CN114806159A - Flame-retardant moisture-absorbing nylon composite material and preparation method thereof - Google Patents
Flame-retardant moisture-absorbing nylon composite material and preparation method thereof Download PDFInfo
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- CN114806159A CN114806159A CN202210502747.1A CN202210502747A CN114806159A CN 114806159 A CN114806159 A CN 114806159A CN 202210502747 A CN202210502747 A CN 202210502747A CN 114806159 A CN114806159 A CN 114806159A
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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
- C08K5/529—Esters containing heterocyclic rings not representing cyclic esters of phosphoric or phosphorous acids
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
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Abstract
The invention discloses a flame-retardant moisture-absorption nylon composite material and a preparation method thereof, wherein the flame-retardant moisture-absorption nylon composite material is prepared from nylon, melamine polyphosphate, glass fiber and purified water sludge by adopting a screw extruder; the amount of the melamine polyphosphate is 5-18% of the mass of the nylon. According to the invention, under the technical idea of blending flame-retardant nylon, the flame retardant is matched with the auxiliary flame retardant, namely purified water sludge, so that the moisture absorption performance of the nylon can be maintained while the flame retardance is improved.
Description
Technical Field
The invention belongs to a plastic modification technology, and particularly relates to a flame-retardant moisture-absorbing nylon composite material and a preparation method thereof.
Background
Polyamides are linear polymers having a main chain of a molecule containing a repeating amide group, and among them, polyamides having an aliphatic main chain are called nylons, and are the earliest synthetic fibers to be industrially used. The nylon has certain flame retardant property, but in the industries such as fabrics and the like with high requirements on the flame retardance of materials, the flame retardant property of the nylon cannot meet the existing use requirements. The prior art finds that the nylon material containing glass fiber is easy to generate the candle wick effect and is easier to burn when burning, and the conventional glass fiber reinforced modified nylon material can not meet the requirement of flame retardant application.
The textile is applied to clothing household and industrial production, agriculture, forestry, animal husbandry, fishery, medical construction, energy conservation, environmental protection, transportation and the like, and the textile is very easy to ignite during combustion due to the large surface area and can generate a large amount of melting, dripping and smog. As a common sense, combustible substances, a heat source and oxygen are essential three elements for combustion, flame retardance of a polymer is mainly started from the three aspects, oxygen is isolated, and the possibility of combustion is reduced to the minimum. Compared with other methods, the existing textile flame retardance comprises a copolymerization method, a blending method, a sheath-core composite spinning method and a flame-retardant post-finishing method, and has the advantages of poor durability, complex preparation, convenience in operation of the blending method and no change of the spinning process.
The nylon fiber has excellent rebound resilience, particularly has higher wear resistance compared with natural fibers, although the hygroscopicity of the nylon fiber is not higher than that of natural fibers such as cotton and hemp, the nylon fiber has the best hygroscopicity in synthetic fibers and has certain microbial resistance, so the nylon fiber has very wide application direction; but the moisture absorption performance is reduced while the flame retardant performance is improved by combining the existing blending flame retardant modification. In the prior art, after vermiculite is subjected to sodium modification and organic modification, a nylon 610/vermiculite nano composite material is prepared by a melt blending method, and the barrier flame retardant property of the composite material is researched; research results show that the water vapor permeability rate and the water absorption rate of the nylon 610/vermiculite composite material are remarkably reduced along with the increase of the content of vermiculite, when the mass fraction of the vermiculite is 5%, the water vapor permeability rate capacity of the composite material is only 39.4% of that of nylon 610, the water absorption rate is 55% of that of the nylon 610, and the addition of the vermiculite remarkably improves the barrier property of the nylon 610. In the prior art, hydroxide is selected as a main flame retardant, inorganic mineral is selected as a synergistic flame retardant, inorganic glass fiber is selected as a reinforcing agent, POE-G-MAH is selected as a toughening agent, and the halogen-free flame retardant reinforced nylon 612 composite material is successfully prepared; the experimental result proves that the material can well meet the requirement of the field of electronic and electric appliances on the flame retardant property, and simultaneously, the saturated water absorption rate is also controlled due to the molecular structure of the material.
Disclosure of Invention
The moisture absorption is one of indexes of physical properties of fibers, and the degree of hydrophilicity and hydrophobicity to water is considered, and PA6 and PA66 are used as the most commonly used polyamide materials, and have good moisture absorption capacity because the molecular structures contain hydrophilic amide groups, so that the polyamide materials are different from plastics such as polyformaldehyde, polycarbonate and ABS. In the prior art, glass fiber and inorganic mineral are used as main means for blending and flame retarding, and the water absorption performance of nylon is reduced, so that the method is favorable for some engineering applications, but is unfavorable for the application utilizing the water absorption performance. According to the invention, under the technical idea of blending flame retardant nylon, the flame retardant is matched with the auxiliary flame retardant, namely the purified water sludge, so that the moisture absorption performance of the nylon can be maintained while the flame retardant is improved.
The invention adopts the following technical scheme:
a flame-retardant moisture-absorbing nylon composite material comprises nylon, a phosphorus-nitrogen flame retardant, glass fiber and purified water sludge; the phosphorus-nitrogen flame retardant is melamine polyphosphate; the amount of the melamine polyphosphate is 5-18% of the mass of the nylon. Preferably, the weight of the nylon is 100%, the weight of the melamine polyphosphate is 10-15%, the weight of the glass fiber is 2-4%, and the weight of the water purification sludge is 0.5-1.5%. More preferably, the weight of the nylon is 100%, the weight of the melamine polyphosphate is 11-12%, the weight of the glass fiber is 2-3%, and the weight of the water purification sludge is 1.0-1.3%.
In the invention, the nylon is one or more of PA6, PA11, PA12, PA46, PA66, PA610, PA612 and PA 1010. The preparation method comprises the following steps of melting and mixing nylon, melamine polyphosphate, glass fiber and purified water sludge to obtain the flame-retardant moisture-absorbing nylon composite material, wherein the specific preparation method is the prior art, such as screw extrusion. It is known that the combustion process of polymers, firstly heat is supplied by an external heat source, so that the temperature of the polymers is raised, softening, creep or deformation and the like occur, further more heat is released, chemical bonds begin to break, small molecules are released, combustion is carried out in the presence of oxygen, a decomposition reaction is initiated in a solid phase, and the combustion is accelerated and circulated. Flame retardants are functional additives that retard or retard the polymer combustion process by physical or chemical action, thereby extinguishing or slowing the flame daughter-in-law. The invention adopts melamine polyphosphate as a main flame retardant, has good stability, low cost and low toxicity, is heated and decomposed into flame retardant gas, blocks the action of a fire element and oxygen, and combines glass fiber and water purification sludge to modify nylon from a combustible material into a flame retardant material. In addition, the glass fiber is beneficial to improving the strength of nylon, and particularly, the moisture absorption performance of the nylon is unexpectedly maintained by adding the purified water sludge.
In the invention, the flame-retardant moisture-absorbing nylon composite material can be directly used for preparing corresponding flame-retardant materials, and can also be used for preparing the required flame-retardant materials together with conventional additives such as dispersing agents and the like, which is the application common knowledge in the field, but the invention does not adopt other resins or plastics as raw materials. Through customer experiments, the flame-retardant moisture-absorbing nylon composite material disclosed by the invention has spinnability and can be used as a spinning raw material.
The flame retardance is realized by a reactive flame retardant and an additive flame retardant, the reactive flame retardant is taken as a monomer to participate in reaction and is combined on a nylon main chain or a side chain, so that the advantage of good flame retardance stability is brought, for example, in the process of polymerization of hexamethylene diamine and adipic acid, a flame retardant bis (2-carboxyethyl) methylphosphine oxide (CEMPO) is added to prepare flame-retardant PA plastic in a literature report, the flame-retardant PA plastic has better flame retardance compared with common PA66, the LOI is improved to a certain extent, but the processing technology is complex, the cost is high, and the flame-retardant PA plastic is unfavorable for common industrial production; the mechanical blending mixes the flame retardant and the nylon, accords with the conventional double-screw extrusion process, is easy to control, has low cost and is suitable for conventional flame-retardant nylon. The combustion process is a very complex process, and the flame retardance of polymers is often the combined action of the two flame retardant mechanisms. With the improvement of the flame-retardant requirement of polymers, a synergistic flame-retardant system is widely applied. According to the invention, the nylon has a certain flame retardant effect, melamine polyphosphate is adopted as a main flame retardant to combine with the glass fiber and the water purification sludge, and the proper flame retardant property is displayed under the combined action, and the flame retardant effect is far greater than the sum of the flame retardant effects of single components.
Drawings
FIG. 1 shows the oxygen index at different ratios in the examples.
FIG. 2 shows water absorption ratios at different ratios in the examples.
Detailed Description
The water purification sludge has the general characteristics of soil, namely caking property, mainly takes inorganic matters as main materials, and researches show that the aluminum iron hydroxide in the water purification sludge exists in an amorphous state, the main components of the water purification sludge are minerals such as quartz, muscovite, kaolin and the like, and the water purification sludge does not contain harmful metals or has very low content (see the properties and resource utilization of the water purification sludge). The direct discharge of waterworks sludge will have a number of adverse effects on the quality of water sources in towns near waterworks and on the daily lives of residents. At present, the purified water sludge is mainly prepared into functional materials such as ceramics, buildings and the like and agricultural fertilizers by improving and improving the components and properties of the purified water sludge through chemical, physical, biological and other methods, and useful components are extracted from the purified water sludge and converted into available resources, and a disposal mode of removing toxic and harmful ions in wastewater by using the purified water sludge to prepare an adsorbent is one of research hotspots (see the purified water sludge dewatering efficiency and resource utilization research).
For nylon flame retardation enhancement, the conventional blended flame retardants comprise halogen flame retardants, phosphorus flame retardants, nitrogen flame retardants and inorganic flame retardants; the halogen flame retardant releases strong carcinogenic substances such as kaempe and benzofuran after combustion, and is eliminated gradually. The invention selects the melamine polyphosphate with low toxicity and low cost as the main flame retardant, combines the glass fiber and the water purification sludge, realizes the technical effect of flame retardancy, and simultaneously maintains the moisture absorption capacity of the nylon. The raw materials are conventional materials, PA6 is made from plastic (unmodified) of hundred million Cisco in Dongguan, melamine polyphosphate is made from star flame retardant, glass fiber is giant stone 910, the length is about 1mm, and the purified water sludge is the purified water sludge of Suzhou water works, which is calcined at 500 ℃ for 3 hours after being cleaned and dried, and is crushed to 50-100 micrometers, particularly from Suzhou colleges and universities. The specific preparation method and the test method disclosed by the invention are conventional technologies in the field, the raw materials are dried conventionally before being added into an extruder, a JF-5 touch screen control full-automatic oxygen index tester is adopted to measure the oxygen index, a sample strip of 50mm multiplied by 10mm multiplied by 3mm is soaked in water at 40 ℃ for 2 hours, the weight before and after soaking is tested, and the increment/initial weight is the water absorption rate and is expressed in percentage.
In the embodiment, a product is prepared by nylon, melamine polyphosphate, glass fiber and purified water sludge, the raw materials are dried and then added into a double-screw extruder, the temperature from a feed inlet to a machine head is 210 ℃, 220 ℃, 235 ℃, 240 ℃, 235 ℃, 230 ℃ and 230 ℃ in sequence, the flame-retardant moisture-absorbing nylon composite material is obtained by extrusion, and then a test sample strip is prepared by a plate vulcanizer at 5 MPa. The results are shown in FIG. 1 and FIG. 2. The extrusion parameters can be adjusted according to the nylon material, and the method is a conventional technology.
Example one
Adding dried nylon 6, melamine polyphosphate and synergistic flame retardant water purification sludge into a high-speed stirrer in proportion, stirring at the speed of 280 rpm for 3 min, and discharging to obtain a premix; and adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material.
Example two
Adding dried nylon 6, melamine polyphosphate and synergistic flame retardant water purification sludge into a high-speed stirrer in proportion, stirring at the speed of 280 rpm for 3 min, and discharging to obtain a premix; and adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material.
EXAMPLE III
Adding dried nylon 6, melamine polyphosphate and synergistic flame retardant water purification sludge into a high-speed stirrer in proportion, stirring at the speed of 280 rpm for 3 min, and discharging to obtain a premix; and adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material.
Example four
Adding dried nylon 6, melamine polyphosphate and synergistic flame retardant water purification sludge into a high-speed stirrer in proportion, stirring at the speed of 280 rpm for 3 min, and discharging to obtain a premix; and adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material.
Comparative example 1
The raw materials are 100Kg of dried PA6, 12Kg of melamine polyphosphate and 2.5Kg of glass fiber, the same process as the examples is adopted, the premix is added into a double screw extruder hopper, the glass fiber is fed, and then the flame retardant nylon composite material is obtained after extrusion, cooling, grain cutting and packaging, and the water absorption rate is 0.832%.
Comparative example No. two
The raw materials are 100Kg of dried PA6, 12Kg of melamine, 2.5Kg of glass fiber and 1.0 Kg of purified water sludge, the same process as the embodiment is adopted, the premix is added into a double screw extruder hopper, the glass fiber is fed, and then the flame retardant nylon composite material is obtained after extrusion, cooling, grain cutting and packaging, and the water absorption rate is 0.905%.
Comparative example No. three
The raw materials are 100Kg of dried PA6, 12Kg of melamine polyphosphate, 2.5Kg of glass fiber and 1.0 Kg of magnesium hydroxide (Yabao), the same process as the example is adopted, the premix is added into a double screw extruder hopper, the glass fiber is fed, and then the flame retardant nylon composite material is obtained after extrusion, cooling, grain cutting and packaging, and the water absorption rate is 0.805%.
EXAMPLE five
Adding dried nylon 6, melamine polyphosphate and synergistic flame retardant water purification sludge into a high-speed stirrer according to the proportion of the second embodiment, stirring at the speed of 350 rpm for 2min, and discharging to obtain a premix; adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material, and maintaining the moisture absorption capacity of nylon while realizing the technical effect of flame retardancy.
EXAMPLE six
Adding dried nylon 66, melamine polyphosphate and synergistic flame retardant purified water sludge into a high-speed stirrer in proportion according to the proportion of the first embodiment, stirring at the speed of 400 rpm for 5 min, and discharging to obtain a premix; adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material, and maintaining the moisture absorption capacity of nylon while realizing the technical effect of flame retardancy.
EXAMPLE seven
Adding the dried nylon 12, melamine polyphosphate and the synergistic flame retardant water purification sludge into a high-speed stirrer according to the proportion of the second embodiment, stirring at the speed of 300 rpm for 3 min, and discharging to obtain a premix; the premix is added into a double-screw extruder hopper, glass fiber is fed, and then the flame-retardant nylon composite material is obtained through extrusion, cooling, grain cutting and packaging, so that the technical effect of flame retardancy is realized, and the PA12 has low water absorption rate in the existing nylon products due to the fact that the methylene molecules in the nylon 12 greatly reduce hydrophilic groups.
Example eight
Adding the dried nylon 610, melamine polyphosphate and the synergistic flame retardant water purification sludge into a high-speed stirrer according to the proportion of the second embodiment, stirring at the speed of 250 rpm for 4 min, and discharging to obtain a premix; and adding the premix into a double-screw extruder hopper, feeding glass fiber, extruding, cooling, granulating and packaging to obtain the flame-retardant moisture-absorbing nylon composite material.
The sludge is waste, is used as a raw material for preparing an adsorbent and a ceramic material, can also be used as a light bone material, and has certain mechanical strength. In the prior art, oil field sludge rich in calcium carbonate is used as a flame retardant additive, and an ethylene-vinyl acetate copolymer (EVA)/oil field sludge (OS)/Graphite (GP) composite material is prepared by a melt blending method; in the prior art, a paper mud/epoxy phenolic composite material is prepared by using thermoplastic epoxy phenolic resin and paper mud, a halogen-containing flame retardant tri-2-chloroethylphosphonate and an inorganic flame retardant are added into the epoxy phenolic resin and the paper mud/epoxy phenolic polymer, and the combustion grade of a system is determined by using a UL-94 grade combustion test method. For the existing paper sludge for flame retardance, the paper sludge is not suitable for being doped with nylon, and the pure water sludge is not reported for flame retardance.
The fabric has excellent moisture absorption and quick drying performance, and can keep relatively dry and comfortable in the taking process, so that the fabric has better taking comfort and health care performance. The high-moisture-conductivity polyamide fabric absorbs sweat in the inner layer of the fabric to the outer layer of the fabric mainly through a capillary effect, and the sweat is evaporated from the outer layer of the fabric, so that the moisture conductivity and the quick drying of the fabric are realized. In the prior art, a polymer containing hydrophilic groups and nylon chips are subjected to mixed spinning by a polymer blending or composite spinning method; or by utilizing a graft copolymerization method, hydrophilic groups are introduced into the macromolecular structure so as to increase the moisture absorption and sweat releasing functions of the fiber.
The nylon has high strength and good wear resistance, also has good moisture absorption capacity and is an excellent raw material of the fabric, but the moisture absorption capacity of the nylon is often weakened while flame retardant modification is carried out in the prior art, which is an advantage in the aspect of electronic and electric appliance application, but is not suitable for the application utilizing the moisture absorption capacity. According to the invention, the melamine polyphosphate is used as a main flame retardant, the glass fiber is used as an auxiliary material for reinforcement, and the combination of the melamine polyphosphate, the glass fiber and the purified water sludge with adsorption capacity is found to obtain a flame-retardant effect under the condition of relatively low filling amount, and maintain the good moisture absorption capacity of nylon.
Claims (10)
1. The flame-retardant moisture-absorption nylon composite material comprises nylon, a phosphorus-nitrogen flame retardant, glass fiber and purified water sludge, and is characterized in that the amount of the phosphorus-nitrogen flame retardant is 5-18% of the mass of the nylon.
2. The flame-retardant moisture-absorbing nylon composite material as claimed in claim 1, wherein the weight of nylon is 100%, the weight of the phosphorus-nitrogen flame retardant is 10-15%, the weight of the glass fiber is 2-4%, and the weight of the purified water sludge is 0.5-1.5%.
3. The flame-retardant moisture-absorbing nylon composite material as claimed in claim 1, wherein the flame-retardant moisture-absorbing nylon composite material is prepared from nylon, a phosphorus-nitrogen flame retardant, glass fiber and purified water sludge.
4. The flame retardant and moisture absorbent nylon composite material of claim 1, wherein the nylon is one or more of PA6, PA11, PA12, PA46, PA66, PA610, PA612 and PA 1010.
5. The method for preparing a flame-retardant moisture-absorbing nylon composite material according to claim 1, wherein the flame-retardant moisture-absorbing nylon composite material is obtained by melt-mixing nylon with a flame retardant, glass fiber and purified water sludge.
6. The method for preparing a flame retardant moisture absorption nylon composite material according to claim 5, wherein the flame retardant moisture absorption nylon composite material is prepared by a screw extruder.
7. The method for preparing the flame-retardant moisture-absorbing nylon composite material as claimed in claim 5, wherein the phosphorus-nitrogen flame retardant is melamine polyphosphate.
8. Use of the flame retardant absorbent nylon composite of claim 1 for the preparation of a flame retardant material.
9. Use of the flame retardant absorbent nylon composite of claim 1 for the preparation of flame retardant textiles.
10. A flame retardant plastic, characterized by being prepared from the flame retardant moisture absorption nylon composite material of claim 1, or prepared from the flame retardant moisture absorption nylon composite material of claim 1 and other high molecular materials.
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| US20020103273A1 (en) * | 2000-10-27 | 2002-08-01 | Yasuhito Inagaki | Additive for resin, additive-containing resin, and method for producing the same |
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| CN103937229A (en) * | 2013-01-17 | 2014-07-23 | 上海杰事杰新材料(集团)股份有限公司 | Fire retardant glass fiber reinforced nylon composite material, and preparation method thereof |
| CN104017356A (en) * | 2014-06-09 | 2014-09-03 | 上海众力汽车部件有限公司 | Preparation method of flame retardant nylon material |
| CN106479165A (en) * | 2016-09-30 | 2017-03-08 | 宋兰兰 | Halogen-free flame-retardant long fiberglass reinforced PA 6 composite and its one-step preppn process |
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2022
- 2022-05-10 CN CN202210502747.1A patent/CN114806159A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020103273A1 (en) * | 2000-10-27 | 2002-08-01 | Yasuhito Inagaki | Additive for resin, additive-containing resin, and method for producing the same |
| JP2013226523A (en) * | 2012-04-26 | 2013-11-07 | Kyushu Koatsu Concrete Kogyo Kk | Hygroscopic material, method for producing the same, and concrete sludge for water retention agent |
| CN103937229A (en) * | 2013-01-17 | 2014-07-23 | 上海杰事杰新材料(集团)股份有限公司 | Fire retardant glass fiber reinforced nylon composite material, and preparation method thereof |
| CN104017356A (en) * | 2014-06-09 | 2014-09-03 | 上海众力汽车部件有限公司 | Preparation method of flame retardant nylon material |
| CN106479165A (en) * | 2016-09-30 | 2017-03-08 | 宋兰兰 | Halogen-free flame-retardant long fiberglass reinforced PA 6 composite and its one-step preppn process |
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