CN102532875A - 6000-mesh inorganic powder-filled modified PA (Polyamide)6 master batch and preparation method thereof - Google Patents
6000-mesh inorganic powder-filled modified PA (Polyamide)6 master batch and preparation method thereof Download PDFInfo
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- CN102532875A CN102532875A CN2010106219014A CN201010621901A CN102532875A CN 102532875 A CN102532875 A CN 102532875A CN 2010106219014 A CN2010106219014 A CN 2010106219014A CN 201010621901 A CN201010621901 A CN 201010621901A CN 102532875 A CN102532875 A CN 102532875A
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Abstract
The invention discloses a 6000-mesh inorganic powder-filled modified PA (Polyamide)6 master batch and a preparation method thereof and belongs to the technical field of high-molecular materials. The PA6 master batch comprises the following main raw materials: PA6, a surface treating agent, polyethylene wax, paraffin wax and 6000-mesh inorganic powder, and the preparation method of the PA6 master batch comprises the following steps of: putting the 6000-mesh inorganic powder into a high-speed mixer for agitation and dehumidification, adding the surface treating agent for mixing and agitation and putting in a cold mixer for cooling, putting the PA6, the polyethylene wax and the paraffin wax into the high-speed mixer in sequence for mixing and agitation, adding the modified 6000-mesh inorganic powder for mixing and agitation, putting in the cold mixer for cooling and discharging and pelleting with an extruder to prepare the 6000-mesh inorganic powder-filled modified PA6 master batch. The 6000-mesh inorganic powder-filled modified PA6 master batch and the preparation method thereof have the beneficial effects that after the 6000-mesh inorganic powder-filled modified PA6 master batch is mixed with matrix resin, a whole system has good compatibility, dispersibility, flowability and processing performance, and a produced product has good mechanical property, dimension stability, toughness and impact resistance and the 6000-mesh inorganic powder-filled modified PA6 master batch is particularly suitable for manufacturing PA6 water supply pipes, PA6 double-walled corrugated tubes, plastic turnover boxes and automotive interior products.
Description
Technical field
The present invention relates to technical field of polymer materials, especially a kind of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof.
Background technology
The widespread use with plastics that develops rapidly along with plastics industry; The filling-modified technology of plastics obtains people's attention day by day, in resin, adds various mineral fillers mixing moulding then, not only can reduce the cost of goods greatly; But also can significantly improve some performances of plastics; Like mechanical energy, thermal property, wear resistance and ageing-resistant performance, thereby give material new characteristic, to satisfy the needs of different purposes.
PA6 (nylon 6) filling master batch comprises vector resin, filler and auxiliary agent three parts.Vector resin is PA6, and filler is often selected lime carbonate, the mineral filler of kaolin isopolarity for use, and consistency between the two is poor, and the interface is difficult to form good bonding.Combine with the interface of mineral filler in order to improve resin, make between resin and the mineral filler to form the good interface clinging power, mechanicalness, the dimensional stability of whole system all can not reach the ideal requirement to cause the master batch of manufacturing to mix afterwards with matrix resin.
Summary of the invention
The objective of the invention is to overcome the deficiency of prior art, a kind of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof are provided.This 6000 mesh inorganic powder filling-modified PA6 master batch with can make whole system have good consistency, dispersiveness, flowability and processing characteristics after matrix resin mixes; And can make the product of producing have mechanicalness, dimensional stability preferably; Toughness and shock resistance, but also can reduce the products production cost.
The present invention solves its technical problem and realizes through following technical scheme: a kind of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof, and the weight part of its each component is:
10～30 parts of PA6;
60～85 parts of 6000 order inorganic material powders;
0.5～3 part of surface treatment agent;
0.5～5 part of polyethylene wax;
0.5～1.5 part in paraffin.
Described inorganic material powder is 6000 purpose water-ground limestones or light calcium carbonate or kaolin or talcum powder or silicon-dioxide or Marinco H or white lake or wollastonite, and above-mentioned substance make a gesture of measuring mixture, its particle diameter of 90%≤2 μ m arbitrarily.
Described surface treatment agent is silane or titanic acid ester or aluminate coupling agent or Triple Pressed Stearic Acid, and the arbitrary combination mixture of above-mentioned substance.
Its preparation method may further comprise the steps:
1) 6000 order inorganic material powders are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 80 ℃ to 90 ℃, after temperature reaches 110 ℃ to 160 ℃, adds surface treatment agent and mixes stirring 5 to 10 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order inorganic material powders that discharging after 30 ℃ to 50 ℃ obtains modification;
3) PA6, polyethylene wax, paraffin are put into high-speed mixer and mixing successively and stirred 1 to 5 minute, add 6000 order inorganic material powders after the modification then and continue to mix and stirred 1 to 5 minute;
4) compound in the high mixer is put in the cold mixer cooled off, discharging after cooling temperature is reduced to 30 ℃ to 50 ℃, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof;
5) with the special-purpose powder of PA6 extruding pelletization on twin screw extruder, one district's temperature is 200～220 ℃ from the spout to the die head, 220～240 ℃ of two district's temperature; 230～250 ℃ of three district's temperature, 230～250 ℃ of four district's temperature, 230～250 ℃ of five district's temperature; 220～240 ℃ of six district's temperature, 235～255 ℃ of seven district's temperature, residence time is 0.5～2min; Engine speed is 200r/min, and pressure is 10～15Mpa, discharging, extrudes postcooling, drying; Pelletizing, 6000 mesh inorganic powder filling-modified PA6 master batches.
Beneficial effect of the present invention is:
1. the present invention is with the 6000 order inorganic material powders of surface treatment agent and its particle diameter of the 90%≤2 μ m component as 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof; Adopt the operation of dehumidifying and modification; The inorganic material powder that makes interpolation by inorganic nature to organic sex reversal; By the surface hydrophilic oleophobic property; Change into lipophilic-hydrophobic property, and the problem of particle aggregation and bad dispersibility when successfully having solved 6000 order inorganic material powders and adding, can make whole system have good consistency, dispersiveness, flowability and processing characteristics after making 6000 mesh inorganic powder filling-modified PA6 master batches and matrix resin mixing.
The present invention's 6000 order inorganic material powders of having added its particle diameter of 90%≤2 μ m make its with can make the product of producing have mechanicalness, dimensional stability, toughness and shock resistance preferably after matrix resin mixes.
3. the present invention is under the prerequisite that guarantees the plastics performance; The addition of 6000 order inorganic material powders can reach 85%; Reducing production costs greatly, practiced thrift raw material, is the best filler parent granule of making PA6 water-feeding pipes, plastic box and automotive trim goods.
Embodiment
Further specify the present invention below in conjunction with embodiment, the scheme of embodiment described here does not limit protection scope of the present invention.
Embodiment 1
Raw material:
PA6 (nylon 6) 15kg
Triple Pressed Stearic Acid (HSt) 0.8kg
Polyethylene wax 3kg
Paraffin (WAX) 0.6kg
6000 order water-ground limestone 70kg.
Its preparation method is:
1) 70kg 6000 order water-ground limestones are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 80 ℃, after temperature reaches 110 ℃, adds Triple Pressed Stearic Acid and mixes stirring 5 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order water-ground limestones that 30 ℃ of dischargings obtain modification;
3) PA6, polyethylene wax, paraffin are put into high-speed mixer and mixing successively and stirred 1 minute, add 6000 order water-ground limestones after the modification then and continue to mix and stirred 1 minute;
4) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to 30 ℃ of dischargings, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches;
6000 order inorganic material powders in this prescription adopt water-ground limestone, also can adopt light calcium carbonate, kaolin, talcum powder, silicon-dioxide, Marinco H, white lake, wollastonite or their mixture.
5) ME of its 6000 mesh inorganic powder filling-modified PA6 master batches is:
Go up extruding pelletization by following processing condition at twin screw extruder (unit is extruded in the compounding of KY50/100 parallel dual-screw), its extruding and pelletizing process (temperature ℃) parameter is following:
Residence time is 0.5～2min, and engine speed is 200r/min, and pressure is 10～15Mpa, discharging, extrudes postcooling, drying, pelletizing, 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof finished product.
Embodiment 2
Raw material:
PA6 (nylon 6) 15kg
Triple Pressed Stearic Acid/titanic acid ester 0.8kg
Polyethylene wax 5kg
Paraffin (WAX) 0.8kg
6000 order water-ground limestone 80kg.
Its step of manufacturing is:
1) 80kg 6000 order water-ground limestones are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 85 ℃, after temperature reaches 120 ℃, adds Triple Pressed Stearic Acid/titanic acid ester and mixes stirring 5 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order water-ground limestones that 50 ℃ of dischargings obtain modification;
3) with PA6, polyethylene wax, paraffin is put into high-speed mixer and mixing successively and was stirred 2 minutes, adds 6000 order water-ground limestones after the modification then and continues to mix and stirred 3 minutes;
4) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to 50 ℃ of dischargings, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches;
5) identical with embodiment 1, promptly process 6000 mesh inorganic powder filling-modified PA6 master batch finished products.
Embodiment 3:
Raw material:
PA6 (nylon 6) 15kg
Triple Pressed Stearic Acid/aluminic acid ester 0.8kg
Polyethylene wax 3kg
Paraffin (WAX) 0.6kg
6000 order water-ground limestone 70kg.
6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof step is:
1) 70kg 6000 order water-ground limestones are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 90 ℃, after temperature reaches 120 ℃, adds Triple Pressed Stearic Acid/aluminic acid ester and mixes stirring 5 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order water-ground limestones that 45 ℃ of dischargings obtain modification;
3) with PA6, polyethylene wax, paraffin is put into high-speed mixer and mixing successively and was stirred 3 minutes, adds 6000 order water-ground limestones after the modification then and continues to mix and stirred 2 minutes;
4) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to 40 ℃ of dischargings, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches.
5) identical with embodiment 1, promptly process 6000 mesh inorganic powder filling-modified PA6 master batch finished products.
Embodiment 4:
Raw material:
PA6 (nylon 6) 20kg
Triple Pressed Stearic Acid/aluminic acid ester 0.8kg
Polyethylene wax 3kg
Paraffin (WAX) 0.6kg
6000 order water-ground limestone 85kg.
The step of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof is:
1) 85kg 6000 order water-ground limestones are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 90 ℃, after temperature reaches 160 ℃, adds Triple Pressed Stearic Acid/aluminic acid ester and mixes stirring 10 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order water-ground limestones that 45 ℃ of dischargings obtain modification;
3) with PA6, polyethylene wax, paraffin is put into high-speed mixer and mixing successively and was stirred 4 minutes, adds 6000 order water-ground limestones after the modification then and continues to mix and stirred 4 minutes;
4) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to 30 ℃ of dischargings, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches;
5) identical with embodiment 1, promptly process 6000 mesh inorganic powder filling-modified PA6 master batch finished products.
Above examples of implementation can be according to practical situation; Under the prerequisite that does not reduce performance index; Select for use 6000 order inorganic material powders of different additions to reach the purpose that reduces production costs, can save 5～15% cost according to the different additions and the product comparison of corresponding common fillers.
The made product of present embodiment is detected by Tianjin quality monitoring testing station the 5th station, reaches corresponding national standards fully.
Select for use 6000 order inorganic material powders with inorganic rigid particle strengthen, toughness reinforcing theory is as the research theory foundation.
This theory general solution is interpreted as: inorganic particulate is dispersed in the matrix resin, and when receiving external impacts, because the existence of inorganic particulate has produced stress concentration effect, resin produces crack splitting around causing.Simultaneously, the matrix between the particle has also produced viscous deformation, absorbs striking energy, thereby reaches toughening effect; The existence of inorganic particulate is obstructed and passivation the matrix cracking expansion, finally stops the unlikely destructiveness cracking that develops into of tiny crack; Along with the particle fineness attenuates.The specific surface area of particle increases, and particle and matrix contact area increase, and material is to produce more crack crackle and viscous deformation being hit, thereby absorbs energy.Another kind of mechanism is thought two tensile stresss very that act on of matrix and particle, and the position is a stress under the line.Because the effect of power, near the effect that can be stressed the equator of particle helps surrender and occurs; In addition, because the two poles of the earth receive action of pulling stress, when the interface cementability is more weak; The interface unsticking can at first take place at the two poles of the earth; Form a hole around being equivalent to make particle, according to the stress distribution for the hole, the stress on the equatorial plane of hole is 3 times of this body stress.Therefore, when this body stress did not reach the matrix yielding stress as yet, partial points had begun to produce surrender, promptly equally also impelled the matrix surrender, and comprehensive effect improves the toughness of superpolymer.
Through to different-grain diameter CaCO
3With discovering of PA6 compound system performance: under the situation that inorganic rigid particle is not reunited, the more little resulting composite property of particle diameter is good more, especially adds an amount of nanometer CaCO in the co-mixing system
3During particle, its shock strength, tensile strength and elongation at break all can be improved simultaneously.Chemical process modified Nano CaCO
3, its interaction between homodisperse and interface in the PA6 matrix is strengthened, thereby cause its shock strength, elongation at break, tensile modulus all to increase considerably, and tensile strength almost remains unchanged; But, work as CaCO
3Consumption surpasses at 15% o'clock, nano level CaCO
3The matrix material of modification all is lower than by micron order CaCO on tensile strength and notched Izod impact strength
3The composite system of modification.Through analyzing; Particle diameter is thin more, and the phenomenon of powder generation secondary agglomeration is serious more, though the particle diameter of addition material is thin more in theory; Add the enhancing that obtains in the polymkeric substance to, toughness reinforcing mechanical property is outstanding more; Because the as easy as rolling off a log generation secondary agglomeration of nano-powder, the true particle diameter of nano-powder is often much larger than theoretical particle diameter during application but in fact.May command still under laboratory environment, in case be amplified to semipilot, the quality of product not only can not improve and occurs the phenomenon that descends on the contrary.Therefore, the 6000 order inorganic material powders that the present invention uses, its particle diameter of 90%≤2 μ m (can be expressed as D
90≤2 μ m), both had the advantage of part nano-powder, solved the shortcoming that nano-powder " is prone to reunion, the difficult dispersion " again basically.
The result of study of the comprehensive domestic and international 6000 order powders of the present invention, it is increasingly high to think that 6000 status of order powder in the modifying plastics field are bound to, and it uses the more and more maturation that also is bound to; Start with from the utilisation technology of micron order 6000 order powders, overcome the problem that nano-powder runs into.
Claims (4)
1. mesh inorganic powder filling-modified PA6 master batch, it is characterized in that: its component and weight part are:
10～30 parts of PA6;
60～85 parts of 6000 order inorganic material powders;
0.5～3 part of surface treatment agent;
0.5～5 part of polyethylene wax;
0.5～1.5 part in paraffin.
2. according to claim 1 6000 mesh inorganic powder filling-modified PA6 master batches; It is characterized in that: described inorganic material powder is 6000 purpose water-ground limestones or light calcium carbonate or kaolin or talcum powder or silicon-dioxide or Marinco H or white lake or wollastonite; And the arbitrary proportion mixture of above-mentioned substance, its particle diameter of 90%≤2 μ m.
3. according to claim 1 6000 mesh inorganic powder filling-modified PA6 master batches is characterized in that: described surface treatment agent is silane or titanic acid ester or aluminate coupling agent or Triple Pressed Stearic Acid, and the arbitrary combination mixture of above-mentioned substance.
4. the preparation method of claim 1 described 6000 mesh inorganic powder filling-modified PA6 master batches is characterized in that: may further comprise the steps:
1) 6000 order inorganic material powders are put into the high mixer high speed and mix, temperature begins dehumidifier when reaching 80 ℃ to 90 ℃, after temperature reaches 110 ℃ to 160 ℃, adds surface treatment agent and mixes stirring 5 to 10 minutes;
2) compound in the high mixer is put in the cold mixer cooled off, when cooling temperature is reduced to the 6000 order inorganic material powders that discharging after 30 ℃ to 50 ℃ obtains modification;
3) PA6, polyethylene wax, paraffin are put into high-speed mixer and mixing successively and stirred 1 to 5 minute, add 6000 order inorganic material powders after the modification then and continue to mix and stirred 1 to 5 minute;
4) compound in the high mixer is put in the cold mixer cooled off, discharging after cooling temperature is reduced to 30 ℃ to 50 ℃, the material of emitting is the special-purpose powder of 6000 mesh inorganic powder filling-modified PA6 master batches and preparation method thereof;
5) with the special-purpose powder of PA6 extruding pelletization on twin screw extruder, 6000 mesh inorganic powder filling-modified PA6 master batches.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2010106219014A CN102532875A (en) | 2010-12-27 | 2010-12-27 | 6000-mesh inorganic powder-filled modified PA (Polyamide)6 master batch and preparation method thereof |
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| CN2010106219014A CN102532875A (en) | 2010-12-27 | 2010-12-27 | 6000-mesh inorganic powder-filled modified PA (Polyamide)6 master batch and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641321A (en) * | 2017-09-20 | 2018-01-30 | 优矿塑新材料科技（苏州）有限公司 | A kind of PA66 carriers master batch |
| CN111349331A (en) * | 2020-04-20 | 2020-06-30 | 江苏京利华新材料有限公司 | Mineral-filled PC alloy material with high impact resistance and low warpage and preparation method thereof |
| CN111592691A (en) * | 2020-05-25 | 2020-08-28 | 贵州利东环保科技有限公司 | Phosphogypsum filled plastic modified particle and preparation method thereof |
-
2010
- 2010-12-27 CN CN2010106219014A patent/CN102532875A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107641321A (en) * | 2017-09-20 | 2018-01-30 | 优矿塑新材料科技（苏州）有限公司 | A kind of PA66 carriers master batch |
| CN111349331A (en) * | 2020-04-20 | 2020-06-30 | 江苏京利华新材料有限公司 | Mineral-filled PC alloy material with high impact resistance and low warpage and preparation method thereof |
| CN111592691A (en) * | 2020-05-25 | 2020-08-28 | 贵州利东环保科技有限公司 | Phosphogypsum filled plastic modified particle and preparation method thereof |
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Application publication date: 20120704 |