the components can be effectively enhanced, the connection between the glass fiber and the resin is more compact, and the phenomenon of fiber floating is inhibited; through the precursor ultrasonic crushing treatment of the lubricant and the pigment, the pigment can be more uniformly distributed in the mixing process, the coloring capability of the final product can be still ensured even if a large content of flame retardant is introduced into the components, and the condition of pigment precipitation cannot occur. The invention also discloses a preparation method of the dark flame-retardant nylon, which has simple operation steps and can realize industrialized large-scale products.
Description
Technical Field
The invention relates to the field of nylon material reinforcement, in particular to a dark flame-retardant nylon and a preparation method thereof.
Background
PA6, also known as nylon 6, is widely used in industrial products due to its excellent strength and resistance, good processability and extremely high thermal stability. In the prior art, the PA6 is enhanced and modified by the multi-purpose glass fiber, so that the product has higher strength, but in the periphery of heating elements of some electric tools and in industrial electrical aspects, the product is required to have certain flame retardant performance, and some products even require the flame retardant grade of the material to reach V0. Therefore, a large amount of flame retardant is added into the nylon materials, however, the mutual fusion of the pigment, the glass fiber and the PA6 resin is hindered, the insufficient fusion of the glass fiber and the PA6 resin causes serious fiber floating on the surface of the product, and the insufficient fusion of the pigment and the PA6 resin causes the coloring capacity of the pigment to be reduced (taking a dark blue product as an example, the product defects are particularly represented by larger L value and B value); in addition, after the products are continuously injected for a period of time, pigments are separated out and adhered to the surface of a mold, so that the injection molding efficiency of the products is reduced.
Disclosure of Invention
Based on the defects in the prior art, the invention aims to provide the dark flame-retardant nylon, and the product not only improves the coloring capability of toner in the components by special component selection and treatment, but also fully fuses the components, thereby solving the problems of toner precipitation and surface floating fiber of the conventional flame-retardant nylon product.
In order to achieve the purpose, the invention adopts the technical scheme that:
the dark flame-retardant nylon comprises the following components in parts by weight:
42-44 parts of PA6 resin, 30-35 parts of glass fiber, 20-30 parts of flame retardant, 0.15-0.25 part of antioxidant and 0.3-0.6 part of lubricant; the nylon also comprises a pigment, wherein the pigment comprises 0.25-0.35 part of white toner and 1.5-1.7 parts of dark toner; the pigment and the lubricant are subjected to ultrasonic crushing treatment, and the lubricant is a hyperbranched lubricant.
In the components of the dark flame-retardant nylon, the specific hyperbranched lubricant is added, so that the fusion property among the components can be effectively enhanced, the connection between glass fiber and resin is more compact, and the phenomenon of fiber floating is inhibited; by the ultrasonic crushing of the lubricant and the pigment, the pigment can be more uniformly distributed in the mixing process, the coloring capability of the final product can be still ensured even if a flame retardant with large content is introduced into the components, and the condition of pigment precipitation cannot occur.
Preferably, the hyperbranched lubricant comprises hydroxyl-terminated polyesters of hyperbranched structure;
more preferably, the hyperbranched lubricant is a wuhan hyperbranched resin HyPer C100.
The HyPer C100 lubricant has hydroxyl-terminated polyester with a hyperbranched structure, and a special structure of the HyPer C100 lubricant can penetrate into the interior of a molecular chain, so that the acting force among the molecular chains is reduced, the molecular chain is driven to move rapidly, the processing temperature is reduced, the melt index is improved, the filler consumption is increased, the cost is reduced, and the fiber floating phenomenon is eliminated; the component has strong wetting ability, can be fully compatible with the components in the nylon, avoids the precipitation of the components, particularly the pigment, and simultaneously keeps the original mechanical property.
Preferably, the weight part of the lubricant is 0.4-0.5 part.
The lubricant in the optimal range can fully fuse all components in the product, and the phenomena of pigment precipitation and fiber floating are avoided after the product is prepared.
Preferably, the frequency of the ultrasonic crushing treatment is 24-26 kHz, and the treatment time is 3.5-4.5 h.
More preferably, the particle size of the coloring material and the lubricant after ultrasonic crushing treatment is less than or equal to 200 nm.
The lubricant and the pigment under the particle size can be fully fused with the resin and the glass fiber, and the prepared product has more stable property.
Preferably, the glass fiber is a chopped glass fiber, and the length of the chopped glass fiber is 3-25 mm.
The chopped glass fiber has low impurity content and excellent dry-state fluidity, can be effectively combined with each component and uniformly distributed in the preparation process of the nylon, and effectively improves the mechanical property of the product.
More preferably, the glass fiber is selected from Chongqing glass fiber ECS301 HP-3-H.
The product has high fiber uniformity, can be effectively combined with resin, fully improves the mechanical and stability performance of the whole material, and reduces the occurrence of fiber floating phenomenon.
Preferably, the flame retardant comprises brominated polystyrene.
Preferably, the antioxidant comprises at least one of amine antioxidants, hindered phenol antioxidants and phosphite antioxidants.
More preferably, the antioxidant is antioxidant 1098.
The antioxidant with the content can effectively inhibit the natural oxidation of the nylon product in a wet environment, and further ensures the strong colorability of the product. Preferably, the antioxidant 1098 is a high-performance general antioxidant which is free from color change, pollution and thermal oxidation, can be effectively combined with pigments and glass fibers in the nylon component, and is not easy to deteriorate.
Preferably, the white powder comprises zinc sulfide.
Preferably, the dark toner is a mixture of carbon black, anthraquinone blue 38 and anthraquinone violet 03; more preferably, in the dark color toner, the mass ratio of the carbon black, the anthraquinone blue 38 and the anthraquinone violet 03 is carbon black: anthraquinone blue 38: anthraquinone violet 03 ═ 3:4: 6.
The invention also aims to provide a preparation method of the dark flame-retardant nylon, which comprises the following steps: and (3) stirring and mixing the lubricant and the pigment after ultrasonic crushing treatment, uniformly mixing the lubricant and the pigment with other components according to the proportion, melting, extruding and granulating to obtain the dark flame-retardant nylon.
The preparation method of the dark flame-retardant nylon has simple operation steps and can realize industrialized large-scale products.
Preferably, the stirring time is 20-25 min, and the melting temperature is 220-240 ℃.
The invention has the beneficial effects that the invention provides the dark flame-retardant nylon, and the product can effectively enhance the fusion property among the components by adding the specific hyperbranched lubricant into the components, promote the connection between the glass fiber and the resin to be more compact and inhibit the phenomenon of fiber floating; through the ultrasonic crushing treatment of the lubricant and the pigment, the pigment can be more uniformly distributed in the mixing process, the coloring capacity of the final product can be still ensured even if a flame retardant with large content is introduced into the components, and the condition of pigment precipitation cannot occur. The invention also provides a preparation method of the dark flame-retardant nylon, which has simple operation steps and can realize industrialized large-scale products.
Detailed Description
In order to better illustrate the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to specific examples and comparative examples, which are intended to be understood in detail, but not intended to limit the invention. All other embodiments obtained by a person skilled in the art without making any inventive step are within the scope of protection of the present invention. The experimental reagents and instruments designed for the practice of the present invention and the comparative examples are common reagents and instruments unless otherwise specified.
Examples 1 to 4
According to the embodiment of the dark flame-retardant nylon, the preparation method of the product comprises the following steps:
and (3) placing the lubricant and the coloring material into an ultrasonic cell crusher, crushing at the normal temperature at the frequency of 25kHz for 4 hours until the particle size is less than or equal to 200nm, mixing and stirring for 20min, then uniformly mixing with other components in proportion, transferring into a double-screw extruder, melting and blending at 230 ℃, extruding and granulating to obtain the dark flame-retardant nylon.
The raw materials used in the examples are as follows, and the proportions of the raw materials are shown in Table 1.
PA6 resin: high viscosity PA6 resin, designation HY-2800;
glass fiber: the glass fiber is chopped, the length of the chopped glass fiber is 3-25 mm, and the Chongqing glass fiber is ECS301 HP-3-H;
antioxidant: an antioxidant 1098;
flame retardant: brominated polystyrene, trade name XZ 6700;
lubricant 1: wuhan hyper branched HyperC 100;
and lubricant 2: a honievir product, lubricant-a-C540A, which does not contain hydroxyl-terminated polyester with hyperbranched structure, nor is a hyperbranched lubricant;
white powder: zinc sulfide;
dark color powder: carbon black, a mixture of anthraquinone blue 38 and anthraquinone violet 03 (carbon black: anthraquinone blue 38: anthraquinone violet 03: 3:4: 6).
Comparative examples 1 to 4
The products described in comparative examples 1 to 4 are different from the products described in examples 1 to 4 only in the formula or the mixture ratio of the component raw materials, and the mixture ratio of the raw materials is shown in table 1.
Comparative examples 5 to 8
The products of comparative examples 5 to 8 are different from the products of examples 1 to 4 only in the formula or the mixture ratio of the component raw materials, and the pigments and the lubricants are not subjected to ultrasonic crushing treatment in the preparation process of the products, and the mixture ratio of the raw materials is shown in table 1.
Example 5
The difference between this example and example 1 is only that the ultrasonication treatment was carried out for 2 hours, and the particle diameters of the lubricant and the coloring material after the treatment were > 200nm (particle diameter distribution: 500nm to 5 μm).
TABLE 1
Effect example 1
In order to verify the reinforcing performance of the nylon obtained in the examples of the present invention, the performance of the nylon obtained in the examples 1 to 5 and the nylon obtained in the comparative examples 1 to 8 was characterized by injection molding with a single screw injection molding machine to form a 4cm x 6cm x 2mm color plate, and the test results are shown in table 2, and the test items and methods are shown below.
The test method comprises the following steps:
(1) the coloring performance is as follows: the L value and B value of the color plate were measured by an Alice 7000A color difference meter (the smaller the two values, the higher the tinting strength of the pigment in the resulting product is indicated);
(2) pigment precipitation: after the material particles are continuously injected into a 50-mold, wiping the mold by alcohol cotton, and judging the precipitation condition of the material during continuous injection molding according to the color of the alcohol cotton; the precipitation conditions are divided into three grades: no, mild, severe; wherein, no indicates that the original color is kept after the alcohol cotton is wiped; "slight" means that the alcohol cotton is stained with other colors after being wiped, but the natural color and the dyeing can still be distinguished; "serious" means that the color of the alcohol cotton is changed seriously after the alcohol cotton is wiped, and the natural color and dyeing of the alcohol cotton cannot be distinguished.
(3) Fiber floating condition: observing the condition of fiber floating on the surface of the color plate visually; the floating fiber condition is divided into three grades: none, mild, severe; wherein, none indicates that the surface of the color plate has no fiber floating phenomenon; "slight" means that less than 20 floating fibers are present on the surface of the color plate; "severe" means more than 20 floating fibers are present on the surface of the panel.
TABLE 2
As can be seen from table 2, the example products prepared by the preferred formulation and treatment method have better coloring ability than the comparative example products, and the pigment precipitation and fiber floating phenomenon thereof are significantly reduced; the performance of the products obtained in the examples 1 and 2 is optimal, and the phenomena of precipitation and fiber floating are not generated.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (6)
1. The dark flame-retardant nylon is characterized by comprising the following components in parts by weight:
42-44 parts of PA6 resin, 30-35 parts of glass fiber, 20-30 parts of flame retardant, 0.15-0.25 part of antioxidant and 0.4-0.5 part of lubricant; the nylon also comprises a pigment, wherein the pigment comprises 0.2 part of white toner and 1.5-1.7 parts of dark toner; the white toner is zinc sulfide, and the dark toner is a mixture of carbon black, anthraquinone blue 38 and anthraquinone violet 03; the mass ratio of the carbon black to the anthraquinone blue 38 to the anthraquinone violet 03 is 3:4: 6; the lubricant is hydroxyl-terminated polyester with a hyperbranched structure; the pigment and the lubricant further comprise the following treatment: putting the lubricant and the pigment into an ultrasonic cell crusher, carrying out ultrasonic crushing treatment until the particle size is less than or equal to 200nm, and mixing and stirring.
2. The dark flame retardant nylon of claim 1, wherein the ultrasonication treatment frequency is 24 to 26kHz and the treatment time is 3.5 to 4.5 hours.
3. The dark flame retardant nylon of claim 1, wherein the glass fibers are chopped glass fibers having a length of 3 to 25 mm.
4. The dark flame retardant nylon of claim 1, wherein the antioxidant comprises at least one of an amine antioxidant, a hindered phenol antioxidant, and a phosphite antioxidant.
5. The preparation method of the dark flame-retardant nylon according to any one of claims 1 to 4, which is characterized by comprising the following steps: and (3) placing the lubricant and the pigment into an ultrasonic cell crusher, performing ultrasonic crushing treatment, stirring and mixing, uniformly mixing with other components according to a ratio, melting, extruding and granulating to obtain the dark flame-retardant nylon.
6. The method for preparing the dark flame-retardant nylon according to claim 5, wherein the stirring time is 20-25 min, and the melting temperature is 220-240 ℃.
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| CN113999497B (en) * | 2021-10-25 | 2023-09-26 | 金发科技股份有限公司 | Organic black powder composition and preparation method and application thereof |
| CN114182365A (en) * | 2021-12-13 | 2022-03-15 | 浙江宝力特种丝业有限公司 | Production process of high-modulus low-shrinkage polyester monofilament |
| CN116496619B (en) * | 2023-05-10 | 2024-05-14 | 金发科技股份有限公司 | Red nylon composite material and preparation method and application thereof |
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| WO2007135032A2 (en) * | 2006-05-23 | 2007-11-29 | Basf Se | Use of hyperbranched polycarbonates as a dispersing agent for pigments |
| CN103087517A (en) * | 2013-02-20 | 2013-05-08 | 上海俊尔新材料有限公司 | Glass-reinforced nylon 6 material and preparation method thereof |
| CN104212239B (en) * | 2014-09-04 | 2016-06-29 | 江南大学 | The method that the multi-functional hyperbranched dispersant of a kind of use improves paint ink color fixation fastness |
| CN104211849B (en) * | 2014-09-04 | 2016-09-07 | 江南大学 | A kind of preparation method of hyperbranched Multi-functional dispersion agent |
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| CN108587133A (en) * | 2018-05-02 | 2018-09-28 | 合肥卡洛塑业科技有限公司 | A kind of anti-electrostatic fire retardant PA Masterbatch and preparation method thereof |
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