CN1288199C - Process for increasing polyolefin nano composite material through catalytic charcoal forming - Google Patents
Process for increasing polyolefin nano composite material through catalytic charcoal forming Download PDFInfo
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- CN1288199C CN1288199C CNB2004100113148A CN200410011314A CN1288199C CN 1288199 C CN1288199 C CN 1288199C CN B2004100113148 A CNB2004100113148 A CN B2004100113148A CN 200410011314 A CN200410011314 A CN 200410011314A CN 1288199 C CN1288199 C CN 1288199C
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Abstract
本发明属于催化成炭提高聚烯烃纳米复合材料的阻燃性能的方法，该方法中采用镍负载催化剂作为成炭催化剂，与聚烯烃、增容剂和改性蒙脱土熔融混合，制备无卤阻燃聚烯烃纳米复合材料。利用成炭催化剂与蒙脱土协同相应，在燃烧过程中促进聚烯烃本身转化为石墨结构炭，从而减少燃烧过程中聚合物裂解释放出的可燃气体含量，降低材料的燃烧速度，使材料具有自我保护作用。聚烯烃与阻燃组分混合的工艺简单，阻燃效率高。The invention belongs to a method for improving the flame retardancy of polyolefin nanocomposites by catalyzing carbon formation. In the method, a nickel-supported catalyst is used as a carbon formation catalyst, which is melted and mixed with polyolefin, compatibilizer and modified montmorillonite to prepare halogen-free Flame retardant polyolefin nanocomposites. Using the synergistic reaction between the carbon-forming catalyst and montmorillonite, it promotes the transformation of polyolefin itself into graphite-structured carbon during the combustion process, thereby reducing the content of combustible gases released by the cracking of the polymer during the combustion process, reducing the burning speed of the material, and making the material self-sufficient. Protective effects. The mixing process of polyolefin and flame retardant components is simple, and the flame retardant efficiency is high.
Description
Technical field
The present invention relates to the method that a kind of catalysis carbon-forming improves the flame retardant properties of olefin polymerization nanometer composite material.
Background technology
Polyolefine material is low with its price, the characteristics of good combination property and easily machine-shaping are widely used in fields such as automobile, electric wire, building materials, indoor article and furniture.The quality of fire retardant performance is the key technical index that can the product innovation be made up of polyolefine material of decision be used by the user.The flame resistant method that in the past was applied to polyolefine material has the halogen-containing fire retardant of adding, perhaps adds expansion type flame retardant, perhaps adds the fire retardant of inorganic type, as: magnesium hydroxide, aluminium hydroxide etc.In actual application, the problem that this three based flame retardant mainly exists is: 1, halogen-containing fire retardant systems discharges poisonous gas in combustion processes, is used by the restriction of many countries; 2, the flame retarding efficiency of the fire retardant of expansion type flame retardant and inorganic type is not high, is embodied in to have only when adding a large amount of these fire retardants just to give polymkeric substance enough good flame retardant properties.
Chem.Mater. (2000,12,1866-1873) reported a small amount of organically-modified laminar silicic acid salt formation nano composite material of adding in polyolefine, when adopting the flame retardant properties of tapered calorimeter evaluating material, can obviously reduce heat release rate in the polyolefine combustion processes, the fall maximum reaches 70-75%, has reduced the danger of fire.Studies show that by the mechanism that layered silicate is improved the polyolefine flame retardant properties, the layered silicate lamella burning surface assemble produce to cracking group divide and oxygen can not to volatilize or permeate be the reason of raising Flame Retardancy energy.Yet the formed barrier layer of layered silicate lamella can not can form three-dimensional protective layer to expansion type flame retardant.This has influenced the raising of layered silicate polyolefine flame retardant properties to a certain extent.Further improving the layered silicate lamella is the problem that faces at present to polyolefinic fire retardation.Chem.Mater. (2002,14,189-193) reported layered silicate and decabromodiphenyl oxide, the compound flame retardant properties of ANTIMONY TRIOXIDE SB 203 99.8 PCT fire retardant with further raising polyolefine-Nano composite material of montmorillonite, but result and bad.
Summary of the invention
The purpose of this invention is to provide the method that a kind of catalysis carbon-forming improves the flame retardant properties of olefin polymerization nanometer composite material.
The present invention is the catalyzer that adds a spot of catalysis carbon-forming in olefin polymerization nanometer composite material, utilizes the iris action of montmorillonite layer to polyolefine cracking volatiles, makes volatiles be converted into solid carbon, further improves the flame retardant properties of material.
The present invention has overcome the shortcoming that generation poison gas causes material property to descend with needing to add a large amount of fire retardants in the material combustion process in the above-mentioned prior art, utilize polyolefine-Nano composite material of montmorillonite becoming under the effect of charcoal supported catalyst, improve the flame retardant properties of olefin polymerization nanometer composite material by the synergistic effect of polynite and catalyzer.
The present invention makes olefin polymerization nanometer composite material with polyolefine, expanding material and organic modification montmonrillonite, metal supported catalyst by carry out melting mixing in mixed with polymers equipment, measures the flame retardant properties of material then by the method for tapered calorimeter evaluation.Its basic step and processing condition are:
With polyolefine, expanding material, organic modification montmonrillonite and ni-loaded catalyst in Banbury mixer in 160-200 ℃, rotating speed 60-100 revolutions per second melting mixing 8-10 minute, make polyolefin blend; Ratio of components by weight wherein, polyolefine is 75-90%, and expanding material is 5-10%, and modified montmorillonoid is greater than 0 and smaller or equal between 10%, and catalyzer is that ni-loaded catalyst is greater than 0 and smaller or equal between 5%;
Earlier with the pre-mixing at room temperature of polyolefine, expanding material and modified montmorillonoid, from main charging opening this mixture is entered that melting mixing prepares masterbatch the forcing machine, from the 2nd charging opening supported catalyst is added then and proceed melting mixing, each section of forcing machine temperature is in 160-200 ℃ of scope, the extruder screw rotating speed is 200-300 rev/min, gets the olefin polymerization nanometer mixture.
Wherein polyolefine comprises polypropylene or polyethylene; Expanding material is acid anhydrides polypropylene or acid anhydrides polyethylene, and maleic anhydride content is the 1-2.5% weight ratio; The used tensio-active agent of modified montmorillonoid is an alkylamine salt, and its structure is trimethylammonium hexadecyl brometo de amonio, octadecyl ammonium chloride or dimethyl-dihydro tallow ammonium chloride; The particle diameter of used modified montmorillonoid is at the 10-50 micron; Catalyst system therefor is that nickel particles loads on the micron-sized aluminium oxide-silicon oxide hybrid of 20-50, and nickel content is 50% weight ratio in the supported catalyst.
Polynite has collaborative corresponding in char forming catalyst that adopts among the present invention and the olefin polymerization nanometer composite material, can promote that in combustion processes polyolefine itself is converted into graphite-structure carbon, thereby the inflammable gas content that polymer cracking discharges in the minimizing combustion processes, reduce the combustionvelocity of material, heat release rate fall maximum reaches 85-90%.And polyolefine and flame retardance element blended technology are simple, the flame retarding efficiency height.
Embodiment
Embodiment 1
With polypropylene and maleic anhydride content is that the acid anhydrides polypropylene of 1% weight ratio enters in the Banbury mixer simultaneously by 90: 10 weight ratios, carries out melting mixing 10 minutes under 200 ℃ and 70 rev/mins, obtains polypropylene miser.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 1850 kilowatts/square metre, and duration of combustion is 420 seconds.
Embodiment 2
With polypropylene, maleic anhydride content be the polynite of the acid anhydrides polypropylene of 1% weight ratio and the trimethylammonium hexadecyl brometo de amonio modification that particle diameter is 10 microns, supported catalyst that particle diameter is 30 microns by 80: 10: 5: 5 weight ratios enter in the Banbury mixer simultaneously, under 200 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polypropylene composite.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 320 kilowatts/square metre, and duration of combustion is 1110 seconds.
Embodiment 3
Be that the acid anhydrides polypropylene of 2.5% weight ratio and the octadecyl ammonium chloride modified montmorillonoid that 2.5% particle diameter is 30 microns, the supported catalyst that 2.5% particle diameter is 20 microns enter in the Banbury mixer simultaneously with 87.5% polypropylene, 7.5% maleic anhydride content by weight, under 200 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polypropylene composite.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 490 kilowatts/square metre, and duration of combustion is 850 seconds.
Embodiment 4
By weight with 5% particle diameter be 50 microns supported catalyst and 75% polypropylene, the 10% maleic anhydride content acid anhydrides polypropylene that is 2% weight ratio and 10% particle diameter be 40 microns dimethyl-dihydro tallow ammonium chloride modified montmorillonoid adds in the Banbury mixer simultaneously, under 200 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polypropylene miser.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 280 kilowatts/square metre, and duration of combustion is 1650 seconds.
Embodiment 5
By weight being that used modified montmorillonoid adds in the Banbury mixer simultaneously in the acid anhydrides polyethylene of 2.5% weight ratio and 5% example 3 with supported catalyst used in 5% example 2 and 80% polyethylene, 10% maleic anhydride content, under 160 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polyethylene composite.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 360 kilowatts/square metre, and duration of combustion is 990 seconds.
Embodiment 6
Adopting supported catalyst used in modified montmorillonoid used in the example 4 of weight ratio 10%, 5% example 2 and 75% polyethylene and 10% maleic anhydride content is that the acid anhydrides polyethylene of 1% weight ratio carries out two and goes on foot melting mixing in twin screw extruder, screw speed is 200 rev/mins, and four sections temperature are respectively 160 ℃, 170 ℃, 170 ℃ and 170 ℃.In twin screw extruder, will contain polyethylene and modified montmorillonoid earlier and add, at the 2nd charging opening supported catalyst be added again at the 1st charging opening.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 290 kilowatts/square metre, and duration of combustion is 1350 seconds.
Embodiment 7
Adopting supported catalyst used in modified montmorillonoid used in the example 2 of weight ratio 10%, 5% example 3 and 75% polypropylene and 10% maleic anhydride content is that the acid anhydrides polypropylene of 1.5% weight ratio carries out two and goes on foot melting mixing in twin screw extruder, screw speed is 300 rev/mins, and four sections temperature are respectively 180 ℃, 190 ℃, 200 ℃ and 200 ℃.In twin screw extruder, will contain polypropylene and modified montmorillonoid earlier and add, at the 2nd charging opening supported catalyst be added again at the 1st charging opening.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 270 kilowatts/square metre, and duration of combustion is 1680 seconds.
Embodiment 8
Adopting supported catalyst used in modified montmorillonoid used in the example 4 of weight ratio 7%, 3% example 3 and 80% polypropylene and 10% maleic anhydride content is that the acid anhydrides polypropylene of 1.5% weight ratio carries out two and goes on foot melting mixing in twin screw extruder, screw speed is 250 rev/mins, and four sections temperature are respectively 180 ℃, 190 ℃, 200 ℃ and 200 ℃.In twin screw extruder, will contain polypropylene and modified montmorillonoid earlier and add, at the 2nd charging opening supported catalyst be added again at the 1st charging opening.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 300 kilowatts/square metre, and duration of combustion is 1250 seconds.
Embodiment 9
Adopting modified montmorillonoid used in the example 4 of weight ratio 5% and 85% polypropylene and 10% maleic anhydride content is that the acid anhydrides polypropylene of 1.5% weight ratio adds in the Banbury mixer simultaneously, under 200 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polypropylene composite.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 370 kilowatts/square metre, and duration of combustion is 850 seconds.
Embodiment 10
Adopting used supported catalyst and 85% polypropylene and 10% maleic anhydride content in the example 4 of weight ratio 5% is that the acid anhydrides polypropylene of 1.5% weight ratio adds in the Banbury mixer simultaneously, under 200 ℃ and 70 rev/mins, carry out melting mixing 10 minutes, and obtained polypropylene composite.
With compression molding above-mentioned sample is made and to be of a size of 100 millimeters * 100 millimeters * 6 millimeters test specimen, measure the polymkeric substance flame retardant properties according to the tapered calorimeter method of ASTM E 1354 regulations.35 kilowatts/square metre of the yield of radiation of well heater.Sample heat release rate peak value in combustion processes is 700 kilowatts/square metre, and duration of combustion is 410 seconds.
Claims (6)
1, a kind of catalysis carbon-forming improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that, with polyolefine, expanding material, organic modification montmonrillonite and ni-loaded catalyst in Banbury mixer in 160-200 ℃, rotating speed 60-100 revolutions per second melting mixing 8-10 minute, make polyolefin blend; Ratio of components by weight wherein, polyolefine is 75-90%, and expanding material is 5-10%, and modified montmorillonoid is greater than 0 and smaller or equal between 10%, and catalyzer is that ni-loaded catalyst is greater than 0 and smaller or equal between 5%;
Earlier with the pre-mixing at room temperature of polyolefine, expanding material and modified montmorillonoid, from main charging opening this mixture is entered that melting mixing prepares masterbatch the forcing machine, from the 2nd charging opening supported catalyst is added then and proceed melting mixing, each section of forcing machine temperature is in 160-200 ℃ of scope, the extruder screw rotating speed is 200-300 rev/min, get the olefin polymerization nanometer mixture, wherein said catalyzer is that nickel particles loads on the micron-sized aluminium oxide-silicon oxide hybrid of 20-50.
2, catalysis carbon-forming as claimed in claim 1 improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that described polyolefine is polypropylene or polyethylene.
3, catalysis carbon-forming as claimed in claim 1 improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that described expanding material is acid anhydrides polypropylene or acid anhydrides polyethylene, and wherein maleic anhydride content is the 1-2.5% weight ratio.
4, catalysis carbon-forming as claimed in claim 1 improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that the particle diameter of described modified montmorillonoid is at the 10-50 micron.
5, catalysis carbon-forming as claimed in claim 1 improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that, the used tensio-active agent of described modified montmorillonoid is an alkylamine salt, and its structure is trimethylammonium hexadecyl brometo de amonio, octadecyl ammonium chloride or dimethyl-dihydro tallow ammonium chloride.
6, catalysis carbon-forming as claimed in claim 1 improves the method for the flame retardant properties of olefin polymerization nanometer composite material, it is characterized in that nickel content is 50% weight ratio in the supported catalyst.
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| CNB2004100113148A CN1288199C (en) | 2004-12-08 | 2004-12-08 | Process for increasing polyolefin nano composite material through catalytic charcoal forming |
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| CNB2004100113148A CN1288199C (en) | 2004-12-08 | 2004-12-08 | Process for increasing polyolefin nano composite material through catalytic charcoal forming |
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| CN1288199C true CN1288199C (en) | 2006-12-06 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9134989B2 (en) | 2002-01-31 | 2015-09-15 | Qualcomm Incorporated | System and method for updating dataset versions resident on a wireless device |
| US9143560B2 (en) | 2007-06-19 | 2015-09-22 | Qualcomm Incorporated | Methods and apparatus for dataset synchronization in a wireless environment |
| US9386397B2 (en) | 2003-10-29 | 2016-07-05 | Qualcomm Incorporated | Method, software and apparatus for performing actions on a wireless device using action lists and versioning |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101453418B (en) * | 2007-12-05 | 2011-01-12 | 高德软件有限公司 | Updating method for synchronization between customer terminal and server |
| CN104177705A (en) * | 2014-08-22 | 2014-12-03 | 华东理工大学 | Method for preparing halogen-free flame retardant polyolefin material by utilizing multi-metal composite catalyst |
| CN108034126B (en) * | 2017-11-30 | 2020-07-31 | 中国科学院长春应用化学研究所 | Halogen-free flame retardant polyolefin composite material and preparation method thereof |
| CN110903552B (en) * | 2019-11-11 | 2022-04-08 | 珠海格力绿色再生资源有限公司 | High-flame-retardant modified polypropylene and preparation method thereof |
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2004
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9134989B2 (en) | 2002-01-31 | 2015-09-15 | Qualcomm Incorporated | System and method for updating dataset versions resident on a wireless device |
| US9386397B2 (en) | 2003-10-29 | 2016-07-05 | Qualcomm Incorporated | Method, software and apparatus for performing actions on a wireless device using action lists and versioning |
| US9591428B2 (en) | 2003-10-29 | 2017-03-07 | Qualcomm Incorporated | Method, software and apparatus for performing actions on a wireless device using action lists and versioning |
| US9143560B2 (en) | 2007-06-19 | 2015-09-22 | Qualcomm Incorporated | Methods and apparatus for dataset synchronization in a wireless environment |
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| CN1635021A (en) | 2005-07-06 |
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