CN110452462A - A kind of enhancing flame-retardant polypropylene composite material and preparation method thereof - Google Patents
A kind of enhancing flame-retardant polypropylene composite material and preparation method thereof Download PDFInfo
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- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
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Abstract
The present invention provides a kind of enhancing flame-retardant polypropylene composite material, it is characterized in that, according to parts by weight, it is made of following raw material: 75-80 parts of polypropylene, 8-10 parts of nano titanium diboride, 3-5 parts of three phosphonitrile of poly- amino ring, three 3-5 parts of (2- ethoxy) chlorinated isocyanurates, 1-2 parts of white carbon black, 2-4 parts of compatilizer, 5-7 parts of toughener, 0.5-1.5 parts of antioxidant, 1-3 parts of coupling agent；Wherein compatilizer is a kind of special alkylation modification chitosan, and wherein O- alkylated reaction degree of substitution is 0.45-0.62.Enhancing flame-retardant polypropylene composite material limit oxygen index value prepared by the present invention reaches 34.5-35.8%, vertical combustion performance reaches FV-0 grades, with excellent flame retardant property, while tensile strength reaches 34.2-35.5MPa, PP composite material rigidity with higher.
Description
Technical field
The invention belongs to field of composite material preparation, and in particular to a kind of enhancing flame-retardant polypropylene composite material and its preparation
Method.
Background technique
Polypropylene (PP) has good mechanical property, processing performance, chemical corrosion resistance, electrical insulating property and non-toxic light
The features such as, it is a kind of general-purpose plastics of high comprehensive performance, is widely used in household electrical appliances, electronics, construction material, auto industry, spinning
The fields such as knit, decorate.But due to the structure of polypropylene itself, oxygen index (OI) is low, meets fiery easy firing, calorific value height, burning velocity
Fastly, a large amount of molten drop can be generated when burning, if burning is insufficient to release the toxic gas such as CO, fire hazard compared with
Greatly, its application field is significantly limited.As polypropylene there are certain requirements product flame retardant property in building, auto industry etc.
Field be widely applied, polyacrylic flame retardant property is improved under the premise of guaranteeing that Mechanical Properties of PP reaches product requirement is
One highly important project.
CN103524885 provides a kind of by poly- three phosphonitrile of amino ring and three (2- ethoxy) chlorinated isocyanurates (referred to as match gram)
The expansion type flame retardant for compounding composition, is compounded with three (2- ethoxy) chlorinated isocyanurates by 1:1, and add in poly- three phosphonitrile of amino ring
When aggregation amount accounts for PP composite material 20%, the polypropylene material obtained after extrusion, vulcanization, compression molding, limit oxygen index
LOI is 27%, and vertical combustion rank reaches FV-0 grades.But actually poly- three phosphonitrile of amino ring and synergist match gram and polypropylene
Compatibility it is bad, the addition of a large amount of fire retardants will lead to polyacrylic mechanical property and substantially reduce, and limit polypropylene material
Comprehensive performance.
Summary of the invention
To solve problems of the prior art, prior art is advanced optimized, the present invention provides a kind of increasing
Strong flame-retardant polypropylene composite material and preparation method thereof, to realize that raising oxygen index (OI), raising fire retardant and polypropylene compatible are same
The goal of the invention of the mechanical property of Shi Tigao material.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of enhancing flame-retardant polypropylene composite material, which is characterized in that according to parts by weight, be made of following raw material: polypropylene
75-80 parts, it is 8-10 parts of nano titanium diboride, 3-5 parts of three phosphonitrile of poly- amino ring, three 3-5 parts of (2- ethoxy) chlorinated isocyanurates, white
1-2 parts of carbon black, 2-4 parts of compatilizer, 5-7 parts of toughener, 0.5-1.5 parts of antioxidant, 1-3 parts of coupling agent；
The polypropylene is isotactic or syndiotactic polypropylene, and melt index is 4 ~ 10g/10min；
The nano titanium diboride granularity 50-100nm, specific surface area 70-80m2/g；
The white carbon black, 98% or more purity；
The compatilizer is alkylation modification chitosan, and O- alkylated reaction degree of substitution is 0.45-0.62；
The toughener includes esters of acrylic acid rubber powder, maleic anhydride inoculated polypropylene, polyvinyl alcohol and peroxidating diisopropyl
Benzene, four mass ratioes are 8-10:13-18:15-18:1；
The antioxidant is antioxidant 1010；
The coupling agent is two (dioctyl phosphite base) tetraisopropyl titanates or pentaerythritol stearate；
The preparation of the enhancing flame-retardant polypropylene composite material, which is characterized in that preparation, increasing including alkylation modification chitosan
The strong preparation of master batch and the preparation of composite material；
The preparation of the alkylation modification chitosan, which is characterized in that including alkalization, temperature reaction and post-processing；
The alkalization is that chitosan is added in the isopropanol alkaline solution of NaOH to carry out ultrasound, supersonic frequency 320-
400MHz, ultrasonic time 20-25min；The chitosan, deacetylation 70%-90%, granularity are 40-70 μm；Chitosan with
The mass ratio of NaOH solid is 1:1.5-2.5；Quantity of isopropanol is 10-15 times of chitosan mass；
The temperature reaction is that ultrasound terminates, and phase transfer catalyst tetrabutylammonium bromide is first added, adds the bromo- 4- of 1- positive ten
Dialkyl benzene is reacted, and temperature is 55-60 DEG C, and insulated and stirred reacts 3.5-4h；The dosage of phase transfer catalyst accounts for reactant
It is the 6-8% of gross mass；The addition mass ratio of the bromo- 4- dodecyl benzene of 1- and chitosan is 9.1-9.5:2；
The post-processing, be added dropwise glacial acetic acid adjust pH to 6-7, alkylation modification chitosan crude product Precipitation, with 5wt% alcohol/
Hydrochloric acid solution washing, 5wt% alcohol/hydrochloric acid solution usage amount are 10-15 times of alkylation modification chitosan crude product quality；
The preparation of the enhancing master batch, nano titanium diboride, white carbon black, toughener and antioxidant through mixed at high speed and are squeezed out
It is granulated, screw speed 80rpm-100rpm, extruder temperature is 110 DEG C -120 DEG C, partial size 2-5mm；
The preparation of the composite material carries out in double screw extruder, is set separately from feed opening to head outlet temperature:
180 DEG C, 185 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, revolving speed 200-250rpm.
By adopting the above technical scheme, the invention has the benefit that
1, enhancing flame-retardant polypropylene composite material prepared by the present invention, according to GB/T2406-1993 standard testing, limit oxygen refers to
Numerical value reaches 34.5-35.8%, has excellent flame retardant property；
2, enhancing flame-retardant polypropylene composite material prepared by the present invention, according to GB/T2408-1996 standard testing, vertical burn flammability
FV-0 grades can be reached, object ignites absorbent cotton phenomenon without dripping off, flaming combustion time 3-5s, and glowing time is no more than 2s；
3, enhancing flame-retardant polypropylene composite material prepared by the present invention, tensile strength 34.2-35.5MPa, PP composite material
Rigidity with higher；
4, enhancing flame-retardant polypropylene composite material prepared by the present invention, bending strength 38.9-40.2MPa, elongation at break 28.4-
33.6%, notch impact strength 14.5-15.2KJ/m2, bending resistance is high, and toughness of material is good.
Detailed description of the invention:
Fig. 1 is the TEM photo of PP composite material described in embodiment 3.
Specific embodiment:
Below with reference to specific embodiment, the present invention is further explained.
A kind of enhancing flame-retardant polypropylene composite material of embodiment 1
The composite material, in parts by weight, including following components:
It is 75 parts of polypropylene, 8 parts of nano titanium diboride, 3 parts of three phosphonitrile of poly- amino ring, three 4 parts of (2- ethoxy) chlorinated isocyanurates, white
2 parts of carbon black, 2 parts of compatilizer, 5 parts of toughener, 1 part of antioxidant, 1 part of coupling agent；
The polypropylene is syndiotactic polypropylene, and melt index is 8 ~ 10g/10min；
The nano titanium diboride granularity 50-53nm, specific surface area 76-80m2/g；
The white carbon black, purity 98.8%；
The compatilizer is alkylation modification chitosan, and O- alkylated reaction degree of substitution is 0.45；
The toughener includes esters of acrylic acid rubber powder, maleic anhydride inoculated polypropylene, polyvinyl alcohol and peroxidating diisopropyl
Benzene, four mass ratioes are 8:15:15:1；
The antioxidant is antioxidant 1010；
The coupling agent is two (dioctyl phosphite base) tetraisopropyl titanates；
The preparation method of above-mentioned composite material, comprising the following steps:
1, the preparation of alkylation modification chitosan
1) it alkalizes
NaOH solid is added in isopropanol to strong basicity, chitosan is added thereto and is sufficiently stirred, is placed on ultrasonic response
Ultrasound is carried out in device at room temperature, is sufficiently alkalized, supersonic frequency 320MHz, ultrasonic time 25min；
The chitosan, deacetylation 70%-73%, granularity 40-45m；
The mass ratio of the chitosan and NaOH solid is 1:1.5；
The quantity of isopropanol is 10 times of chitosan mass；
2) temperature reaction
Ultrasound terminates, and phase transfer catalyst tetrabutylammonium bromide is first added, after being completely dissolved, adds the bromo- 4- n-dodecane of 1-
Base benzene is reacted, and increasing the temperature to temperature is 55 DEG C, and insulated and stirred reacts 4h；
The dosage of the phase transfer catalyst accounts for the 6% of reaction system gross mass；
The addition mass ratio of the bromo- 4- dodecyl benzene of the 1- and chitosan is 9.5:2；
3) it post-processes
Reaction terminates, and glacial acetic acid is added dropwise and adjusts pH to 6-7, alkylation modification chitosan crude product Precipitation, filtering；Afterwards by alkyl
Change modification of chitosan crude product, which is added in 5wt% alcohol/hydrochloric acid solution, to be washed, and suction filtration is placed in 40 DEG C of vacuum drying ovens and does
It is dry to constant weight；
The usage amount of the 5wt% alcohol/hydrochloric acid solution is 10 times of alkylation modification chitosan crude product quality.
2, enhance the preparation of master batch
Nano titanium diboride, white carbon black, toughener and antioxidant are pre-mixed uniformly through high-speed mixer, rear extruding pelletization
Master batch, screw speed 80rpm must be enhanced, extruder temperature is 110 DEG C, partial size 2-3mm.
3, the preparation of composite material
Polypropylene, alkylation modification chitosan, poly- three phosphonitrile of amino ring, three (2- ethoxy) chlorinated isocyanurates and coupling agent are added
Enter twin-screw extrusion owner's spout, weighs enhancing master batch and be added from side spout, is extruded into jointly in extruder melt blending
Type is set separately from feed opening to head outlet temperature: 180 DEG C, 185 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, revolving speed
200rpm。
A kind of enhancing flame-retardant polypropylene composite material of embodiment 2
The composite material, in parts by weight, including following components:
80 parts of polypropylene, 10 parts of nano titanium diboride, 5 parts of three phosphonitrile of poly- amino ring, three 5 parts of (2- ethoxy) chlorinated isocyanurates,
2 parts of white carbon black, 2 parts of compatilizer, 6 parts of toughener, 1.5 parts of antioxidant, 2 parts of coupling agent；
The polypropylene is isotactic polypropylene, and melt index is 5 ~ 8g/10min；
The nano titanium diboride granularity 50-60nm, specific surface area 73-76m2/g；
The white carbon black, purity 98.5%；
The compatilizer is alkylation modification chitosan, and O- alkylated reaction degree of substitution is 0.62；
The toughener includes esters of acrylic acid rubber powder, maleic anhydride inoculated polypropylene, polyvinyl alcohol and peroxidating diisopropyl
Benzene, four mass ratioes are 8:13:18:1；
The antioxidant is antioxidant 1010；
The coupling agent is pentaerythritol stearate；
The preparation method of above-mentioned composite material, comprising the following steps:
1, the preparation of alkylation modification chitosan
1) it alkalizes
NaOH solid is added in isopropanol to strong basicity, chitosan is added thereto and is sufficiently stirred, is placed on ultrasonic response
Ultrasound is carried out in device at room temperature, is sufficiently alkalized, supersonic frequency 400MHz, ultrasonic time 20min；
The chitosan, deacetylation 78%-80%, granularity are 50-55 μm；
The mass ratio of the chitosan and NaOH solid is 1:2.5；
The quantity of isopropanol is 15 times of chitosan mass；
2) temperature reaction
Ultrasound terminates, and phase transfer catalyst tetrabutylammonium bromide is first added, after being completely dissolved, adds the bromo- 4- n-dodecane of 1-
Base benzene is reacted, and increasing the temperature to temperature is 60 DEG C, and insulated and stirred reacts 4h；
The dosage of the phase transfer catalyst accounts for the 8% of reaction system gross mass；
The addition mass ratio of the bromo- 4- dodecyl benzene of the 1- and chitosan is 9.1:2；
3) it post-processes
Reaction terminates, and glacial acetic acid is added dropwise and adjusts pH to 6-7, alkylation modification chitosan crude product Precipitation, filtering；Afterwards by alkyl
Change modification of chitosan crude product, which is added in 5wt% alcohol/hydrochloric acid solution, to be washed, and suction filtration is placed in 40 DEG C of vacuum drying ovens and does
It is dry to constant weight；
The usage amount of the 5wt% alcohol/hydrochloric acid solution is 12 times of alkylation modification chitosan crude product quality.
2, enhance the preparation of master batch
Nano titanium diboride, white carbon black, toughener and antioxidant are pre-mixed uniformly through high-speed mixer, rear extruding pelletization
Master batch, screw speed 100rpm must be enhanced, extruder temperature is 110 DEG C DEG C, partial size 3-5mm.
3, the preparation of composite material
Polypropylene, alkylation modification chitosan, poly- three phosphonitrile of amino ring, three (2- ethoxy) chlorinated isocyanurates and coupling agent are added
Enter twin-screw extrusion owner's spout, weighs enhancing master batch and be added from side spout, is extruded into jointly in extruder melt blending
Type is set separately from feed opening to head outlet temperature: 180 DEG C, 185 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, revolving speed
250rpm。
A kind of enhancing flame-retardant polypropylene composite material of embodiment 3
The composite material, in parts by weight, including following components:
It is 80 parts of polypropylene, 8 parts of nano titanium diboride, 3 parts of three phosphonitrile of poly- amino ring, three 5 parts of (2- ethoxy) chlorinated isocyanurates, white
1 part of carbon black, 4 parts of compatilizer, 7 parts of toughener, 0.5 part of antioxidant, 3 parts of coupling agent
The polypropylene is isotactic polypropylene, and melt index is 4 ~ 5g/10min；
The nano titanium diboride granularity 90-100nm, specific surface area 70-72m2/g；
The white carbon black, purity 99.5；
The compatilizer is alkylation modification chitosan, and O- alkylated reaction degree of substitution is 0.55；
The toughener includes esters of acrylic acid rubber powder, maleic anhydride inoculated polypropylene, polyvinyl alcohol and peroxidating diisopropyl
Benzene, four mass ratioes are 10:13:18:1；
The antioxidant is antioxidant 1010；
The coupling agent is two (dioctyl phosphite base) tetraisopropyl titanates；
The preparation method of above-mentioned composite material, comprising the following steps:
1, the preparation of alkylation modification chitosan
1) it alkalizes
NaOH solid is added in aqueous isopropanol to strong basicity, chitosan is added thereto and is sufficiently stirred, is placed on ultrasonic wave
Ultrasound is carried out in reactor at room temperature, is sufficiently alkalized, supersonic frequency 400MHz, ultrasonic time 20min；
The chitosan, deacetylation 85%-90%, granularity are 60-70 μm；
The mass ratio of the chitosan and NaOH solid is 1:2.5；
The quantity of isopropanol is 15 times of chitosan mass；
2) temperature reaction
Ultrasound terminates, and phase transfer catalyst tetrabutylammonium bromide is first added, after being completely dissolved, adds the bromo- 4- n-dodecane of 1-
Base benzene is reacted, and increasing the temperature to temperature is 60 DEG C, and insulated and stirred reacts 4h；
The dosage of the phase transfer catalyst accounts for the 8% of reaction system gross mass；
The addition mass ratio of the bromo- 4- dodecyl benzene of the 1- and chitosan is 9.1:2；
3) it post-processes
Reaction terminates, and glacial acetic acid is added dropwise and adjusts pH to 6-7, alkylation modification chitosan crude product Precipitation, filtering；Afterwards by alkyl
Change modification of chitosan crude product, which is added in 5wt% alcohol/hydrochloric acid solution, to be washed, and suction filtration is placed in 40 DEG C of vacuum drying ovens and does
It is dry to constant weight；
The usage amount of the 5wt% alcohol/hydrochloric acid solution is 10 times of alkylation modification chitosan crude product quality.
2, enhance the preparation of master batch
Nano titanium diboride, white carbon black, toughener and antioxidant are pre-mixed uniformly through high-speed mixer, rear extruding pelletization
Master batch, screw speed 80rpm-100rpm must be enhanced, extruder temperature is 110 DEG C -120 DEG C, partial size 2-5mm.
3, the preparation of composite material
Polypropylene, alkylation modification chitosan, poly- three phosphonitrile of amino ring, three (2- ethoxy) chlorinated isocyanurates and coupling agent are added
Enter twin-screw extrusion owner's spout, weighs enhancing master batch and be added from side spout, is extruded into jointly in extruder melt blending
Type is set separately from feed opening to head outlet temperature: 180 DEG C, 185 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, 190 DEG C, revolving speed
250rpm。
Comparative example 1:
Common compatilizer polypropylene grafted maleic anhydride is added in formula, its grafting rate of polypropylene grafted maleic anhydride is 2%,
Remaining component is same as Example 1, and preparation method, technological parameter are same as Example 1.
Comparative example 2:
Compatilizer is added without in formula, remaining component is same as Example 1, preparation method, technological parameter with 1 phase of embodiment
Together.
The Properties of Polypropylene Composite data of embodiment 1-3 and comparative example 1-2 preparation are as follows:
According to comparative example as it can be seen that the intensity and notch impact strength of obtained PP composite material are significantly lower than preparation of the present invention
PP composite material, it is seen that be added the present invention self-control compatilizer, the compatibility of fire retardant and polypropylene matrix can be improved, mentioned
The mechanical property of high PP composite material.
Finally, it should be noted that the above description is only a preferred embodiment of the present invention, it is not intended to restrict the invention, although
It describes the invention in detail with reference to the foregoing embodiments, it for those skilled in the art, still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in protection model of the invention
Within enclosing.
Claims (10)
1. a kind of enhancing flame-retardant polypropylene composite material, which is characterized in that according to parts by weight, be made of following raw material: poly- third
75-80 parts of alkene, 8-10 parts of nano titanium diboride, 3-5 parts of three phosphonitrile of poly- amino ring, three 3-5 parts of (2- ethoxy) chlorinated isocyanurates,
1-2 parts of white carbon black, 2-4 parts of compatilizer, 5-7 parts of toughener, 0.5-1.5 parts of antioxidant, 1-3 parts of coupling agent；
The compatilizer is alkylation modification chitosan, and O- alkylated reaction degree of substitution is 0.45-0.62.
2. enhancing flame-retardant polypropylene composite material according to claim 1, which is characterized in that the nano titanium diboride grain
Spend 50-100nm, specific surface area 70-80m2/g。
3. enhancing flame-retardant polypropylene composite material according to claim 1, which is characterized in that the toughener includes propylene
Esters of gallic acid rubber powder, maleic anhydride inoculated polypropylene, polyvinyl alcohol and cumyl peroxide, esters of acrylic acid rubber powder, horse
Maleic anhydride grafted polypropylene, polyvinyl alcohol and cumyl peroxide mass ratio are 8-10:13-18:15-18:1.
4. enhancing flame-retardant polypropylene composite material according to claim 1, which is characterized in that the polypropylene be isotactic or
Syndiotactic polypropylene, melt index are 4 ~ 10g/10min.
5. a kind of preparation method for enhancing flame-retardant polypropylene composite material, which is characterized in that including alkylation modification chitosan
Preparation, the preparation of the alkylation modification chitosan, including alkalization, temperature reaction and post-processing.
6. enhancing the preparation method of flame-retardant polypropylene composite material according to claim 5, which is characterized in that the alkalization,
It is that chitosan is added in the isopropanol alkaline solution of NaOH to carry out ultrasound, supersonic frequency 320-400MHz, ultrasonic time 20-
25min。
7. enhancing the preparation method of flame-retardant polypropylene composite material according to claim 5, which is characterized in that the heating is anti-
It answers, phase transfer catalyst tetrabutylammonium bromide is first added, adds the bromo- 4- dodecyl benzene of 1- and is reacted, reaction temperature
It is 55-60 DEG C, insulated and stirred reacts 3.5-4h.
8. enhancing the preparation method of flame-retardant polypropylene composite material according to claim 7, which is characterized in that the phase transfer
The dosage of catalyst accounts for the 6-8% of reaction system gross mass；The addition mass ratio of the bromo- 4- dodecyl benzene of 1- and chitosan is
9.1-9.5:2。
9. enhancing the preparation method of flame-retardant polypropylene composite material according to claim 6, which is characterized in that the shell is poly-
Sugar, deacetylation 70%-90%, granularity are 40-70 μm；The mass ratio of chitosan and NaOH solid is 1:1.5-2.5；Isopropanol
Additional amount is 10-15 times of chitosan mass.
10. enhancing the preparation method of flame-retardant polypropylene composite material according to claim 5, which is characterized in that place after described
Reason is added dropwise glacial acetic acid and adjusts pH to 6-7, and alkylation modification chitosan crude product Precipitation is washed with 5wt% alcohol/hydrochloric acid solution
It washs, 5wt% alcohol/hydrochloric acid solution usage amount is 10-15 times of alkylation modification chitosan crude product quality.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113756130A (en) * | 2020-06-04 | 2021-12-07 | 南京工业大学 | Porous polymer flame retardant and preparation method and application thereof |
| CN118108997A (en) * | 2024-04-30 | 2024-05-31 | 广东骊虹新材料有限公司 | Antibacterial plastic sealing nozzle and preparation method thereof |
-
2019
- 2019-08-31 CN CN201910819203.6A patent/CN110452462A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113756130A (en) * | 2020-06-04 | 2021-12-07 | 南京工业大学 | Porous polymer flame retardant and preparation method and application thereof |
| CN118108997A (en) * | 2024-04-30 | 2024-05-31 | 广东骊虹新材料有限公司 | Antibacterial plastic sealing nozzle and preparation method thereof |
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