CN108610626A - A kind of preparation method of novel flame-retardant PA6 composite materials - Google Patents
A kind of preparation method of novel flame-retardant PA6 composite materials Download PDFInfo
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- CN108610626A CN108610626A CN201611144198.6A CN201611144198A CN108610626A CN 108610626 A CN108610626 A CN 108610626A CN 201611144198 A CN201611144198 A CN 201611144198A CN 108610626 A CN108610626 A CN 108610626A
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- Prior art keywords
- retardant
- flame
- magaldrates
- novel flame
- modified layered
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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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
- 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
-
- 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
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
-
- 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
- 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
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- 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
- 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
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The present invention relates to the preparation methods of novel flame-retardant PA6 of technical field of polymer materials a kind of.The each component and the weight percent of each component weight and PA6 of the flame-proof PA 6 be：Modified layered double magaldrates 5%~12%, microcapsule red phosphorus 5%~15%；The preparation method of the flame-proof PA 6 includes the following steps：The modification of the double magaldrates of stratiform；Each component is weighed by said ratio, is put into high-speed mixer and mixes, then melt blending and extruding pelletization in double screw extruder, up to novel flame-retardant PA6 masterbatch after drying.Flame-proof PA 6 prepared by the present invention enables flame-proof PA 6 vertical combustion to reach V -0 grades, and the influence to mechanical property is little due to the synergistic effect of microcapsule red phosphorus and modified layered double magaldrates.
Description
Technical field
The present invention relates to the preparations of flame-proof PA 6.Especially a kind of preparation method of novel flame-retardant PA6.
Background technology
PA6 is most representative nylon resin, is a kind of to be widely used general engineering plastics.In PA6 strands
Amide group has polarity, can form hydrogen bond, therefore mechanical performance is excellent, if tensile strength is high, good toughness, is resistant to repeated stock
Vibrations, while it is also with good electrical property, oil resistivity, self lubricity, sound-deadening properties, wearability and workability
Deng but its L0I is only 23% or so, and when burning generates a large amount of flammable molten drops, thus to make it have broader application range just
It must be carried out flame-retardant modified.
Invention content
It is an object of the invention to propose a kind of novel flame-retardant PA6, it is intended to overcome the feature of PA6 combustibilities difference, and add
Enter microcapsule red phosphorus, form synergistic effect with modified layered double magaldrates, flame-proof PA 6 vertical combustion is enable to reach V -0 grades,
And the influence to mechanical property is little.
It is a further object to provide the preparation methods of above-mentioned novel flame-retardant PA6.
Realizing the technical solution of the object of the invention is：First the double magaldrates of stratiform are modified, then will be modified
The double magaldrate of stratiform, microcapsule red phosphorus, with PA6 blending extrusions according to a certain ratio, obtain product, its step are as follows：
（1）Weigh the Mg (NO of certain mol proportion3)2·6H2O and Al (NO3)3·9H2O is dissolved in the deionized water of 1L, is made into Mg/
The mixing salt solution that Al molar ratios are 1 ~ 3, is subsequently poured into three-necked flask, with vigorous stirring, will prepare the NaOH of concentration
Solution is slowly dropped to base buret in mixing salt solution, then adjusts pH value.0.5 h ~ 2h is reacted, and is added dropwise 100
The sodium stearate solution of 1.6 mol/L of mL.Continue to be aged gained slurries for 24 hours under 80 DEG C of water-baths after stirring 0.5 h ~ 2h,
It is crushed afterwards for 24 hours up to modified layered double magaldrates through dry at deionized water centrifuge washing 5 times, 80 DEG C；
（2）Weigh respectively according to a certain ratio modified layered double magaldrates, microcapsule red phosphorus with and PA6 pellets, drying；
（3）By above-mentioned each component in double screw extruder melt blending, extruding pelletization, up to novel flame-retardant PA6 after drying.
In the present invention, the microcapsule red phosphorus preparation method is specially：It coats to obtain using melamine formaldehyde resin,
Wherein, microcapsule red phosphorus grain size is 0.5-35 um, and heat decomposition temperature reaches 396 DEG C;
Compared with prior art, the present invention the advantage is that：Microcapsule red phosphorus forms synergistic with modified layered double magaldrates
Effect, enables flame-proof PA 6 vertical combustion to reach V -0 grades, and the influence to mechanical property is little.
Description of the drawings
Fig. 1 is a kind of novel flame-retardant PA6 preparation technology flow charts of the present invention.
Specific implementation mode
In conjunction with attached drawing, a kind of preparation method of novel flame-retardant PA6 of the present invention is as follows：
（1）Weigh the Mg (NO of certain mol proportion3)2·6H2O and Al (NO3)3·9H2O is dissolved in the deionized water of 1L, is made into Mg/
The mixing salt solution that Al molar ratios are 1 ~ 3, is subsequently poured into three-necked flask, with vigorous stirring, will prepare the NaOH of concentration
Solution is slowly dropped to base buret in mixing salt solution, then adjusts pH value.0.5 h ~ 2h is reacted, and is added dropwise 100
The sodium stearate solution of 1.6 mol/L of mL.Continue to be aged gained slurries for 24 hours under 80 DEG C of water-baths after stirring 0.5 h ~ 2h,
It is crushed afterwards for 24 hours up to modified layered double magaldrates through dry at deionized water centrifuge washing 5 times, 80 DEG C；
（2）PA6, stratiform double magaldrate, microcapsule red phosphorus, drying are weighed respectively；The weight of its each component and the weight of PA6
Percentage is：Modified layered double magaldrates 5%~12%, microcapsule red phosphorus 5%~15%；
（3）Above-mentioned material is put into high-speed mixer and is mixed, then melt blending and extruding pelletization in double screw extruder,
Up to novel flame-retardant PA6 after drying.
Embodiment 1
（1）Weigh 0.2 mol/L Mg (NO3)2·6H2O、0.2 mol/L Al(NO3)3·9H2O is dissolved in the deionized water of 1L,
It is made into the mixing salt solution that Mg/Al molar ratios are 1, is subsequently poured into the three-necked flask of 3 L, with vigorous stirring, will prepare
The 1.5mol/L NaOH solutions of 1L be slowly dropped in mixing salt solution with base buret, then adjust pH value 10.5 ~
11.After reacting 0.5 h, and the sodium stearate solution of 100 mL, 1.6 mol/L is added dropwise.Continue stir 2 h after by gained slurries in
It is aged under 80 DEG C of water-baths for 24 hours, is crushed afterwards for 24 hours up to modified layered double hydrogen-oxygens through dry at deionized water centrifuge washing 5 times, 80 DEG C
Change magnalium；
（2）1000 grams of PA6,50 grams of modified layered double magaldrates, 50 grams of microcapsule red phosphorus are weighed respectively, are dried；
（3）Above-mentioned material is put into high-speed mixer and is mixed, melt blending and extruding pelletization in double screw extruder, drying
Afterwards up to novel flame-retardant PA6.
Embodiment 2
（1）Weigh 0.4 mol/L Mg (NO3)2·6H2O、0.2 mol/L Al(NO3)3·9H2O is dissolved in the deionized water of 1L,
It is made into the mixing salt solution that Mg/Al molar ratios are 2, is subsequently poured into the three-necked flask of 3 L, with vigorous stirring, will prepare
The 1.5mol/L NaOH solutions of 1L be slowly dropped in mixing salt solution with base buret, then adjust pH value 10.5 ~
11.After reacting 2h, and the sodium stearate solution of 100 mL, 1.6 mol/L is added dropwise.Continue stir 1 h after by gained slurries in 80
It is aged under DEG C water-bath for 24 hours, is crushed afterwards for 24 hours up to modified layered double hydroxides through dry at deionized water centrifuge washing 5 times, 80 DEG C
Magnalium.
（2）1000 grams of PA6,120 grams of modified layered double magaldrates, 100 grams of microcapsule red phosphorus are weighed respectively, are dried；
（3）Above-mentioned material is put into high-speed mixer and is mixed, melt blending and extruding pelletization in double screw extruder, drying
Afterwards up to novel flame-retardant PA6.
Embodiment 3
(1) 0.6 mol/L Mg (NO are weighed3)2·6H2O、0.2 mol/L Al(NO3)3·9H2O is dissolved in the deionized water of 1L,
It is made into the mixing salt solution that Mg/Al molar ratios are 3, is subsequently poured into the three-necked flask of 3 L, with vigorous stirring, will prepare
The 1.5mol/L NaOH solutions of 1L be slowly dropped in mixing salt solution with base buret, then adjust pH value 11 ~
11.5.After reacting 2h, and the sodium stearate solution of 100 mL, 1.6 mol/L is added dropwise.Continue stir 1 h after by gained slurries in
It is aged under 80 DEG C of water-baths for 24 hours, is crushed afterwards for 24 hours up to modified layered double hydrogen-oxygens through dry at deionized water centrifuge washing 5 times, 80 DEG C
Change magnalium.
（2）1000 grams of PA6,90 grams of modified layered double magaldrates, 90 grams of microcapsule red phosphorus are weighed respectively, are dried；
（3）Above-mentioned material is put into high-speed mixer and is mixed, melt blending and extruding pelletization in double screw extruder, drying
Afterwards up to novel flame-retardant PA6.
Embodiment 4
（1）Weigh 0.6 mol/L Mg (NO3)2·6H2O、0.2 mol/L Al(NO3)3·9H2O is dissolved in the deionized water of 1L,
It is made into the mixing salt solution that Mg/Al molar ratios are 3, is subsequently poured into the three-necked flask of 3 L, with vigorous stirring, will prepare
The 1.5mol/L NaOH solutions of 1L be slowly dropped in mixing salt solution with base buret, then adjust pH value 11.5 ~
12.After reacting 2h, and the sodium stearate solution of 100 mL, 1.6 mol/L is added dropwise.Continue stir 1.5 h after by gained slurries in
It is aged under 80 DEG C of water-baths for 24 hours, is crushed afterwards for 24 hours up to sample through dry at deionized water centrifuge washing 5 times, 80 DEG C.
（2）1000 grams of PA6,10 grams of modified layered double magaldrates, 15 grams of microcapsule red phosphorus are weighed respectively, are dried；
（3）Above-mentioned material is put into high-speed mixer and is mixed, melt blending and extruding pelletization in double screw extruder, drying
Afterwards up to novel flame-retardant PA6.
Claims (1)
1. a kind of preparation method of novel flame-retardant PA6, it is characterised in that the method includes following preparation processes：
（1）Weigh the Mg (NO of certain mol proportion3)2·6H2O and Al (NO3)3·9H2O is dissolved in the deionized water of 1L, is made into Mg/
The mixing salt solution that Al molar ratios are 1 ~ 3, is subsequently poured into three-necked flask, with vigorous stirring, will prepare the NaOH of concentration
Solution is slowly dropped to base buret in mixing salt solution, then adjusts pH value；0.5 h ~ 2h is reacted, and is added dropwise 100
The sodium stearate solution of 1.6 mol/L of mL；Continue to be aged gained slurries for 24 hours under 80 DEG C of water-baths after stirring 0.5 h ~ 2h,
It is crushed afterwards for 24 hours up to modified layered double magaldrates through dry at deionized water centrifuge washing 5 times, 80 DEG C；
（2）Weigh respectively according to a certain ratio modified layered double magaldrates, microcapsule red phosphorus with and PA6 pellets, drying；
（3）By above-mentioned each component in double screw extruder melt blending, extruding pelletization, up to novel flame-retardant PA6 after drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611144198.6A CN108610626A (en) | 2016-12-13 | 2016-12-13 | A kind of preparation method of novel flame-retardant PA6 composite materials |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611144198.6A CN108610626A (en) | 2016-12-13 | 2016-12-13 | A kind of preparation method of novel flame-retardant PA6 composite materials |
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| Publication Number | Publication Date |
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| CN108610626A true CN108610626A (en) | 2018-10-02 |
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| CN201611144198.6A Pending CN108610626A (en) | 2016-12-13 | 2016-12-13 | A kind of preparation method of novel flame-retardant PA6 composite materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592693A (en) * | 2019-10-10 | 2019-12-20 | 嘉兴冰火新材料科技有限公司 | Special black flame retardant for microfiber and preparation method thereof |
| CN116180256A (en) * | 2023-03-06 | 2023-05-30 | 湖北博韬合纤有限公司 | Flame-retardant polypropylene staple fiber and preparation method thereof |
-
2016
- 2016-12-13 CN CN201611144198.6A patent/CN108610626A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110592693A (en) * | 2019-10-10 | 2019-12-20 | 嘉兴冰火新材料科技有限公司 | Special black flame retardant for microfiber and preparation method thereof |
| CN116180256A (en) * | 2023-03-06 | 2023-05-30 | 湖北博韬合纤有限公司 | Flame-retardant polypropylene staple fiber and preparation method thereof |
| CN116180256B (en) * | 2023-03-06 | 2023-09-19 | 湖北博韬合纤有限公司 | Flame-retardant polypropylene staple fiber and preparation method thereof |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20181002 |
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| WD01 | Invention patent application deemed withdrawn after publication |