CN106398163A - Low temperature resistant and high impact resistant polycarbonate and preparation method thereof - Google Patents
Low temperature resistant and high impact resistant polycarbonate and preparation method thereof Download PDFInfo
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- CN106398163A CN106398163A CN201610870667.6A CN201610870667A CN106398163A CN 106398163 A CN106398163 A CN 106398163A CN 201610870667 A CN201610870667 A CN 201610870667A CN 106398163 A CN106398163 A CN 106398163A
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2369/00—Characterised by the use of polycarbonates; 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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/53—Core-shell polymer
Abstract
The invention provides a low temperature resistant and high impact resistantpoly carbonate and a preparation method thereof. The preparation method comprises the following steps of selecting and using composite synergistic of tremolite powder, azodiisobutyronitrile, an antioxygen, a core-shell nanoparticle emulsion, a bulking agent and other aid agents for improving the product performance; stirring for 4 to 5 minutes in a high-speed mixer at the temperature of 65 DEG C to 95 DEG C, feeding uniformly mixed mixture into a high polymer material stirring machine for stirring, wherein the stirring speed is 250r/min, and the stirring time is 70min; when the stirred material reaches 30 to 35 DEG C, discharging. The product effectively solves the problems of low anti-shock capability and wear-resisting property, easiness in stress cracking, notch sensitivity and the like of existing polycarbonate under the low temperature condition; a test proves that the low temperature resistant and high impact resistant polycarbonate has the tensile strength being 75Mpa at the temperature of -70 DEG C, the bending strength being 131MPa at the temperature of -70 DEG C, the notch impact strength being 460J/M at the temperature of -70 DEG C, and the notch impact strength being 707J/M at the temperature of 23 DEG C, and is applicable to various meter cases or accessories such as light shells and auto spare parts working under a cold environment.
Description
Technical field
The present invention relates to macromolecule engineering plastic applications, more particularly, to a kind of low temperature resistant high impact poly carbonic ester and its preparation
Method.
Background technology
Merlon（PC）It is a kind of superior engineering plastics of combination property, be also the fastest general of growth rate in recent years
Engineering plastics, have excellent impact flexibility, dimensional stability, electric insulating quality, creep resistant, weatherability, the transparency and nothing
The advantages of toxicity, it is now widely used for automobile, electric, building, office equipment, packaging, sports equipment, health care etc.
Field, deepening continuously with study on the modification, just it is being extended to rapidly the high-tech areas such as Aero-Space, computer, CD but it
There is also some shortcomings, as poor in processing fluidity, be easy to stress cracking, and wearability more sensitive to breach be not good enough etc..
Simultaneously as the amorphism of Merlon, intermolecular pile up not fine and close, in low temperature even ultralow temperature ring
Under border, the mechanical property of Merlon changes, and impact resistance reduces, remitted its fury.Although being currently fed impact modification
- 30 DEG C～-40 DEG C of the cryogenic property of the low temperature resistant flame retardant Merlon of agent and fire retardant, even lower, and can reach higher
Fire-retardant rank, but the high transparent of makrolon material itself will be by large effect.
Formerly disclose a kind of Merlon and methyl methacrylate/methacrylic acid in patent CN101454210B
The mixture of naphthalene ester, this mixture maintains splendid optical property, but does not refer to resistance to low temperature and the resistance of this mixture
Combustion performance.
Formerly patent JP2010185031A discloses a kind of Merlon/ABS containing polyurethane-type resin of hydrolysis
Alloy resin composition, wherein polyurethane-type resin are polyamide resin and/or polyacrylate resin.But, this gathers
Ammonia ester type resin is not TPUE, and shock resistance and heat resistance are still inadequate.
Therefore, how to obtain and a kind of take into account good low temperature resistant, and preferable shock resistance, production cost and phase simultaneously
To rational method, still it is worth people to be continually striving to explore.
Content of the invention
In order to overcome the problems referred to above, the invention provides a kind of polycarbonate composite material with low temperature resistant high-impact and
Its preparation method.
For achieving the above object, the technical scheme of present invention offer is：
A kind of low temperature resistant high impact poly carbonic ester, its composition of raw materials is made up of each component of following parts by weight：
Merlon 65-80 part；
Amphibole powder 10-20 part；
Azodiisobutyronitrile 1-2.5 part；
Antioxidant 0.2-1.2 part；
Core-shell nano emulsion 5.5-8 part；
Bulking agent 4-6 part；
Light diffusing agent 5-9 part；
Lubricant 0.5-1.5 part；
Fire retardant 0.5-1.8 part.
Described amphibole powder is natural inorganic mineral powder to coexist through superfine powder by formed after dolomite and quartzy mixed deposit
Broken for particle diameter 2000 mesh -6000 mesh powder.
A kind of preparation method of low temperature resistant high impact poly carbonic ester it is characterised in that：It comprises the following steps：
1）Amphibole powder is dried at a temperature of 65 °C -95 °C 1-2 hour, stand-by；
2）Weighing dry amphibole powder by weight ratio adds barrel temperature in 65 DEG C -95 DEG C of high-speed mixer, stirs 4-
5 minutes, then weigh 2.5 parts of azodiisobutyronitrile by weight ratio and 7 parts of core-shell nano emulsion stirs 10～15 points
Clock, then adds 78 parts of Merlon by weight ratio, weighs bulking agent, light diffusing agent, antioxidant, profit simultaneously by weight ratio
Lubrication prescription and fire retardant 5-10 minute, are sufficiently mixed uniformly；
3）By step 2）In mix after compound, be sent into macromolecular material mixer in be stirred, mixing speed is
250r/min, mixing time is 70min, when stirring material reaches 30-35 °C, discharging；
4）By step 3）Stirring material after middle stirring puts in twin screw extruder, and barrel heat temperature is 120-160 °C, mouth
Mould temperature is 120-150 °C, and screw speed is 12-55rpm, charging rotating speed is for, under conditions of 10-40rpm, extruding；
5）By step 4）Middle extruded stock is introduced in pelleter and carries out pelletizing operation, collects pellet and is low temperature resistant high impact poly carbonic acid
Ester.
Technique scheme is beneficial in that：
1 the invention provides a kind of low temperature resistant high impact poly carbonic ester and preparation method thereof, selected amphibole powder,
Azodiisobutyronitrile, antioxidant, core-shell nano emulsion, bulking agent and other auxiliary agents combine the property that synergistic strengthens product
Can, and the ratio of each material component is optimized, efficiently solve existing Merlon erosion-resisting characteristics under cryogenic
And anti-wear performance low, be easy to stress cracking and the shortcomings of to notch sensitive, the product being produced by the preparation method of the present invention its
Tensile strength under conditions of -70 °C up to 75Mpa, bending strength under conditions of -70 °C can 131Mpa greatly, notch shock is strong
Up to 460J/M under conditions of -70 °C, notch impact strength up to 707 J/M, is proven under conditions of 23 °C degree,
This product good combination property it is adaptable to work in psychro-environment lamp housing, all kinds of meter cases or the accessory such as auto parts machinery.
2nd, the preparation method process is simple of the present invention, convenient operation and control, steady quality, production efficiency is high, can be extensive
Industrialized production.
Technical scheme is clearly and completely described it is clear that being retouched below in conjunction with specific embodiment
The embodiment stated is a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this area
The every other embodiment that those of ordinary skill is obtained under the premise of not making creative work, broadly falls into present invention protection
Scope.
Specific embodiment
Embodiment 1
A kind of low temperature resistant high impact poly carbonic ester, its composition of raw materials is made up of each component of following parts by weight：
78 parts of Merlon；
16 parts of amphibole powder；
2.5 parts of azodiisobutyronitrile；
0.8 part of antioxidant；
7 parts of core-shell nano emulsion；
4.5 parts of bulking agent；
9 parts of light diffusing agent；
0.5 part of lubricant；
1 part of fire retardant.
Described amphibole powder is natural inorganic mineral powder to coexist through superfine powder by formed after dolomite and quartzy mixed deposit
Broken for particle diameter 6000 mesh powder.
A kind of preparation method of low temperature resistant high impact poly carbonic ester it is characterised in that：It comprises the following steps：
1) described amphibole powder is dried 1.7 hours at a temperature of 78 °C, stand-by.
2) the amphibole powder being dried is added barrel temperature in 75 DEG C of high-speed mixer, stir 4.7 minutes, then press
Weight proportion weighs 2.5 parts of azodiisobutyronitrile and 7 parts of core-shell nano emulsion stirs 12 minutes, then adds by weight ratio
Enter 78 parts of Merlon, weigh bulking agent, light diffusing agent, antioxidant, lubricant and fire retardant 7 minutes simultaneously by weight ratio,
It is sufficiently mixed uniformly.
3) compound after mixing, is sent in macromolecular material mixer and is stirred, and mixing speed is 250r/
Min, mixing time is 70min, when stirring material reaches 33 °C, discharging.
4) the stirring material after stirring is put in twin screw extruder, barrel heat temperature is 130 °C, die temperature
For 128 °C, screw speed is 42rpm, charging rotating speed is for, under conditions of 33rpm, extruding.
5) extruded stock is introduced in pelleter and carries out pelletizing operation, collects pellet and is low temperature resistant high impact poly carbonic ester.
Performance test
Tested using the low temperature resistant high impact poly carbonic ester that ASTM international standard is obtained to the present embodiment, its result such as following table
Shown in 1：
As seen from the above table, the low temperature resistant high impact poly carbonic ester that the present embodiment is provided, also shows under conditions of -70 °C of low temperature
Go out excellent impact strength, in addition its tensile strength at low temperature and bending strength also ratio like product superior performance.
Embodiment 2
A kind of low temperature resistant high impact poly carbonic ester as described in Example 1, its composition of raw materials can also be by following parts by weight
Each component composition：
74 parts of Merlon；
10 parts of amphibole powder；
1.5 parts of azodiisobutyronitrile；
1.2 parts of antioxidant；
8 parts of core-shell nano emulsion；
6 parts of bulking agent；
7 parts of light diffusing agent；
1 part of lubricant；
1.8 parts of fire retardant.
Described amphibole powder is natural inorganic mineral powder to coexist through superfine powder by formed after dolomite and quartzy mixed deposit
Broken for particle diameter 2000 mesh powder.
A kind of preparation method of low temperature resistant high impact poly carbonic ester it is characterised in that：It comprises the following steps：
1）Described amphibole powder is dried 1 hour at a temperature of 65 °C, stand-by.
2）The amphibole powder being dried is added barrel temperature in 65 DEG C of high-speed mixer, stirring 4 minutes, then by weight
Proportioning weighs 2.5 parts of azodiisobutyronitrile and 7 parts of core-shell nano emulsion stirs 10 minutes, then adds poly- by weight ratio
78 parts of carbonic ester, weighs bulking agent, light diffusing agent, antioxidant, lubricant and fire retardant 5 minutes, fully simultaneously by weight ratio
Mix.
3）Compound after mixing, is sent in macromolecular material mixer and is stirred, and mixing speed is 250r/
Min, mixing time is 70min, when stirring material reaches 30 °C, discharging.
4）Stirring material after stirring is put in twin screw extruder, barrel heat temperature is 120 °C, die temperature is
120 °C, screw speed is 25rpm, charging rotating speed is for, under conditions of 10rpm, extruding.
Performance test
Tested using the low temperature resistant high impact poly carbonic ester that ASTM international standard is obtained to the present embodiment, its result such as following table
Shown in 2：
As seen from the above table, the low temperature resistant high impact poly carbonic ester that the present embodiment is provided, also shows under conditions of -70 °C of low temperature
Go out excellent impact strength, in addition its tensile strength at low temperature and bending strength also ratio like product superior performance.
Embodiment 3
A kind of low temperature resistant high impact poly carbonic ester as described in Example 1, its composition of raw materials can also be by following parts by weight
Each component composition：
80 parts of Merlon；
20 parts of amphibole powder；
1 part of azodiisobutyronitrile；
0.7 part of antioxidant；
5.5 parts of core-shell nano emulsion；
4 parts of bulking agent；
5 parts of light diffusing agent；
1.5 parts of lubricant；
0.5 part of fire retardant.
Described amphibole powder is natural inorganic mineral powder to coexist through superfine powder by formed after dolomite and quartzy mixed deposit
Broken for particle diameter 4000 mesh powder.
A kind of preparation method of low temperature resistant high impact poly carbonic ester it is characterised in that：It comprises the following steps：
1）Described amphibole powder is dried 2 hours at a temperature of 95 °C, stand-by.
2）The amphibole powder being dried is added barrel temperature in 95 DEG C of high-speed mixer, stirring 5 minutes, then by weight
Proportioning weighs 2.5 parts of azodiisobutyronitrile and 7 parts of core-shell nano emulsion stirs 15 minutes, then adds poly- by weight ratio
78 parts of carbonic ester, weighs bulking agent, light diffusing agent, antioxidant, lubricant and fire retardant 10 minutes, fully simultaneously by weight ratio
Mix.
3）Compound after mixing, is sent in macromolecular material mixer and is stirred, and mixing speed is 250r/
Min, mixing time is 70min, when stirring material reaches 35 °C, discharging.
4）Stirring material after stirring is put in twin screw extruder, barrel heat temperature is 160 °C, die temperature is
150 °C, screw speed is 55rpm, charging rotating speed is for, under conditions of 40rpm, extruding.
Performance test
Tested using the low temperature resistant high impact poly carbonic ester that ASTM international standard is obtained to the present embodiment, its result such as following table
Shown in 3：
As seen from the above table, the low temperature resistant high impact poly carbonic ester that the present embodiment is provided, also shows under conditions of -70 °C of low temperature
Go out excellent impact strength, in addition its tensile strength at low temperature and bending strength also ratio like product superior performance.
By various embodiments above, low temperature resistant high impact poly carbonic ester finally all can be obtained；It should be noted that this area
Technical staff should be noted that in preparation method in the present invention when implementing, step 2）、3）、4）The macromolecule material being adopted
Material mixer can directly adopt existing fusion apparatus, mixing plant；The high anti-Merlon of low temperature of this department offer is be provided
Produce use fusion apparatus, mixing plant, through the applicant it was verified that through this department offer engineering plastics fusion apparatus and height
The material that molecular material mixer is processed can make material have the higher uniformity, can be for high-quality low temperature resistant height is obtained
Anti-impact Merlon provides one preferably to ensure.
Test two：Low temperature resistant, impact and fire resistance for finished product make mensure.
Test sample：The product being obtained through technical scheme described in above-mentioned 3 embodiments of the present invention and on the market common
Product.
Result of the test is as shown in table 1：
Table 1
Conclusion (of pressure testing)：
Addition amphibole powder, azodiisobutyronitrile warp and core-shell nano emulsion be can be seen that by the test performance result of table 1
Greatly improved low-temperature impact-resistant performance Deng fire retardant, and there is excellent anti-flammability, in addition the injection pressure of the present invention and
Injection temperature is decreased obviously, and has and is easy to mold filling.Wherein with poly- obtained by the raw material proportioning described in embodiment 1 and preparation method
Carbonic ester performance highest, compare like product, and lifting is substantially.
Claims (8)
1. a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Its composition of raw materials is by each component of following parts by weight
Composition：
Merlon 65-80 part；
Amphibole powder 10-20 part；
Azodiisobutyronitrile 1-2.5 part；
Antioxidant 0.2-1.2 part；
Core-shell nano emulsion 5.5-8 part；
Bulking agent 4-6 part；
Light diffusing agent 5-9 part；
Lubricant 0.5-1.5 part；
Fire retardant 0.5-1.8 part.
2. as claimed in claim 1 a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Its composition of raw materials is by following
The each component composition of parts by weight：
78 parts of Merlon；
16 parts of amphibole powder；
2.5 parts of azodiisobutyronitrile；
0.8 part of antioxidant；
7 parts of core-shell nano emulsion；
4.5 parts of bulking agent；
9 parts of light diffusing agent；
0.5 part of lubricant；
1 part of fire retardant.
3. a kind of low temperature resistant high impact poly carbonic ester as described in claim 1-2 it is characterised in that：Described amphibole powder is by white
Formed after marble and quartzy mixed deposit natural coexist inorganic mineral powder through ultra-fine grinding for particle diameter in 2000 mesh -6000 purpose
Powder.
4. a kind of low temperature resistant high impact poly carbonic ester as described in claim 1-2 preparation method it is characterised in that：It includes
Following steps：
1）Amphibole powder is dried at a temperature of 65 °C -95 °C 1-2 hour, stand-by；
2）Weighing dry amphibole powder by weight ratio adds barrel temperature in 65 DEG C -95 DEG C of high-speed mixer, stirs 4-
5 minutes, then weigh 2.5 parts of azodiisobutyronitrile by weight ratio and 7 parts of core-shell nano emulsion stirs 10～15 points
Clock, then adds 78 parts of Merlon by weight ratio, weighs bulking agent, light diffusing agent, antioxidant, profit simultaneously by weight ratio
Lubrication prescription and fire retardant 5-10 minute, are sufficiently mixed uniformly；
3）By step 2）In mix after compound, be sent into macromolecular material mixer in be stirred, mixing speed is
250r/min, mixing time is 70min, when stirring material reaches 30-35 °C, discharging；
4）By step 3）Stirring material after middle stirring puts in twin screw extruder, and barrel heat temperature is 120-160 °C, mouth
Mould temperature is 120-150 °C, and screw speed is 12-55rpm, charging rotating speed is for, under conditions of 10-40rpm, extruding；
5）By step 4）Middle extruded stock is introduced in pelleter and carries out pelletizing operation, collects pellet and is low temperature resistant high impact poly carbonic acid
Ester.
5. as claimed in claim 4 a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Step 1）In, described amphibole
Powder is dried 1.7 hours at a temperature of 78 °C, stand-by.
6. as claimed in claim 4 a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Step 2）In, described drying
Amphibole powder add barrel temperature in 75 DEG C of high-speed mixer, stir 4.7 minutes, then weigh azo two by weight ratio
2.5 parts of isobutyronitrile and 7 parts of core-shell nano emulsion stir 12 minutes, then add 78 parts of Merlon by weight ratio, with
When weigh bulking agent, light diffusing agent, antioxidant, lubricant and fire retardant 7 minutes by weight ratio, be sufficiently mixed uniformly.
7. as claimed in claim 4 a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Step 3）In, mix
Compound afterwards, is sent in macromolecular material mixer and is stirred, and mixing speed is 250r/min, and mixing time is 70min,
When stirring material reaches 33 °C, discharging.
8. as claimed in claim 4 a kind of low temperature resistant high impact poly carbonic ester it is characterised in that：Step 4）In, after stirring
Stirring material puts in twin screw extruder, and barrel heat temperature is 130 °C, and die temperature is 128 °C, and screw speed is
Under conditions of 42rpm, charging rotating speed are 33rpm, extrusion.
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