CN116355405A - Low-modulus scale halogen-free flame-retardant reinforced nylon material and preparation method thereof - Google Patents
Low-modulus scale halogen-free flame-retardant reinforced nylon material and preparation method thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- 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
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- 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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2244—Oxides; Hydroxides of metals of zirconium
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34924—Triazines containing cyanurate groups; Tautomers thereof
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/5205—Salts of P-acids with N-bases
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
Abstract
The invention discloses a low-modulus halogen-free flame-retardant reinforced nylon material and a preparation method thereof, belonging to the technical field of high polymer materials. Under the condition of not changing halogen-free flame-retardant components or processing technology, the inorganic zirconium hydroxide with special composition is introduced, the components can fix acidic substances and decomposed small molecular substances, then three special components contained in the inorganic zirconium hydroxide react with the acidic substances generated by decomposing the halogen-free flame-retardant components, so that the nylon resin in the product is prevented from being degraded, the mold scale amount generated in the production injection molding process is reduced, and the tensile strength and the flame retardant performance of the product are not influenced.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-modulus halogen-free flame-retardant reinforced nylon material and a preparation method thereof.
Background
The halogen-free flame-retardant reinforced nylon material generally refers to a nylon material which is prepared by taking halogen-free flame-retardant components as raw materials and matching with reinforcing fillers (such as glass fibers, talcum powder and the like) and has high flame retardance, high strength and environmental friendliness. However, as the halogen-free flame retardant component in the material is easy to generate decomposition reaction and acidic substances in the processing process, the nylon resin serving as a main component is degraded and the service performance of the nylon resin is reduced, and meanwhile, small molecular substances generated by decomposition are continuously enriched in the production injection mold to generate mold scales, so that the purity of the product is reduced, the mold is even required to be cleaned frequently, and the production efficiency is obviously reduced.
In order to solve the problems, attempts are made to reduce the decomposition reaction of the halogen-free flame retardant component and the formation of mold scales by modifying the chemical properties of the halogen-free flame retardant component or introducing an alkaline neutralizer with high compatibility with nylon resin, but the halogen-free flame retardant reinforced nylon material has a limited degree of modification effect due to higher processing temperature, and meanwhile, the polarity of the modified halogen-free flame retardant component is easy and the polarity difference of the reinforced filler is increased, so that the uniformity of each component of the final product is low, and even the mechanical property (especially tensile strength) and flame retardant property of the product are influenced; in addition, attempts have been made to reduce mold deposit formation by stepwise melting based on the original formulation, but such processes are time-consuming and require multiple heating zones, which are energy-intensive.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide a low-mold-scale halogen-free flame-retardant reinforced nylon material, which introduces inorganic zirconium hydroxide with special composition under the condition of not changing halogen-free flame-retardant components or processing technology, the components can fix acidic substances and decomposed small molecular substances, then the acidic substances generated by decomposing the halogen-free flame-retardant components react with the three special components contained in the inorganic zirconium hydroxide, so that the nylon resin in the product is prevented from being degraded, the mold scale amount generated in the production injection molding process is reduced, and the intrinsic tensile strength and the flame retardant performance of the product are not influenced.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the low-modulus non-halogen flame-retardant reinforced nylon material comprises the following components in parts by weight:
40-60 parts of nylon resin, 20-40 parts of glass fiber, 14-20 parts of halogen-free flame retardant, 0.1-1 part of zirconium hydroxide and 0.8-2 parts of processing aid; the zirconium hydroxide is a mixture of isomers including alpha- [ Zr (OH) 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]。
Zirconium hydroxide is a water-insoluble hydroxide with amphoteric properties, which reacts with acidic substances, but which exists in three isomers, alpha- [ Zr (OH), respectively 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]The chemical activity of the three are different due to the difference of crystals, and alpha- [ Zr (OH) is generally adopted 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]The activity decreases in turn, and it is theoretically supposed to be the most active alpha- [ Zr (OH) 4 ]The use effect is optimal, however, in the components of the low-scale halogen-free flame-retardant reinforced nylon material, the thermal decomposition of the halogen-free flame retardant is not performed instantaneously, so that the generated acidic substances or the small molecular substances obtained after the decomposition are continuously increased, and zirconium hydroxide is required to continuously act at a proper adsorption reaction rate. The inventors found that alpha- [ Zr (OH) with step activity was used as the catalyst based on the ratio of the components of the product 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]Together as a modification ofThe sex agent is introduced into the components, so that the long-acting effect can be effectively realized under the condition of lower introduction amount, the stability effect of the product is finally ensured, and meanwhile, the product can not generate a large amount of mold scales in the production injection molding process, and the production efficiency is high. Meanwhile, if the adding amount of zirconium hydroxide is too high, the mechanical property of the product can be influenced, and meanwhile, the fluidity of the nylon material in the injection molding process is increased, so that small molecular substances can not be effectively and stably adsorbed.
In addition, the inventor also found that if other substances (such as aluminum hydroxide) with amphoteric properties are selected as the modifier, the generation amount of mold deposit cannot be reduced, and even the mechanical properties of the product are weakened.
Preferably, the low-modulus halogen-free flame-retardant reinforced nylon material comprises the following components in parts by weight: 45-58 parts of nylon resin, 25-35 parts of glass fiber, 16-18 parts of halogen-free flame retardant, 0.2-0.5 part of zirconium hydroxide and 0.8-2 parts of processing aid.
The introduction condition of nylon resin and glass fiber can influence the initial mechanical strength of the product, the adding amount of the halogen-free flame retardant can determine the probability of subsequent decomposition reaction, the nylon resin and the glass fiber are matched with the adding amount of zirconium hydroxide, and the low-modulus-scale halogen-free flame-retardant reinforcing material prepared by the mixture ratio has better comprehensive effect through screening.
In the invention, the content of the nylon resin in the low-modulus halogen-free flame-retardant reinforced nylon material is not less than 30wt%, and the additive amount meets the raw materials and production requirements of the conventional nylon composite material. Preferably, said α - [ Zr (OH) 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]Is a molar ratio of alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：(0.2～0.4)：(0.15～0.2)。
As described above, due to the activity difference of the three isomers, effective fixation and elimination of side reaction products generated in the whole preparation and production process of the product can be realized, while the total mold deposit generated in the preparation and production injection molding process of the product is minimized at the above ratio.
Preferably, the ratio test method of the three isomers of zirconium hydroxide is as follows: the zirconium hydroxide is kept at 120 ℃ to constant weight in an oven, then a thermogravimetric analyzer is adopted to heat up to 550 ℃ under the air atmosphere, and the component proportion is determined according to the thermal weight loss area and the thermal weight loss rate; wherein alpha- [ Zr (OH) 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]The weight loss rates of the three are 26 to 27 percent, 17.5 to 18.5 percent and 12 to 13 percent respectively; meanwhile, zirconium hydroxide can be directly tested by XRD to obtain a map, and then fitting software is adopted to count the proportion of components according to the difference of characteristic peaks of three isomers.
Preferably, the zirconium hydroxide has an average pore diameter of 2 to 4nm and a particle diameter D50 of 25 to 35 μm.
Preferably, the nylon resin is at least one of hexamethylenediamine adipate copolymer and caprolactam copolymer.
Preferably, the glass fibers have an average diameter of 8 μm to 15 μm.
Preferably, the halogen-free flame retardant is diethyl aluminum phosphinate and melamine polyphosphate according to the mass ratio of (2.5-3.5): 1, and a mixture of the compounds.
It should be noted that the halogen-free flame retardant is not limited to the above-mentioned type, and the low-mold-scale halogen-free flame-retardant reinforced nylon material has good effect on other types of halogen-free flame retardants and can effectively reduce the mold scale of the product.
Preferably, the processing aid is at least one of a lubricant and an antioxidant.
More preferably, the lubricant is at least one of an organosilicon lubricant, an amide lubricant, a stearic acid lubricant and an ester lubricant, and the antioxidant is at least one of a hindered phenol antioxidant and a phosphite antioxidant.
The invention further aims at providing a preparation method of the low-scale halogen-free flame-retardant reinforced nylon material, which comprises the following steps:
and uniformly mixing all components except glass fibers, then adding the components into a double-screw extruder from a main feeding port, adding the glass fibers into a side feeding port, mixing, melting, extruding and granulating to obtain the low-scale halogen-free flame-retardant reinforced nylon material.
Preferably, the temperature of the melt extrusion is 240 to 270 ℃.
The low-scale halogen-free flame-retardant reinforced nylon material disclosed by the invention is free from adopting a special process for production due to an improved formula, is simple in operation steps, and can realize industrial mass production.
The invention also aims to provide an electronic and electric appliance part prepared from the low-modulus halogen-free flame-retardant reinforced nylon material.
The low-mold-scale halogen-free flame-retardant reinforced nylon material can obviously improve the stability of a product under the condition of not obviously reducing the expected mechanical strength by introducing a small amount of special zirconium hydroxide on the premise of not changing the basic formula or the production process of the original nylon resin and the reinforced filler, is particularly suitable for preparing electronic and electric parts with higher requirements on flame retardance, mechanical strength and stability, and has low mold scale produced in the production process.
The invention has the beneficial effects that the invention provides the low-mould-scale halogen-free flame-retardant reinforced nylon material, inorganic zirconium hydroxide with special composition is introduced under the condition of not changing halogen-free flame-retardant components or processing technology, the components can fix acidic substances and decomposed micromolecule substances, then three special components contained in the inorganic zirconium hydroxide react with the acidic substances generated by decomposing the halogen-free flame-retardant components, so that the nylon resin in the product is prevented from being degraded, the mould scale amount generated in the production injection molding process is reduced, and the tensile strength and flame retardant performance of the product are not influenced.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and the object of the present invention is to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents and instruments involved in the practice of the present invention are common reagents and instruments unless otherwise specified.
Examples 1 to 11
In the embodiment of the low-modulus non-halogen flame-retardant reinforced nylon material, the components of the low-modulus non-halogen flame-retardant reinforced nylon material are shown in the table 1.
The preparation method of the product comprises the following steps:
uniformly mixing all components except glass fibers, then adding the components into a double-screw extruder from a main feeding port, adding the glass fibers into a side feeding port, mixing, melting, extruding and granulating to obtain the low-scale halogen-free flame-retardant reinforced nylon material; the temperature of the melt extrusion is 240-270 ℃.
Comparative examples 1 to 5
The comparative examples differ from the examples only in the kinds and proportions of the components, as shown in Table 2.
Among the components described in each example and comparative example,
nylon resin 1: adipic acid hexamethylenediamine copolymer, infludary Nylon chemical Co., ltd., PA 66U 3600;
nylon resin 2: caprolactam copolymer, PA 6M 2800, available from guangdong new merda chinlon, inc;
glass fiber: 584 type fiber produced by China boulder Co., ltd., average diameter 11 μm;
halogen-free flame retardant 1: the compound: aluminum diethylphosphinate (OP-1230, clariant chemical company, limited) and melamine polyphosphate (Budenheim, BUDIT 3141) are compounded according to a mass ratio of 3:1;
halogen-free flame retardant 2: melamine cyanurate (MCA-F, institute of fine chemical engineering, tetrac);
an antioxidant: a mixture of commercially available hindered phenol antioxidants and phosphite antioxidants according to a mass ratio of 1:1;
and (3) a lubricant: commercially available silicone-based lubricants;
the zirconium hydroxide 1-3 and 5 are all from Jiangxi Jing An high-tech Co., ltd;
zirconium hydroxide 1: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：0.3：0.18；
Zirconium hydroxide 2: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：0.2：0.2；
Zirconium hydroxide 3: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：0.4：0.15；
Zirconium hydroxide 4: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝0.5：1：0.2；
Zirconium hydroxide 5: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：0.5：0.1；
Zirconium hydroxide 6: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：1：0；
Zirconium hydroxide 7: alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：0：0；
Aluminum hydroxide: luoyang Zhongfu, AH-01DG.
The raw materials of the components used in each example and comparative example of the present invention are all commercially available raw materials, and the raw materials of the components used in each parallel experiment are the same, unless otherwise specified. Meanwhile, the zirconium hydroxide 1-3 and the zirconium hydroxide 5 are all commercial products in practice, and the content ratio of the isomers in the products is different due to the difference of the products among batches; zirconium hydroxide 4, 6 and 7 are self-made products, an acid solution of a zirconium source is adopted to react in an ammonia water environment, zirconium hydroxide with different crystal forms is separated out through adjusting the pH value of the solution, and then the zirconium hydroxide is ground, sieved and combined, and the method is referred to in the prior art, namely, preparation of powdery zirconium hydroxide, rare metal express, wang Zebin and the like. The inventor confirms that products distributed in different proportions are subjected to example/comparative example implementation and test by adopting an isomer analysis method and a thermal weightlessness method; the average pore diameter of the zirconium hydroxide is 2-4 nm, and the particle diameter D50 is 25-35 mu m. .
TABLE 1
TABLE 2
Effect example 1
In order to verify the performance of the products according to the invention, the following performance tests were carried out on the products of the examples and comparative examples, in particular with the following steps:
(1) And (3) testing the mold scale: continuously injecting the products into the mold for 200 times at the injection temperature of 280-300 ℃, and then collecting the scale on the mold for weighing;
(2) Tensile strength test: according to GB/T1040.1-2018, products are injection molded into I-shaped tensile bars for testing, and the testing conditions are as follows: the stretching rate is 10mm/min;
(4) Flame retardant rating: the materials of the examples and comparative examples were tested for vertical burn performance according to GB/T2408-2008 standard, with test bars having a thickness of 0.8mm, and the flame retardant grade being classified into V-0 grade, V-1 grade, V-2 grade and no grade.
The test results are shown in tables 3 and 4.
TABLE 3 Table 3
TABLE 4 Table 4
As can be seen from tables 3 and 4, compared with the comparative example 1 product of the original formulation, the low-scale halogen-free flame retardant reinforced nylon material of the embodiments of the invention has no influence on tensile strength (more than 100MPa is still reserved) and flame retardant property, and meanwhile, the residual scale amount after 200 times of mold injection is reduced from 2.30mg of comparative example 1 to less than 1.5mg, which indicates that the product effectively solves the negative influence caused by decomposition of flame retardant components of the existing product, and the product has better stability. While comparing the products according to examples 1-5, when the product components are preferably: 45-58 parts of nylon resin, 25-35 parts of glass fiber, 16-18 parts of halogen-free flame retardant, 0.2-0.5 part of zirconium hydroxide and 0.8-2 parts of processing aid. As can be seen from comparative examples 1 and examples 7 to 10 and comparative examples 3 to 5, when zirconium hydroxide in the product is replaced with similar other hydroxide species, the product is difficult to achieve good stability, the problem of mold deposit cannot be solved, and even intrinsic tensile strength may be affected, and when zirconium hydroxide is introduced, if the collocation of three isomers cannot be achieved, the product is also difficult to achieve the expected effect; while the ratio of the three isomers was maintained at 1: (0.2-0.4): in the range of (0.15-0.2), the mold deposit yield of the product is the lowest. However, when the amount of zirconium hydroxide added is too large, the performance of the product is lowered again as shown in comparative example 2.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The low-modulus non-halogen flame-retardant reinforced nylon material is characterized by comprising the following components in parts by weight:
40-60 parts of nylon resin, 20-40 parts of glass fiber, 14-20 parts of halogen-free flame retardant, 0.1-1 part of zirconium hydroxide and 0.8-2 parts of processing aid; the zirconium hydroxide is a mixture of isomers including alpha- [ Zr (OH) 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]。
2. The low-modulus halogen-free flame retardant reinforced nylon material according to claim 1, which is characterized by comprising the following components in parts by weight: 45-58 parts of nylon resin, 25-35 parts of glass fiber, 16-18 parts of halogen-free flame retardant, 0.2-0.5 part of zirconium hydroxide and 0.8-2 parts of processing aid.
3. The low-modulus, halogen-free, flame retardant, reinforced nylon material of claim 1, wherein the α - [ Zr (OH) 4 ]、β-[Zr 4 O 2 (OH) 12 ]And gamma- [ Zr 4 O 4 (OH) 8 ]Is a molar ratio of alpha- [ Zr (OH) 4 ]：β-[Zr 4 O 2 (OH) 12 ]：γ-[Zr 4 O 4 (OH) 8 ]＝1：(0.2～0.4)：(0.15～0.2)。
4. The low-mold-scale halogen-free flame-retardant reinforced nylon material according to claim 1, wherein the nylon resin is at least one of hexamethylenediamine adipate copolymer and caprolactam copolymer.
5. The low-scale halogen-free flame retardant reinforced nylon material of claim 1, wherein the glass fiber has an average diameter of 8 μm to 15 μm.
6. The low-modulus halogen-free flame-retardant reinforced nylon material according to claim 1, wherein the halogen-free flame retardant is diethyl aluminum phosphinate and melamine polyphosphate according to the mass ratio of (2.5-3.5): 1, and a mixture of the compounds.
7. The low-modulus halogen-free flame retardant reinforced nylon material according to claim 1, wherein the processing aid is at least one of a lubricant and an antioxidant.
8. The method for preparing the low-scale halogen-free flame retardant reinforced nylon material according to any one of claims 1 to 7, which is characterized by comprising the following steps:
and uniformly mixing all components except glass fibers, then adding the components into a double-screw extruder from a main feeding port, adding the glass fibers into a side feeding port, mixing, melting, extruding and granulating to obtain the low-scale halogen-free flame-retardant reinforced nylon material.
9. An electronic and electrical component made from the low mold-scale halogen-free flame retardant reinforced nylon material of any one of claims 1-7.
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