CN106147009A - A kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof - Google Patents
A kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof Download PDFInfo
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- CN106147009A CN106147009A CN201510152574.5A CN201510152574A CN106147009A CN 106147009 A CN106147009 A CN 106147009A CN 201510152574 A CN201510152574 A CN 201510152574A CN 106147009 A CN106147009 A CN 106147009A
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Abstract
The present invention provides a kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof, it is made up of regenerating polypropylene, grafting compatilizer, inorganic mineral filler, coupling agent, antioxidant, lubricant, and the weight of wherein said coupling agent accounts for the 2% of inorganic mineral filler weight；Described regenerating polypropylene, grafting compatilizer, the weight portion sum of inorganic mineral filler are 100 parts；Described regenerating polypropylene be reclaim after through sort, cleans, crush, dry the injection grade polypropylene being fabricated to, its moisture content is less than 0.5%, combustion residue is less than 3%, melt index is 15-60g/10min at 2.16kg, under the conditions of 230 DEG C.The present invention prepares filler parent granule by regenerating polypropylene and grafting compatilizer, inorganic mineral filler etc. for raw material, and use spray mode to add coupling agent, make the master batch prepared have good dispersibility, a compatibility, and expand the range of regenerated plastics, reduce production cost.
Description
Technical field
The invention belongs to field of compound material, be specifically related to a kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof.
Background technology
For correlated performances such as the mechanical performance of reinforced plastic material, density, typically all add a little modifying agent it is modified, originally modifying plastics directly uses powder body at filling-modified aspect, on the one hand this modification mode can have bigger pollution to production environment, on the other hand to be added on dispersion aspect poor for powder body, affects final products performance.In recent years, along with continuous renewal and the development of plastics modification technology, use filler parent granule as the filling-modified production form becoming many enterprises, effectively improve polluting and being obtained in terms of processing technique.
At present, the base material that on market, substantial amounts of filler parent granule mainly uses is virgin material polypropylene, polyethylene, polyolefin elastomer (POE) etc., and the cost of raw material aspect of production is higher.And use regenerated plastics to be filled with master batch as base material and produce, it is equipped with corresponding auxiliary agent again, can not only effectively reduce the cost of raw material, and the filler parent granule that dispersive property, the compatibility are good can be obtained, modifying plastics industry can be widely used in, such as automobile, pipeline, cable etc..
Summary of the invention
It is an object of the invention to provide a kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof.
For achieving the above object, the technical solution used in the present invention is: a kind of filler parent granule prepared by regenerating polypropylene, it is characterised in that: this material is prepared from by weight by following components:
Regenerating polypropylene
10～20；
Grafting compatilizer
2～6；
Inorganic mineral filler
75～85；
Coupling agent
1.5～1.7；
Antioxidant
0.5～1.0
Lubricant
1.5～3；
The weight of described coupling agent accounts for the 2% of inorganic mineral filler weight；
Described regenerating polypropylene, grafting compatilizer, the weight portion sum of inorganic mineral filler are 100 parts；
Described regenerating polypropylene be reclaim after through sort, cleans, crush, dry the injection grade polypropylene being fabricated to, its moisture content is less than 0.5%, combustion residue is less than 3%, melt index is 15-60g/10min at 2.16kg, under the conditions of 230 DEG C.
Further, described grafting compatilizer is polypropylene and the graft (POE-g-MAH) of the graft (PP-g-MAH) of maleic anhydride or polyolefin elastomer with maleic anhydride, and wherein the percent grafting of maleic anhydride reaches more than 1.5%.
Described inorganic mineral filler is one or more that particle diameter is more than in the Pulvis Talci of 1200 mesh, calcium carbonate or Muscovitum.
One or more in silane coupler, titanate coupling agent, aluminate coupling agent of described coupling agent.
Described antioxidant is that four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester (1010) compounds for 1:2 in mass ratio with tricresyl phosphite (2,4--di-tert-butyl-phenyl) ester (168).
Described lubricant is that white mineral oil, ethylene bis stearamide (EBS) and calcium stearate compound for 2:1:1 in mass ratio.
Another goal of the invention of the present invention is to provide a kind of method preparing above-mentioned filler parent granule, comprises the following steps:
(1) regenerating polypropylene of dried, grafting compatilizer, antioxidant, lubricant are poured in temperature control high-speed mixer mixing 2-3min by formula proportion；The temperature of described mixer is 75 DEG C-90 DEG C, rotating speed is 500-800r/min；
(2) compound in (1) adds inorganic mineral filler, after using spray mode to be uniformly added into coupling agent in whipping process, continue stirring mixing 10-15min, obtain premix material；
(3) premix material is put in the double screw extruder of L/D=44:1, after first preheating 2～4 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein double screw extruder temperature is set to: pre-tabetisol 140～155 DEG C, the first melting zone 190～200 DEG C, first shear at high temperature district 200～210 DEG C, second shear at high temperature district 210～220 DEG C, second melts warm area 200～210 DEG C, and discharging opening melts warm area 190～200 DEG C.The rotating speed of course of processing double screw extruder is 300～500 revs/min.
The present invention compared with prior art has the advantage that
(1) present invention prepares filler parent granule by regenerating polypropylene and grafting compatilizer, inorganic mineral filler etc. for raw material, and uses spray mode to add the master batch that coupling agent prepares.Add grafting compatilizer and introduce highly polar reactive group, make material have high polarity and reactivity, improve the compatibility of polypropylene and mineral filler；Coupling agent makes filling surface be become lipophile by hydrophilic, thus reaches and the combining closely of polymer, and makes the intensity of material, cohesion, dispersive property etc. significantly improve, and the most after all makes the master batch prepared have good dispersibility, the compatibility；
(2) present invention uses the regenerating polypropylene of recovery to prepare filler parent granule as base material, and it, compared with the filler parent granule using new resin binder, can be greatly reduced the cost of raw material.
(3) reduce the waste or used plastics pollution to environment, promote regenerated plastics and be worth；
(4) present invention solves the problems such as the cost height of Conventional filler master batch in the market, bad dispersibility, poor compatibility, extends the range of regenerated plastics simultaneously.Filler parent granule after this invention processed can be used for being widely used in the filling-modified of the materials such as automobile, pipeline, cable, significantly can reduce cost by modified raw material meeting, improve the use value of regenerated plastics in the case of properties of product require.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, and following example are only that the present invention will be described rather than is limited it.
Table 1 below is the material mixture ratio situation of embodiment 1-6, wherein: antioxidant is by four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester (1010) and tricresyl phosphite (2,4--di-tert-butyl-phenyl) ester (168) carry out compounding composition for 1:2 in mass ratio.
Described lubricant is carried out compounding composition for 2:1:1 in mass ratio by white mineral oil, ethylene bis stearamide (EBS) and calcium stearate.
Regenerating polypropylene be select reclaim after through sort, cleans, crush, dry the injection grade polypropylene being fabricated to, its moisture content is less than 0.5%, combustion residue is less than 3%, melt index is 15-60g/10min at 2.16kg, under the conditions of 230 DEG C.
Polypropylene is the PP K7926 of Shanghai match section.
Table 1: the proportioning of embodiment 1-6
| Material | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Regenerating polypropylene | 10 | 13 | 15 | 20 | 16 | 14 |
| PP-g-MAH | 5 | 5 | 4 | 6 | ||
| POE-g-MAH | 2 | 5 | ||||
| Calcium carbonate | 85 | 55 | 50 | |||
| Pulvis Talci | 30 | 45 | 75 | |||
| Mica powder | 35 | 30 | 80 | |||
| Silane coupler | 1.7 | 1.3 | 1.1 | 1.6 | 1.2 | |
| Titanate coupling agent | 0.4 | 1 | 0.4 | |||
| Aluminate coupling agent | 0.6 | 0.4 | ||||
| Antioxidant | 0.8 | 0.8 | 0.5 | 1 | 0.9 | 0.7 |
| Lubricant | 1.6 | 3 | 2.5 | 1.5 | 2 | 2.8 |
Embodiment
1
Regenerating polypropylene 10 parts, grafting Compatibilizer PP-g-MAH 5 parts, 0.8 part of antioxidant, lubricant 1.6 parts are put into mixing 2min in temperature control high-speed mixer, and temperature controls at 80 DEG C, rotating speed 700r/min；Then by 85 parts of addition high-speed mixers of inorganic mineral filler calcium carbonate, stirring and use spray mode to be uniformly added into silane coupler 1.7 parts, high mixer rotating speed controls at 750 r/min, continues stirring 12min, obtain premix material after adding；Finally premix material is fed in the double screw extruder of L/D=44:1, after preheating 3 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 140 DEG C of pre-tabetisol, first melting zone 195 DEG C, first 205 DEG C of shear at high temperature district, the second 210 DEG C of shear at high temperature district, second melts warm area 205 DEG C, discharging opening melts warm area 195 DEG C, and screw speed is 350 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Embodiment
2
Regenerating polypropylene 13 parts, grafting compatilizer POE-g-MAH 2 parts, 0.8 part of antioxidant, lubricant 3 parts are put into mixing 3min in temperature control high-speed mixer, and temperature controls at 75 DEG C, rotating speed 600r/min；Then by inorganic mineral filler calcium carbonate 55 parts, 30 parts of addition high-speed mixers of Pulvis Talci, stir while using spray mode to be uniformly added into silane coupler 1.3 parts, titanate coupling agent 0.4 part, high mixer rotating speed controls at 650 r/min, continue stirring 15min after adding, obtain premix material；Finally premix material is fed in double screw extruder, after preheating 2 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 155 DEG C of pre-tabetisol, first melting zone 200 DEG C, first 210 DEG C of shear at high temperature district, the second 220 DEG C of shear at high temperature district, second melts warm area 210 DEG C, discharging opening melts warm area 200 DEG C, and screw speed is 400 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Embodiment
3
Regenerating polypropylene 15 parts, grafting Compatibilizer PP-g-MAH 5 parts, 0.5 part of antioxidant, lubricant 2.5 parts are put into mixing 3min in temperature control high-speed mixer, and temperature controls at 90 DEG C, rotating speed 800r/min；Then by inorganic mineral filler mica powder 35 parts, 45 parts of addition high-speed mixers of Pulvis Talci, stir while using spray mode to be uniformly added into aluminate coupling agent 0.6 part, titanate coupling agent 1 part, high mixer rotating speed controls at 800 r/min, continue stirring 12min after adding, obtain premix material；Finally premix material is fed in double screw extruder, after preheating 3 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 140 DEG C of pre-tabetisol, first melting zone 190 DEG C, first 200 DEG C of shear at high temperature district, the second 210 DEG C of shear at high temperature district, second melts warm area 200 DEG C, discharging opening melts warm area 190 DEG C, and screw speed is 300 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Embodiment
4
Regenerating polypropylene 20 parts, grafting compatilizer POE-g-MAH 5 parts, 1 part of antioxidant, lubricant 1.5 parts are put into mixing 3min in temperature control high-speed mixer, and temperature controls at 75 DEG C, rotating speed 600r/min；Then by 75 parts of addition high-speed mixers of inorganic mineral filler Pulvis Talci, stir while using spray mode to be uniformly added into silane coupler 1.1 parts, aluminate coupling agent 0.4 part, high mixer rotating speed controls at 500 r/min, continues stirring 10min, obtain premix material after adding；Finally premix material is fed in double screw extruder, after preheating 2 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 145 DEG C of pre-tabetisol, first melting zone 200 DEG C, first 205 DEG C of shear at high temperature district, the second 215 DEG C of shear at high temperature district, second melts warm area 205 DEG C, discharging opening melts warm area 195 DEG C, and screw speed is 500 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Embodiment
5
Regenerating polypropylene 16 parts, grafting Compatibilizer PP-g-MAH 4 parts, 0.9 part of antioxidant, lubricant 2 parts are put into mixing 2min in temperature control high-speed mixer, and temperature controls at 90 DEG C, rotating speed 500r/min；Then by inorganic mineral filler calcium carbonate 50 parts, 30 parts of addition high-speed mixers of mica powder, stir while using spray mode to be uniformly added into silane coupler 1.6 parts, high mixer rotating speed controls at 600 r/min, continues stirring 13min, obtain premix material after adding；Finally premix material is fed in double screw extruder, after preheating 2 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 150 DEG C of pre-tabetisol, first melting zone 200 DEG C, first 205 DEG C of shear at high temperature district, the second 220 DEG C of shear at high temperature district, second melts warm area 205 DEG C, discharging opening melts warm area 195 DEG C, and screw speed is 450 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Embodiment
6
Regenerating polypropylene 14 parts, grafting Compatibilizer PP-g-MAH 6 parts, 0.7 part of antioxidant, lubricant 2.8 parts are put into mixing 3min in temperature control high-speed mixer, and temperature controls at 85 DEG C, rotating speed 650r/min；Then by 80 parts of addition high-speed mixers of inorganic mineral filler mica powder, stir while using spray mode to be uniformly added into silane coupler 1.2 parts, titanate coupling agent 0.4 part, high mixer rotating speed controls at 550 r/min, continues stirring 14min, obtain premix material after adding；Finally premix material is fed in double screw extruder, after preheating 4 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein each district temperature of double screw extruder is: 145 DEG C of pre-tabetisol, first melting zone 195 DEG C, first 210 DEG C of shear at high temperature district, the second 215 DEG C of shear at high temperature district, second melts warm area 200 DEG C, discharging opening melts warm area 195 DEG C, and screw speed is 400 revs/min.
Again through melting, extrude and to obtain composite after above-mentioned prepared filler parent granule and polypropylene are mixed for 25:75 in mass ratio.
Comparative example 1-6 is the filler parent granule selecting Anhui Banni New Material Co., Ltd. to produce, its base material is selected and is melted the virgin material polypropylene referred to as 20-60g/10min, other components and preparation method correspond respectively to embodiment 1-6, the filler parent granule prepared and polypropylene mix for 25:75 in mass ratio after again through melting, extrude and to obtain composite.
Composite prepared by the PP composite material obtained by above-described embodiment 1-6 and comparative example 1-6 carries out physical property detection and is shown in Table 2, and the method for testing of the most each physical property is as follows:
Melt flow rate (MFR) is tested according to GB/T 3682-2000
Hot strength, elongation at break measure according to GB/T 1040.2-2006；
Bending strength, bending modulus measure according to GB/T 9341-2008；
Izod notched impact strength measures according to GB/T 1834-2008；
Load deformation temperature measures according to GB/T 1634.2-2004；
Table 2: performance indications:
Be can be seen that by embodiment in table 2 and comparative example result, filler parent granule is prepared compared with the master batch that commercially available same ratio is filled by this patent, they are suitable with PP matrix compound tense performance, and than comparative example, there is more preferable rigidity, toughness, intensity and thermostability, it also has clear superiority in terms of the compatibility, dispersibility.The regrown material source selected additionally, due to the present invention is relatively wide, and production technology is simple, greatly saves the cost of raw material.
These embodiments are merely to illustrate the present invention and should not limit the scope of this invention.Additionally, after having read content of the present invention, the present invention is made change or the amendment of the various equivalent form of value by those skilled in the art, these equivalent form of values also belong to following claims limited range.
Claims (10)
1. the filler parent granule prepared by regenerating polypropylene, it is characterised in that: this material is prepared from by weight by following components:
Regenerating polypropylene
10～20；
Grafting compatilizer
2～6；
Inorganic mineral filler
75～85；
Coupling agent
1.5～1.7；
Antioxidant
0.5～1.0
Lubricant
1.5～3.
Filler parent granule the most according to claim 1, it is characterised in that: the weight of described coupling agent accounts for the 2% of inorganic mineral filler weight.
Filler parent granule the most according to claim 1, it is characterised in that: described regenerating polypropylene, grafting compatilizer, the weight portion sum of inorganic mineral filler are 100 parts.
Filler parent granule the most according to claim 1, it is characterized in that: described regenerating polypropylene be reclaim after through sort, cleans, crush, dry the injection grade polypropylene being fabricated to, its moisture content is less than 0.5%, combustion residue is less than 3%, melt index is 15-60g/10min at 2.16kg, under the conditions of 230 DEG C.
Filler parent granule the most according to claim 1, it is characterised in that: described grafting compatilizer is polypropylene and the graft of the graft of maleic anhydride or polyolefin elastomer with maleic anhydride, and wherein the percent grafting of maleic anhydride reaches more than 1.5%.
Filler parent granule the most according to claim 1, it is characterised in that: described inorganic mineral filler is one or more that particle diameter is more than in the Pulvis Talci of 1200 mesh, calcium carbonate or Muscovitum.
Filler parent granule the most according to claim 1, it is characterised in that: one or more in silane coupler, titanate coupling agent, aluminate coupling agent of described coupling agent.
Filler parent granule the most according to claim 1, it is characterized in that: described antioxidant is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester and tricresyl phosphite (2,4--di-tert-butyl-phenyl) ester compound for 1:2 in mass ratio.
Filler parent granule the most according to claim 1, it is characterised in that: described lubricant is that white mineral oil, ethylene bis stearamide and calcium stearate compound for 2:1:1 in mass ratio.
10. the method preparing filler parent granule as claimed in claim 1, it is characterised in that: comprise the following steps:
(1) regenerating polypropylene of dried, grafting compatilizer, antioxidant, lubricant are poured in temperature control high-speed mixer mixing 2-3min by formula proportion；The temperature of described mixer is 75 DEG C-90 DEG C, rotating speed is 500-800r/min；
(2) compound in (1) adds inorganic mineral filler, after using spray mode to be uniformly added into coupling agent in whipping process, continue stirring mixing 10-15min, obtain premix material；
(3) premix material is put in the double screw extruder of L/D=44:1, after first preheating 2～4 minutes, again through melted, extrusion, evacuation, air-cooled, pelletizing and dry, i.e. preparing filler parent granule, wherein double screw extruder temperature is set to: pre-tabetisol 140～155 DEG C, the first melting zone 190～200 DEG C, first shear at high temperature district 200～210 DEG C, second shear at high temperature district 210～220 DEG C, second melts warm area 200～210 DEG C, and discharging opening melts warm area 190～200 DEG C；The rotating speed of course of processing double screw extruder is 300～500 revs/min.
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| CN201510152574.5A CN106147009A (en) | 2015-04-01 | 2015-04-01 | A kind of filler parent granule prepared by regenerating polypropylene and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589619A (en) * | 2016-11-30 | 2017-04-26 | 浙江中财管道科技股份有限公司 | Multi-element toughened and modified special material for PP-R pipe and preparation method thereof |
| CN111100378A (en) * | 2018-10-29 | 2020-05-05 | 泉州市旭丰粉体原料有限公司 | Low-odor functional talc master batch and preparation method thereof |
| CN111117061A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特复合材料股份有限公司 | Novel environment-friendly low-cost long glass fiber reinforced polypropylene composite material and preparation method thereof |
| CN113789027A (en) * | 2021-01-04 | 2021-12-14 | 海信（山东）冰箱有限公司 | Heat-resistant regenerated polypropylene material and preparation method thereof |
| CN114318683A (en) * | 2022-01-07 | 2022-04-12 | 东莞市悠悠美居家居制造有限公司 | Preparation process of spunbonded non-woven fabric |
| CN115584080A (en) * | 2022-08-23 | 2023-01-10 | 始命再生新材料(江苏)有限公司 | PP material recycling and modifying method and application |
-
2015
- 2015-04-01 CN CN201510152574.5A patent/CN106147009A/en active Pending
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| 孔萍等: "《塑料配混技术》", 31 August 2009, 中国轻工业出版社 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106589619A (en) * | 2016-11-30 | 2017-04-26 | 浙江中财管道科技股份有限公司 | Multi-element toughened and modified special material for PP-R pipe and preparation method thereof |
| CN106589619B (en) * | 2016-11-30 | 2019-10-01 | 浙江中财管道科技股份有限公司 | A kind of PP-R pipe PP Pipe Compound of polynary toughening modifying and preparation method thereof |
| CN111100378A (en) * | 2018-10-29 | 2020-05-05 | 泉州市旭丰粉体原料有限公司 | Low-odor functional talc master batch and preparation method thereof |
| CN111117061A (en) * | 2019-12-12 | 2020-05-08 | 上海普利特复合材料股份有限公司 | Novel environment-friendly low-cost long glass fiber reinforced polypropylene composite material and preparation method thereof |
| CN113789027A (en) * | 2021-01-04 | 2021-12-14 | 海信（山东）冰箱有限公司 | Heat-resistant regenerated polypropylene material and preparation method thereof |
| CN114318683A (en) * | 2022-01-07 | 2022-04-12 | 东莞市悠悠美居家居制造有限公司 | Preparation process of spunbonded non-woven fabric |
| CN115584080A (en) * | 2022-08-23 | 2023-01-10 | 始命再生新材料(江苏)有限公司 | PP material recycling and modifying method and application |
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Application publication date: 20161123 |