CN104830041A - Low-thermal-release polycarbonate material and preparation method thereof - Google Patents
Low-thermal-release polycarbonate material and preparation method thereof Download PDFInfo
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- CN104830041A CN104830041A CN201510258014.8A CN201510258014A CN104830041A CN 104830041 A CN104830041 A CN 104830041A CN 201510258014 A CN201510258014 A CN 201510258014A CN 104830041 A CN104830041 A CN 104830041A
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- polycarbonate
- thermal release
- polycarbonate material
- low thermal
- release
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The invention discloses a low-thermal-release polycarbonate material and a preparation method thereof, belonging to the technical filed of polycarbonate materials. The polycarbonate material comprises the following raw materials in percentage by weight: 5-40 percent of a brominated flame retardant based on mass of bromine in the total amount of the composition, 2-50 percent of semi-aromatic polyesters and 30-90 percent of siloxane polycarbonate. The preparation method comprises the following steps: performing mechanical melt blending on the brominated flame retardant, the semi-aromatic polyesters and the siloxane polycarbonate composition, thereby obtaining the low-thermal-release polycarbonate of which the total thermal release amount is less than 65kW.min/m<2> within 2 minutes and of which the peak thermal release rate is less than 65kW/m<2> within 5 minutes. The requirement of FAR25.853 on the thermal release level of cabin materials is met.
Description
Technical field
The present invention relates to technical field of polycarbonate, particularly relate to a kind of low Thermal release polycarbonate material and preparation method thereof.
Background technology
Common application field generally uses UL (Underwriters Laboratories) system to carry out the flameproof effect of assessment material, and this system examines or check emphatically the initial combustibility of material.For the relatively narrow and small closed aircraft cabin in personnel's high concentration, space, material is once ignition, oxygen, release of heat produce poisonous flammable gas will be consumed in a large number, the more heats of further combustion-supporting generation known from experience by combustible gas, heat concentrates release will build the hot environment of a local, causes material accelerated degradation and produces more toxic combustible gas.Only can be suitable for Initial Stage of Fire by Flame Retardancy in UL system assessment cabin, once localized hyperthermia's environment is formed, occupant's escape time will be decided by the speed (in other words oxygen consumption rate) of material inflammable gas burst size in cabin.
1917, when Thornton finds that most of superpolymer burns, the inflammable gas of generation often consumed 1kg oxygen, will release (13.1 ± 0.7) MJ heat.1980, Huggett established the method estimating its heat release rate by measuring superpolymer burning oxygen-consumption.According to this principle, Babrauskas has invented cone calorimetry in nineteen eighty-two, and Ohio State University also improves and produced high-precision OSU calorimeter.1984, FAA has promulgated Federal Aviation Regulation (FAR), establish Flame Retardancy in cabin can airworthiness standard FAR25.853, it is FAR25.853 (d) that corresponding Thermal release controls clause, recommendation OSU calorimeter as standard method of test.The controlling indicator of FAR25.853 (d) progressively improves, and promotes the sustainable development of Novel low releasable material.1996, FAA and FTT company developed again the miniature calorimeter of FAA cooperatively, Thermal release is tested and becomes more convenient.
Since FAA in 1984 issues FAR, oneself aviation has been formulated in other countries and area one after another as source, its content is also substantially identical.For calendar year 2001 revised airplane in transportation category airworthiness standard FAR25 portion, wherein cabin interior facility Thermal release controlled clause is FAR25.853 (d), and under the thermal radiation that its acceptance criterion specifies, the mean value of cabin materials 2 minutes total thermal discharges must not more than 65kWmin/m
2, in 5 minutes, the mean value of peak heat rate of release must not more than 65kWmin/m
2.Correspondingly, the relevant provision of EASA (EASA) and Civil Aviation Administration of China (CAAC) airworthiness standard is EASA25.853 (d) and CCAR25.853 (d), and the sequence number of regulations is all identical with content.Various countries flyer manufacturer is as Boeing and Air Passenger, although also there is respective materials'use standard, all this clause is followed in unification.
Polycarbonate (PC) excellent combination property, be easier to realize the raising of flame retardant properties and the reduction of Thermal release by modification, it is a kind of desirable aeronautical material development object, have wide practical use at engine room inside, such as luggage carrier parts, seat component, walkie fork lift truck parts, air supply rate, bin element, top ceiling, porthole, wallboard, meal plate, floor, cargo hold ground cushion, aviation tray etc., owing to having low-gravity characteristic, can effectively reduce aircraft load, save fuel oil, reduce Carbon emission.
Up to now, there is multiple method to reduce the Thermal release of polycarbonate material, reached materials'use standard in cabin to make it.
USP4629759 discloses the flame resistant method of a kind of polycarbonate and blend polyetherimides, obtains Thermal release peak value be less than 100KW/m by interpolation brominated Polystyrene fire retardant
2material.
USP4923933, by copolymer blended to the polycarbonate containing dihydroxyphenyl propane, m-phthalic acid and terephthalic acid, the polycarbonate containing tetrabromo-bisphenol and polyimide-siloxane, obtained Thermal release peak value and has been less than 50KW/m
2low Thermal release polycarbonate.
CN94115303.7 select containing the polycarbonate of m-phthalic acid and terephthalic acid and polyetherimide and polyimide-siloxane copolymer blended, obtained the cabin panel material of low Thermal release.
CN200680049993.5 and USP7652107 by containing the poly-aryl ester of Resorcinol or poly-aryl carbonates and polyimide-siloxane copolymer blended, obtain the thermoplastic material of low Thermal release.
USP7790262 discloses carbonate copolymer of a kind of polysiloxane, Resorcinol and dihydroxyphenyl propane and preparation method thereof, and this multipolymer has low heat emission characteistics.
These methods have by polyetherimide and common polycarbonate blended, have will to introduce polycarbonate to, isophthalic structure copolymer blended with polyimide-siloxane again, what have directly will introduce polycarbonate to, isophthalic structure and polysiloxane.The blended temperature needed more than 300 degrees Celsius of polyetherimide and polycarbonate, this can cause polycarbonate to be degraded, and, be usually difficult to obtain light effect.Polycarbonate or the polyarylester with isophthalic structure need special synthesis, are not a kind of technique of simple possible.
Summary of the invention
For solving the shortcoming of existing polycarbonate material, the object of this invention is to provide a kind of low Thermal release polycarbonate material and preparation method thereof, bromide fire retardant, semi-aromatic polyester and siloxane polycarbonate composition by melt blending, are obtained 2 minutes Thermal release total amounts and are less than 65kWmin/m by the present invention
2, 5 minute-peak heat release rate are less than 65kW/m
2low Thermal release polycarbonate, meet the requirement of FAR25.853 to material Thermal release level in cabin.
The formula of low Thermal release polycarbonate material of the present invention comprises the raw material of following weight percent: the 5%-40% that bromide fire retardant is total composition with the Mass Calculation of bromine, semi-aromatic polyester 2%-50%, siloxane polycarbonate 30%-90%.
Described bromide fire retardant is decabromodiphynly oxide, brominated Polystyrene, three (tribromo phenyl) cyanurate, containing the polycarbonate of tetrabromo-bisphenol or the tetrabromobisphenol a polycarbonate oligopolymer of tribromophenol end-blocking, in described bromide fire retardant, the mass percentage of bromine is at 30%-90%.
Preferably described bromide fire retardant is with the 10%-25% of the Mass Calculation of bromine for polycarbonate material total amount.
Described semi-aromatic polyester is common PET polyester slice or flame-proof copolyester that is brominated or phosphorus composition.
It is 5%-30% that preferably described semi-aromatic polyester adds quality in polycarbonate material.
Described siloxane polycarbonate preferably but be not limited only to commercially available prod.
It is 40%-80% that preferably described siloxane polycarbonate adds quality in polycarbonate material.
In described siloxane polycarbonate, siloxanes is present in polycarbonate with copolymerized form, and siloxanes mass percentage is 1%-10%.
Also containing additive in described low Thermal release polycarbonate material, described additive is one or more in pigment, weighting agent, toughener, oxidation inhibitor, anti ultraviolet agent, lubricant, releasing agent or anti-dripping agent, and additive addition in polycarbonate material is 0.1%-30%.
The concrete steps of the preparation method of low Thermal release polycarbonate material of the present invention are as follows:
(1) raw material is taken by proportioning;
(2) raw material that step (1) takes is carried out drying;
(3) dried raw material is passed through Banbury mixer or screw extrusion press melting mixing within the scope of 250 DEG C-330 DEG C, after extruding cooling, obtain low Thermal release polycarbonate material of the present invention.
Compared with prior art, technique effect of the present invention is as follows:
The present invention is by the method for melt blending, bromide fire retardant is added siloxane polycarbonate, although significantly can reduce its Thermal release numerical value, under suitable addition, the mean value that still can not reach 2 minutes total thermal discharges that FAR25.853 (d) requires must not more than 65kWmin/m
2, the mean value of peak heat rate of release must not more than 65kWmin/m in 5 minutes
2.Surprisingly, in above-mentioned two kinds of compositions, add polyethylene terephthalate (PET), significantly reduce Thermal release numerical value further, be met the fire-retardant blend that FAR25.853 (d) requires.
The present invention all adopts marketable material, does not adopt special synthesis material, and wherein polyethylene terephthalate can also be reworked material, not only with low cost, and has special environment protection significance.
So, the invention provides a kind of raw material sources extensive, the formula that working method is simple and technique, obtain 2 minutes Thermal release total amounts and be less than 65kWmin/m
2, 5 minute-peak heat release rate are less than 65kW/m
2low Thermal release polycarbonate, meet the requirement of FAR25.853 to material Thermal release level in cabin.
Embodiment
The following examples describe in further detail of the present invention.
The method of gained target product of the present invention being carried out to Thermal release test can be OSU calorimeter, cone calorimetry, also can be micro-combustion calorimeter.
OSU calorimeter is the pyrolysis-type calorimeter invented by Ohio State University, obtains FAA accreditation, and is the testing tool that FAR25.853 standard method of test is specified.Cone calorimetry all adopts the principle of work identical with OSU with micro-combustion calorimeter, utilizes the amount of oxygen of materials pyrolysis burning consumption to measure its parameter such as Thermal release peak rate and Thermal release total amount.But the sample size that they adopt is different with quality, and structure and using method also have larger difference, the test result obtained does not have the possibility mutually converted yet.According to the research of FAA, there is good dependency in the test result of micro-combustion calorimeter and cone calorimetry, but also not much else, not there are some researches show to there is conversion relation between the two.For investigator, OSU and cone calorimetry is used to there is many difficulties, sample requirements is large, sample preparation difficulty, test duration is long, and testing expense is high, is unfavorable for carrying out research work in enormous quantities, micro-combustion calorimeter solves this problem well, only needs several milligrams of samples and very short time just can test out the Thermal release feature of material.Therefore, micro-combustion calorimeter be have also been obtained the license of FAA as one of material Thermal release research method.
In order to prove that described PET has the effect of unique reduction Thermal release level to polycarbonate, the present invention first adopts MCC-2 micro-combustion calorimeter to analyze the Thermal release parameter of different content PET/PC blend, the results are shown in Table the embodiment 1-6 listed by 1.The all comparative examples of table 2 and embodiment adopt OSU calorimeter to measure Thermal release parameter, and test condition is FAR25.853 (IV) specified standards condition.
The full name of FAR25.853 is that US Airways management rules-airplane in transportation category-engine room inside is implemented, FAA.FAR.25.853 (CCAR 25.853) has done requirement to material in cabin and chair cushion respectively in a) and b) bar row, specified in more detail is set forth in annex F. and annex F comprises I, II, III, IV, V 5 partial contents, and here is the related introduction for this 5 part.
I is light performance test requirement to material, the regulation such as method and judgement.This part is the main experimental section of FAR 25.853, the horizontal firing that everybody knows usually, vertical combustion, miter angle burns, 60 degree of angle burnings are exactly for this, concrete have more introductions below. and it should be noted that and must note Sorting Materials before test, in order to avoid the testing method of the mistake used.
II is the composite test about aircraft seat cushion, it is to be noted that the test about aircraft seat cushion not only requires that starting material meet the requirement of annex F I, also will by the combined test of II, just calculate by test .FAR25.853 (c) Appendix F, Part II is an oil burner nozzle for the combined burning source of seat, provides standard model respectively to seat chair pad and backrest:
Seat chair pad dimensional requirement: [(18 ± 1/8) * (20 ± 1/8) * (4 ± 1/8)] in.;
Backrest dimensional requirement: [(18 ± 1/8) * (25 ± 1/8) * (2 ± 1/8)] in
Above size does not all comprise the size of braiding sealing and seam lap,
III is the test method about cargo hold cushioning material fire-resistance flame burn-through resistance, comprises cargo hold sidewall and top ceiling liner.
IV is the test measuring cabin materials heat release rate under thermal radiation, requires that total anti-heat mean value is no more than 65KW.MIN/M
2, heat release rate peak value is no more than 65KW.M
2.
V is the test method measuring material smoke generation characteristics, and smoke-producing amount quantizes according to optical density readings, be averaging Ds and be no more than 200.
Test relates to material
First kind material
The paving on top ceiling inside panel dividing plate kitchen structure large cabinet wall panel structure floor and the material for the manufacture of (except the chest of the bin under seat and storage magazine map one class smallclothes) between storage
Equations of The Second Kind material
Floor covering, textiles (comprising tent and cover), seat chair pad, liner, there are coated fabric (ornamental and non-decorative) leatherware, pallet and galley equipment etc.
Embodiment 1-6
Embodiment 1-6 composition composition and the performance test results as shown in table 1:
The concrete steps of the preparation method of material are as follows:
(1) raw material is taken by proportioning;
(2) raw material that step (1) takes is carried out drying;
(3) dried raw material is passed through Banbury mixer or screw extrusion press melting mixing within the scope of 250 DEG C-330 DEG C, after extruding cooling, obtain target product.
Table 1 PET is on the impact of PC Thermal release level
Each routine peak heat rate of release from table 1, because itself mass percent of reduction Amplitude Ratio reduction amplitude of adding the peak heat rate of release of PET, PC is much bigger, such as add the PC of 20%PET, its peak heat rate of release reduces 56.5%.Clear and definite thus, PET has remarkable effect to the Thermal release peak rate reducing PC.
Comparative example 7-10 and embodiment 11,12
The composition of comparative example 7-10 and embodiment 11,12 form and the performance test results as shown in table 1:
The concrete steps of the preparation method of material are as follows:
(1) raw material is taken by proportioning;
(2) raw material that step (1) takes is carried out drying;
(3) dried raw material is passed through Banbury mixer or screw extrusion press melting mixing within the scope of 250 DEG C-330 DEG C, after extruding cooling, obtain target product.
Table 2 comparative example and embodiment
Note: EXL1414-siloxane polycarbonate, XHT8141-high heat polycarbonates, DBDPO-decabromodiphynly oxide, PBBC-tetrabromobisphenol a polycarbonate, TF1645-tetrafluoroethylene anti-dripping agent, Irganox 168-oxidation inhibitor
Comparative example 7-10 presents the remarkably influenced added Thermal release level of fire retardant kind, amount of flame-retardant agent, siloxanes composition and PET under OSU test condition further, highlight bromide fire retardant, siloxanes composition and PET adds necessity of the present invention simultaneously, embodiment 11-12 is that two of these influence factors optimize special case, show that composition and engineering disclosed by the invention is effective, the requirement of FAA to material Thermal release in cabin can be reached: within 2 minutes, Thermal release total amount is less than 65kWmin/m
2, 5 minute-peak heat release rate are less than 65kW/m
2.
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (10)
1. a low Thermal release polycarbonate material, is characterized in that: the formula of described polycarbonate material comprises the raw material of following weight percent: the 5%-40% that bromide fire retardant is total composition with the Mass Calculation of bromine, semi-aromatic polyester 2%-50%, siloxane polycarbonate 30%-90%.
2. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: described bromide fire retardant be decabromodiphynly oxide, brominated Polystyrene, three (tribromo phenyl) cyanurate, containing the polycarbonate of tetrabromo-bisphenol or the tetrabromobisphenol a polycarbonate oligopolymer of tribromophenol end-blocking.
3. low Thermal release polycarbonate material as claimed in claim 2, is characterized in that: in described bromide fire retardant, the mass percentage of bromine is at 30%-90%.
4. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: described bromide fire retardant is with the 10%-25% of the Mass Calculation of bromine for polycarbonate material total amount.
5. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: described semi-aromatic polyester is common PET polyester slice or flame-proof copolyester that is brominated or phosphorus composition.
6. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: it is 5%-30% that described semi-aromatic polyester adds quality in polycarbonate material.
7. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: it is 40%-80% that described siloxane polycarbonate adds quality in polycarbonate material.
8. low Thermal release polycarbonate material as claimed in claim 1, is characterized in that: in described siloxane polycarbonate, and siloxanes is present in polycarbonate with copolymerized form, and siloxanes mass percentage is 1%-10%.
9. low Thermal release polycarbonate material as claimed in claim 1, it is characterized in that: also containing additive in described low Thermal release polycarbonate material, described additive is one or more in pigment, weighting agent, toughener, oxidation inhibitor, anti ultraviolet agent, lubricant, releasing agent or anti-dripping agent, and additive addition in polycarbonate material is 0.1%-30%.
10. prepare a method for the low Thermal release polycarbonate material as described in any one of claim 1-9, it is characterized in that: the concrete steps of described method are as follows:
(1) raw material is taken by proportioning;
(2) raw material that step (1) takes is carried out drying;
(3) dried raw material is passed through Banbury mixer or screw extrusion press melting mixing within the scope of 250 DEG C-330 DEG C, after extruding cooling, obtain low Thermal release polycarbonate material of the present invention.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105315645A (en) * | 2015-10-12 | 2016-02-10 | 深圳市富恒新材料股份有限公司 | Transparent PC composite and preparation method thereof |
| CN109305796A (en) * | 2018-10-11 | 2019-02-05 | 山东奥福环保科技股份有限公司 | A kind of gasoline engine exhaust aftertreatment honeycomb ceramic filter body and preparation method thereof |
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| CN103534315A (en) * | 2011-03-31 | 2014-01-22 | 沙特基础创新塑料Ip私人有限责任公司 | Aircraft component comprising flame retardant s iloxane - containing polymer compositions |
| CN104039890A (en) * | 2012-01-19 | 2014-09-10 | 沙伯基础创新塑料知识产权有限公司 | Polycarbonate-polyester compositions, methods of manufacture, and articles thereof |
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2015
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Patent Citations (3)
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| CN103282433A (en) * | 2010-11-05 | 2013-09-04 | 沙伯基础创新塑料知识产权有限公司 | Flame-resistant polyester-olycarbonate compositions, methods of manufacture, and articles thereof |
| CN103534315A (en) * | 2011-03-31 | 2014-01-22 | 沙特基础创新塑料Ip私人有限责任公司 | Aircraft component comprising flame retardant s iloxane - containing polymer compositions |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105315645A (en) * | 2015-10-12 | 2016-02-10 | 深圳市富恒新材料股份有限公司 | Transparent PC composite and preparation method thereof |
| CN109305796A (en) * | 2018-10-11 | 2019-02-05 | 山东奥福环保科技股份有限公司 | A kind of gasoline engine exhaust aftertreatment honeycomb ceramic filter body and preparation method thereof |
| CN109305796B (en) * | 2018-10-11 | 2021-08-27 | 山东奥福环保科技股份有限公司 | Honeycomb ceramic filter body for gasoline engine exhaust aftertreatment and preparation method thereof |
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