CN108976594A - A kind of flame retardant polyolefin compound and preparation method thereof - Google Patents
A kind of flame retardant polyolefin compound and preparation method thereof Download PDFInfo
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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
- C08K5/00—Use of organic ingredients
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
- C08K5/523—Esters of phosphoric acids, e.g. of H3PO4 with hydroxyaryl compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5313—Phosphinic compounds, e.g. R2=P(:O)OR'
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/10—Peculiar tacticity
- C08L2207/14—Amorphous or atactic polypropylene
Abstract
The invention discloses a kind of flame retardant polyolefin compounds, by weight, including following components: 100 parts of polyolefin resin；Three .5-10 parts of phosphoesterase 30 of (tribromo neopentyl)；0.5-10 parts of phosphorus flame retardant；0.1-2 parts of fire retarding synergist.The phosphorus flame retardant is selected from least one of hypophosphites, phosphate, Quadrafos.In the case that flame retardant polyolefin compound of the invention has many advantages, such as excellent anti-flammability, surface gloss, transparency, especially three (tribromo neopentyl) phosphates and phosphate, fire retarding synergist compounding, surface gloss, transparency are preferable.
Description
Technical field
The present invention relates to technical field of macromolecules, more particularly to a kind of flame retardant polyolefin compound and preparation method thereof.
Background technique
Polyolefin resin includes polyethylene, polypropylene, polyvinyl acetate and various olefin copolymers, wherein poly- third
Alkene becomes the general plastic being most widely used because of its excellent comprehensive performance and good cost performance, wider machine-shaping conditions
One of material.Polyolefin resin is mostly red label goods, and such as polyacrylic limit oxygen index is 17-18%, is easily burnt,
Self-extinguishment is unable to after fire, with being gradually increased for material safety requirements, the polyolefin resins such as polypropylene must carry out flame-retardant modified.
Fire retardant for polyolefin is broadly divided into bromide fire retardant and halogen-free flame retardants, existing flame-retardant modified polyolefin
In, in order to meet non-halogen requirement, need to select to add the fire retardant of phosphorous, nitrogen or its compound system.Present use is most general
Time phosphonium flame retardant and combinations thereof mainly have phosphate, Intumscent Flame Retardant System based on ammonium polyphosphate etc..But these
Flame-retardant system compared with the bromo- antimony compounding flame retardant of tradition, there are additive amounts it is big, physical property is poor the disadvantages of, be widely applied
There is also biggish limitations.
Chinese patent 201010154587.3 discloses one kind using phosphinates, Tripolycyanamide hydrobromide as main component
Fire retardant combination, polypropylene can be made to reach UL94 V-2 fire-retardant rank, but the fire retarding synergist in its component contains
The elements such as antimony, bismuth can reduce the transparency of material.Meanwhile antimony and its compound are as typical heavy metal non-renewable mineral
Resource, it is expensive, and be easy to bring environmental pollution and Health cost problem in process, no antimony flame-retardant formulations system has
Effect solves these problems.Chinese patent 200980131213.5 disclose it is a kind of with tricresyl phosphate (tribromo neopentyl) ester with
The mixture of carbon-to-carbon initiator is the polypropene composition of flame retardant constituent, does not contain antimony oxide, can satisfy UL94
V-1 or V-0 fire-retardant rank, but fire retardant additive amount is higher.
With the continuous improvement of downstream industry application demand, in addition to being wanted to traditional performances such as flame retardant property, physical properties
Ask outer, more and more products wish material also while having preferable surface gloss and transparency, existing common bromo-
The performance of the flame-retardant systems such as antimony, halogen-free expandable in these areas is unsatisfactory.
Summary of the invention
The object of the present invention is to provide a kind of flame retardant polyolefin compounds, have excellent anti-flammability, lustrous surface
In the case where the advantages that degree, transparency, especially three (tribromo neopentyl) phosphates and phosphate, fire retarding synergist compounding, table
Face glossiness, transparency are best.
Another object of the present invention is to provide the preparation methods of above-mentioned flame retardant polyolefin compound.
The present invention is achieved by the following technical solutions:
A kind of flame retardant polyolefin compound, by weight, including following components:
100 parts of polyolefin resin；
Three .5-10 parts of phosphoesterase 30 of (tribromo neopentyl)；
0.5-10 parts of phosphorus flame retardant；
0.1-2 parts of fire retarding synergist.
Including following components preferably, by weight:
100 parts of polyolefin resin；
Three 1-5 parts of phosphate of (tribromo neopentyl)；
1-5 parts of phosphorus flame retardant；
0.15-1 parts of fire retarding synergist.
It is furthermore preferred that by weight, including following components:
100 parts of polyolefin resin；
Three 1-3 parts of phosphate of (tribromo neopentyl)；
1-3 parts of phosphorus flame retardant；
5 parts of fire retarding synergist 0.2-0..
The phosphorus flame retardant is selected from least one of hypophosphites, phosphate, Quadrafos；Preferably, it is selected from
At least one of phosphate；The hypophosphites is selected from hypo-aluminum orthophosphate, calcium hypophosphite, dimethyl hypo-aluminum orthophosphate, diethyl
At least one of hypo-aluminum orthophosphate, Methylethyl hypo-aluminum orthophosphate；The phosphate is selected from triphenyl phosphate, resorcinol bis- (two
Phenyl phosphate ester), at least one of bisphenol-A-bis- (diphenyl phosphoesters), oligomeric aryl phosphate ester；The Quadrafos choosing
From ammonium polyphosphate, at least one of melamine phosphate, melamine pyrophosphate, melamine polyphosphate.Wherein, institute
The oligomeric aryl phosphate ester degree of polymerization stated is 2-10.
The average grain diameter of the phosphorus flame retardant is 1-10 microns；Preferably, the average grain of the phosphorus flame retardant
Diameter is 1-5 microns.Partial size is too big, and the dispersion effect of fire retardant is poor, and lustrous surface and the transparency decline of product are more.
The fire retarding synergist is selected from least one of at least one of compound (I) and/or compound (II)；
The general formula of compound (I) is
Wherein, R1, R2, R3 or R4 are respectively in C1-12 alkyl, C1-12 alkoxy, C6-12 aromatic radical or C6-12 fragrance oxygroup
Any one；Preferably C1-12 alkyl；More preferably C1-4 alkyl；X or Y be H, C1-12 alkyl, C1-12 alkoxy,
Any one in C6-12 aromatic radical, C6-12 fragrance oxygroup, halogen, nitro, sulfonic group or polysubstituted aromatic radical；Preferably H
Or C1-12 alkyl；
The general formula of compound (II) is
Wherein, R5 is any one in C1-12 alkyl, C1-12 alkoxy, C6-12 aromatic radical or C6-12 fragrance oxygroup；It is excellent
It is selected as C1-12 alkyl；More preferably C1-4 alkyl；N is 2-20；Preferably 2-10；More preferably 3-6.
For example poly- 1,4- diisopropyl benzene (n 3-10) of fire retarding synergist, 2,3- dimethyl -2,3- diphenyl butane.
The polyolefin resin is selected from least one of polyvinyl resin, acrylic resin.Such as random copolymerization poly- third
Alkene, homopolypropylene, high density polyethylene (HDPE) etc..
By weight, further include 0-1 parts antioxidant, 0-1 parts of processing aids；The antioxidant is selected from phenols, amine
At least one of class, phosphorous acid esters, half Hinered phenols, calixarene kind, dilauryl thiodipropionate；The processing helps
Agent is selected from least one of low molecule lipid, metal soap, the compound esters of stearic acid, amides.Such as: processing aid can be
Lubricant stearic acid calcium；Antioxidant can be antioxidant 1010, irgasfos 168.
Flame retardant polyolefin compound surface gloss >=79 degree, light transmittance >=78%, mist degree≤84%, lustrous surface
Degree uses GB 8807-1988 standard, and light transmittance uses 2008 standard of GB/T2410-, and mist degree is marked using GB/T2410- 2008
It is quasi-.
Flame retardant polyolefin compound of the invention, the partial size of fire retardant in the product is to surface gloss, light transmittance, mist degree
It is affected, the partial size of fire retardant is big, and the dispersion of fire retardant in the product can be inhomogenous, causes under surface gloss, light transmittance
Drop, mist degree rise.
The preparation method of above-mentioned flame retardant polyolefin compound, comprising the following steps:
A) polyolefin resin, three (tribromo neopentyl) phosphates, phosphorus flame retardant, fire retarding synergist are passed through after weighing proportionally
High-speed mixer is uniformly mixed；
B) melting extrusion, granulation at 180-200 DEG C by double screw extruder, obtains fire retardant polyolefin combination after dry
Object.
Can also be in step A) in be added antioxidant, processing aid.
The invention has the following beneficial effects:
The present invention is compounded using three (tribromo neopentyl) phosphates, phosphorus flame retardant, fire retarding synergist, combines fire retardant polyolefin
Object can have the flame retardant rating (0.8-3.2 mm) of UL-94 V-2 in the case where only adding a small amount of fire retardant, and
Flame retardant polyolefin compound has the advantages that excellent surface gloss, transparency.Especially three (tribromo neopentyl) phosphates,
In the case where phosphate, fire retarding synergist compounding, composition surface gloss, transparency are preferable.
Specific embodiment
Further illustrate that the present invention, following embodiment are the preferable embodiment party of the present invention below by specific embodiment
Formula, but embodiments of the present invention are not limited by following embodiments.
Embodiment and comparative example it is raw materials used be following raw material, remaining raw material sources is in commercially available, but the present invention is not by following
Raw material limitation:
High density polyethylene (HDPE): Dow Chemical；
Homopolypropylene: Exxon Mobil Corporation；
Atactic copolymerized polypropene: Exxon Mobil Corporation；
2,3- dimethyl -2,3- diphenyl butane: Wuxi City Mount Everest Fine Chemical Co., Ltd；
Poly- 1,4- diisopropyl benzene: n 3-10；Wuxi City Mount Everest Fine Chemical Co., Ltd；
Poly- 1,4- diisopropyl benzene: n 3-6；Wuxi City Mount Everest Fine Chemical Co., Ltd；
Diethyl hypo-aluminum orthophosphate A: average grain diameter is 1.5 microns；
Diethyl hypo-aluminum orthophosphate B: average grain diameter is 5.5 microns；
Melamine pyrophosphate: average grain diameter is 2.0 microns；
Remaining raw material sources is in commercially available.
The preparation method of embodiment, comparative example flame retardant polyolefin compound:
Polyolefin resin, three (tribromo neopentyl) phosphates, phosphorus flame retardant, fire retarding synergist, antioxidant, processing aid are pressed
Ratio is uniformly mixed after weighing by high-speed mixer, then melting extrusion, granulation at 200 DEG C by double screw extruder,
Flame retardant polyolefin compound is obtained after drying.
Each performance test methods:
(1) UL-94,3.2mm: according to UL-94 standard, test bars are with a thickness of 3.2mm；
(2) UL-94,1.6mm: according to UL-94 standard, test bars are with a thickness of 1.6mm；
(3) UL-94,0.8mm: according to UL-94 standard, test bars are with a thickness of 0.8mm；
(4) surface gloss: press 8807-1988 standard of GB, 60 ° of test angle；
(5) light transmittance: according to 2008 standard of GB/T2410-, test sample is with a thickness of 1.0mm；
(6) mist degree: according to 2008 standard of GB/T2410-, test sample is with a thickness of 1.0mm；
Note: the standard of transparency includes light transmittance and mist degree two, and light transmittance is higher, the more low then transparency of mist degree is better.
(7) fire retardant average grain diameter detection method: being prepared into print for compound, be placed in liquid nitrogen freeze it is crisp after five minutes
It is disconnected, then using the fire retardant pattern and size in SEM observation 50 × 50 micron range of section, count fire retardant within the scope of this
Average grain diameter.
Table 1: embodiment and comparative example each group distribution ratio (parts by weight) and each the performance test results
Continued 1
Note: NR indicates that the lowest class is all not achieved
It can be seen that the fire-retardant rank that the present invention uses small amount fire retardant to can reach UL-94 V-2 from embodiment 1-6, and
And there is high surface gloss and transparency, wherein amount of flame-retardant agent is fewer, and surface gloss and transparency are higher；From implementation
In the case that example 2/7/8 can be seen that three (tribromo neopentyl) phosphates, phosphate, fire retarding synergist compounding, product surface light
Damp degree, transparency are higher；From embodiment 7 and embodiment 13 as can be seen that when the average grain diameter of phosphorus flame retardant is 1-5 microns
When, surface gloss, light transmittance are higher.From embodiment 2 and embodiment 9 as can be seen that fire retarding synergist dosage has been more than 0.5
Part, flame retardant property is not promoted, but transparency can be reduced.From embodiment 2 and embodiment 14 as can be seen that using poly- Isosorbide-5-Nitrae-
The embodiment transparency of diisopropyl benzene (n 3-6) is preferable.
Claims (10)
1. a kind of flame retardant polyolefin compound, which is characterized in that by weight, including following components:
100 parts of polyolefin resin；
Three .5-10 parts of phosphoesterase 30 of (tribromo neopentyl)；
0.5-10 parts of phosphorus flame retardant；
0.1-2 parts of fire retarding synergist.
2. flame retardant polyolefin compound according to claim 1, which is characterized in that by weight, including following components:
100 parts of polyolefin resin；
Three 1-5 parts of phosphate of (tribromo neopentyl)；
1-5 parts of phosphorus flame retardant；
0.15-1 parts of fire retarding synergist.
3. flame retardant polyolefin compound according to claim 2, which is characterized in that by weight, including following components:
100 parts of polyolefin resin；
Three 1-3 parts of phosphate of (tribromo neopentyl)；
1-3 parts of phosphorus flame retardant；
5 parts of fire retarding synergist 0.2-0..
4. flame retardant polyolefin compound according to claim 1-3, which is characterized in that the phosphorus flame retardant
Selected from least one of hypophosphites, phosphate, Quadrafos；Preferably, selected from least one of phosphate；Described
Hypophosphites is selected from hypo-aluminum orthophosphate, calcium hypophosphite, dimethyl hypo-aluminum orthophosphate, diethyl hypo-aluminum orthophosphate, Methylethyl hypo-aluminum orthophosphate
At least one；The phosphate is selected from triphenyl phosphate, resorcinol bis- (diphenyl phosphoesters), the bis- (hexichol of bisphenol-A-
Base phosphate), at least one of oligomeric aryl phosphate ester；The Quadrafos be selected from ammonium polyphosphate, melamine phosphate,
At least one of melamine pyrophosphate, melamine polyphosphate.
5. flame retardant polyolefin compound according to claim 4, which is characterized in that the average grain of the phosphorus flame retardant
Diameter is 1-10 microns；Preferably, the average grain diameter of the phosphorus flame retardant is 1-5 microns.
6. flame retardant polyolefin compound according to claim 1-3, which is characterized in that the fire retarding synergist
Selected from least one of compound (I) and/or at least one of compound (II)；
The general formula of compound (I) is
Wherein, R1, R2, R3 or R4 are respectively in C1-12 alkyl, C1-12 alkoxy, C6-12 aromatic radical or C6-12 fragrance oxygroup
Any one；Preferably C1-12 alkyl；More preferably C1-4 alkyl；X or Y be H, C1-12 alkyl, C1-12 alkoxy,
Any one in C6-12 aromatic radical, C6-12 fragrance oxygroup, halogen, nitro, sulfonic group or polysubstituted aromatic radical；Preferably H
Or C1-12 alkyl；
The general formula of compound (II) is
Wherein, R5 is any one in C1-12 alkyl, C1-12 alkoxy, C6-12 aromatic radical or C6-12 fragrance oxygroup；It is excellent
It is selected as C1-12 alkyl；More preferably C1-4 alkyl；N is 2-20；Preferably 2-10；More preferably 3-6.
7. flame retardant polyolefin compound according to claim 1-3, which is characterized in that the polyolefin resin
Selected from least one of polyvinyl resin, acrylic resin.
8. flame retardant polyolefin compound according to claim 1-3, which is characterized in that by weight, also wrap
Include 0-1 parts antioxidant, 0-1 parts of processing aids；The antioxidant is selected from phenols, amine, phosphorous acid esters, half hindered phenol
At least one of class, calixarene kind, dilauryl thiodipropionate；The processing aid is selected from low molecule lipid, metal
At least one of the compound esters of soaps, stearic acid, amides.
9. flame retardant polyolefin compound according to claim 1-8, which is characterized in that the fire retardant polyolefin
Composition surface gloss >=79 degree, light transmittance >=78%, mist degree≤84%, surface gloss use GB 8807-1988 standard,
Light transmittance uses 2008 standard of GB/T2410-, and mist degree uses 2008 standard of GB/T2410-.
10. the preparation method of the described in any item flame retardant polyolefin compounds of claim 1-9, which is characterized in that including following
Step:
A) polyolefin resin, three (tribromo neopentyl) phosphates, phosphorus flame retardant, fire retarding synergist are passed through after weighing proportionally
High-speed mixer is uniformly mixed；
B) melting extrusion, granulation at 180-200 DEG C by double screw extruder, obtains fire retardant polyolefin combination after dry
Object.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004041919A2 (en) * | 2002-11-04 | 2004-05-21 | Ciba Specialty Chemicals Holding Inc. | Flame retardant compositions |
| CN1743369A (en) * | 2004-09-01 | 2006-03-08 | 第一Fr株式会社 | Flame retardant compositions for flammable plastics and flame retarded plastic compositions containing the same |
| JP2016501963A (en) * | 2012-12-20 | 2016-01-21 | ポリアド サービシズ エルエルシー | Flame retardant polymer composition |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2004041919A2 (en) * | 2002-11-04 | 2004-05-21 | Ciba Specialty Chemicals Holding Inc. | Flame retardant compositions |
| CN1743369A (en) * | 2004-09-01 | 2006-03-08 | 第一Fr株式会社 | Flame retardant compositions for flammable plastics and flame retarded plastic compositions containing the same |
| JP2016501963A (en) * | 2012-12-20 | 2016-01-21 | ポリアド サービシズ エルエルシー | Flame retardant polymer composition |
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