CN106751772B - Class graphene g-C3N4 fire-retardant nylon and preparation method thereof - Google Patents
Class graphene g-C3N4 fire-retardant nylon and preparation method thereof Download PDFInfo
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- 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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Abstract
The invention belongs to high molecular fire retardant Material Fields, a more particularly to type graphene g-C3N4 fire-retardant nylon and preparation method thereof, raw material are by nylon 6 resin 200-250 parts by weight, class graphene g-C3N4 material 7-10 parts by weight, inorganic filler 10-20 parts by weight, synergistic fire retardant 2-7 parts by weight and processing aid 1-5 parts by weight, the solvent that molten caprolactam had both been used as g-C3N4 to prepare in whole preparation process, polymerized monomer as nylon 6 again, fire-retardant Nylon 6 composite material prepared by this method has fire retardant additive amount few, green, the features such as composite material combination property is excellent.
Description
Technical field
The invention belongs to high molecular fire retardant Material Field more particularly to a type graphene g-C3N4 fire-retardant nylon and its systems
Preparation Method.
Background technique
Nylon resin, i.e. polyamide have excellent mechanical strength, wearability, self-lubrication, corrosion resistance and preferable
Machine-shaping property is widely applied in fields such as automobile, electronic apparatus and machinery, has become five big general engineerings at present
Yield is maximum in plastics, kind is most, purposes is most wide, high comprehensive performance base resin.But nylon resin limit oxygen index
It is not high, and the nylon resin composition heat resistance of tradition preparation is not strong, easy firing, therefore it is limited in many fields into one
Step application, needs to carry out flame retardant treatment.Although halogen containing flame-retardant good flame retardation effect, smoke amount is big when burning, and generates toxic
Gas causes secondary pollution.Melamine cyanurate is a kind of nitrogenous compound that melamine and cyanuric acid are polymerized.
As a kind of nitrogenated flame retardant, compared with halogenated flame retardant, toxicity is lower, has excellent flame-retardant comprehensive performance.
The patent of invention of 1013013104 B of Authorization Notice No. CN discloses a kind of Halogen filling fire-retardant Nylon 6 composite wood
Material and preparation method thereof, the Halogen are filled fire-retardant Nylon 6 composite material, are made of the following raw material: nylon 6 resin 53-70
Parts by weight；Melamine cyanurate 7-15 parts by weight；Inorganic filler 20-30 parts by weight；Synergistic fire retardant 0-5 parts by weight；Add
Work auxiliary agent 1-5 parts by weight.Compared with prior art, the Halogen filling fire-retardant Nylon 6 composite material of the invention can pass through 960 DEG C
Under GWFI test, have the characteristics such as low cost, high-modulus, high intensity and excellent dimensional stability, environmental protection flame retardant, have good
Good application prospect.But melamine cyanurate is directly passed through melting extrusion modification of nylon, this method preparation by this method
Nitrogenated flame retardant using 6 ontology of nylon carry out it is fire-retardant, the usage amount of fire retardant is bigger.
Summary of the invention
The present invention in order to solve nitrogenated flame retardant it is fire-retardant when, the big problem of the usage amount of fire retardant provides a type graphite
Alkene g-C3N4 fire-retardant nylon and preparation method thereof.
In order to achieve the above object, first foundation scheme of the invention provides a type graphene g-C3N4 fire-retardant nylon,
It is made of the following raw material:
Class graphene g-C3N4 is that dicyanodiamine and the synthesis of N2 atmosphere are made, and inorganic modifier is graphene oxide, nanometer
At least one of silica, montmorillonite, synergistic fire retardant are aluminium hydroxide, magnesium hydroxide, red phosphorus, ammonium polyphosphate, boron
At least one of sour zinc, antimony oxide and molybdenum compound.
The principle of this base case is: class graphene g-C3N4 is to be closed using dicyanodiamine as raw material by heat treating process
At the g-C3N4 of synthesis carries out amination in N2 atmosphere, and the g-C3N4 after amination carries out calcining heat treatment in tube furnace and obtains
Class graphite ene-type g-C3N4 reacts g-C3N4 under certain temperature and pH value, and water, inorganic modifier are added during the reaction
Or the predecessor and other processing aids of inorganic modifier are generated, inorganic modified g-C3N4 composite flame-retardant agent is made, then one
Determine using molten caprolactam (nylon 6 resin) ontology as reaction medium under temperature and pressure, in-situ polymerization prepares inorganic modified
Class graphene g-C3N4 fire-retardant nylon.
Wherein, inorganic modifier be at least one of graphene oxide, nano silica, montmorillonite, it is inorganic modified
Agent has harmfulness small, and smoke suppressing effect is good, can form inierpeneirating network structure with body surface, and adhesive force is good, have it is certain every
The protective effect of hot, anti-oxidation, anti-corrosion, fire-retardant fireproof can extend the service life of matrix, energy conservation and environmental protection；Synergistic fire retardant can
To select halogen system, phosphorus system, nitrogen system and other organic fire-retardants, it is fire-retardant that its can be significantly improved by the cooperation with synergistic fire retardant
Effect；Processing aid is that fire retardant is promoted to carry out fire-retardant auxiliary agent.
The beneficial effect of this base case is: 1, by dicyanodiamine be heat-treated and in N2 atmosphere amination prepare class
Graphite ene-type g-C3N4 has 50-100m2The specific surface area of/g, and the interlamellar spacing of class graphite ene-type g-C3N4 is 2-3nm thick,
It can be evenly dispersed in water, in ethyl alcohol；2, since class graphene g-C3N4 has carried out amination treatment, the by-product ammonia that amination generates
Gas can carry out polycondensation reaction with molten caprolactam, so that class graphene g-C3N4 fire retardant is obtained, this type graphene g-
C3N4 fire retardant can consume a part of caprolactam, and the interlamellar spacing of class graphite ene-type g-C3N4 is bigger, be seven yuan a kind of
Molten caprolactam can be wrapped in outside by mechanism of nucleation by the layer structure of ring, in this way that molten caprolactam is uniform
It is dispersed in outside class graphene g-C3N4 fire retardant, so that fire-retardant contact area increases, flame retardant effect is more preferable；This type graphene g-
C3N4 fire retardant both polymerize using a part of molten caprolactam as monomer, can also be wrapped in molten caprolactam outside,
And such graphene g-C3N4 fire retardant is a kind of halogen-free flame retardants, it is this to pass through into class graphene g-C3N4 halogen-free flame retardants
Core mechanism is wrapped in the fire-retardant nylon in nylon 6 resin, has that fire retardant usage amount is few, environmentally protective and composite material is comprehensive
Can be excellent the features such as.
Scheme two: this is the preferred of basic scheme, and the raw material for preparing of class graphene g-C3N4 further includes urea, melamine
Amine.The utility model has the advantages that urea and melamine also can produce class graphite at a high temperature of 550 DEG C or so, through the method for sintering
Alkene g-C3N4.
Scheme three: this is the preferred of basic scheme, and nylon 6 resin is the nylon 6 resin that relative viscosity is 2.0-2.2.Have
Beneficial effect: the nylon 6 resin mobility of low viscosity is preferable, can sufficiently polymerize with class graphene g-C3N4, generates class graphene
G-C3N4 fire retardant；Furthermore the dispersion of the class graphene g-C3N4 fire retardant of generation can be improved in nylon 6 resin good fluidity
Property, enhance flame retardant effect.
Scheme four: this for scheme two or three it is preferred, processing aid be carbon forming agent, glass fibre, silicon glass fiber, polytetrafluoro
At least one of vinyl fiber, silico-tungstic acid, zinc borate.The utility model has the advantages that carbon forming agent, glass fibre, silicon glass fiber, polytetrafluoroethyl-ne
The compatibility of these processing aids of alkene fiber, silico-tungstic acid, zinc borate and nylon 6 resin is preferable, can be very good to inhibit melting Buddhist nun
The burning of imperial 6 resins.
Second base case of the invention provides the preparation method of a type graphene g-C3N4 fire-retardant nylon, specific steps
Are as follows:
Step 1: by dicyanodiamine calcination processing, by temperature programmed control, within the temperature range of 450 DEG C -600 DEG C,
It is reacted 6-8 hours under N2 atmosphere, synthesizes class graphene g-C3N4, class graphene g-C3N4 and NH4Cl solution is mixed, is put into
In hydrothermal reaction kettle, reaction temperature is 150 DEG C-200 DEG C, and the reaction time 20-30 hours, pH value range was 2.0-10.0, instead
It is cooled to room temperature after answering, forms amination carbon nitride material；Amination carbon nitride material is extracted by water and in room temperature ring
It is 5-7 hours dry under border, then the amination carbon nitride material after drying is put into tube furnace, it is passed through N2 protection gas, reaction temperature is
It 350 DEG C-450 DEG C, was heat-treated within the reaction time 4-6 hours, obtains class graphene g-C3N4 material.
Step 2: by nylon 6 resin 200-250 parts by weight, class graphene g-C3N4 material 7-10 parts by weight, inorganic filler
High mixer mixing is added in 10-20 parts by weight, synergistic fire retardant 2-7 parts by weight and processing aid 1-5 parts by weight, obtains premix；
Step 3: the premix that second step is obtained is placed in reaction kettle, adjusting pH value range is 2.0-5.0, when reaction
Between be 2-3 hours, by the air in high pure nitrogen displacement kettle, be warming up to 180 DEG C, be forced into 1.0MPa, polyase 13 hour, then
It is decompressed to -1.0MPa, is polymerize 13 hours, material is taken out after being cooled to room temperature, material carries out melting extrusion, cooling granulation.
Scheme six: this is preferred for scheme five, and material is extracted after being cooled to room temperature with water, carries out extruding pelletization after dry.
The utility model has the advantages that, good flame retardation effect relatively high by water class graphene g-C3N4 material purity extracted.
Specific embodiment
Below by specific embodiment, the present invention is described in further detail:
In the raw material that embodiment 1-7 is used, nylon 6 resin PA6M2400；Class graphene g-C3N4 is by dicyan two
Amine and the synthesis of N2 atmosphere are made, and inorganic modifier is at least one of graphene oxide, nano silica, montmorillonite, association
With at least one that fire retardant is in aluminium hydroxide, magnesium hydroxide, red phosphorus, ammonium polyphosphate, zinc borate, antimony oxide and molybdenum compound
Kind.
For the weight of each raw material according to shown in table 1, preparation method is as follows in embodiment 1-7 and comparative example:
1, class graphene g-C3N4 is prepared first, by dicyanodiamine calcination processing, by temperature programmed control, in 450 DEG C -600
Reacted 6-8 hours within the temperature range of DEG C and under N2 atmosphere, synthesize class graphene g-C3N4, by class graphene g-C3N4 and
NH4Cl solution mixing, be put into hydrothermal reaction kettle, reaction temperature be 150 DEG C-200 DEG C, the reaction time 20-30 hours, pH value
Range is 2.0-10.0, is cooled to room temperature after reaction, and amination carbon nitride material is formed；Amination carbon nitride material is passed through
Water extraction and drying 5-7 hours under room temperature environment, then the amination carbon nitride material after drying is put into tube furnace, it is passed through
N2 protects gas, and reaction temperature is 350 DEG C-450 DEG C, was heat-treated within the reaction time 4-6 hours, obtains class graphene g-C3N4
Material.
2, each raw material addition high mixer is mixed to get premix according to each material content (parts by weight), premix is placed in
In reaction kettle, adjusting pH value range is 2.0-5.0, and the reaction time is 2-3 hours, passes through the sky in high pure nitrogen displacement kettle
Gas is warming up to 180 DEG C, is forced into 1.0MPa, polyase 13 hour, then be decompressed to -1.0MPa, polymerize 13 hours, after being cooled to room temperature
Material is taken out, material is added in double screw extruder from the main spout of double screw extruder, carries out melting extrusion, cooling is made
Grain obtains the class graphene g-C3N4 fire-retardant nylon of Halogen filling, wherein double screw extruder is divided into nine areas, wherein an area
Temperature is 210 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 250 DEG C, and four area's temperature are 250 DEG C, and five area's temperature are 240 DEG C,
Six area's temperature are 240 DEG C, and seven area's temperature are 240 DEG C, and eight area's temperature are 230 DEG C, and nine area's temperature are 240 DEG C；Engine speed 350
Rev/min.
Mechanical property test method of the present invention and standard are respectively as follows: tensile strength and are tested according to ISO527-2 standard；
Bending strength and bending modulus are tested according to ISO178 standard；Notch impact strength is tested according to ISO179 standard；
Furthermore flame retardant property is characterized by limit oxygen index, UL94 vertical combustion performance, glowing filament fire burning index GWFI, each test knot
Fruit is as shown in table 1.
Table 1:
It is tensile strength, curved from table 1 it follows that class graphene g-C3N4 fire-retardant nylon prepared in accordance with the present invention
Qu Qiangdu and impact strength are not much different with comparative example, it is seen that and the addition of the g-C3N4 of class graphene-like influences less nylon,
Its bending modulus and comparative example slightly improve, and molten caprolactam is wrapped in outside the class graphene g-C3N4 of nanometer shape, increases
Its bending modulus；The limit epoxy index of class graphene g-C3N4 fire-retardant nylon prepared by the present invention is greater than 26, and is greater than comparison
The limit epoxy index of example, belongs to nonflammable material；Class graphene g-C3N4 fire-retardant nylon prepared by the present invention has passed through the U.S.
The test of UL94 vertical combustion performance, and the test of maximum temperature in glowing filament fire burning index (960 DEG C, 1mm) has been passed through,
When burning, low cigarette, low toxicity, while material keeps the modulus of good mechanical property, especially material to significantly improve on the whole, and
And the good fluidity of system, it is conducive to production and processing.Compared with other flame-retardant nylon 6 materials, fire proofing of the invention is efficient
The fire proofing of halogen-free environmental；In addition, the class graphene g-C3N4 fire-retardant nylon of preparation method preparation, is to pass through Review On The Nucleation Mechanism
The fire-retardant nylon being wrapped in nylon 6 resin has used nylon-6 matrix body material during fire-retardant, and fire retardant makes when fire-retardant
Dosage is few, environmentally protective and composite material combination property is excellent.
What has been described above is only an embodiment of the present invention, and the common sense such as well known specific structure and characteristic are not made herein in scheme
Excessive description.It, without departing from the structure of the invention, can be with it should be pointed out that for those skilled in the art
Several modifications and improvements are made, these also should be considered as protection scope of the present invention, these all will not influence what the present invention was implemented
Effect and patent practicability.The scope of protection required by this application should be based on the content of the claims, in specification
The records such as specific embodiment can be used for explaining the content of claim.
Claims (5)
1. class graphene g-C3N4 fire-retardant nylon, which is characterized in that be made of the following raw material:
The g-C3N4 is that dicyanodiamine and the synthesis of N2 atmosphere are made, and the inorganic modifier is graphene oxide, nanometer two
At least one of silica, montmorillonite, the synergistic fire retardant be aluminium hydroxide, magnesium hydroxide, red phosphorus, ammonium polyphosphate,
At least one of zinc borate, antimony oxide and molybdenum compound, the processing aid are carbon forming agent, glass fibre, silicon glass fiber, gather
At least one of tetrafluoroethylene fiber, silico-tungstic acid, zinc borate.
2. class graphene g-C3N4 fire-retardant nylon as described in claim 1, which is characterized in that the raw material for preparing of g-C3N4 also wraps
Include urea, melamine.
3. class graphene g-C3N4 fire-retardant nylon as described in claim 1, which is characterized in that the nylon 6 resin is opposite
Viscosity is the nylon 6 resin of 2.2-2.5.
4. the method for preparing class graphene g-C3N4 fire-retardant nylon as described in claim 1, which is characterized in that specific steps
Are as follows:
Step 1: by dicyanodiamine calcination processing, by temperature programmed control, within the temperature range of 450 DEG C -600 DEG C, in N2 gas
It is reacted 6-8 hours under atmosphere, synthesizes class graphene g-C3N4, class graphene g-C3N4 and NH4Cl solution is mixed, hydro-thermal is put into
In reaction kettle, reaction temperature is 150 DEG C-200 DEG C, and the reaction time 20-30 hours, pH value range was 2.0-10.0, reaction knot
It is cooled to room temperature after beam, forms amination carbon nitride material；Amination carbon nitride material is extracted by water and under room temperature environment
It is 5-7 hours dry, then the amination carbon nitride material after drying is put into tube furnace, it is passed through N2 protection gas, reaction temperature 350
It DEG C-450 DEG C, was heat-treated within the reaction time 4-6 hours, obtains class graphene g-C3N4 material；
Step 2: by nylon 6 resin 200-250 parts by weight, class graphene g-C3N4 material 7-10 parts by weight, inorganic filler 10-
High-speed mixer and mixing is added in 20 parts by weight, synergistic fire retardant 2-7 parts by weight and processing aid 1-5 parts by weight, obtains premix；
Step 3: the premix that second step is obtained is placed in reaction kettle, adjusting pH value range is 2.0-5.0, and the reaction time is
2-3 hours, by the air in high pure nitrogen displacement kettle, 180 DEG C are warming up to, is forced into 1.0MPa, polyase 13 hour, then depressurize
To -1.0MPa, it polymerize 13 hours, material is taken out after being cooled to room temperature, material carries out melting extrusion, cooling granulation.
5. the preparation method of class graphene g-C3N4 fire-retardant nylon as claimed in claim 4, which is characterized in that the material is cold
But to being extracted after room temperature with water, extruding pelletization is carried out again after dry.
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| CN109054151B (en) * | 2018-07-11 | 2021-04-02 | 河南科技大学 | Polyolefin flame-retardant composite material and preparation method thereof |
| CN109880211A (en) * | 2019-02-25 | 2019-06-14 | 牟富书 | Antibiotic plastic and preparation method thereof |
| CN109824942B (en) * | 2019-02-26 | 2021-04-20 | 西北师范大学 | Preparation and application of organic-inorganic hybrid material composite flame retardant |
| CN110183831A (en) * | 2019-05-21 | 2019-08-30 | 南京工业大学 | A kind of metal organic frame modification graphitic nitralloy carbon/unsaturated polyester resin composite flame-proof material preparation method and applications |
| CN113087970B (en) * | 2020-01-08 | 2024-01-30 | 中国石油化工股份有限公司 | Halogen-free flame retardant and application thereof in preparation of halogen-free flame retardant PA6 |
| CN113186727A (en) * | 2021-05-08 | 2021-07-30 | 兰州大学 | Inorganic-bio-based anti-photoaging flame retardant and application thereof in textiles |
| CN113737302B (en) * | 2021-07-22 | 2023-06-23 | 常州恒利宝纳米新材料科技有限公司 | Method for modifying nylon 6 fiber by using graphene oxide |
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Effective date of registration: 20191213 Address after: 511825 north side of Yinying Road, Shengping Industrial Park, Feilaixia Town, Qingcheng District, Qingyuan City, Guangdong Province Patentee after: QINGYUAN CITY YICHENG FLAME RETARDANT MATERIALS CO., LTD. Address before: 511500 Guangdong city of Qingyuan province science and Technology Innovation Park, hi tech Industrial Development Zone, Chong Hing Road No. 18 Tian Chi Valley Exhibition Center by 19 Co-patentee before: Guangdong Nanfang fountain Plastic Technology Co., Ltd. Patentee before: Guangdong New Material Research Institute Co., Ltd. |
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