CN108102222A - A kind of resistance to stress whitens master batch and resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material and preparation method thereof - Google Patents
A kind of resistance to stress whitens master batch and resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material and preparation method thereof Download PDFInfo
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- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
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Abstract
Whiten master batch the invention discloses a kind of resistance to stress and resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material and preparation method thereof.A kind of resistance to stress master batch that whitens is to be made of following raw material：Propylene-based elastomeric, POE g MAH, HDPE, double 25 and antioxidant.Also disclose that this resistance to stress is whitened the preparation method of master batch simultaneously.It also discloses and a kind of whitens halogen-free expanded flame-retardant polypropylene composite material and this resistance to stress is whitened the preparation method of halogen-free expanded flame-retardant polypropylene composite material comprising the whiten resistance to stress of master batch of the resistance to stress.The PP composite material that the present invention is prepared its Δ E values are dropped to from 3.89 within 1.0, and stress whitening degree drops to very slight, the degree that even up to can not visually perceive from obvious.The purpose for understanding stress whitening of determining is not only reached, while the flame retardant property for also overcoming PP composite material in the case of toughening declines and strong and unyielding unbalanced disadvantage.
Description
Technical field
Whiten master batch the present invention relates to a kind of resistance to stress and resistance to stress whiten halogen-free expanded flame-retardant polypropylene composite material and
Its preparation method.
Background technology
Polypropylene is widely used in building as a kind of light, nontoxic, acid and alkali-resistance, the plastics variety of relative low price,
Traffic, agricultural and industrial circle.However polyacrylic oxygen index (OI) is only 17.4%, belongs to combustible material.In addition, polypropylene material
Be subject to extraneous stress (stretch, bending or impact when) when, it is easy to appear blushing, i.e., so-called stress for stress area
Whiten, the generation of stress whitening not only influences the appearance of product, it is also possible to damage product service life.Therefore, modification is passed through
Means come assign its flame-retarding characteristic and improve resistance to stress whiten it is very necessary.
Since European Union implements RoHS instructions, people constantly strengthen the consciousness of environmental protection, to the nothing of modified plastics product
Halogenation cry also grows to even greater heights.It is the halogen-free expanded flame-retardant agent (N-P systems) that primary raw material compounds with ammonium polyphosphate (APP),
Because it is added to fire-retardant high into carbon effect in polypropylene, few cigarette during burning, low toxicity, no pernicious gas generates and does not occur molten drop
Phenomenon meets halogen-free environmental development trend, thus becomes the research hotspot of academia and obtain being widely recognized as industrial quarters.However
The APP of commercialization at present is because its own design feature is there are certain hygroscopicity, and the relatively large reason of additive amount, it is caused to add
It is added in polypropylene matrix, is easier to occur top in vain compared with traditional bromine sb system.
Current most of patents concentrate on non-flame resistant modified field, though CN104059297A and patent CN103881233A
Be related to it is fire-retardant, but the fire retardant be bromine antimony type fire retardant.In addition, although based on formula level, increase polyethylene, POE, Weida
The elastomers such as U.S. are a kind of feasible schemes, but due to the particularity of N-P intumescent systems, are caused in addition to Weida is beautiful, the overwhelming majority
Toughener can all reduce flame retardant property to varying degrees.U.S. of Weida is also right except the flame retardant property on composite material is without influence
The improvement that polypropylene resistance to stress is whitened is had outstanding performance, but its there is also toughening effect is poor and modulus decline it is serious not
Foot.
The content of the invention
Based on problem existing in the prior art, whiten master batch and resistance to stress it is an object of the invention to provide a kind of resistance to stress
Whiten halogen-free expanded flame-retardant polypropylene composite material and preparation method thereof.
The present invention is screened in terms of raw material first, rejects the anti-impact type polypropylene for being easier to trigger stress whitening
(or block copolymerization polypropylene) and not surface treated anti-dripping agent polytetrafluoroethylene (PTFE).Meanwhile add in surface modifier pair
The inorganic additives such as APP, wollastonite are pre-processed, and to improve compatibility, reduce the anaclasis caused by boundary defect, so as to
Improve stress whitening phenomenon.Finally, whitened by adding a kind of resistance to stress, while flame retardant property does not decline and rigidity-toughness balanced
Resistance to stress is whitened master batch, to realize halogen-free expanded flame-retardant polypropylene composite material that resistance to stress is whitened excellent.
The technical solution used in the present invention is：
A kind of resistance to stress is whitened master batch, is made of the raw material of following mass parts：
Propylene-based elastomeric be U.S. of Weida elastomer, melt index≤10g/10min under 190 DEG C, 2.16kg.
Melt index of the POE-g-MAH under 190 DEG C, 2.16kg is 0.5g/10min~4.0g/10min；HDPE is 190
DEG C, the melt index under 2.16kg is 1.0g/10min~5.0g/10min.
This resistance to stress is whitened the preparation method of master batch, is weighed raw material by above-mentioned composition, is melted in double screw extruder
Melt blending, squeeze out, obtain resistance to stress and whiten master batch.
A kind of resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material, the raw material composition of following mass parts：45~65
Part acrylic resin, 20~30 parts of N-P compound flame retardants, 8~15 parts of above-mentioned resistance to stress are whitened master batch, 1~10 part of filler,
0.1~0.5 part of coupling agent, 0.1~0.3 part of anti-dripping agent, 0.2~0.5 part of antioxidant, 0.2~0.8 part of lubricant.
Melt index of the acrylic resin under 230 DEG C, 2.16kg is 5g/10min~35g/10min.
Filler is wollastonite, and grain size is the mesh of 1250 mesh~4000.
Anti-dripping agent is polytetrafluoroethylene (PTFE) after the processing of surface cladding.
Coupling agent is at least one in silane coupling agent, titanate coupling agent, acrylic acid coupling agent, stearic acid coupling agent
Kind；Antioxidant is antioxidant 1010,168,1098,1075,1076,245, at least one of 626；Lubricant is polyethylene
At least one of wax, ethylene bis stearamide, calcium stearate, zinc stearate.
This resistance to stress is whitened the preparation method of halogen-free expanded flame-retardant polypropylene composite material, and original is weighed by above-mentioned composition
Material, mixing, squeezes out in double screw extruder, is granulated, and obtains resistance to stress and whitens halogen-free expanded flame-retardant polypropylene composite material.
The beneficial effects of the invention are as follows：
Surface treatment of the present invention by the preferred of formula for raw stock and to relevant raw materials finally adds one when being granulated
Homemade resistance to stress is whitened master batch kind in advance, the PP composite material being prepared its Δ E values from 3.89 drop to 1.0 with
Interior, stress whitening degree drops to very slight, the degree that even up to can not visually perceive from obvious.It does not only reach
The purpose of stress whitening is solved, while the flame retardant property for also overcoming PP composite material in the case of toughening declines and strong and unyielding
Unbalanced disadvantage.
Specific embodiment
A kind of resistance to stress is whitened master batch, is made of the raw material of following mass parts：
Preferably, propylene-based elastomeric is U.S. of Weida elastomer of Exxon Mobil production, at 190 DEG C, under 2.16kg
Melt index≤10g/10min.
Preferably, melt index of the POE-g-MAH under 190 DEG C, 2.16kg is 0.5g/10min~4.0g/10min.
Preferably, the grafting rate of POE-g-MAH is 0.6%~1.2%.
Preferably, melt index of the HDPE under 190 DEG C, 2.16kg is 1.0g/10min~5.0g/10min.
Double 25 its scientific name are 2,5- dimethyl -2,5- bis(t-butylperoxy) hexanes.
This resistance to stress is whitened the preparation method of master batch, is weighed raw material by above-mentioned composition, is melted in double screw extruder
Melt blending, squeeze out, obtain resistance to stress and whiten master batch.
Preferably, resistance to stress whiten master batch preparation method in, the draw ratio of extruder is (40~50)：1, extrusion temperature
For 180 DEG C~190 DEG C；It is further preferred that resistance to stress is whitened in the preparation method of master batch, the draw ratio of extruder is 44：1,
Extrusion temperature is 185 DEG C.
A kind of resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material, the raw material composition of following mass parts：45~65
Part acrylic resin, 20~30 parts of N-P compound flame retardants, 8~15 parts of above-mentioned resistance to stress are whitened master batch, 1~10 part of filler,
0.1~0.5 part of coupling agent, 0.1~0.3 part of anti-dripping agent, 0.2~0.5 part of antioxidant, 0.2~0.8 part of lubricant.
Preferably, acrylic resin is at least one of homopolypropylene, atactic copolymerized polypropene resin.
Preferably, melt index of the acrylic resin under 230 DEG C, 2.16kg is 5g/10min~35g/10min.
Further, N-P compound flame retardants are commercial goods product, and main component is ammonium polyphosphate, Ji Wusi
The mixed thing of alcohol or triazines macromolecular as compositions such as carbon forming agents.
Preferably, during resistance to stress whitens halogen-free expanded flame-retardant polypropylene composite material, resistance to stress whitens master batch at 230 DEG C,
Melt index under 2.16kg is 2.0g/10min~5.0g/10min.
Preferably, filler is wollastonite, and grain size is the mesh of 1250 mesh~4000.
Preferably, anti-dripping agent is polytetrafluoroethylene (PTFE) after the processing of surface cladding.
Preferably, coupling agent is silane coupling agent, in titanate coupling agent, acrylic acid coupling agent, stearic acid coupling agent
It is at least one.
Preferably, lubricant is at least one of polyethylene wax, ethylene bis stearamide, calcium stearate, zinc stearate.
Preferably, the antioxygen that resistance to stress whitens master batch or resistance to stress is whitened used in halogen-free expanded flame-retardant polypropylene composite material
Agent is antioxidant 1010,168,1098,1075,1076,245, at least one of 626.
This resistance to stress is whitened the preparation method of halogen-free expanded flame-retardant polypropylene composite material, and original is weighed by above-mentioned composition
Material, mixing, squeezes out in double screw extruder, is granulated, and obtains resistance to stress and whitens halogen-free expanded flame-retardant polypropylene composite material.
Preferably, resistance to stress whiten halogen-free expanded flame-retardant polypropylene composite material preparation method in, double screw extruder
Technological parameter it is as follows：180~195 DEG C, engine speed 300rpm~400rpm of processing temperature, draw ratio 40:1, vacuum degree<
0.06MPa。
Present disclosure is described in further detail below by way of specific embodiment.
The trade mark of PP resins used in following examples and comparative example for 5090T (platform mould atactic copolymerized polypropene,
MI is 15g/10min), the commercialization trades mark of N-P fire retardants used is EPFR-100C, and resistance to stress is whitened propylene used in master batch
Based elastomeric is U.S. of Weida 6102 (MI 1.3g/10min) of Exxon Mobil production, and POE-g-MAH gives birth to for Exxon Mobil
The VA1803 of production, HDPE raw material are the 5000S (MI 1.2g/10min) of Daqing Refinery, and double 25 carry for Akzo Nobel
For.
Resistance to stress is whitened the preparation of master batch：By 60 parts of U.S.s of Weida 6102,15 parts of VA1803,24.5 parts of 5000S, 0.2 part double
25 and 0.3 parts of antioxidant 1010s after stirring evenly, use double screw extruder (draw ratio 44:1) in 185 DEG C of conditions
Lower melting extrusion is granulated, and it is that resistance to stress is whitened master batch to obtain particle.
Filler used is wollastonite, and mesh number is 3000 mesh.
The polytetrafluoroethylene (PTFE) that anti-dripping agent used is handled for surface cladding, it is commercially available.
Antioxidant used is for 1010 and 168 according to 1:2 ratios are compounded.
Lubricant used is for polyethylene wax (PE waxes) with ethylene bis stearamide (EBS) according to 1:1 ratio is compounded.
The injection temperature of batten is 185 DEG C, and test method used is normal unless otherwise specified in following embodiments
Rule method is carried out according to relevant criterion requirement.Other raw materials used, unless otherwise specified, being can be from routine business
The raw material that approach obtains.
Stress-whitening resistance can be according to germany volkswagen PV3966 standard testings.Final result is with table before and after ball falling impact sample
The scattering difference DELTA E values in face judge the quality of its stress-whitening resistance energy.The Δ E values measured are smaller, stress-whitening resistance energy
Better.
Embodiment：
Table 1 lists embodiment 1-4 resistance to stress and whitens the formula of halogen-free expanded flame-retardant polypropylene composite material, according to table 1
Ingredients listed and its mass parts are 180~195 DEG C in processing temperature after high speed machine mixing 2min, engine speed for 300~
400rpm, draw ratio 40:1 double screw extruder is granulated, and vacuum degree in the process is necessarily less than 0.06Mpa, gained
To particle be that resistance to stress is whitened halogen-free expanded flame-retardant polypropylene composite material.
Comparative example：
Table 1 lists 1~6 test recipe of comparative example, according to 1 ingredients listed of table and its mass parts, is made through twin-screw extrusion
Grain, process condition and embodiment are consistent.
1 embodiment of table is matched with comparative example experiment
Table 2 show embodiment and the PP composite material of comparative example its performance test results.
The Properties of Polypropylene Composite test result of 2 embodiment of table and comparative example
The results of property of table 2 is understood：In conjunction with the embodiments with from the point of view of comparative example, the resistance to stress master batch that whitens efficiently solves poly- third
Alkene N-P halogen-free expansion composite material easily generates the situation of stress whitening, and Δ E values are dropped to from 3.89 within 1.0, stress whitening
Degree drops to very slight, the degree that even up to can not visually perceive from obvious.It is serious that it is applied to stress whitening
Impact polypropylene on also there is obvious improvement (Δ E values drop to 2.53 from 6.76).In addition, it sends out in resistance to stress
POE and LDPE is substantially better than in white improvement degree, also efficiently solves what flame retardant property caused during traditional POE toughenings declined
Problem.Finally, on the premise of itself beautiful excellent improvement stress whitening effect of Weida is kept not decline, the U.S. increasing of Weida is overcome
Tough not sufficiently effective and modulus declines the shortcomings that notable, has reached the initial purpose of the present invention.
More than detailed description of the invention is only presently preferred embodiments of the present invention, it is impossible to be construed as limiting the present invention
Practical range.Any changes and modifications in accordance with the scope of the present application, the patent that should all belong to the present invention cover
Within the scope of.
Claims (10)
- The master batch 1. a kind of resistance to stress is whitened, it is characterised in that：It is made of the raw material of following mass parts：
- The master batch 2. a kind of resistance to stress according to claim 1 is whitened, it is characterised in that：Propylene-based elastomeric is U.S. of Weida bullet Property body, at 190 DEG C, melt index≤10g/10min under 2.16kg.
- The master batch 3. a kind of resistance to stress according to claim 1 is whitened, it is characterised in that：POE-g-MAH at 190 DEG C, Melt index under 2.16kg is 0.5g/10min~4.0g/10min；Melt index of the HDPE under 190 DEG C, 2.16kg be 1.0g/10min~5.0g/10min.
- The preparation method of master batch 4. a kind of resistance to stress is whitened, it is characterised in that：It is formed by claims 1 to 3 any one of them Raw material is weighed, the melt blending in double screw extruder squeezes out, and obtains resistance to stress and whitens master batch.
- The halogen-free expanded flame-retardant polypropylene composite material 5. a kind of resistance to stress is whitened, it is characterised in that：By the raw material of following mass parts Composition：45~65 parts of acrylic resins, 20~30 parts of N-P compound flame retardants, 8~15 parts of claims 1 to 3 any one of them Resistance to stress is whitened master batch, 1~10 part of filler, 0.1~0.5 part of coupling agent, 0.1~0.3 part of anti-dripping agent, 0.2~0.5 part of antioxygen Agent, 0.2~0.8 part of lubricant.
- The halogen-free expanded flame-retardant polypropylene composite material 6. a kind of resistance to stress according to claim 5 is whitened, it is characterised in that： Melt index of the acrylic resin under 230 DEG C, 2.16kg is 5g/10min~35g/10min.
- The halogen-free expanded flame-retardant polypropylene composite material 7. a kind of resistance to stress according to claim 5 is whitened, it is characterised in that： Filler is wollastonite, and grain size is the mesh of 1250 mesh~4000.
- The halogen-free expanded flame-retardant polypropylene composite material 8. a kind of resistance to stress according to claim 5 is whitened, it is characterised in that： Anti-dripping agent is polytetrafluoroethylene (PTFE) after the processing of surface cladding.
- The halogen-free expanded flame-retardant polypropylene composite material 9. a kind of resistance to stress according to claim 5 is whitened, it is characterised in that： Coupling agent is at least one of silane coupling agent, titanate coupling agent, acrylic acid coupling agent, stearic acid coupling agent；Antioxidant For antioxidant 1010,168,1098,1075,1076,245, at least one of 626；Lubricant is polyethylene wax, ethylene is double hard At least one of acyl amine, calcium stearate, zinc stearate.
- The preparation method of halogen-free expanded flame-retardant polypropylene composite material 10. a kind of resistance to stress is whitened, it is characterised in that：It will by right 5~9 any one of them composition is asked to weigh raw material, mixes, is squeezed out in double screw extruder, is granulated, is obtained resistance to stress and whiten Halogen-free expanded flame-retardant polypropylene composite material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774362A (en) * | 2018-06-15 | 2018-11-09 | 广东美的环境电器制造有限公司 | Proof stress whitens master batch and preparation method thereof, halogen-free anti-flaming polypropylene material and preparation method thereof and electric appliance |
| CN109971071A (en) * | 2019-04-02 | 2019-07-05 | 金旸（厦门）新材料科技有限公司 | A kind of filter bottle of water purifier shell PP composite material, Preparation method and use |
| CN110964259A (en) * | 2019-09-04 | 2020-04-07 | 上海日之升科技有限公司 | Efficient halogen-free flame-retardant master batch with polypropylene carrier and preparation method thereof |
| CN112552608A (en) * | 2020-11-18 | 2021-03-26 | 上海日之升科技有限公司 | Low-temperature impact-resistant stress whitening-resistant polypropylene material and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108774362A (en) * | 2018-06-15 | 2018-11-09 | 广东美的环境电器制造有限公司 | Proof stress whitens master batch and preparation method thereof, halogen-free anti-flaming polypropylene material and preparation method thereof and electric appliance |
| CN108774362B (en) * | 2018-06-15 | 2021-05-25 | 广东美的环境电器制造有限公司 | Stress whitening resistant master batch and preparation method thereof, halogen-free flame-retardant polypropylene material and preparation method thereof, and electric appliance |
| CN109971071A (en) * | 2019-04-02 | 2019-07-05 | 金旸（厦门）新材料科技有限公司 | A kind of filter bottle of water purifier shell PP composite material, Preparation method and use |
| CN109971071B (en) * | 2019-04-02 | 2021-05-11 | 金旸（厦门）新材料科技有限公司 | Polypropylene composite material for water purifier filter bottle shell, preparation method and application |
| CN110964259A (en) * | 2019-09-04 | 2020-04-07 | 上海日之升科技有限公司 | Efficient halogen-free flame-retardant master batch with polypropylene carrier and preparation method thereof |
| CN110964259B (en) * | 2019-09-04 | 2022-07-29 | 上海日之升科技有限公司 | Efficient halogen-free flame-retardant master batch with polypropylene carrier and preparation method thereof |
| CN112552608A (en) * | 2020-11-18 | 2021-03-26 | 上海日之升科技有限公司 | Low-temperature impact-resistant stress whitening-resistant polypropylene material and preparation method thereof |
| CN112552608B (en) * | 2020-11-18 | 2022-06-17 | 上海日之升科技有限公司 | Low-temperature impact-resistant stress whitening-resistant polypropylene material and preparation method thereof |
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| CN108102222B (en) | 2020-07-10 |
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