CN109294226A - A kind of fire-retardant PA composite material and preparation method of enhancing - Google Patents
A kind of fire-retardant PA composite material and preparation method of enhancing Download PDFInfo
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- CN109294226A CN109294226A CN201811049322.XA CN201811049322A CN109294226A CN 109294226 A CN109294226 A CN 109294226A CN 201811049322 A CN201811049322 A CN 201811049322A CN 109294226 A CN109294226 A CN 109294226A
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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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
- 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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- 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
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Abstract
The present invention relates to a kind of fire-retardant PA composite material and preparation methods of enhancing.The fire-retardant PA composite material of the enhancing, the component including following parts by weight: 10~80 parts of polyamide；2~15 parts of bonding agent；15~25 parts of fireproof agent；1~5 part of toughener；15~60 parts of filler；Wherein, the bonding agent is the bonding agent containing highly polar functional group, and the highly polar functional group is selected from-COOH ,-MAH ,-GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO.The fire-retardant PA composite material of enhancing of the invention has the strong cementability to metal such as brass etc., not easy to crack, leakage characteristic；In addition, each ingredient gives full play to synergistic effect in composition, good fire protecting performance and excellent mechanical property are kept.
Description
Technical field
The present invention relates to functionalization modifying plastics field more particularly to a kind of fire-retardant PA composite material of enhancing and its preparations
Method.
Background technique
Polyamide PA resin (nylon) is that the Carothers of DuPont is succeeded in developing at first, in nineteen thirty-nine reality
Now industrialize.Initial 30 years which are mainly applied to fiber art, the 1950s initially as engineering plastics application, and
Growth momentum is swift and violent, becomes five large-engineering plastics together with PC, POM, PPO, PBT, and there is a sharp increase in output, and extend be applied to it is each
Field.
Containing there are many amide groups of repetitive unit on polyamide PA main chain, claim nylon when as plastics, is used as synthetic fibers
When, PA6 is known as polyamide fibre.PA has good comprehensive performance, including mechanical property, heat resistance, wear resistance, chemical-resistant resistance
Property and self-lubrication, and coefficient of friction is low, there is certain anti-flammability, it is easy to process, suitable for being filled out with glass fibre and other fillers
It fills enhancing to be modified, improve performance and expands application range.
Polyamide PA can be produced by diamine and binary acid, can also be synthesized with omega-amino acid or cyclic lactam.Root
According to the difference containing carbon atom number in diamine and binary acid or amino acid, a variety of different polyamide can be made, wherein with
PA6, PA66 and PA610's is most widely used, other nylon PA11, PAl2, PA46, PA610, PAl010 are also quickly sent out
Exhibition, the seventies, semi-aromatic nylon PA6T also started to rise with extraordinary nylon, and sharp increase at the beginning of the eighties to 2000 is domestic
Also sharp increase after 2010.
PA6 is mainly used in automobile, machinery, electrical apparatus product functional parts currently on the market；PA66 is sent out applied to automobile
Motivation periphery heat-resistant part, 610 and 612 often do wire and cable covering material, high temperature PA material using its flexibility, wearability length
Expect applying electronic appliance field, the precise parts such as connector, connector, Tack switch, type-C, water treatment field, light
Volt industry automobile oil guide pipe, cooling system, grid also have fairly large application.
Enhance fire-retardant PA composite material, is being applied to connector, when the fields such as connector, is often being connect with brass ware
Touching, cladding or insertion, however, in bonding site, often due to the bonding of enhancing fire-retardant PA composite material and brass ware
Property poor and generate Welding Problems, infiltration, leakage such as scaling powder, so as to cause metal parts loosening, setup error, even
Lead to scrap of the product.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of fire-retardant PA composite materials of enhancing, it is intended to it is fire-retardant to solve enhancing
The poor technical problem of the caking property of PA composite material and metal.
Its technical solution is as follows:
A kind of fire-retardant PA composite material of enhancing, the component including following parts by weight:
Wherein, the bonding agent be the bonding agent containing highly polar functional group, and the highly polar functional group be selected from-
COOH ,-MAH ,-GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO.
Further, the bonding agent is selected from the grafting of polyester-type thermoplastic polyurethane elastomer, the graft of PE, EVA
One or more of object, styrene maleic anhydride copolymer.
It is described poly- in the fire-retardant PA composite material of enhancing described in every 100 parts by weight in one of them embodiment
The parts by weight of amide PA are 25~65 parts.
It is described viscous in the fire-retardant PA composite material of enhancing described in every 100 parts by weight in one of them embodiment
The parts by weight for connecing agent are 2~10 parts.
Further, the filler is one or both of talcum powder or glass；And/or the toughener is benzene
Ethylene-butadiene-styrene block copolymer.
Further, the partial size of the talcum powder is 800~2000 mesh；The glass diameter is 10~17um, is selected short
Cut glass or continuous glass-fiber.
In one of them embodiment, the parts by weight of the toughener are 2~5 parts.
Further, enhancing fire-retardant PA composite material further includes the lubricant and 0.1~2 that parts by weight are 0.1~1 part
The antioxidant of part.
Further, the polyamide PA, relative density are 1.01~1.20g/cm3。
Another object of the present invention is to provide a kind of preparation methods for enhancing fire-retardant PA composite material, including following step
It is rapid:
The formula of the S1 fire-retardant PA composite material of enhancing according to any one of claims 1 to 8 weighs each component, will
Each component is mixed, and is kept each component fully dispersed uniformly, is obtained mixture；
S2 is squeezed out in the resulting mixture investment extruder of S1 after melting；
S3 obtains having the fire-retardant PA composite material of the enhancing of good adhesion through supercooling, air-dried and pelletizing.
The extruder is double screw extruder, and the extrusion processing temperature of the double screw extruder is respectively as follows: feed opening
180 DEG C, 210 DEG C~350 DEG C of middle part, 240 DEG C~360 DEG C of head temperature, screw speed is 200rpm~600rpm.
Compared with prior art, the bonding agent of the present invention enhanced in fire-retardant PA composite material containing 2~15 parts,
And the bonding agent be the bonding agent containing highly polar functional group, and the highly polar functional group be selected from-COOH ,-MAH ,-
GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO.When the fire-retardant PA of the enhancing that will contain above-mentioned bonding agent is answered
When condensation material is coated on metal surface, under the action of metal surface, open loop can occur for functional group-MAH ,-GMA ,-epoxy group
Reaction, and stronger bonding force is generated with metal surface, multi-point-anchoring effect is generated in metal surface, to play firm viscous
Connect effect, and functional group-COOH ,-OH ,-NH2,-NCO there is stronger polarity, have with metal surface and stronger be bonded
Power can be strongly adhered on metal surface.Therefore the fire-retardant PA composite material of enhancing provided by the invention has to metal such as
The strong cementability of brass etc., not easy to crack, leakage characteristic.In addition, each in the fire-retardant PA composite material of enhancing provided by the invention
Ingredient gives full play to synergistic effect, keeps good fire protecting performance and excellent mechanical property.
The preparation method process of the fire-retardant PA composite material of enhancing provided by the present invention is simple, process conditions are reasonable, manufacture
It is at low cost.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to this hair
It is bright to be further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, not
For limiting the present invention.
The fire-retardant PA composite material of the enhancing of the embodiment of the present invention, the component including following parts by weight:
10~80 parts of polyamide PA, 2~15 parts of bonding agent, 15~25 parts of fireproof agent and 1~5 part of toughening
Agent, 15~60 parts of filler；
Wherein, the bonding agent be the bonding agent containing highly polar functional group, and the highly polar functional group be selected from-
COOH ,-MAH ,-GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO.
In above scheme, when the fire-retardant PA composite material of the enhancing for containing above-mentioned bonding agent is coated on metal surface
When, under the action of metal surface, ring-opening reaction can occur for functional group-MAH ,-GMA ,-epoxy group, and generate with metal surface
Stronger bonding force generates multi-point-anchoring effect in metal surface, so that firm adhesive effect is played, and functional group-COOH ,-
OH、-NH2,-NCO have stronger polarity, with metal surface have stronger bonding force, metal watch can be strongly adhered to
On face.Therefore, the resulting fire-retardant PA composite material of enhancing of the present invention has the strong cementability to metals such as brass.
In the embodiment of the present invention, bonding agent is selected from polyester-type thermoplastic polyurethane elastomer, the graft of PE, EVA
One or more of graft, styrene maleic anhydride copolymer.The bonding agent that this programme is selected, it is preferable with PA compatibility,
While increasing the adhesive property for enhancing fire-retardant PA composite material, the influence to other performance is smaller.In addition, this programme selects
Bonding agent is cheap, and cost is relatively low.
Further, in the fire-retardant PA composite material of enhancing described in every 100 parts by weight, the parts by weight of polyamide are preferred
It is 25~65 parts.It is more appropriate in the polyamide of this programme, while meeting other performance, there is lower cost.
Further, in the fire-retardant PA composite material of enhancing described in every 100 parts by weight, the parts by weight of bonding agent are preferred
It is 2~10 parts.It is bonding with metal can to improve the fire-retardant PA composite material of enhancing for the bonding agent content that this programme uses
Property, and it can be reduced to the intensity bring counter productive for enhancing fire-retardant PA composite material.
Further, in the fire-retardant PA composite material of enhancing described in every 100 parts by weight, the parts by weight of toughener are preferred
It is 2~5 parts.
The filler that the embodiment of the present invention uses is one or both of talcum powder or glass；Wherein talcum powder
Partial size is preferably 800~2000 mesh；The glass diameter is 10~17um, selects chopped glass fiber or continuous glass-fiber.In can be used
The glass 568H of megalith limited liability company of state production, 540, the glass ECS- of Chongqing Polycomp International Co., Ltd's production
301H, the glass 910-10P of OWENS CORNING company production, 995.When the partial size of talcum powder is too small or the diameter of glass is too small
When, the diffusion effect in PA is poor, cannot be well dispersed in system, causes the intensity of finished product uneven.This programme
In, the particle size range of the talcum powder of selection and the diameter range of glass then can be fully scattered in PA, have finished product uniform
Intensity.
The toughener that the embodiment of the present invention uses is Styrene-Butadiene-Styrene Block Copolymer (SBS).It can adopt
3501F, the 3540F produced with Lee Chang Yung Chemical Indust, 475P, 501P of LG chemistry, the U.S.
The 840A of Firestone company, 8508；POE LC150, the LC175 of LG company, the POE 8150 and three wells of DuPont Dow Elastomers
The DF610 etc. of chemistry.
It is able to satisfy environmental requirement simultaneously for enhancing flame retardant effect, the fireproof agent of the present embodiment selects aromatic radical or alkylation
The phosphate of aromatic radical, tert-butyl benzene diphenylphosphoric acid enzyme, decabromodiphenylethane, brominated Polystyrene, brominated polystyrene,
Brominated epoxy resin, diethyl hypophosphites (the OP fire-retardant agent of such as Clariant), polypentabrombenzamide acrylate, three oxygen
Change one or more of compounds of the kinds such as two antimony, sodium antimonate, sodium stannate, zinc stannate.
In addition, enhancing fire-retardant PA composite material further includes in order to improve the light of product, thermal stability and processing performance
Parts by weight are 0.1~1 part of lubricant and 0.1~2 part of antioxidant.Antioxidant used in the embodiment of the present invention is divided into master
Antioxidant and auxiliary type antioxidant；Primary antioxidant uses four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrites
Ester (trade name IRGANOX1010) or N, N '-hexamethylene bis (3,5- di-t-butyl -4- hydroxyl hydrocinnamamide) (trade name
One or both of IRGANOX1098)；The auxiliary type antioxidant uses three (2,4- di-tert-butyl-phenyl) phosphorous
Acid esters (trade name IRGANOX168) or bis- (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites (trade name
One or both of IRGANOX626,627)；The lubricant uses pentaerythritol stearate (PETS), ethylene
One or more of bis-stearamides (EBS) etc..
Further, enhancing fire-retardant PA composite material can also include other processing aids, such as dispersing agent.The dispersion
Agent is preferably but not limited to the one of which such as 5# White Mineral Oil, silicone oil or two kinds.
Further, the polyamide PA, relative density are 1.01~1.20g/cm3.It is of the present invention poly-
Amide PA material it is from a wealth of sources, as PA6, PA66, PA610, PA612, PA11, PA12, PPA, 6T and copolymer, 66/X are total
Polymers, 10T, 11T, 12T, 13T, MXD6, MXD10.Using PA66 in the present embodiment.
The fire-retardant PA material of the above-mentioned enhancing with good adhesion may be selected double screw extruder, single screw extrusion machine,
Reciprocating extruder etc. is process.
The preparation method of the above-mentioned fire-retardant PA material of enhancing with good adhesion, comprising the following steps:
S1 prepares good material by component and quantity (parts by weight) described in table 1, and each component is mixed in super mixer
It closes, keeps each component fully dispersed uniformly；
S2 is squeezed out in the resulting mixture investment double screw extruder of S1 after melting；
S3 obtains having the fire-retardant PA composite material of the enhancing of good adhesion through supercooling, air-dried and pelletizing.
The extrusion processing temperature of the double screw extruder is respectively 180 DEG C of feed opening, 210 DEG C~350 DEG C of middle part, machine
240 DEG C~360 DEG C of temperature of head, screw speed are 200rpm~600rpm.
It is illustrated combined with specific embodiments below.
Embodiment 1
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 1 of table.
The preparation method of the fire-retardant PA composite material of enhancing, includes the following steps:
S1 prepares good material by the corresponding component of embodiment 1 in table 1 and quantity (parts by weight), and each component is mixed in high speed
It is mixed in clutch, keeps each component fully dispersed uniformly；
S2 is squeezed out in the resulting mixture investment double screw extruder of S1 after melting；
S3 obtains having the fire-retardant PA material of the enhancing of good adhesion through supercooling, air-dried and pelletizing.
The extrusion processing temperature of the double screw extruder is respectively 180 DEG C of feed opening, 210 DEG C~350 DEG C of middle part, machine
240 DEG C~360 DEG C of temperature of head, screw speed are 200rpm~600rpm.
Embodiment 2
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 2 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 3
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 3 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 4
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 4 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 5
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 5 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 6
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 6 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 7
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 7 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Embodiment 8
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 embodiment 8 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Comparative example 1
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 comparative example 1 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
Comparative example 2
A kind of fire-retardant PA composite material of enhancing, each component including parts by weight shown in 1 comparative example 2 of table.
The preparation method of the fire-retardant PA composite material of enhancing is same as Example 1.
The formula composition of the fire-retardant PA material of enhancing of embodiment and comparative example is as shown in table 1 below.
Table 1
The fire-retardant PA material of enhancing prepared to above-described embodiment 1~8 and comparative example 1~2 is tested for the property, test mark
Quasi- and test result is shown in Table 2.
Table 2
Note: red ink leaks time test method: it is soaked in 50 DEG C of red ink, and records the leakage time, 96 hours
It is non-leakage for not occurring leakage phenomenon inside.
From table 1, table 2 it can be seen that
(1) bonding agent is affected to the adhesive strength and red ink osmotic effect of material, and additive amount is more, material
Cementability it is better, but mechanical strength loss it is bigger, as shown in Examples 1 to 44, comparative example 1,2；Therefore bonding agent
Content as mass fraction be preferably 2~10%.
(2) number of bonding agent increases, and has a certain impact to fire prevention, but fire-protection rating is attained by V0 rank；And
With the increase of bonding agent, material is mitigated, and is had a certain upgrade advantage to material cost performance；
(3) although can achieve V0 rank without the material fire-protection rating of glass, its mechanical strength fall compared with
Greatly, intensity only about enhances the 1/3 of fire-retardant PA material；
It is obtained in conjunction with above-mentioned analysis, the present invention uses the bonding agent of 2~10% mass fractions, has highly polar functional group-
COOH ,-MAH ,-GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO, when will contain described in above-mentioned bonding agent
When enhancing fire-retardant PA composite material and being coated on metal surface, under the action of metal surface, functional group-MAH ,-GMA ,-epoxy
Ring-opening reaction can occur for base, and generate stronger bonding force with metal surface, generate multi-point-anchoring effect in metal surface, from
And firm adhesive effect is played, and functional group-COOH ,-OH ,-NH2,-NCO have stronger polarity, have with metal surface
Stronger bonding force can be strongly adhered on metal surface.In addition, the mass fraction of packing material is 15~60%
When, there is preferable mechanical strength；The mass fraction of fireproof agent has preferable flame retardant effect at 15~25%；By this hair
The excellent combination property of the bright enhancing fire-retardant PA material obtained with good adhesion, has good adhesive property, power
Performance and processing performance are learned, and the heatproof with chemical-resistant resistance and wide scope.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (10)
1. a kind of fire-retardant PA composite material of enhancing, which is characterized in that the component including following parts by weight:
Wherein, the bonding agent be the bonding agent containing highly polar functional group, and the highly polar functional group be selected from-COOH ,-
MAH ,-GMA ,-OH ,-epoxy group ,-NH2, one or more of-NCO.
2. enhancing fire-retardant PA composite material as described in claim 1, which is characterized in that the bonding agent is selected from polyester-type thermoplastic
One or more of property polyurethane elastomer, the graft of PE, the graft of EVA, styrene maleic anhydride copolymer.
3. enhancing fire-retardant PA composite material as claimed in claim 1 or 2, which is characterized in that enhancing described in every 100 parts by weight
In fire-retardant PA composite material, the parts by weight of the polyamide are 25~65 parts.
4. enhancing fire-retardant PA composite material as claimed in claim 1 or 2, which is characterized in that enhancing described in every 100 parts by weight
In fire-retardant PA composite material, the parts by weight of the bonding agent are 2~10 parts.
5. enhancing fire-retardant PA composite material as claimed in claim 1 or 2, which is characterized in that the filler be talcum powder or
One or both of glass；And/or the toughener is Styrene-Butadiene-Styrene Block Copolymer.
6. enhancing fire-retardant PA composite material as claimed in claim 5, which is characterized in that the partial size of the talcum powder be 800~
2000 mesh；The glass diameter is 10~17um, selects chopped glass fiber or continuous glass-fiber.
7. enhancing fire-retardant PA composite material as claimed in claim 1 or 2, which is characterized in that further include parts by weight be 0.1~
1 part of lubricant and 0.1~2 part of antioxidant.
8. enhancing fire-retardant PA composite material as claimed in claim 1 or 2, which is characterized in that the relative density of the polyamide
For 1.01~1.20g/cm3。
9. a kind of preparation method for enhancing fire-retardant PA composite material, which comprises the following steps:
The formula of the S1 fire-retardant PA composite material of enhancing according to any one of claims 1 to 8 weighs each component, by each component
It is mixed, keeps each component fully dispersed uniformly, obtain mixture；
S2 is squeezed out in the resulting mixture investment extruder of S1 after melting；
S3 obtains having the fire-retardant PA composite material of the enhancing of good adhesion through supercooling, air-dried and pelletizing.
10. enhancing the preparation method of fire-retardant PA composite material as claimed in claim 9, which is characterized in that the extruder is
Double screw extruder, the extrusion processing temperature of the double screw extruder are respectively as follows: 180 DEG C of feed opening, middle part 210 DEG C~350
DEG C, 240 DEG C~360 DEG C of head temperature, screw speed is 200rpm~600rpm.
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