CN103897372B - A kind of preparation method of transparent flame-retardant polycarbonate - Google Patents
A kind of preparation method of transparent flame-retardant polycarbonate Download PDFInfo
- Publication number
- CN103897372B CN103897372B CN201310094766.6A CN201310094766A CN103897372B CN 103897372 B CN103897372 B CN 103897372B CN 201310094766 A CN201310094766 A CN 201310094766A CN 103897372 B CN103897372 B CN 103897372B
- Authority
- CN
- China
- Prior art keywords
- flame retardant
- low speed
- rotation
- temperature
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 59
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 239000004417 polycarbonate Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920000515 polycarbonate Polymers 0.000 title claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 26
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 11
- 239000012757 flame retardant agent Substances 0.000 claims abstract description 8
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- -1 cyclohexyl methyl siloxanes Chemical class 0.000 claims description 8
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 claims description 7
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 6
- KVCGISUBCHHTDD-UHFFFAOYSA-M sodium;4-methylbenzenesulfonate Chemical compound [Na+].CC1=CC=C(S([O-])(=O)=O)C=C1 KVCGISUBCHHTDD-UHFFFAOYSA-M 0.000 claims description 6
- 235000010290 biphenyl Nutrition 0.000 claims description 5
- 239000004305 biphenyl Substances 0.000 claims description 5
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 5
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 238000010008 shearing Methods 0.000 claims description 4
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 2
- 230000003078 antioxidant effect Effects 0.000 claims description 2
- 239000000314 lubricant Substances 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 238000002156 mixing Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000002932 luster Substances 0.000 description 3
- 239000012994 photoredox catalyst Substances 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 150000004651 carbonic acid esters Chemical class 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The preparation method who the invention discloses a kind of transparent flame-retardant polycarbonate, it comprises the following steps: Al, add 60-80 part Merlon particle; A2, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add liquid flame retardant, its mass percent is 0.08-0.15 part, and mixed on low speed is even; Wherein, the rotating speed of described low speed rotation is 45-50 rpm; A3, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add solid flame retardant and auxiliary agent, described solid flame retardant is 0.08-0.1 part, and described auxiliary agent is 0.3-0.5 part; A4, be High Rotation Speed under 55-60 DEG C of condition in temperature, add 20-40 part Merlon powder; Wherein, the rotating speed of described High Rotation Speed is 200-250 rpm; A5, on double screw extruder, melt extrude granulation, temperature is 270-285 DEG C.
Description
Technical field
The present invention relates to flame retardant products, in particular, a kind of preparation method of transparent flame-retardant polycarbonate.
Background technology
Along with people are more and more higher to product appearance requirement, and the raising of people's awareness of safety, transparent flame-retarding gathers carbonic acidEster (Polycarbonate, PC) is more and more subject to consumer's favor with its excellent performance. The ripe transparent resistance of Halogen at presentThe fire-retardant rank of combustion PC is still the V0 level that thickness is 3.2mm, and V0 level carries out after twice combustion testings of 10 seconds sample, flameIn 30 seconds, extinguish, do not have comburant to fall down. As a rule, all reaching under the prerequisite of V0 level the anti-flammability of thinner materialCan be better. But, aspect the production technology of transparent flame-retarding PC, also exist at present following problem.
1, because the addition of fire retardant is very little, adding proportion is less than 0.1% conventionally, thus in mixing procedure fire retardantBe difficult for disperseing, cause the fire resistance of product unstable.
2, for the distribution that improves micro-fire retardant disperses, conventionally use strong shear screw combination, but strong shear screw combinationVery easily cause the xanthochromia of product, for improving the color and luster of product, conventionally use blue powder to mix colours, the membership that adds of blue powder causesThe reduction of product light transmittance.
Therefore, there is defect in prior art, needs to improve.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of novel transparent flame-retardant polycarbonate.
Technical scheme of the present invention is as follows: a kind of preparation method of transparent flame-retardant polycarbonate, and it comprises the following steps:A1, add 60-80 part Merlon particle; A2, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add liquid flame-proofAgent, its mass percent is 0.08-0.15 part, mixed on low speed is even; Wherein, to be that 45-50 turns every for the rotating speed of described low speed rotationMinute; A3, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add solid flame retardant and auxiliary agent, described solid flame retardantFor 0.08-0.1 part, described auxiliary agent is 0.3-0.5 part; A4, be High Rotation Speed under 55-60 DEG C of condition in temperature, add 20-40 partMerlon powder; Wherein, the rotating speed of described High Rotation Speed is 200-250 rpm; A5, on double screw extruder melting squeezeGo out granulation, temperature is 270-285 DEG C.
Preferably, in described preparation method, the time of described rotation is 3-7 minute.
Preferably, in described preparation method, described solid flame retardant is postassium salt of perfluoroalkane sulfonate, toluenesulfonic acid sodium salt, phosphoric acidTriphenylmethyl methacrylate, HBCD, melamine cyanurate or its combination.
Preferably, in described preparation method, 1 part of described solid flame retardant comprises 0.26 part of toluenesulfonic acid sodium salt, 0.19 partTriphenyl phosphate, 0.47 part of HBCD and 0.08 part of melamine cyanurate.
Preferably, in described preparation method, 1 part of described liquid flame retardant comprises 0.53 part of bisphenol-A-bis-(diphenylphosphinesAcid esters), 0.29 part of dimethyl silicone polymer and 0.18 part of cyclohexyl methyl siloxanes.
Preferably, in described preparation method, described double screw extruder arranges the weak strong screw combinations distributing of shearing.
Preferably, in described preparation method, the screw slenderness ratio of described double screw extruder is 33-39.
Preferably, in described preparation method, the screw slenderness ratio of described double screw extruder is 36.
Preferably, in described preparation method, a little less than described double screw extruder arranges at the rear portion of screw rod, shearing distributes by forceScrewing element.
Preferably, in described preparation method, described screwing element is two head thread elements.
Each technical characterictic of above-mentioned each technical scheme, the preparation method of the transparent flame-retardant polycarbonate being mutually combined to form.
Adopt such scheme, it is V0 (2.0) that the present invention has obtained fire-retardant rank through experiment, the transparent resistance of Halogen that color and luster is stableCombustion PC, has good market using value.
Brief description of the drawings
Fig. 1 is the schematic diagram of one embodiment of the present of invention.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
As shown in Figure 1, one embodiment of the present of invention are, a kind of preparation method of transparent flame-retardant polycarbonate, and it comprisesFollowing steps.
A1, add 60-80 part Merlon particle; For example, add 61,60,62,68,71,79 or 80 parts of Merlon grainsSon, i.e. PC particle.
A2, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add liquid flame retardant, its mass percent is0.08-0.15 part, mixed on low speed is even; Wherein, the rotating speed of described low speed rotation is 45-50 rpm; For example, temperature is31,30,32,33,34 or 35 DEG C; And for example, drip liquid flame retardant, and for example, the speed of dropping is 1/1 second, 1/2 seconds, 1Drip/5 seconds, 1/9 seconds or 1/10 seconds; And for example, add 0.08 part, 0.09,0.1,0.11,0.12,0.13,0.14 or 0.15Part liquid flame retardant; And for example, the rotating speed of described low speed rotation is 45,46,47,48,49 or 50 rpms (RPM). Preferably,The time of described rotation is 3-7 minute, and for example, the time of rotation is 3,3.1,4,5,6,6.9 or 7 minutes. For example, described liquidFire retardant is bisphenol-A-bis-(diphenyl phosphoesters), dimethyl silicone polymer, cyclohexyl methyl siloxanes or its combination.
A3, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add solid flame retardant and auxiliary agent, described solid resistanceCombustion agent is 0.08-0.1 part, and described auxiliary agent is 0.3-0.5 part; Described auxiliary agent is lubricant, flexibilizer, antioxidant, Antidrip agentOr its combination. For example, temperature is 31,30,32,33,34 or 35 DEG C; And for example, adopt the spoon of prefabricated capacity, several times by volumeSequentially add solid flame retardant, auxiliary agent; And for example, be mixed evenly in advance described solid flame retardant and described auxiliary agent, then adopt pre-The spoon of capacity processed, by volume sequentially adds described solid flame retardant and described auxiliary agent several times; For example, dividing 8,9 or 10 times addsEnter solid flame retardant and auxiliary agent. For example, add 0.08 part, 0.09,0.095 or 0.1 part described solid flame retardant; Described solid resistanceCombustion agent is postassium salt of perfluoroalkane sulfonate, toluenesulfonic acid sodium salt, triphenyl phosphate, HBCD HBCD, melamine cyanurateMCA or its combination. And for example, add 0.3,0.34,0.39,0.42,0.45,0.48 or 0.5 part of auxiliary agent. And for example, described low speed revolvesThe rotating speed turning is 45,46,47,48,49 or 50 rpms (RPM). Preferably, the time of described rotation is 3-7 minute, exampleAs, the time of rotation is 3,3.1,4,5,6,6.9 or 7 minutes.
A4, be High Rotation Speed under 55-60 DEG C of condition in temperature, add 20-40 part Merlon powder; Wherein, described high speedThe rotating speed of rotation is 200-250 rpm; For example, temperature is 55,56,57,58,59 or 60 DEG C; For example, described High Rotation SpeedRotating speed be 200,203,211,228,231,246 or 250 rpms. Preferably, the time of described rotation is 3-7 minute,For example, the time of rotation is 3,3.1,4,5,6,6.9 or 7 minutes. Preferably, temperature is that 60 DEG C, time of High Rotation Speed are 3.5Minute, rotating speed is 249RPM.
A5, on double screw extruder, melt extrude granulation, temperature is 270-285 DEG C. For example, temperature be 270,274,278,281,283 or 285 DEG C.
Preferably, Merlon particle and Merlon powder add up to 100 parts. For example, a preferred example is to add62 parts of Merlon particles, add 0.13 part of liquid flame retardant, and 1 part of described liquid flame retardant comprises 0.53 part of bisphenol-A-bis-(diphenyl phosphoester), 0.29 part of dimethyl silicone polymer and 0.18 part of cyclohexyl methyl siloxanes; Add 0.098 part of described solidFire retardant, adds 0.31 part of described auxiliary agent, and 1 part of described solid flame retardant comprises 0.26 part of toluenesulfonic acid sodium salt, 0.19 part of phosphoric acidTriphenylmethyl methacrylate, 0.47 part of HBCD and 0.08 part of melamine cyanurate; And, add 38 parts of Merlon powder;Wherein, add the condition of liquid flame retardant to be, the time of low speed rotation is 5 minutes, and rotating speed is that 47RPM, temperature are 34 DEG C; AddThe condition of solid flame retardant and auxiliary agent is, the time of low speed rotation is 7 minutes, and rotating speed is that 45RPM, temperature are 31 DEG C; High-speed rotaryThe time turning is 4 minutes, and rotating speed is that 245RPM, temperature are 58 DEG C; The sample that reaction obtains 1.6mm is V0 level, and its light transmittance is92.4%. And for example, add 80 parts of Merlon particles, add 0.09 part of liquid flame retardant, 1 part of described liquid flame retardant comprises0.57 part of bisphenol-A-bis-(diphenyl phosphoester), 0.21 part of dimethyl silicone polymer and 0.22 part of cyclohexyl methyl siloxanes; Add0.08 part of described solid flame retardant, adds 0.49 part of described auxiliary agent, and 1 part of described solid flame retardant comprises 0.23 part of toluenesulfonic acidSodium, 0.29 portion of triphenyl phosphate, 0.38 part of HBCD and 0.10 part of melamine cyanurate; And, add 20Part Merlon powder; Wherein, add the condition of liquid flame retardant to be, the time of low speed rotation is 6.8 minutes, rotating speed be 45RPM,Temperature is 30 DEG C; Add the condition of solid flame retardant and auxiliary agent to be, the time of low speed rotation is 3 minutes, and rotating speed is 50RPM, temperatureDegree is 35 DEG C; The time of High Rotation Speed is 4.9 minutes, and rotating speed is that 250RPM, temperature are 60 DEG C; Reaction obtains the sample of 2.0mmFor V0 level, its light transmittance is 90.1%.
Various embodiments of the present invention relate to this class chemical reaction related manufacturing processes, and main evaluation is to see product effect, forThe Merlon of transparent flame-retarding, transparent and fire-retardant is two very important indexs, and adopts above-mentioned each reality of the present inventionExecute example, when Related product can reach thickness and is 2.0mm, transparency be greater than 88.5% and flame retardant rating be V0 technology refers toMark.
Umber described in each embodiment of the present invention, it is relevant to quality, for example, adds the Merlon particle of 60g,Then add the liquid flame retardant of 0.15g, then add the solid flame retardant of 0.08g and the auxiliary agent of 0.3g, then add 40g'sMerlon powder.
In conjunction with the above-mentioned arbitrary embodiment of application, preferred, described double screw extruder arranges the weak strong screw rod distributing that dispersesCombination. For example, the screw slenderness ratio of described double screw extruder is 33 to 39; Preferably, through experiment test, described twin-screw squeezesThe screw slenderness ratio that goes out machine is 35.8 to 36 for good. And for example, described double screw extruder arranges weak shearing by force at the rear portion of screw rodThe screwing element distributing. Preferably, described screwing element is two head thread elements.
Like this, the mixing procedure of optimizing by use, makes micro-fire retardant obtain good distribution, increases product fire-retardantThe stability of performance. Being mainly by improving mixing equipment and optimizing mixing procedure, is exactly specifically by selecting suitable materialMaterial, comprises that mass ratio is the PC powder of 60-80% and the PC particle that ratio is 20-40%; On this basis, additionally addRatio is the liquid flame retardant of 0.08-0.15%, the solid flame retardant that ratio is 0.08-0.1%, and ratio is 0.3-0.5%Other auxiliary agent.
Suitable charging sequence, is specially and first adds particle, adds liquid flame retardant, again reinforcing body fire retardant and auxiliary agent, the most againAfter add PC powder.
For example, feed way is specially and first adds PC particle, then slowly adds liquid flame retardant when low speed batch mixing, mixesAfter add again solid flame retardant and auxiliary agent, low speed mixes, then adds PC powder to mix at a high speed; Control batch mixing speed, be specially low speedBe controlled at 45-50RPM, High-speed Control is at 200-250RPM; Mixture temperature control, controls 30-35 DEG C of left and right while being specially low speed,High-speed Control 55-60 DEG C of left and right; Mixing time general control is at 3-7min, to obtain being evenly stained with of micro-fire retardant and PC raw materialAttached, wherein, such as silicone based and Sulfonates of fire retardant etc., thus reach fire-retardant being uniformly distributed of trace.
And each embodiment uses special screw combinations, this screw combinations main feature is that weak dispersion distributes by force, makes micro-Amount fire retardant can keep good dispersion effect in extrusion, can ensure again the strong distributed function of micro-fire retardant, withTime be within the scope of 270-285 DEG C by controlling melt temperature, promote fire retardant and PC that phase cross-linking reaction occurs, the resistance of increase productCombustion rank and stability. This process also needs to select suitable screw slenderness ratio L/D, and preferred, ratio is 36; And a little less than specialShear the strong screwing element distributing, also relate to special thread position of components simultaneously, consider the plasticizing effect of product, this special spiral shellLine element is placed the rear position of leaning on of screw rod; And consider and the coordinating of other screwing element concrete and thickness cutout and reverseThe problem that is used in conjunction with of screwing element, by using screwing element and the combination of specific function, thereby realizes low shearingThe strong expressing technique distributing, guarantees the xanthochromia that is uniformly distributed and don't causes product of micro-fire retardant aborning, therebyGuarantee, under product color stable case, to have ensured the light transmittance of product. Preferably, adopt two head thread elements.
The optimization of the mixing procedure by various embodiments of the present invention and use transparent flame-retarding bolt special technology, through experiment cardBright, can obtain thickness and be 2.0mm time, fire-retardant rank is V0, and light transmittance > 88.5%, the transparent resistance of Halogen that color and luster is stableCombustion PC, has good market using value.
Further, embodiments of the invention can also be that each technical characterictic of the various embodiments described above, is combined to form mutuallyThe preparation method of transparent flame-retardant polycarbonate.
It should be noted that, above-mentioned each technical characterictic continues combination mutually, forms the various embodiment that do not enumerate in the above,All be considered as the scope that description of the present invention is recorded; And, for those of ordinary skills, can add according to the above descriptionTo improve or conversion, and all these improvement and conversion all should belong to the protection domain of claims of the present invention.
Claims (1)
1. a preparation method for transparent flame-retardant polycarbonate, is characterized in that, comprises the following steps:
A1, add 60-80 part Merlon particle;
A2, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add liquid flame retardant, its mass percent is 0.08-0.15 part, mixed on low speed is even; Wherein, the rotating speed of described low speed rotation is 45-50 rpm, and the time of described rotation is 3-7 minutes; Described liquid flame retardant is bisphenol-A-bis-(diphenyl phosphoesters), dimethyl silicone polymer, cyclohexyl methyl siloxanes or itsCombination;
A3, be low speed rotation under 30-35 DEG C of condition in temperature, slowly add solid flame retardant and auxiliary agent, described solid flame retardantFor postassium salt of perfluoroalkane sulfonate, toluenesulfonic acid sodium salt, triphenyl phosphate, HBCD, melamine cyanurate or its combination,Described auxiliary agent is lubricant, flexibilizer, antioxidant, Antidrip agent or its combination; Described solid flame retardant is 0.08-0.1 part, instituteStating auxiliary agent is 0.3-0.5 part; Wherein, the rotating speed of described low speed rotation is 45-50 rpm, and the time of described rotation is 3-7Minute;
A4, be High Rotation Speed under 55-60 DEG C of condition in temperature, add 20-40 part Merlon powder; Wherein, described High Rotation SpeedRotating speed be 200-250 rpm; The time of described rotation is 3-7 minute;
A5, on double screw extruder, melt extrude granulation, temperature is 270-285 DEG C, a little less than described double screw extruder arranges, cutsCut the screw combinations of strong distribution, screw slenderness ratio is 33-39, and double screw extruder arranges weak strong distribution of shearing at the rear portion of screw rodScrewing element, screwing element is two head thread elements; This screwing element is placed the rear position of leaning on of screw rod;
1 part of described solid flame retardant comprises 0.26 part of toluenesulfonic acid sodium salt, 0.19 portion of triphenyl phosphate, 0.47 part of hexabromo ring 12Alkane and 0.08 part of melamine cyanurate;
1 part of described liquid flame retardant comprises 0.53 part of bisphenol-A-bis-(diphenyl phosphoesters), 0.29 part of dimethyl silicone polymerAnd 0.18 part of cyclohexyl methyl siloxanes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310094766.6A CN103897372B (en) | 2013-03-22 | 2013-03-22 | A kind of preparation method of transparent flame-retardant polycarbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310094766.6A CN103897372B (en) | 2013-03-22 | 2013-03-22 | A kind of preparation method of transparent flame-retardant polycarbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103897372A CN103897372A (en) | 2014-07-02 |
| CN103897372B true CN103897372B (en) | 2016-05-11 |
Family
ID=50988967
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310094766.6A Expired - Fee Related CN103897372B (en) | 2013-03-22 | 2013-03-22 | A kind of preparation method of transparent flame-retardant polycarbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103897372B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106280378A (en) * | 2016-09-30 | 2017-01-04 | 福建华塑新材料有限公司 | One is exempted to spray polycarbonate compositions and preparation method thereof |
| CN109265992A (en) * | 2018-09-18 | 2019-01-25 | 吴立国 | Low-cost high-strength high heat-resistant halogen-free flame-retardant PA66 composition and preparation method thereof |
| CN110330779A (en) * | 2019-08-02 | 2019-10-15 | 横店集团得邦工程塑料有限公司 | A kind of permanent high light transmission fire retardant PC composition material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824213A (en) * | 2009-03-05 | 2010-09-08 | 帝人化成株式会社 | Flame-retardant polycarbonate resin composition |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090312479A1 (en) * | 2008-06-17 | 2009-12-17 | Sabic Innovative Plastics Ip Bv | Polycarbonate compositions |
-
2013
- 2013-03-22 CN CN201310094766.6A patent/CN103897372B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824213A (en) * | 2009-03-05 | 2010-09-08 | 帝人化成株式会社 | Flame-retardant polycarbonate resin composition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103897372A (en) | 2014-07-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101392077B (en) | Polypropylene color master-batch with pearlescent interference effect and preparation method thereof | |
| CN103897372B (en) | A kind of preparation method of transparent flame-retardant polycarbonate | |
| CN102276970B (en) | Halogen-free antiflaming thin-film polycarbonate material and preparation method thereof | |
| DE1931387A1 (en) | Flame protection equipment for glass fiber reinforced polyamide | |
| CN107619520A (en) | For polyethylene or polyacrylic blue phase black agglomerate and preparation method thereof | |
| CN101319068A (en) | White master batch applied for polyolefin film and preparation method thereof | |
| CN103298879B (en) | Elastica/fiber prescription | |
| CN103059542A (en) | Halogen-free flame-retardant PC-PET (polycarbonate-polyethylene terephthalate) alloy film and its making method | |
| CN103649140A (en) | ASA-based graft copolymer composition | |
| CN105086234A (en) | Polyvinyl chloride single-wall corrugated pipe used for buildings and preparation method of polyvinyl chloride single-wall corrugated pipe | |
| CN104072913B (en) | A kind of fastness master batch and manufacture method thereof | |
| CN104404651A (en) | Flame-retardant modified polyester wig fiber textile and manufacturing method thereof | |
| CN103739988A (en) | High-impact hydraulic-pressure-resistant PVC (polyvinyl chloride) irrigation pipe | |
| CN105585801A (en) | Novel low-smoke flame-retardant PVC cable material and preparation method thereof | |
| CN106085021A (en) | Alloy-type coating material and preparation method thereof | |
| CN104804304B (en) | Halogen-free flame retardant polypropylene composite material and preparation method thereof | |
| CN102260398B (en) | Premixed fluororubber gum with improved thermal tear resistance and preparation method thereof | |
| CN102146179B (en) | Full density LLDPE/HDPE (Linear Low Density Polyethylene/High-Density Polyethylene) polyethylene premixing assistant and preparation method thereof | |
| CN101333318A (en) | Precipitate-free polypropylene fire retardant mastre batch and method for preparing same | |
| CN104861585A (en) | Red phosphorus master batch modified composition based on PTT polyesters | |
| CN102604356A (en) | Efficient flame-retardant plastic alloy and preparation method thereof | |
| CN106009364A (en) | Thermoplastic crosslinking sheathing material | |
| CN102485791A (en) | Masterbatch | |
| CN105566739A (en) | Flame-retardant and weather-resistant color masterbatch and production method thereof | |
| CN104194251A (en) | Color masterbatch intermediate for plastic and processing technology thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent of invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 518104 Guangdong city of Shenzhen province Baoan District Tantou town of Songgang West Industrial Park building A16 Applicant after: SHENZHEN HALCYON NEW MATERIALS Co.,Ltd. Address before: 518104 Guangdong city of Shenzhen province Baoan District Tantou town of Songgang West Industrial Park building A16 Applicant before: SHENZHEN HALCYON ENGINEERING PLASTICS Co.,Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: SHENZHEN HALCYON ENGINEERING PLASTICS CO., LTD. TO: SHENZHEN HUALIXING NEW MATERIALS CO., LTD. |
|
| C53 | Correction of patent of invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Lai Hualin Inventor after: Lu Qiyong Inventor before: Lai Hualin |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: LAI HUALIN TO: LAI HUALIN LU QIYONG |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160511 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |