CN106398200A - Water proof flame retardant polyamide material and preparation method thereof - Google Patents
Water proof flame retardant polyamide material and preparation method thereof Download PDFInfo
- Publication number
- CN106398200A CN106398200A CN201611053987.9A CN201611053987A CN106398200A CN 106398200 A CN106398200 A CN 106398200A CN 201611053987 A CN201611053987 A CN 201611053987A CN 106398200 A CN106398200 A CN 106398200A
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- parts
- chopped fiber
- flame retardant
- polyamide material
- water
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The invention provides a water proof flame retardant polyamide material. The polyamide material is prepared from, by weight, 100 parts of polyamide, 0.5-1 part of antioxidant, 1-1.5 parts of lubricant, 0.7-1.2 parts of thermal stabilizer, 1.3-1.8 parts of light stabilizer, 6-11 parts of fortifying agent, 4-9 parts of toughening agent, 3-3.5 parts of anti-friction agent, and 10-15 parts of modified compound brucite short fiber. The invention also discloses a preparation method for the polyamide material. The provided polyamide material has good water proof ability and strong flame retardant ability.
Description
Technical field
The present invention relates to a kind of macromolecular material, more particularly to a kind of polyamide material of waterproof flame retardant and manufacturer
Method.
Background technology
Polyamide is commonly called as nylon (Nylon), English name Polyamide (abbreviation PA), is to contain on molecular backbone to repeat
The thermoplastic resin general name of amide group [NHCO], including aliphatic PA, aliphatic-aromatic PA and aromatic series PA.Its
In, aliphatic PA is wide in variety, and yield is big, is widely used, depending on its name is by the specific carbon number of synthon.Due to polyamides
Amine has nontoxic, light weight, excellent mechanical strength, wearability and preferable corrosion resistance, is therefore widely used in replacing copper etc.
Metal manufactures bearing, gear, pump leaf and other parts in the industry such as machinery, chemical industry, instrument, automobile.Molten polyamide is spun into
There is very high intensity after silk, mainly make synthetic fibers can be used as medical suture.Polyamide is one of most important engineering plastics,
Yield ranks first in five big general engineering plastic.
It is limited that Publication No. CN102604371B, the day for announcing are 2014.04.16, grand science and technology share is gathered in the artificial Nanjing of application
The Chinese invention of company discloses " a kind of high performance-price ratio insulating heat-conductive polyamide compoiste material and preparation method thereof ", its weight hundred
Divide and be divided into than group：Polyamide：40%～95%, modifying common graphite：5%～35%, modified expanded graphite：1%～10%, change
Property flaky inorganic filler：1%～10%, lubricant：1%～5%, antioxidant：0.1%～1%, that above each group is divided and be
100%；Preparation method：Modifying common graphite, modified expanded graphite and modified sheeted filler are added in blender, 50 DEG C～90
5min～10min is blended at DEG C, obtains modified heat filling；By polyamide, modified heat filling, antioxidant and lubricant by joining
Ratio adds in blender, and 5～10min is blended；The material mixing is added in twin-screw extrusion owner's feed hopper,
Granulation is melt extruded at 230～260 DEG C.Although the composite of this invention has good insulation heat-conducting property and preferably comprehensive
Close mechanical property, but its water imbibition is still bigger than normal, resistance to water is not good, but also there is a problem of that anti-flammability is poor.
Content of the invention
The technical problem to be solved in the present invention is to provide a kind of polyamide material of waterproof flame retardant, and its resistance to water preferably and hinders
Combustion property is stronger.
For solving above-mentioned technical problem, the technical scheme is that：
A kind of polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of polyamide, antioxidant
0.5～1 part, 1～1.5 part of lubricant, 0.7～1.2 part of heat stabilizer, 1.3～1.8 parts of light stabilizer, 6～11 parts of reinforcing agent,
4～9 parts of toughener, 3～3.5 parts of anti-wear agent, modified compound 10～15 parts of shepardite chopped fiber.
Preferably, polyamide of the present invention is PA6 or PA12.
Preferably, antioxidant of the present invention is antioxidant KY-405.
Preferably, lubricant of the present invention is odium stearate.
Preferably, heat stabilizer of the present invention is cuprous halide compound stabilizer.
Preferably, light stabilizer of the present invention is phenyl salicylate.
Preferably, reinforcing agent of the present invention is talcum powder.
Preferably, toughener of the present invention is grafted EP rubbers for maleic anhydride.
Preferably, anti-wear agent of the present invention is silicone.
The invention solves the problems that another technical problem be the polyamide material that above-mentioned waterproof flame retardant is provided manufacture method.
For solving above-mentioned technical problem, technical scheme is：
A kind of manufacture method of the polyamide material of waterproof flame retardant, comprises the following steps：
(1) shepardite chopped fiber is added to the water stirring uniformly mixing slurry, soaks under room temperature after adding water reducer OT
15 hours, it is subsequently placed in vane type beater, stirring under 800 revs/min of speed stood 1 hour, by mixing slurry magnetic after 50 minutes
After choosing, deionized water is rinsed 10 minutes, obtains pretreated water magnesite chopped fiber after drying, wherein, shepardite chopped fiber, water, subtracts
The part by weight of aqua OT is 1:90:0.1；
(2) pretreated water magnesite chopped fiber is added in absolute ethyl alcohol, 45 DEG C of stirring in water bath uniformly add afterwards ammoniacal liquor, go from
Sub- water and tetraethyl orthosilicate, 45 DEG C, constant temperature stirring ageing 6 hours under 450 revs/min of speed, by the product obtaining absolute ethyl alcohol
With deionized water cyclic washing, it is placed in roasting at 450 DEG C in roaster and obtains within 4 hours compound shepardite chopped fiber, wherein, pre- place
Reason shepardite chopped fiber, absolute ethyl alcohol, ammoniacal liquor, deionized water, the part by weight of tetraethyl orthosilicate are 1:12:1:1:1；
(3) compound shepardite chopped fiber ultrasonic disperse is obtained the slurry that suspends for 30 minutes in absolute ethyl alcohol, by stearic acid plus
Enter and suspend in slurry, 75 DEG C of oil baths are stirred 2 hours, the product obtaining is filtered post-drying, after extracting removes unreacted stearic acid
Drying obtains modified compound shepardite chopped fiber, and wherein, compound shepardite chopped fiber, absolute ethyl alcohol, stearic weight ratio are
1:20:0.015；
(4) by weight the component in addition to modified compound shepardite chopped fiber is added 5 points of high-speed mixer and mixing
Clock obtains compound, adds mixture in double screw extruder, and modified compound shepardite chopped fiber is added with side feeding manner
At entering 230-280 DEG C in extruder, extruding pelletization obtains pellet, pellet is placed in drying at 90 DEG C in convection oven and obtains within 5 hours
The polyamide material of waterproof flame retardant.
Compared with prior art, the invention has the advantages that：
Shepardite chopped fiber is the mineral fibres that main chemical compositions are magnesium hydroxide, and its anti-flammability is very good, Bu Guoqi
Acid resistance is poor, there are a large amount of fibre bundles in structure, and impurity is more, leads to it to be difficult to be uniformly dispersed in polyamide, therefore originally
Invention is first disperseed by water reducer OT so as to fibre bundle decomposition is come, and impurity is also released simultaneously, Ran Houtong
Cross magnetic separation and eliminate major impurity magnetic iron ore, then other impurities are eliminated by deionized water rinsing and obtain purity and dispersiveness
The pretreated water magnesite chopped fiber all greatly improving, then with pretreated water magnesite chopped fiber as core, by sol-gel process
Obtain compound shepardite chopped fiber in its Surface coating silica shell, the acid resistance of silica is very good, compensate for water
The poor defect of magnesite chopped fiber acid resistance, but the silica in compound shepardite chopped fiber and shepardite chopped fiber are equal
Poor for the compatibility between hydrophilic material, and oil loving polyamide, therefore the present invention uses stearic acid to Compound Water magnesium
Stone chopped fiber has carried out surface modification, stearic acid is coated on the surface of compound shepardite chopped fiber, reduces its hydrophily, carry
Itself compatibility and polyamide between high has obtained modified compound shepardite chopped fiber, post-modification is blended with components such as polyamide
Compound shepardite chopped fiber can be uniformly dispersed in system, and then significantly improves the anti-flammability of polyamide material；On the other hand,
The water absorption rate of silica itself is less, and modified compound shepardite chopped fiber with polyamide blended after can be formed with polyamide
Preferably interface cohesion, thus improve the compactness of polyamide and producing good humidification, can reduce polyamides further
The water imbibition of amine, thus significantly improve the resistance to water of polyamide material.
Specific embodiment
To describe the present invention, the illustrative examples of the here present invention and explanation below in conjunction with specific embodiment in detail
It is used for explaining the present invention, but not as a limitation of the invention.
Embodiment 1
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA12, antioxidant KY-405
0.9 part, 1.1 parts of odium stearate, 1.2 parts of cuprous halide compound stabilizer, 1.3 parts of phenyl salicylate, 8 parts of talcum powder, maleic acid
Acid anhydride is grafted 7 parts of EP rubbers, 3 parts of silicone, modified compound 15 parts of shepardite chopped fiber.
The manufacture method of this polyamide material comprises the following steps：
(1) shepardite chopped fiber is added to the water stirring uniformly mixing slurry, soaks under room temperature after adding water reducer OT
15 hours, it is subsequently placed in vane type beater, stirring under 800 revs/min of speed stood 1 hour, by mixing slurry magnetic after 50 minutes
After choosing, deionized water is rinsed 10 minutes, obtains pretreated water magnesite chopped fiber after drying, wherein, shepardite chopped fiber, water, subtracts
The part by weight of aqua OT is 1:90:0.1；
(2) pretreated water magnesite chopped fiber is added in absolute ethyl alcohol, 45 DEG C of stirring in water bath uniformly add afterwards ammoniacal liquor, go from
Sub- water and tetraethyl orthosilicate, 45 DEG C, constant temperature stirring ageing 6 hours under 450 revs/min of speed, by the product obtaining absolute ethyl alcohol
With deionized water cyclic washing, it is placed in roasting at 450 DEG C in roaster and obtains within 4 hours compound shepardite chopped fiber, wherein, pre- place
Reason shepardite chopped fiber, absolute ethyl alcohol, ammoniacal liquor, deionized water, the part by weight of tetraethyl orthosilicate are 1:12:1:1:1；
(3) compound shepardite chopped fiber ultrasonic disperse is obtained the slurry that suspends for 30 minutes in absolute ethyl alcohol, by stearic acid plus
Enter and suspend in slurry, 75 DEG C of oil baths are stirred 2 hours, the product obtaining is filtered post-drying, after extracting removes unreacted stearic acid
Drying obtains modified compound shepardite chopped fiber, and wherein, compound shepardite chopped fiber, absolute ethyl alcohol, stearic weight ratio are
1:20:0.015；
(4) by weight the component in addition to modified compound shepardite chopped fiber is added 5 points of high-speed mixer and mixing
Clock obtains compound, adds mixture in double screw extruder, and modified compound shepardite chopped fiber is added with side feeding manner
At entering 230-280 DEG C in extruder, extruding pelletization obtains pellet, pellet is placed in drying at 90 DEG C in convection oven and obtains within 5 hours
The polyamide material of waterproof flame retardant.
Embodiment 2
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA6, antioxidant KY-405
0.7 part, 1.3 parts of odium stearate, 1 part of cuprous halide compound stabilizer, 1.5 parts of phenyl salicylate, 6 parts of talcum powder, maleic anhydride
9 parts of EP rubbers of grafting, 3.2 parts of silicone, modified compound 13 parts of shepardite chopped fiber.
The manufacture method of this polyamide material is same as Example 1.
Embodiment 3
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA12, antioxidant KY-405
0.5 part, 1.5 parts of odium stearate, 0.8 part of cuprous halide compound stabilizer, 1.7 parts of phenyl salicylate, 10 parts of talcum powder, maleic acid
Acid anhydride is grafted 5 parts of EP rubbers, 3.4 parts of silicone, modified compound 11 parts of shepardite chopped fiber.
The manufacture method of this polyamide material is same as Example 1.
Embodiment 4
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA6, antioxidant KY-405
1 part, 1 part of odium stearate, 0.9 part of cuprous halide compound stabilizer, 1.6 parts of phenyl salicylate, 9 parts of talcum powder, maleic anhydride connects
8 parts of EP rubbers of branch, 3.5 parts of silicone, modified compound 10 parts of shepardite chopped fiber.
The manufacture method of this polyamide material is same as Example 1.
Embodiment 5
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA6, antioxidant KY-405
0.8 part, 1.2 parts of odium stearate, 1.1 parts of cuprous halide compound stabilizer, 1.4 parts of phenyl salicylate, 11 parts of talcum powder, maleic acid
Acid anhydride is grafted 4 parts of EP rubbers, 3.3 parts of silicone, modified compound 12 parts of shepardite chopped fiber.
The manufacture method of this polyamide material is same as Example 1.
Embodiment 6
The polyamide material of waterproof flame retardant, is made up of the component of following parts by weight：100 parts of PA12, antioxidant KY-405
0.6 part, 1.4 parts of odium stearate, 0.7 part of cuprous halide compound stabilizer, 1.8 parts of phenyl salicylate, 7 parts of talcum powder, maleic acid
Acid anhydride is grafted 6 parts of EP rubbers, 3.1 parts of silicone, modified compound 14 parts of shepardite chopped fiber.
The manufacture method of this polyamide material is same as Example 1.
By test, the resistance to water of embodiment 1-6 and comparative example and anti-flammability are as shown in the table, wherein, comparative example
For the Chinese patent of Publication No. CN102604371B, resistance to water aspect tests out the suction of each material with reference to GB/T1034-2008
Water rate, the more little then resistance to water of water absorption rate is better, and the oxygen that fire resistance aspect tests out each material with reference to GB/T 2406-2008 refers to
Number, the more high then fire resistance of oxygen index (OI) is stronger：
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example | |
| Water absorption rate/% | 0.35 | 0.34 | 0.30 | 0.36 | 0.33 | 0.32 | 3.41 |
| Oxygen index (OI)/% | 28.8 | 28.9 | 29.2 | 28.7 | 29.0 | 29.3 | 25.3 |
As seen from the above table：The water absorption rate of embodiment 1-6 is significantly less than comparative example, and oxygen index (OI) is apparently higher than contrast simultaneously
Example, preferably and anti-flammability is stronger for the resistance to water of the surface present invention.
Above-described embodiment only principle of the illustrative present invention and effect, not for the restriction present invention.Any ripe
The personage knowing this technology all can carry out modifications and changes without prejudice under the spirit and the scope of the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete with institute under technological thought without departing from disclosed spirit such as
All equivalent modifications becoming or change, must be covered by the claim of the present invention.
Claims (10)
1. a kind of polyamide material of waterproof flame retardant is it is characterised in that be made up of the component of following parts by weight：Polyamide 100
Part, 0.5～1 part of antioxidant, 1～1.5 part of lubricant, 0.7～1.2 part of heat stabilizer, 1.3～1.8 parts of light stabilizer, reinforcing agent
6～11 parts, 4～9 parts of toughener, 3～3.5 parts of anti-wear agent, modified compound 10～15 parts of shepardite chopped fiber.
2. a kind of waterproof flame retardant according to claim 1 polyamide material it is characterised in that：Described polyamide is PA6
Or PA12.
3. a kind of waterproof flame retardant according to claim 2 polyamide material it is characterised in that：Described antioxidant is antioxygen
Agent KY-405.
4. a kind of waterproof flame retardant according to claim 3 polyamide material it is characterised in that：Described lubricant is tristearin
Sour sodium.
5. a kind of waterproof flame retardant according to claim 4 polyamide material it is characterised in that：Described heat stabilizer is halogen
Change cuprous compound stabilizer.
6. a kind of waterproof flame retardant according to claim 5 polyamide material it is characterised in that：Described light stabilizer is water
Poplar acid phenenyl ester.
7. a kind of waterproof flame retardant according to claim 6 polyamide material it is characterised in that：Described reinforcing agent is talcum
Powder.
8. a kind of waterproof flame retardant according to claim 7 polyamide material it is characterised in that：Described toughener is Malaysia
Acid anhydrides is grafted EP rubbers.
9. a kind of waterproof flame retardant according to claim 8 polyamide material it is characterised in that：Described anti-wear agent is silicon
Ketone.
10. the manufacture method of the polyamide material of a kind of waterproof flame retardant according to claim 1～9 any one, it is special
Levy and be, comprise the following steps：
(1) shepardite chopped fiber is added to the water stirring uniformly mixing slurry, soaks 15 under room temperature after adding water reducer OT little
When, it is subsequently placed in vane type beater, stirring under 800 revs/min of speed stood 1 hour, after mixing slurry magnetic separation after 50 minutes
Deionized water is rinsed 10 minutes, obtains pretreated water magnesite chopped fiber, wherein, shepardite chopped fiber, water, water reducer after drying
The part by weight of OT is 1:90:0.1；
(2) pretreated water magnesite chopped fiber is added in absolute ethyl alcohol, 45 DEG C of stirring in water bath uniformly add ammoniacal liquor, deionized water afterwards
And tetraethyl orthosilicate, 45 DEG C, constant temperature stirring ageing 6 hours under 450 revs/min of speed, by the product obtaining absolute ethyl alcohol with go
Ionized water cyclic washing, is placed in roasting at 450 DEG C in roaster and obtains within 4 hours compound shepardite chopped fiber, wherein, pretreated water
Magnesite chopped fiber, absolute ethyl alcohol, ammoniacal liquor, deionized water, the part by weight of tetraethyl orthosilicate are 1:12:1:1:1；
(3) compound shepardite chopped fiber ultrasonic disperse is obtained the slurry that suspends for 30 minutes in absolute ethyl alcohol, stearic acid is added outstanding
In laitance, 75 DEG C of oil baths are stirred 2 hours, and the product obtaining is filtered post-drying, and extracting removes unreacted stearic acid post-drying
Obtain modified compound shepardite chopped fiber, wherein, compound shepardite chopped fiber, absolute ethyl alcohol, stearic weight ratio is for 1:20:
0.015；
(4) by weight the component in addition to modified compound shepardite chopped fiber is added high-speed mixer and mixing to obtain for 5 minutes
To compound, add mixture in double screw extruder, modified compound shepardite chopped fiber is added with side feeding manner and squeezes
At going out 230-280 DEG C in machine, extruding pelletization obtains pellet, by pellet be placed at 90 DEG C in convection oven drying obtain within 5 hours water-fast
Fire-retardant polyamide material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611053987.9A CN106398200A (en) | 2016-11-25 | 2016-11-25 | Water proof flame retardant polyamide material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611053987.9A CN106398200A (en) | 2016-11-25 | 2016-11-25 | Water proof flame retardant polyamide material and preparation method thereof |
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| CN106398200A true CN106398200A (en) | 2017-02-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611053987.9A Pending CN106398200A (en) | 2016-11-25 | 2016-11-25 | Water proof flame retardant polyamide material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054373A (en) * | 2018-06-28 | 2018-12-21 | 西安永兴科技发展有限公司 | A kind of contact nets in electrified railways are fixed to hang device for carrying a tripot nylon material and preparation method thereof |
| CN115746570A (en) * | 2022-12-07 | 2023-03-07 | 华力通线缆股份有限公司 | Ceramic fire-resistant sheath material and medium-voltage fire-resistant cable |
Citations (1)
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| CN101747622A (en) * | 2008-12-22 | 2010-06-23 | 上海日之升新技术发展有限公司 | Brucite flame-retardant reinforced nylon compound and preparation method thereof |
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2016
- 2016-11-25 CN CN201611053987.9A patent/CN106398200A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747622A (en) * | 2008-12-22 | 2010-06-23 | 上海日之升新技术发展有限公司 | Brucite flame-retardant reinforced nylon compound and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张伟娜等: "纤维增强型二氧化硅气凝胶的制备条件优化研究", 《吉林师范大学学报（自然科学版）》 * |
| 曹曦等: "纤水镁石的提纯与改性", 《矿物学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109054373A (en) * | 2018-06-28 | 2018-12-21 | 西安永兴科技发展有限公司 | A kind of contact nets in electrified railways are fixed to hang device for carrying a tripot nylon material and preparation method thereof |
| CN115746570A (en) * | 2022-12-07 | 2023-03-07 | 华力通线缆股份有限公司 | Ceramic fire-resistant sheath material and medium-voltage fire-resistant cable |
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Application publication date: 20170215 |