CN103937192A - PC/PA 11 (polycarbonate/polyamide 11) composition and preparation method thereof - Google Patents
PC/PA 11 (polycarbonate/polyamide 11) composition and preparation method thereof Download PDFInfo
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- 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
- B29C48/50—Details of extruders
- B29C48/505—Screws
- B29C48/625—Screws characterised by the ratio of the threaded length of the screw to its outside diameter [L/D ratio]
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- 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
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- 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
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- 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
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- 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
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
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- 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
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- 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
- B29C2948/92704—Temperature
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- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92838—Raw material pre-treatment, e.g. drying or cleaning
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- 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
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
Abstract
The invention discloses a PC/PA 11 (polycarbonate/polyamide 11) composition and a preparation method thereof, belonging to the technical field of materials. The PC/PA 11 composition is prepared from the following raw materials in parts by weight: 65-90 parts of PC, 10-35 parts of PA 11, 0.1-3 parts of toluene diisocyanate, 0.1-3 parts of 2,2'-(1,3-phenylene)-dioxazoline, 0.1-6 parts of styrene-maleic anhydride copolymer, 0.1-2 parts of anti-dripping agent, 0.1-1 part of hindered phenol antioxidant, 0.1-1 part of phosphite antioxidant and 0.1-1 part of lubricant, wherein the sum of the PC and PA 11 is 100 parts. The in-situ reaction compatibilization process is utilized to prepare the PC/PA 11 composition with favorable mechanical properties, high flame retardancy, favorable chemical resistance and favorable processability; and the PC/PA 11 composition can be used in automobiles (front and back baffles, post hoods, wheel covers and instrument masks), electronic and electric appliances (electric tool shells, wiring instruments and relays) and other industries.
Description
Technical field
The present invention relates to Material Field, particularly relate to a kind of PC/PA11 composition and method of making the same.
Background technology
The develop rapidly of China in Recent Years industry, constantly expands the application surface of polycarbonate (PC), and its demand also constantly increases.But along with science and technology progress with rapid changepl. never-ending changes and improvements, the continuous renewal of Industrial products is regenerated, requirement to material property is more and more harsh, the polycarbonate of conventional model can not meet all types of requirements of product in product performance, and PC exists that melt viscosity is large, poor fluidity, high temperature facile hydrolysis, poor solvent resistance, susceptibility to breach is high, easily there is swelling and stress cracking, and the shortcomings such as frictional coefficient is large, higher, the special trade mark price of melt temperature height, thereby directly affect its further deeply application and popularization.
Polymeric amide, claims again nylon (PA), is that in five large general engineering plastic, purposes is the widest, kind is maximum, output is maximum, the base resin of high comprehensive performance.Polymeric amide 11 (PA11) is the long carbochain softness polymeric amide synthetic taking Viscotrol C as raw material, compares with PA66 with PA6, and it has the advantages such as low water-absorbent, good dimensional stability and lower temperature resistance, good electrical insulation capability; And have elastic memory, in the time that external force is removed, PA11 can return to original shape; Stress cracking resistance is good, can embed therein metal parts and not easy to crack; Can meet the injection moulding of various melt viscosity scopes and extrude processing; The erosion of termite-proof moth, harmless, be a kind of bio-based materials.Thereby PA11 is widely used in the fields such as automobile, machinery, electronics, military project, medical treatment, food and physical culture.
By PC and PA11 blend, can obviously improve PC mobility, improve its processing characteristics, stress crack resistance performance and chemical resistance, simultaneously can keep thermotolerance and the shock-resistance etc. that PC is higher.PC/PA11 blend has good solvent resistance, wear resistance, dimensional stability and stress cracking resistance, and processing characteristics is better, heat-drawn wire is high, can be applicable to the industry such as automobile (front and rear baffle, post cover, wheel cover, instrument mask) and electronic apparatus (electric power tool shell, distribution apparatus, rly.).
But because two kinds of component crystal properties in PC/PA11 co-mixing system exist greatest differences, compatibility performance is not good enough, has affected performance and the application of co-mixing system.Although some performance of alloy that adopts simple blend method to prepare improves, and because two-phase interface adhesiveproperties is bad, can cause unstable properties, some performance also can decline.In PC/PA11 co-mixing system, add the 3rd component expanding material, can further improve the performance of blend, obtain the alloy material having compared with stability.At present, in prior art, the modification of PC is done to some researchs, all to have added compatilizer in PC/PA11 co-mixing system, patent CN200910048187.1 discloses a kind of polycarbonate/polyamide alloy and preparation method thereof, its compatilizer is vinylbenzene (ST)-maleic anhydride (MAH) binary polymer and the compound that reacts the ABS-g-GMA extruding, or contains vinylbenzene (ST) ter-polymers of glycidyl methacrylate (GMA) and maleic anhydride (MAH) bi-functional monomer; Patent CN201080033771.0 discloses polycarbonate/polyester or the polycarbonate/daiamid composition of impact modification, a kind of blend polymer that it comprises polycarbonate and polyester and/or polymeric amide, adds a kind of anti-impact modifier blend of coker/shell and Functional Polyolefine anti-impact modifier; Patent CN201310300517.8 discloses anti-aging PA/PC polyblend, and its compatilizer is SEBS-g-MAH; Patent CN201310687754.4 discloses rat-and-ant proof PA/PC environmentally-friendly plastic, and its compatilizer is PP-g-MAH.
The preparation method of the PC/PA11 blend of prior art all adopts two step method, its essence is that first preparation is containing the compatilizer of polar functional group, as: ABS-g-GMA, MAH-g-ST-g-GMA, SEBS-g-MAH, PP-g-MAH etc.Then, then by PC, PA11, carry out blending extrusion containing compatilizer and the toughner of polar functional group, thereby reach the object of toughness reinforcing increase-volume.
Summary of the invention
The deficiency existing for prior art, the object of the invention is to prepare have that mechanical property is good, flame retardant resistance is high, the PC/PA11 composition of chemical resistant properties and good processability, can be applicable to the industry such as automobile (front and rear baffle, post cover, wheel cover, instrument mask) and electronic apparatus (electric power tool shell, distribution apparatus, rly.).
The following scheme of the concrete employing of the present invention:
A kind of PC/PA11 composition, is prepared from by the raw material of following weight part:
Described anti-dripping agent is fluoropolymer;
Described Hinered phenols antioxidant is the positive octadecanol ester of β-(4-hydroxy phenyl-3,5-di-t-butyl) propionic acid; Described phosphite ester kind antioxidant is tricresyl phosphite (2,4-di-tert-butyl-phenyl) ester.
In some embodiment, PC/PA11 composition, is prepared from by the raw material of following weight part therein:
In some embodiment, PC/PA11 composition, is prepared from by the raw material of following weight part therein:
In some embodiment, described polycarbonate is dihydroxyphenyl propane aromatic copolycarbonate therein, and number-average molecular weight is 15000～30000; The number-average molecular weight of described polymeric amide 11 is 20000～30000; In described styrene-maleic anhydride copolymer, the content of maleic anhydride is 15%～20%.
Therein in some embodiment, the number-average molecular weight of described polycarbonate is for being 18000～27000; The number-average molecular weight of described polymeric amide 11 is 22000～26000.
In some embodiment, described lubricant is pentaerythritol stearate therein; Described anti-dripping agent is tetrafluoroethylene.
Another object of the present invention is to provide the preparation method of PC/PA11 composition.
The preparation method of above-mentioned PC/PA11 composition, concrete technical scheme, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 100～120 DEG C, dry 4～12 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 220～240 DEG C, two district's temperature: 230～250 DEG C, three district's temperature are 230～250 DEG C, four district's temperature: 230～250 DEG C, five district's temperature are 230～250 DEG C, six district's temperature: 230～250 DEG C, die head temperature: 230～250 DEG C, driving screw rotating speed is: 100～400rpm.
In some embodiment, in described step (1), polycarbonate and polymeric amide 11 are placed in 110 DEG C therein, dry 4～6 hours; Processing parameter in described step (3) is: district's temperature is 220～230 DEG C, two district's temperature: 230～240 DEG C, three district's temperature are 230～240 DEG C, four district's temperature: 230～240 DEG C, five district's temperature are 230～240 DEG C, six district's temperature: 230～240 DEG C, die head temperature: 230～240 DEG C, driving screw rotating speed is: 150～250rpm.
In some embodiment, the screw rod of described parallel double-screw extruder is shaped as single thread therein; The ratio L/D of spiro rod length L and diameter D is 35～60; Described screw rod is provided with 1 above gear block district and 1 above left-hand thread district.
In some embodiment, the ratio L/D of described spiro rod length L and diameter D is 40～55 therein; Described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Principle of the present invention is as follows:
In situ reactive compatibilization mechanism of the present invention is two kinds of superpolymer, puts in the lump in parallel double-screw extruder containing the monomer of double reactive functional group, in the extrusion of melt blending, react at two-phase interface place, generate random, grafting or segmented copolymer, produce on the spot compatilizer, should react with these two kinds of superpolymer respectively containing the monomer of double reactive functional group, form the compatilizer of superpolymer-co-containing monomer-co-superpolymer of double reactive functional group.
The present invention adopts the method for in situ reactive compatibilization, in parallel double-screw extruder, the terminal hydroxy group of polycarbonate can be respectively and the isocyanate groups of tolylene diisocyanate, 2, 2'-(1, 3-phenylene) the oxazoline group of-bisoxazoline reacts, the end amino of polymeric amide 11, end carboxyl can be respectively and the isocyanate groups of tolylene diisocyanate, 2, 2'-(1, 3-phenylene) the oxazoline group of-bisoxazoline reacts, form compatilizer PC-co-TDI-co-PA11, compatilizer PC-co-PBO-co-PA11, thereby improve the consistency of PC/PA11 system, obtain having mechanical property good, flame retardant resistance is high, the PC/PA11 composition of chemical resistant properties and good processability.
The styrene-maleic anhydride copolymer (SMA) that the present invention adds plays the effect of auxiliary compatilizer, its principle is that the anhydride group in styrene-maleic anhydride copolymer can react and form SMA-g-PA11 with the end amino of PA11, and the consistency of styrol structural unit in SMA-g-PA11 and polycarbonate is fabulous, thereby further improve the consistency of PC/PA11 system.
Compared with prior art, the present invention has following beneficial effect:
1, PC/PA11 composition of the present invention, have that mechanical property is good, flame retardant resistance is high, the advantage such as chemical resistant properties and good processability, can be applicable to the industry such as automobile (front and rear baffle, post cover, wheel cover, instrument mask) and electronic apparatus (electric power tool shell, distribution apparatus, rly.).
2, adopt method of the present invention to prepare PC/PA11 composition, belong to single stage method (In Situ Compatibilization reaction), it has minimizing operation compared to two step method, shortens flow process, reduces costs the advantage of boosting productivity.And this preparation method's technique is simple, be easy to control, not high to equipment requirements, the equipment using is general polymer processing equipment, invests not high.
Brief description of the drawings
Figure 1 shows that preparation technology's schema of PC/PA11 composition of the present invention.
Embodiment
For further understanding feature of the present invention, technique means and the specific purposes that reach, function, resolve the advantages and spirit of the present invention, by following examples, the present invention is further elaborated.
The reaction mechanism following (preparation technology's schema is asked for an interview Fig. 1) of PC/PA11 composition of the present invention:
Reaction mechanism
From upper reaction formula, the terminal hydroxy group of polycarbonate can be respectively and the isocyanate groups of tolylene diisocyanate, 2, 2'-(1, 3-phenylene) the oxazoline group of-bisoxazoline reacts, the end amino of polymeric amide 11, end carboxyl can be respectively and the isocyanate groups of tolylene diisocyanate, 2, 2'-(1, 3-phenylene) the oxazoline group of-bisoxazoline reacts, form compatilizer PC-co-TDI-co-PA11, compatilizer PC-co-PBO-co-PA11, thereby improve the consistency of PC/PA11 system, obtain having mechanical property good, flame retardant resistance is high, the PC/PA11 composition of chemical resistant properties and good processability.
The raw material that the embodiment of the present invention is used is as follows:
Polycarbonate, is dihydroxyphenyl propane aromatic copolycarbonate, is selected from Dow Chemical company, and number-average molecular weight is 15000.
Polycarbonate, is dihydroxyphenyl propane aromatic copolycarbonate, is selected from Japanese Supreme Being people and changes into company, and number-average molecular weight is 23000.
Polycarbonate, is dihydroxyphenyl propane aromatic copolycarbonate, is selected from Korea S three and supports company, and number-average molecular weight is 30000.
Polycarbonate, is dihydroxyphenyl propane aromatic copolycarbonate, is selected from Korea S three and supports company, and number-average molecular weight is 50000.
Polymeric amide 11, is selected from Lian Zenong Chemical Co., Ltd. in Taiyuan, and number-average molecular weight is 20000.
Polymeric amide 11, is selected from Lian Zenong Chemical Co., Ltd. in Taiyuan, and number-average molecular weight is 24000.
Polymeric amide 11, is selected from Lian Zenong Chemical Co., Ltd. in Taiyuan, and number-average molecular weight is 30000.
Tolylene diisocyanate, is selected from Shanghai Sheng Yu Chemical Co., Ltd..
2,2'-(1,3-phenylene)-bisoxazoline, is selected from colon, Nanjing medication chemistry company limited.
Styrene-maleic anhydride copolymer A, is selected from Sheyang Ketong Plastic Co., Ltd., maleic anhydride content 15%～18%.
Styrene-maleic anhydride copolymer B, is selected from Rizhisheng New Technology Development Co., Ltd., Shanghai, maleic anhydride content 18%～20%.
Anti-dripping agent (tetrafluoroethylene), is selected from Minnesota ,USA mines and production company (3M), trade mark TF-1645.
β-(4-hydroxy phenyl-3,5-di-t-butyl) positive octadecanol ester of propionic acid (antioxidant 1076), as primary antioxidant, is selected from Switzerland's vapour Bagong department.
Tricresyl phosphite (2,4-di-tert-butyl-phenyl) ester (irgasfos 168), as auxiliary antioxidant, is selected from Switzerland's vapour Bagong department.
Pentaerythritol stearate, is selected from Clariant company of the U.S..
Comparative example 1:
A kind of In situ Reactive Compatibility of this comparative example is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 200rpm.
The screw rod of described parallel double-screw extruder is shaped as double thread, and the ratio L/D of spiro rod length L and diameter D is 20, and described screw rod is provided with 1 gear block district, without left-hand thread district.
Comparative example 2:
A kind of In situ Reactive Compatibility of this comparative example is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant are joined in another homogenizer and mixed, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 200rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 50, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Comparative example 3:
A kind of In situ Reactive Compatibility of this comparative example is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 200rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 50, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 1:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 230 DEG C, two district's temperature: 240 DEG C, three district's temperature are 240 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 240 DEG C, die head temperature: 240 DEG C, driving screw rotating speed is: 400rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 60, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 2:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer A (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 220 DEG C, two district's temperature: 230 DEG C, three district's temperature are 230 DEG C, four district's temperature: 230 DEG C, five district's temperature are 230 DEG C, six district's temperature: 230 DEG C, die head temperature: 230 DEG C, driving screw rotating speed is: 100rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 35, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 3:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 240 DEG C, three district's temperature are 240 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 230 DEG C, driving screw rotating speed is: 150rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 40, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 4:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 200rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 50, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 5:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer A (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 230 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 250rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 45, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Embodiment 6:
A kind of In situ Reactive Compatibility of the present embodiment is prepared PC/PA11 composition, is prepared from by following raw material:
The preparation method of above-mentioned PC/PA11 composition, comprises the following steps:
(1) described polycarbonate (PC) and polymeric amide 11 (PA11) are placed in to 110 DEG C, dry 4 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate (TDI), 2,2'-(1,3-phenylene)-bisoxazoline (PBO), styrene-maleic anhydride copolymer B (SMA), anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 225 DEG C, two district's temperature: 235 DEG C, three district's temperature are 235 DEG C, four district's temperature: 240 DEG C, five district's temperature are 240 DEG C, six district's temperature: 235 DEG C, die head temperature: 235 DEG C, driving screw rotating speed is: 250rpm.
The screw rod of described parallel double-screw extruder is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 55, and described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
Be below comparative example and embodiment table look-up:
Table 1 comparative example and embodiment raw material composition weight part table look-up
Anti-dripping agent, primary antioxidant, auxiliary antioxidant and the lubricant of above comparative example and embodiment is respectively 0.3 part, 0.1 part, 0.1 part, 0.1 part.
Above-mentioned comparative example and the made sample of embodiment are carried out to following performance test:
Tensile property: press GB/T1042-1992 standard testing, rate of extension 50mm/min.
Impact property: press GB/T1843-1996 standard testing, batten thickness is 3.2mm.
Flame retardant resistance: the XZT-100A oxygen index measurer test oxygen index that the batten of 130mm × 6.5mm × 3.0mm is produced with Chengde great Hua trier company limited.
Chemical resistant properties: tensile bars is put into after Glacial acetic acid 3min, tested its elongation at break.The elongation at break of Glacial acetic acid tensile bars after treatment is not with larger by the ratio of the elongation at break of the tensile bars of Glacial acetic acid processing, and its chemical resistant properties is better.
Melting index: press ASTM D1238 test, 250 DEG C of probe temperatures, load 5kg.
Table 2 comparative example and embodiment performance table look-up
Comparative example 1 is for screw rod is shaped as double thread, and the ratio L/D of spiro rod length L and diameter D is 20, and screw rod is provided with 1 gear block district, the PC/PA11 composition preparing without the twin screw extruder in left-hand thread district; Embodiment 4 is for screw rod is shaped as single thread, and the ratio L/D of spiro rod length L and diameter D is 50, and screw rod is provided with the PC/PA11 composition that the twin screw extruder in 2 gear block districts and 2 left-hand thread districts prepares.Can find out by contrast, adopt screw rod of the present invention to be shaped as single thread, the ratio L/D of spiro rod length L and diameter D is 50, when screw rod is provided with 2 gear block districts and 2 left-hand thread districts, tensile strength, notched Izod impact strength, oxygen index, chemical resistant properties and the melting index of PC/PA11 composition are greatly improved, and obtain that mechanical property is good, flame retardant resistance is high, the beneficial effect of the PC/PA11 composition of chemical resistant properties and good processability.
Comparative example 2 is not for adding the PC/PA11 composition containing the monomer of double reactive functional group; Embodiment 4 is for adding tolylene diisocyanate (TDI), 2, the PC/PA11 composition of 2'-(1,3-phenylene)-bisoxazoline (PBO).Can find out by contrast, add containing tensile strength, notched Izod impact strength, oxygen index, chemical resistant properties and the melting index of the PC/PA11 composition of the monomer of double reactive functional group and be better than and do not add containing the PC/PA11 composition of the monomer of double reactive functional group.
The PC/PA11 composition that the number-average molecular weight that comparative example 3 is polycarbonate is 50000; The PC/PA11 composition that the number-average molecular weight that embodiment 4 is polycarbonate is 23000.Can find out by contrast, the number-average molecular weight of polycarbonate is that tensile strength, notched Izod impact strength and the chemical resistant properties outline of 50000 PC/PA11 composition is better than PC/PA11 composition that the number-average molecular weight of polycarbonate is 23000, and the melting index of the PC/PA11 composition that the number-average molecular weight of polycarbonate is 50000 only has 7g/10min, its processing characteristics is poor.
Embodiment 1～6 is for adjusting the weight part of PC and PA11, and as can be seen from Table 2, along with the addition of PA11 increases, the tensile strength of PC/PA11 composition and notched Izod impact strength present the variation tendency of minimizing; The chemical resistant properties of PC/PA11 composition and melting index present the variation tendency of increase.Wherein, over-all properties the best of embodiment 4.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a PC/PA11 composition, is characterized in that, is prepared from by the raw material of following weight part:
Described anti-dripping agent is fluoropolymer;
Described Hinered phenols antioxidant is the positive octadecanol ester of β-(4-hydroxy phenyl-3,5-di-t-butyl) propionic acid;
Described phosphite ester kind antioxidant is tricresyl phosphite (2,4-di-tert-butyl-phenyl) ester.
2. PC/PA11 composition according to claim 1, is characterized in that, is prepared from by the raw material of following weight part:
3. PC/PA11 composition according to claim 2, is characterized in that, is prepared from by the raw material of following weight part:
4. according to the PC/PA11 composition described in claim 1～3 any one, it is characterized in that, described polycarbonate is dihydroxyphenyl propane aromatic copolycarbonate, and number-average molecular weight is 15000～30000; The number-average molecular weight of described polymeric amide 11 is 20000～30000; In described styrene-maleic anhydride copolymer, the content of maleic anhydride is 15%～20%.
5. PC/PA11 composition according to claim 4, is characterized in that, the number-average molecular weight of described polycarbonate is for being 18000～27000; The number-average molecular weight of described polymeric amide 11 is 22000～26000.
6. PC/PA11 composition according to claim 4, is characterized in that, described lubricant is pentaerythritol stearate; Described anti-dripping agent is tetrafluoroethylene.
7. a preparation method for the PC/PA11 composition described in claim 1～6 any one, is characterized in that, comprises the following steps:
(1) described polycarbonate and polymeric amide 11 are placed in to 100～120 DEG C, dry 4～12 hours, cooling after, polycarbonate and polymeric amide 11 are joined and in homogenizer, carry out pre-mixing;
(2) by tolylene diisocyanate, 2,2'-(1,3-phenylene)-bisoxazoline, styrene-maleic anhydride copolymer, anti-dripping agent, Hinered phenols antioxidant, phosphite ester kind antioxidant and lubricant join in another homogenizer and mix, then the mixture obtaining is joined in the homogenizer in step (1) and mixed;
(3) premixture step (2) being mixed is placed in parallel double-screw extruder and melt extrudes, granulation, processing parameter is as follows: district's temperature is 220～240 DEG C, two district's temperature: 230～250 DEG C, three district's temperature are 230～250 DEG C, four district's temperature: 230～250 DEG C, five district's temperature are 230～250 DEG C, six district's temperature: 230～250 DEG C, die head temperature: 230～250 DEG C, driving screw rotating speed is: 100～400rpm.
8. preparation method according to claim 7, is characterized in that, in described step (1), polycarbonate and polymeric amide 11 are placed in 110 DEG C, dry 4～6 hours; Processing parameter in described step (3) is: district's temperature is 220～230 DEG C, two district's temperature: 230～240 DEG C, three district's temperature are 230～240 DEG C, four district's temperature: 230～240 DEG C, five district's temperature are 230～240 DEG C, six district's temperature: 230～240 DEG C, die head temperature: 230～240 DEG C, driving screw rotating speed is: 150～250rpm.
9. preparation method according to claim 7, is characterized in that, the screw rod of described parallel double-screw extruder is shaped as single thread; The ratio L/D of spiro rod length L and diameter D is 35～60; Described screw rod is provided with 1 above gear block district and 1 above left-hand thread district.
10. preparation method according to claim 9, is characterized in that, the ratio L/D of described spiro rod length L and diameter D is 40～55; Described screw rod is provided with 2 gear block districts and 2 left-hand thread districts.
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