CN106854295A - A kind of whiteness red phosphorus, nylon distribute whiteness red phosphorus flame-retardant masterbatch and preparation method thereof with low smell is low - Google Patents
A kind of whiteness red phosphorus, nylon distribute whiteness red phosphorus flame-retardant masterbatch and preparation method thereof with low smell is low Download PDFInfo
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- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch and preparation method thereof, it is prepared from by weight by following components：50 85 parts of whiteness red phosphorus, 15 parts of hydrophobic type odor adsorption master batch, 0.2~1.0 part of antioxidant, 0.2 1 parts of lubricant.The red phosphorus flame-retardant masterbatch versatility for preparing of the invention is wide, active ingredient is high, low without obvious smell, addition, and preparation method is simple, while also breaching the limitation in color, product is not limited to dark product, and dust pollution can be effectively reduced, improve work situation.
Description
Technical field
The present invention relates to a kind of whiteness red phosphorus, low smell, low distribute modified red phosphorus flame-retardant nylon material and its preparation side
Method, belongs to technical field of polymer materials.
Background technology
Nylon is the general engineering plastic with excellent comprehensive performance, with excellent mechanical performance and wear-resisting, solvent resistant,
The advantages of oil resistant, it is widely used in every profession and trade.But nylon belongs to combustible material, in order to meet flame retardant products requirement, it is necessary to
Numerous studies are carried out to fire-retardant aspect.And red phosphorus is a kind of excellent halogen-free environment-friendly type flame-proof agent, flame retarding efficiency is high, with other resistances
Combustion agent is compared, and addition needed for reaching identical fire-retardant rank is few, thus small on the physical and mechanical property influence of material.But it is also deposited
Such as oxidizable rotten in atmosphere in some shortcomings, the easy moisture absorption, oxidation generate phosphoric acid and discharge severe toxicity in atmosphere for exposure
Phosphine gas, the aubergine of itself has limitation to preparing light plastic products.Therefore, red phosphorus is used as fire retardant, only
Have by just there is actual application value after surface treatment.
The content of the invention
It is an object of the invention to provide a kind of whiteness red phosphorus, nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain and preparation method thereof.
In order to realize the purpose of the present invention, the invention provides a kind of whiteness red phosphorus, described whiteness red phosphorus is micro-
Capsule red phosphorus, described microcapsule red phosphorus are aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin, the preparation of the microcapsule red phosphorus：
It is made of the raw material including following weight proportion：Red phosphorus 25-35%, aluminum sulfate 5-15%, urea 10-15%, water 50-
59%, oil-soluble phenolic resin resin 1-5%；Aluminium hydroxide coats process：Aluminum sulfate is added to the water first, stirring has been allowed to
CL, then puts into red phosphorus, stirs 20min, then is transferred in ball mill and is ground to red phosphorus particle diameter untill 5-10um,
Then it is transferred in reactor, adds caustic soda (5-15wt% solution) slowly while stirring, untill the PH=5-6 of system, then
It (can be the flocculation agents such as conventional PB1 gene or polyacrylamide PAM, consumption may generally be system to add flocculation agent
The 0.1%-1% of weight), stir, in 75-85 DEG C of scope inside holding 1.5h, filtering is eventually passed, washed, be dried to obtain
Aluminium hydroxide encapsulated red phosphorus；Phenolic resin coats process：Dimethylbenzene first with 2.5-3.0 times of volume is dilute by oil-soluble phenolic resin
Release, then aluminium hydroxide encapsulated red phosphorus are mixed with oil-soluble phenolic resin dilution, stir into pasty state homogeneous state, send into band
Reclaim in the drier of xylene unit, 60 ± 5 DEG C of temperature of control is dried, and obtains final product aluminium hydroxide and phenolic resin double-contracting is covered
Red phosphorus.
Present invention also offers a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, pressed by following components
Weight portion is prepared from：
Whiteness red phosphorus 20-50,
The 45-80 of nylon 6
1-5 parts of hydrophobic type odor adsorption master batch,
Silane coupler 0.5-1 parts
0.2~1.0 part of antioxidant
0.2~1.0 part of lubricant
Described whiteness red phosphorus is microcapsule red phosphorus, and described microcapsule red phosphorus are aluminium hydroxide and phenolic resin double-contracting
Cover red phosphorus.
The described inherent viscosity of nylon 6 is 2.0-3.6.
Described hydrophobic type odor adsorption master batch is made up of the component of following weight portion：40~75 parts of PA6, hydrophobicity silicon
10~20 parts of diatomaceous earth, 1~5 part of ferriferous oxide, 0~10 part of hydrophobic active charcoal, 5~10 parts of needle-like zeolite molecular sieve, castor oil
5~10 parts of sour zinc, 5~10 parts of antiseptic, 0.1-0.5 parts of Benzopyranone kind the free radical scavenger, [β-(3,5- of antioxidant four
Di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 0.2-0.5 parts, antioxidant three [2.4- di-tert-butyl-phenyls] phosphorous acid
Ester 0.2-0.5 parts, 0.5-1.0 parts of lubricant stearic acid zinc；Described antiseptic is the nano-silica of grafting polymer quaternary ammonium salt
SiClx；Described Benzopyranone kind free radical scavenger is 5,7- bis--(2,2- dimethyl ethyls) -3- (3,4- dimethyl benzenes
Base) -2-3 hydrogen-benzofuranone.The ferriferous oxide is ferroso-ferric oxide and di-iron trioxide 1：The active iron oxidation of 1 mixing
Thing.
Described silane coupler is gamma-aminopropyl-triethoxy-silane (KH550) or γ-(methacryloxypropyl) propyl group
Trimethoxy silane (KH570).
Described antioxidant is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters, N, N'- be double-
(3- (3,5- di-tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, the mixing of three [2.4- di-tert-butyl-phenyls] phosphite esters
Thing.
Described lubricant is silicone powder.
It is a further object to provide above-mentioned nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch
Preparation method, comprises the following steps：
Microcapsule red phosphorus, hydrophobicity odor adsorption master batch, nylon, silane coupler, antioxidant and lubricant are poured into height
In fast mixer, high-speed stirred mixes into uniform rear addition double screw extruder, is granulated after melting extrusion, and low gas is obtained
Taste, it is low distribute, high abrasion-proof and high temperature resistant nylon.
The area's temperature of the double screw extruder one is 200-230 DEG C, and two area's temperature are 200-230 DEG C, and three area's temperature are
200-240 DEG C, four area's temperature are 210-240 DEG C, and five area's temperature are 210-250 DEG C, and six area's temperature are 220-250 DEG C；Twin-screw
Engine speed is 250-500rpm.
Beneficial effects of the present invention：
1. hydrophobic type odor adsorption master batch of the present invention significantly reduces phosphatization in red phosphorus flame-retardant masterbatch thermoforming process
The release of hydrogen, significantly reduces total volatile organism TVOC, is also maintained while guarantee fire-retardant master granule low odor property
Relatively low water absorption rate；The molding processibility that does not then interfere with matrix plastic is added in nylon matrix plastics as fire-retardant master granule
Energy.
Whiteness red phosphorus after 2 claddings, substantially overcomes the easy moisture absorption of red phosphorus, oxidizable problem, while in smell
The PH3 generating capacities in thermoforming process are significantly reduced under the synergy for adsorbing master batch, while also breaching in color
Limitation, product is not limited to dark product.
Specific embodiment
Below by way of the description of specific embodiment, the invention will be further described, but this is not to limit of the invention
System, those skilled in the art's basic thought of the invention, various modifications may be made or improves, but without departing from this
The basic thought of invention, within the scope of the present invention.
Specific embodiment
Below by way of the description of specific embodiment, the invention will be further described, used in embodiments below
Whiteness red phosphorus and odor adsorption master batch are prepared from by following method：
The preparation of whiteness red phosphorus：Red phosphorus 30%, aluminum sulfate 10%, urea 5%, water 50%, oil-soluble phenolic resin
5%.Aluminium hydroxide coats process：Aluminum sulfate is added to the water first, stirring is allowed to be completely dissolved, and then puts into red phosphorus, stirs
Mix 20min, then be transferred in ball mill and be ground to red phosphorus particle diameter untill 5-10um, be then transferred in reactor, side stirring
While addition caustic soda (10wt% solution) that blows slowly, untill the PH=5-6 of system, adds flocculation agent polyacrylamide, stir
Uniformly, in 75-85 DEG C of scope inside holding 1.5h, filtering is eventually passed, is washed, is dried to obtain aluminium hydroxide encapsulated red phosphorus.Phenolic aldehyde
Resin-coating process：Oil-soluble phenolic resin is diluted with 2.5-3.0 times of dimethylbenzene first, then by aluminium hydroxide encapsulated red phosphorus with oil
Dissolubility phenolic resin dilution is mixed, and stirs into pasty state homogeneous state, and feeding is controlled with the drier for reclaiming xylene unit
60 ± 5 DEG C of temperature processed is dried, and obtains final product aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin.
The preparation of hydrophobic type odor adsorption master batch：6 50 parts of nylon, 15 parts of hydrophobicity diatomite, 2 parts of ferroso-ferric oxide, three
Aoxidize 2 parts of two iron, 5 parts of hydrophobic active charcoal, 10 parts of needle-like zeolite molecular sieve, 10 parts of zinc ricinate, high molecular quaternary connects
5 parts of nano silicon of branch, 5,7- bis--(2,2- dimethyl ethyl) -3- (3,4- 3,5-dimethylphenyl) -2-3 hydrogen-benzofuranone
0.1 part, antioxidant four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] 0.2 part of pentaerythritol ester, [2.4- of antioxidant three
Di-tert-butyl-phenyl] 0.2 part of phosphite ester, 0.5 part of addition high-speed mixer of zinc stearate is well mixed, then crowded in twin-screw
Go out extruding pelletization in machine and obtain hydrophobic type odor adsorption master batch.
Embodiment 1
By 40 parts of whiteness red phosphorus, 55 parts of nylon, 6,3 parts of hydrophobic type odor adsorption master batches, 0.6 part of silane coupler, 0.2
Part 1098,0.2 part of irgasfos 168 of antioxidant and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, be obtained the low smell of nylon, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
Embodiment 2
By 20 parts of whiteness red phosphorus, 77 parts of nylon, 6,1 part of hydrophobic type odor adsorption master batch, 0.8 part of silane coupler, 0.5
Part 1098,0.5 part of irgasfos 168 of antioxidant and 0.2 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to uniform
Afterwards add double screw extruder in, after melting extrusion granulate, be obtained nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant
Master batch.
Wherein the area's temperature of double screw extruder one is 230 DEG C, and two area's temperature are 230 DEG C, and three area's temperature are 240 DEG C, 4th area
Temperature is 240 DEG C, and five area's temperature are 250 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 500rpm.
Embodiment 3
By 50 parts of whiteness red phosphorus, 43 parts of nylon, 6,5 parts of hydrophobic type odor adsorption master batches, 1 part of silane coupler, 0.2 part
1098,0.3 part of irgasfos 168 of antioxidant and 0.5 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, be obtained the low smell of nylon, it is low distribute, whiteness red phosphorus flame-retardant it is female
Grain.
Wherein the area's temperature of double screw extruder one is 205 DEG C, and two area's temperature are 205 DEG C, and three area's temperature are 210 DEG C, 4th area
Temperature is 215 DEG C, and five area's temperature are 220 DEG C, and six area's temperature are 225 DEG C；Twin-screw engine speed is 250rpm.
Comparative example 1
By 40 parts of untreated red phosphorus, 55 parts of nylon, 6,3 parts of hydrophobic type odor adsorption master batches, 0.6 part of silane coupler, 0.2
Part 1098,0.2 part of irgasfos 168 of antioxidant and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed to after uniform
Add in double screw extruder, granulated after melting extrusion, prepared nylon red phosphorus flame-retardant masterbatch.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
Comparative example 2
By 40 parts of untreated red phosphorus, 58 parts of nylon, 6,0.6 part of silane coupler, 0.2 part of antioxidant, 1098,0.2 part of antioxygen
Agent 168 and 1 part of silicone powder are poured into homogenizer, high-speed stirred, are mixed into uniform rear addition double screw extruder, through molten
Granulated after melting extrusion, prepared nylon red phosphorus flame-retardant masterbatch.
Wherein the area's temperature of double screw extruder one is 200 DEG C, and two area's temperature are 210 DEG C, and three area's temperature are 220 DEG C, 4th area
Temperature is 230 DEG C, and five area's temperature are 240 DEG C, and six area's temperature are 250 DEG C；Twin-screw engine speed is 350rpm.
According to the effective flame retardance element of equivalent of embodiment 1, by the nylon made by above-described embodiment 1-3 with low smell, low dissipate
Hair, whiteness red phosphorus flame-retardant masterbatch are respectively applied in PA6, and embodiment 4-6 is obtained.It is effective fire-retardant group according to the equivalent of embodiment 1
Point, the nylon red phosphorus flame-retardant masterbatch made by comparative example 1-2 is respectively applied in PA6, comparative example 3-4 is obtained.According to reality
The effective flame retardance element of equivalent of example 1 is applied, the untreated red phosphorus of equivalent is applied to comparative example 5 is obtained in PA6.Material modified proportioning
And performance is as shown in the table, wherein mechanical property is detected using ASTM standard, and oder levels, TVOC are entered using GMW standards
Row detection, fire resistance is determined according to UL94 standards.
The performance data of table 1
Can be seen by upper table 1, after nylon red phosphorus flame-retardant masterbatch prepared by the present invention mixes with nylon-6 matrix body, its is fire-retardant
Performance can reach UL94V-0 grades, and oder levels reach 6.5 grades, and tensile strength, the impact strength of material have due to not
Treatment red phosphorus institute prepared material, improves the comprehensive mechanical property and processing characteristics of fire proofing to a certain extent.
In addition, using nylon red phosphorus flame-retardant masterbatch of the invention dust pollution can be reduced, improve environmental protection and to human body without
Evil；And compatibility is good between resin matrix, the physical and chemical performance of modified resin is also correspondingly improve.
The description of above specific embodiment is that the invention will be further described, but this is not to limit of the invention
System, those skilled in the art's basic thought of the invention, various modifications may be made or improves, but without departing from this
The basic thought of invention, within the scope of the present invention.
Claims (10)
1. a kind of whiteness red phosphorus, described whiteness red phosphorus is microcapsule red phosphorus, and described microcapsule red phosphorus are aluminium hydroxide
With the double encapsulated red phosphorus of phenolic resin, the preparation of the microcapsule red phosphorus：It is made of the raw material including following weight proportion：Red phosphorus
25-35%, aluminum sulfate 5-15%, urea 10-15%, water 50-59%, oil-soluble phenolic resin resin 1-5%；Hydroxide
Aluminium coats process：Aluminum sulfate is added to the water first, stirring is allowed to be completely dissolved, and then puts into red phosphorus, stirs 20min, then
It is transferred in ball mill and is ground to red phosphorus particle diameter untill 5-10um, be then transferred in reactor, adds slowly while stirring
Caustic soda, untill the PH=5-6 of system, adds flocculation agent, stirs, in 75-85 DEG C of scope inside holding 1.5h, finally
By filtering, washing, being dried to obtain aluminium hydroxide encapsulated red phosphorus；Phenolic resin coats process：First with 2.5-3.0 times the two of volume
Toluene dilutes oil-soluble phenolic resin, then aluminium hydroxide encapsulated red phosphorus are mixed with oil-soluble phenolic resin dilution,
Pasty state homogeneous state is stirred into, with the drier for reclaiming xylene unit, 60 ± 5 DEG C of temperature of control is dried feeding, obtains final product
Aluminium hydroxide and the double encapsulated red phosphorus of phenolic resin.
2. a kind of nylon with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, it is characterised in that：By following components by by weight
Amount part is prepared from：
20-50 parts of whiteness red phosphorus described in claim 1,
45-80 parts of nylon 6
1-5 parts of hydrophobic type odor adsorption master batch,
Silane coupler 0.5-1 parts
0.2~1.0 part of antioxidant
0.2~1.0 part of lubricant.
3. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：Described whiteness red phosphorus is microcapsule red phosphorus, described microcapsule red phosphorus for aluminium hydroxide and phenolic resin double-contracting cover it is red
Phosphorus.
4. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：The described inherent viscosity of nylon 6 is 2.0-3.6.
5. a kind of nylon according to claim 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, its feature exists
In：Described hydrophobic type odor adsorption master batch is made up of the component of following weight portion：40~75 parts of PA6, hydrophobicity diatomite 10
~20 parts, 1~5 part of ferriferous oxide, 0~10 part of hydrophobic active charcoal, 5~10 parts of needle-like zeolite molecular sieve, zinc ricinate 5~
10 parts, 5~10 parts of antiseptic, 0.1-0.5 parts of Benzopyranone kind free radical scavenger, antioxidant four [β-（3,5- bis- tertiary fourths
Base -4- hydroxy phenyls）Propionic acid] pentaerythritol ester 0.2-0.5 parts, antioxidant three [2.4- di-tert-butyl-phenyls] phosphite ester
0.2-0.5 parts, 0.5-1.0 parts of lubricant stearic acid zinc；Described antiseptic is the nanometer titanium dioxide of grafting polymer quaternary ammonium salt
Silicon；Described Benzopyranone kind free radical scavenger is 5,7- bis--(2,2- dimethyl ethyls) -3- (3,4- dimethyl benzenes
Base) -2-3 hydrogen-benzofuranone, the ferriferous oxide is ferroso-ferric oxide and di-iron trioxide by weight 1：The work of 1 mixing
Property ferriferous oxide.
6. a kind of nylon according to right 2 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch, it is characterised in that：Institute
The silane coupler stated be gamma-aminopropyl-triethoxy-silane or γ-（Methacryloxypropyl）Propyl trimethoxy silicane.
7. a kind of low smell according to claim 2, low distribute modified red phosphorus flame-retardant nylon material, it is characterised in that：Institute
The antioxidant stated be four [β-（3,5- di-tert-butyl-hydroxy phenyls）Propionic acid] pentaerythritol ester, N, N'- pair-(3- (3,5- bis-
Tert-butyl-hydroxy phenyl) propiono) hexamethylene diamine, the mixture of three [2.4- di-tert-butyl-phenyls] phosphite esters.
8. a kind of low smell according to claim 2, low distribute modified red phosphorus flame-retardant nylon material, it is characterised in that：Institute
The lubricant stated is silicone powder.
9. a kind of nylon according to claim any one of 1-8 with low smell, it is low distribute, whiteness red phosphorus flame-retardant masterbatch
Preparation method, it is characterised in that comprise the following steps：
Whiteness red phosphorus, hydrophobicity odor adsorption master batch, nylon 6, silane coupler, antioxidant and lubricant are poured into high-speed stirring
In mixing machine, high-speed stirred mixes into adding double screw extruder after uniform, is granulated after melting extrusion, and low smell, low is obtained
Distribute, high abrasion-proof and high temperature resistant nylon.
10. preparation method according to claim 9, it is characterised in that：The area's temperature of the double screw extruder one is 200-
230 DEG C, two area's temperature are 200-230 DEG C, and three area's temperature are 200-240 DEG C, and four area's temperature are 210-240 DEG C, and five area's temperature are
210-250 DEG C, six area's temperature are 220-250 DEG C；Twin-screw engine speed is 250-500rpm.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107793749A (en) * | 2017-09-30 | 2018-03-13 | 中广核俊尔新材料有限公司 | A kind of low smell red phosphorus flame-retardant reinforced polyamide material |
| CN107974257A (en) * | 2017-10-24 | 2018-05-01 | 什邡市太丰新型阻燃剂有限责任公司 | High whiteness red phosphorus of a kind of flame retarding efficiency and preparation method thereof |
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| CN107793749A (en) * | 2017-09-30 | 2018-03-13 | 中广核俊尔新材料有限公司 | A kind of low smell red phosphorus flame-retardant reinforced polyamide material |
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| CN110499671A (en) * | 2019-08-19 | 2019-11-26 | 四川金路高新材料有限公司 | A kind of preparation method of fire resistance fibre wallpaper |
| CN114410056A (en) * | 2022-01-11 | 2022-04-29 | 宁波帅特龙集团有限公司 | Flame-retardant ABS composite material and preparation method thereof |
| CN114410056B (en) * | 2022-01-11 | 2024-03-01 | 宁波帅特龙集团有限公司 | Flame-retardant ABS composite material and preparation method thereof |
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