CN115819961A - Preparation method of nylon 6 flame-retardant composite material - Google Patents
Preparation method of nylon 6 flame-retardant composite material Download PDFInfo
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- CN115819961A CN115819961A CN202211526093.2A CN202211526093A CN115819961A CN 115819961 A CN115819961 A CN 115819961A CN 202211526093 A CN202211526093 A CN 202211526093A CN 115819961 A CN115819961 A CN 115819961A
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- Prior art keywords
- nylon
- flame
- section
- composite material
- retardant
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- 229920002292 Nylon 6 Polymers 0.000 title claims abstract description 65
- 239000003063 flame retardant Substances 0.000 title claims abstract description 61
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 238000002844 melting Methods 0.000 claims abstract description 25
- 230000008018 melting Effects 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 16
- 230000008569 process Effects 0.000 claims description 12
- 238000010008 shearing Methods 0.000 claims description 12
- 150000003254 radicals Chemical class 0.000 abstract description 9
- -1 4-oxygen-2 Chemical class 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 3
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 19
- 239000011159 matrix material Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000002861 polymer material Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 150000002391 heterocyclic compounds Chemical group 0.000 description 1
- 229910000039 hydrogen halide Inorganic materials 0.000 description 1
- 239000012433 hydrogen halide Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- DOTMOQHOJINYBL-UHFFFAOYSA-N molecular nitrogen;molecular oxygen Chemical compound N#N.O=O DOTMOQHOJINYBL-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Abstract
The invention provides a preparation method of a nylon 6 flame-retardant composite material, which comprises the following steps: weighing nylon 6 resin, MCA flame retardant and 4-oxo-2, 6-tetramethylpiperidine-1-oxygen radical, adding into a mixer, and stirring to obtain premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The invention can obviously improve the flame retardant property by adding a halogen-free compound which can be effectively combined with free radicals, namely 4-oxygen-2, 6-tetramethyl piperidine-1-oxygen free radical.
Description
Technical Field
The invention relates to the field of flame-retardant materials, and particularly relates to a preparation method of a nylon 6 flame-retardant composite material.
Background
The nylon 6 has excellent comprehensive performance, and the modified composite material has wide application in various fields, and becomes an important high polymer material from civilian use to military use, from land to air, and from clothes and eating habits to living and daily life of people. Among the whole general engineering plastics, nylon (PA) becomes a high polymer material with the largest yield and the widest application field. However, nylon is easy to burn, the oxygen index of pure nylon 6 is 22.7%, the burning speed is high, and the dripping phenomenon is serious. Melamine Cyanurate (MCA) is a low-cost halogen-free flame retardant suitable for nylon 6, and has the advantages of high nitrogen content, good thermal stability, low toxicity and low smoke. However, during the combustion process, MCA is mainly used for gas-phase flame retardance, the carbon forming amount is small, and the carbon layer is loose, so the flame retardance efficiency is low. The MCA is used for preparing the nylon 6 flame-retardant polymer material, and the flame retardant property of the flame-retardant polymer material can only reach UL94-V2 level.
The brominated flame retardant has high flame retardant efficiency mainly because halogen element substances can be combined and consumed free radicals continuously in the combustion process, the amount of the free radicals is reduced, and the continuous progress of the combustion reaction is prevented. However, the toxic and harmful gas generated by the method, namely the hydrogen halide HX, limits the use of the method under the environment-friendly requirement.
Disclosure of Invention
The invention provides a preparation method of a nylon 6 flame-retardant composite material, which aims to solve at least one technical problem.
In order to solve the above problems, as an aspect of the present invention, there is provided a method for preparing a nylon 6 flame retardant composite, comprising: weighing nylon 6 resin, MCA flame retardant and 4-oxo-2, 6-tetramethylpiperidine-1-oxyl, adding into a mixer, and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating.
Preferably, the temperatures of each section of the extrusion process are respectively: the conveying section is 190-200 ℃, the melting section is 235-245 ℃, the shearing section is 245-265 ℃, the exhaust section is 235-245 ℃ and the extrusion section is 250-255 ℃.
Preferably, the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows: (90-94): (3.5-9): (1-2.5).
Preferably, the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows: 94: (4-45): (1-2.5).
Preferably, the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows: 90: (7.5-9): (1-2.5).
The invention can obviously improve the flame retardant property by adding the halogen-free compound which can be effectively combined with free radicals, namely 4-oxo-2, 6-tetramethyl piperidine-1-oxygen free radical.
Detailed Description
The following detailed description of embodiments of the invention, but the invention can be practiced in many different ways, as defined and covered by the claims.
The invention provides a method for improving halogen-free flame retardant property of nylon 6 by using a nitrogen-oxygen stable free radical, which obviously improves the flame retardant property by adding a halogen-free compound which can be effectively combined with the free radical, namely 4-oxo-2, 6-tetramethylpiperidine-1-oxygen free radical. Possible flame retardant mechanisms are: firstly, the free radicals generated in the combustion process are combined to block the combustion chain reaction; and secondly, the heterocyclic compound structure can effectively promote carbon formation and make up for the defect of insufficient carbon formation in MCA flame retardance.
4-oxo-2, 6-tetramethylpiperidine-1-oxyl radical
Example 1
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 94 parts of nylon 6 resin, 5 parts of MCA flame retardant and 1 part of 4-oxo-2, 6-tetramethylpiperidine-1-oxyl are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the nylon 6 flame-retardant composite material is prepared at the temperature of 190-200 ℃ in the conveying section, 235-2245 ℃ in the melting section, 245-2265 ℃ in the shearing section, 235-2245 ℃ in the exhaust section and 250-2255 ℃ in the extrusion section.
Example 2
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 94 parts of nylon 6 resin, 4.5 parts of MCA flame retardant and 1.5 parts of 4-oxo-2, 6-tetramethyl piperidine-1-oxyl are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 3
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 94 parts of nylon 6 resin, 4 parts of MCA flame retardant and 2 parts of 4-oxo-2, 6-tetramethylpiperidine-1-oxyl radical are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 4
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 94 parts of nylon 6 resin, 3.5 parts of MCA flame retardant and 2.5 parts of 4-oxo-2, 6-tetramethyl piperidine-1-oxyl are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 5
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: weighing 90 parts of nylon 6 resin, 9 parts of MCA flame retardant and 1 part of 4-oxo-2, 6-tetramethylpiperidine-1-oxyl. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 6
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 90 parts of nylon 6 resin, 8.5 parts of MCA flame retardant and 1.5 parts of 4-oxo-2, 6-tetramethyl piperidine-1-oxyl are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 7
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: weighing 90 parts of nylon 6 resin, 8 parts of MCA flame retardant and 2 parts of 4-oxo-2, 6-tetramethylpiperidine-1-oxyl. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Example 8
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 90 parts of nylon 6 resin, 7.5 parts of MCA flame retardant and 2.5 parts of 4-oxo-2, 6-tetramethyl piperidine-1-oxyl are weighed. Adding a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-2200 ℃, the melting section is 235-2245 ℃, the shearing section is 245-2265 ℃, the exhaust section is 235-2245 ℃ and the extrusion section is 250-2255 ℃, so as to prepare the nylon 6 flame-retardant composite material.
Comparative example 1
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: 94 parts of nylon 6 resin and 6 parts of MCA flame retardant are weighed. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the nylon 6 flame-retardant composite material is prepared at 190-200 ℃ in the conveying section, 235-245 ℃ in the melting section, 245-265 ℃ in the shearing section, 235-245 ℃ in the exhaust section and 250-255 ℃ in the extrusion section.
Comparative example 2
The preparation method of the nylon 6 flame-retardant composite material comprises the following steps: taking the matrix resin as nylon 6 as an example: weighing 90 parts of nylon 6 resin and 10 parts of MCA flame retardant. Adding the mixture into a mixer and uniformly stirring to obtain a premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating. The temperature of each section of the extrusion process is respectively as follows: the nylon 6 flame-retardant composite material is prepared at the temperature of 190-200 ℃ in the conveying section, 235-245 ℃ in the melting section, 245-265 ℃ in the shearing section, 235-245 ℃ in the exhaust section and 250-255 ℃ in the extrusion section.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (5)
1. The preparation method of the nylon 6 flame-retardant composite material is characterized by comprising the following steps: weighing nylon 6 resin, MCA flame retardant and 4-oxo-2, 6-tetramethylpiperidine-1-oxygen radical, adding into a mixer, and stirring to obtain premix; adding the premix into a No. 1 weightlessness scale, and adding from a main feeding port of a double-screw extruder; and (4) melting, mixing, extruding and granulating.
2. The preparation method of the nylon 6 flame-retardant composite material according to claim 1, wherein the temperature of each section of the extrusion process is respectively as follows: the conveying section is 190-200 ℃, the melting section is 235-245 ℃, the shearing section is 245-265 ℃, the exhaust section is 235-245 ℃ and the extrusion section is 250-255 ℃.
3. The preparation method of the nylon 6 flame-retardant composite material according to claim 1, wherein the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows:
(90-94)：(3.5-9)：(1-2.5)。
4. the preparation method of the nylon 6 flame-retardant composite material according to claim 1, wherein the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows: 94: (4-45): (1-2.5).
5. The preparation method of the nylon 6 flame-retardant composite material according to claim 1, wherein the parts ratio of the nylon 6 resin, the MCA flame retardant and the 4-oxo-2, 6-tetramethylpiperidine-1-oxyl is as follows: 90: (7.5-9): (1-2.5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211526093.2A CN115819961B (en) | 2022-11-30 | 2022-11-30 | Preparation method of nylon 6 flame-retardant composite material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211526093.2A CN115819961B (en) | 2022-11-30 | 2022-11-30 | Preparation method of nylon 6 flame-retardant composite material |
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| CN115819961A true CN115819961A (en) | 2023-03-21 |
| CN115819961B CN115819961B (en) | 2024-05-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885339A (en) * | 2014-12-26 | 2016-08-24 | 神华集团有限责任公司 | Antioxidant composition, modified polyformaldehyde resin composition and modified polyformaldehyde resin and preparation method thereof |
| CN111500059A (en) * | 2020-05-21 | 2020-08-07 | 新乡市新蒲机械有限责任公司 | Flame-retardant reinforced nylon composite material and preparation method thereof |
| WO2021243836A1 (en) * | 2020-06-03 | 2021-12-09 | 山东科技大学 | Flame-retardant masterbatch, preparation method therefor, and application thereof |
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- 2022-11-30 CN CN202211526093.2A patent/CN115819961B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105885339A (en) * | 2014-12-26 | 2016-08-24 | 神华集团有限责任公司 | Antioxidant composition, modified polyformaldehyde resin composition and modified polyformaldehyde resin and preparation method thereof |
| CN111500059A (en) * | 2020-05-21 | 2020-08-07 | 新乡市新蒲机械有限责任公司 | Flame-retardant reinforced nylon composite material and preparation method thereof |
| WO2021243836A1 (en) * | 2020-06-03 | 2021-12-09 | 山东科技大学 | Flame-retardant masterbatch, preparation method therefor, and application thereof |
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