CN109721809A - A kind of filling-modified composite material and preparation method of rotomoulding polyethylene grade - Google Patents
A kind of filling-modified composite material and preparation method of rotomoulding polyethylene grade Download PDFInfo
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- CN109721809A CN109721809A CN201811409919.0A CN201811409919A CN109721809A CN 109721809 A CN109721809 A CN 109721809A CN 201811409919 A CN201811409919 A CN 201811409919A CN 109721809 A CN109721809 A CN 109721809A
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Abstract
The present invention provides a kind of filling-modified composite material and preparation method of rotomoulding polyethylene grade, wherein, a kind of filling-modified composite material of rotomoulding polyethylene grade includes: 25~90 parts of LLDPE1,0~40 part of LLDPE2,10~50 parts of inorganic fillers, 1~6 part of compatilizer, 0.5~10 part of toughener, 0.1~1 part of antioxidant, 0.2~0.6 part of lubricant in parts by weight；Wherein, LLDPE1 and LLDPE2 is the LLDPE material of two kinds of different performances；Inorganic filler contains glass microballoon；Compatilizer is PE grafted maleic anhydride.The present invention is using linear low density polyethylene resin as matrix, fill inorganic filler, the blendings such as POE-g-GMA, POE-g-MAH are added to be granulated, be milled, rotational moulding material is prepared, it is improved using rotomoulded articles intensity prepared by the rotational moulding material, also there is good wearability, resistance to acid and alkali, geometrical stability and anti-microbial property, furthermore can also reduce production cost.
Description
Technical field
The present invention relates to rotational molding grade material, the filling-modified composite material of especially a kind of rotomoulding polyethylene grade and its preparation side
Method.
Background technique
Rotational molding technique is a kind of thermoplastic hollow forming method, i.e., first leads in powdery or pasty material injection mould
The heating and vertical and horizontal rolling rotation to mold are crossed, material is made to be covered with mould by means of self gravitation effect and centrifugal force even action
Tool and melts inner cavity, demolding after cooling and hollow product.Rotational molding technique starts from the 1940s, in 70 years 20th century
In generation, is widely used in some developed countries such as America and Europe.China realizes industrialized production the 1990s, although starting
Relatively late, but development is very rapid, also achieves some achievements attracted attention.
90% or more rotomoulded articles raw material is polyethylene (PE) in domestic market, wherein 95% is linear low close again
It spends polyethylene (LLDPE), and external market is compared, raw material is single.In addition, in domestic rotomoulded articles manufacturer, one
Man, subsidiary factory directly produces rotomoulded articles using LLDPE raw material, and there are many deficiencies compared with modified materials for LLDPE raw material, for example, power
It learns that performance is poor, intensity is weak, acid and alkali-resistance, antibiotic property are poor, can also have geometrical stability for the rotational moulding product of some large sizes
The problem of difference.
Summary of the invention
That there are mechanical properties to solve the LLDPE raw material of existing rotational moulding mentioned in background technique is poor, intensity is weak, resistance to
The problems such as soda acid, poor antibiotic property；The present invention provides a kind of filling-modified composite material of rotomoulding polyethylene grade, in parts by weight,
Including following component:
LLDPE1:25~90 part；
LLDPE2:0~40 part；
Inorganic filler: 10~50 parts；
Compatilizer: 1~6 part；
Toughener: 0.5~10 part；
Antioxidant: 0.1~1 part；
Lubricant: 0.2~0.6 part；
Wherein, the LLDPE1 and LLDPE2 is the LLDPE material of two kinds of different performances；
The inorganic filler contains glass microballoon；
The compatilizer is PE grafted maleic anhydride.
Further, melt index >=5g/10min of the LLDPE1, tensile yield strength >=12MPa, simply supported beam lack
Mouth impact strength >=70kJ/m2；Melt index >=20g/10min of the LLDPE2, tensile yield strength >=9MPa, simply supported beam
Notch impact strength >=60kJ/m2。
Further, the inorganic filler includes: that 10~50 parts of glass microballoons, 10~50 parts of modifications are super in parts by weight
Thin barium sulfate, 10~50 parts of talcum powder, 10~50 parts of calcium carbonate.
Further, the inorganic filler is powder, and powder diameter is more than 800 mesh.
Further, the antioxidant is at least one of irgasfos 168, antioxidant 1010, antioxidant 1098.
Further, the lubricant is Lubricate EBS-SF.
Further, the toughener is that POE plastics grafted maleic anhydride (POE-g-MAH) and Glycidyl methacrylate are sweet
At least one of grease grafted ethene-octene copolymer (POE-g-GMA).
The present invention also provides a kind of preparation methods of above-mentioned filling-modified composite material of rotomoulding polyethylene grade, including following step
It is rapid:
Step 1 weighs LLDPE, inorganic filler, compatilizer, toughener, antioxidant, lubricant low according to the weight ratio
It is uniformly mixed in fast mixing machine, then puts into extruding pelletization in double screw extruder, drying for standby；
Step 2 fills out the powder that plastic pellet obtained in step 1 wears into 30-40 mesh in flour mill to get polyethylene
Fill modified rotational moulding PP Pipe Compound.
Further, the technological parameter that low speed mixer mixes in step 1 are as follows: 10~50rpm of revolving speed, incorporation time 5~
15min。
Further, double screw extruder is parallel dual-screw extruding machine, melting temperature 180~200 when extrusion in step 1
DEG C, 100~500rpm of engine speed, 8~20Hz of main feeding frequency, melt pressure≤10MPa.
Further, flour mill selects 30~40 mesh screens in step 2, and speed of grinding plate 4000-5000rpm, be milled electric current
50~70A, powder outlet temperature≤70 DEG C.
The filling-modified composite material of rotomoulding polyethylene grade of the invention is compared compared with the LLDPE material of rotational moulding, is had
Following advantages:
(1) present invention using linearly Density Polyethylene Resin as matrix, fill inorganic filler, addition compatilizer, toughener,
Antioxidant and lubricant, to improve the intensity of rotomoulded articles, wearability, resistance to acid and alkali and geometrical stability；
(2) it is filling-modified multiple to cannot be only used for enhancing rotomoulding polyethylene grade using glass microballoon as inorganic filler by the present invention
The wearability of condensation material, while also there is the ability of enhancing resistance to acid and alkali, alternative acidproof modified additive and alkaline-resisting modified additive
Addition, reduce cost；
(3) present invention uses PE grafted maleic anhydride as compatilizer, and using glass microballoon as inorganic filler, PE grafting
Maleic anhydride branch on maleic anhydride can be reacted with the silicone hydroxyl on glass microballoon surface generates a kind of maleic anhydride esters product,
The maleic anhydride esters product has good bacteriostatic activity, especially good to the inhibitory effect of fungi；Equally, POE plastics connect
Branch maleic anhydride can also enhance fungistatic effect as compatilizer.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention
A part of the embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not having
Every other embodiment obtained under the premise of creative work is made, shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: by 72 parts of linear low density polyethylene LLDPE1,
20 parts of glass microballoons, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 5 parts of POE-g-MAH, 3
Part PE grafted maleic anhydride is put into low speed batch mixer, mixing 5min, and batch mixer revolving speed is 20rpm；Then by mixed object
Extruding pelletization in material investment parallel dual-screw extruding machine, extruder parameter are as follows: engine speed 400rpm, main feeding frequency 10Hz,
180~200 DEG C of temperature, melt pressure≤10MPa；The plastic pellet being granulated is put into oven drying, it is 90 DEG C of temperature, dry
2h；Dried plastic pellet is milled in flour mill, flour mill selects 40 mesh screens, speed of grinding plate 4000rpm, milling electricity
Flow 60A, powder outlet temperature≤70 DEG C.
Embodiment 2
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: 66 parts of linear low density polyethylene are added
LLDPE1,25 parts of glass microballoons, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 6 parts of POE-
G-MAH, 3 parts of PE grafted maleic anhydrides put into mixing 8min in low speed batch mixer, and batch mixer revolving speed is 10rpm；Then it will mix
Extruding pelletization in good material investment double screw extruder, extruder parameter are as follows: engine speed 350rpm, main feeding frequency 8Hz,
180~200 DEG C of temperature, melt pressure≤10MPa；The plastic pellet being granulated is put into oven drying, it is 90 DEG C of temperature, dry
2h；Dried plastic pellet is milled in flour mill later, flour mill selects 40 mesh screens, speed of grinding plate 4000rpm, mill
Powder electric current 55A, powder outlet temperature≤70 DEG C.
Embodiment 3
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: 61 parts of linear low density polyethylene are added
LLDPE1,30 parts of glass microballoons, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 5 parts of POE-
G-MAH, 4 parts of PE grafted maleic anhydrides put into mixing 10min in low speed batch mixer, and batch mixer revolving speed is 20rpm；Then it will mix
Extruding pelletization in good material investment double screw extruder, extruder parameter are as follows: engine speed 400rpm, main feeding frequency
12Hz, 180~200 DEG C of temperature, melt pressure≤10MPa；The plastic pellet being granulated is put into oven drying, 90 DEG C of temperature,
Dry 2h；Dried plastic pellet is milled in flour mill later, flour mill selects 40 mesh screens, speed of grinding plate
5000rpm, be milled electric current 60A, powder outlet temperature≤70 DEG C.
Embodiment 4
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: 61 parts of linear low density polyethylene are added
LLDPE1,10 parts of modified superfine barium sulfate, 20 parts of glass microballoons, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of profit
Lubrication prescription EBS-SF, 5 parts of POE-g-MAH, 4 parts of PE grafted maleic anhydrides put into mixing 10min, batch mixer in low speed batch mixer
Revolving speed is 20rpm；Then by extruding pelletization, extruder parameter are as follows: engine speed in mixed material investment double screw extruder
400rpm, main feeding frequency 12Hz, 180~200 DEG C of temperature, melt pressure≤10MPa；The plastic pellet being granulated is put into baking
Case is dry, and 90 DEG C of temperature, dry 2h；Dried plastic pellet is milled in flour mill later, flour mill selects 40 meshes
Net, speed of grinding plate 5000rpm, be milled electric current 60A, powder outlet temperature≤70 DEG C.
Embodiment 5
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: 31 parts of linear low density polyethylene are added
LLDPE1,31 parts of linea low density LLDPE2,15 parts of modified superfine barium sulfate, 15 parts of glass microballoons, 0.1 part of antioxidant 1010,
0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 4 parts of POE-g-MAH, 4 parts of PE grafted maleic anhydrides put into low speed mixing
Mixing 8min in machine, batch mixer revolving speed are 10rpm；Then it by extruding pelletization in mixed material investment double screw extruder, squeezes
Machine parameter out are as follows: engine speed 400rpm, main feeding frequency 10Hz, 180~200 DEG C of temperature, melt pressure≤10MPa；It will make
The good plastic pellet of grain is put into oven drying, 90 DEG C of temperature, dries 2h；Dried plastic pellet is ground in flour mill later
Powder, flour mill select 40 mesh screens, and speed of grinding plate 5000rpm, be milled electric current 60A, powder outlet temperature≤70 DEG C.
Embodiment 6
A kind of preparation of the filling-modified composite material of rotomoulding polyethylene grade: 28 parts of linear low density polyethylene are added
LLDPE1,28 parts of linea low density LLDPE2,10 parts of modified superfine barium sulfate, 25 parts of glass microballoons, 0.1 part of antioxidant 1010,
0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 5 parts of POE-g-MAH, 4 parts of PE grafted maleic anhydrides put into low speed mixing
Mixing 10min in machine, batch mixer revolving speed are 10rpm；Then it by extruding pelletization in mixed material investment double screw extruder, squeezes
Machine parameter out are as follows: engine speed 400rpm, main feeding frequency 10Hz, 180~200 DEG C of temperature, melt pressure≤10MPa；It will make
The good plastic pellet of grain is put into oven drying, 90 DEG C of temperature, dries 2h；Dried plastic pellet is ground in flour mill later
Powder, flour mill select 40 mesh screens, and speed of grinding plate 4000rpm, be milled electric current 55A, powder outlet temperature≤70 DEG C.
Comparative example 1
A kind of preparation of rotomoulding polyethylene grade composite material: weigh 100 parts of linear low density polyethylene LLDPE1,0.1 part it is anti-
1010,0.2 parts of irgasfos 168s of oxygen agent, 0.3 part of Lubricate EBS-SF, the preparation method is the same as that of Example 1.
Comparative example 2
A kind of preparation of rotomoulding polyethylene grade composite material: weigh 50 parts of linear low density polyethylene LLDPE1,50 parts it is linear
Low density polyethylene (LDPE) LLDPE2,0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF.Preparation method
With embodiment 5.
Comparative example 3
It is milled using LLDPE1 raw material as rotational moulding material.Flour milling method is the same as embodiment 3.
The material investment of the rotational moulding of embodiment 1-6 and comparative example 1-3 is kept the temperature in bung Plastic Rolling Molds, in identical work
Production heat preservation bung, rotational molding machine parameter under skill parameter are as follows: outer shaft revolving speed 8rpm, inner shaft revolving speed 6rpm, oven temperature setting 230
DEG C, mold heats 35min, and cooling 25min obtains heat preservation bung after demoulding.
The performance of each heat preservation bung is tested as follows:
Melt index test: according to ISO-1133 standard testing；
Tensile strength test: according to ISO-527 standard testing；
Bending strength test: according to ISO-178:2001 standard testing；
Room temperature simply supported beam notch impact strength test: according to ISO-179:1993 standard testing.
The test result of each heat preservation bung is as shown in table 1:
Table 1
According to table 1 as a result, the tensile strength and bending strength of embodiment 1-6 are above comparative example 1-3, rotational moulding of the invention
The grade filling-modified composite material of polyethylene significantly improves mechanical property in the case where impact strength meets the requirements；With comparative example
The problems such as 3 compare, and rotational moulding PP Pipe Compound of the invention significantly improves current rotomoulding polyethylene grade raw material mechanical property deviation.
Comparative example 4 has also been devised in the present invention: weighing 61 parts of linear low density polyethylene LLDPE1,30 parts of modified superfine sulfuric acid
Barium, 0.1 part of antioxidant 1010,0.2 part of irgasfos 168,0.3 part of Lubricate EBS-SF, 5 parts of POE-g-GMA, 4 parts of PE grafting
Maleic anhydride, preparation method are identical with embodiment 4.The material of comparative example 4 equally puts into heat preservation bung Plastic Rolling Molds and is fabricated to guarantor
Warm bung.
Biocidal property experiment test: it is sub- that sodium nitrate 3g, phosphoric acid hydrogen dimethylamino 1g, magnesium sulfate 0.5g, potassium chloride 0.5g, sulfuric acid are weighed
Iron 0.01g, sucrose 30g, agar 20g add distilled water to 1000mL, dissolve by heating, after packing, high pressure sterilization 20 divides at 121 DEG C
It is spare that culture medium is made in clock；Above-described embodiment 1-6 and comparative example 1-4 the heat preservation bung being made into are made into the slice of 2cm × 2cm,
Slice is respectively put into corresponding 35mm culture dish and is marked, then adds culture medium into culture dish；Not add the culture of slice
Base is as blank control group；2 drop mould bacterium solution (bacterium solution robe numbers 10 are added dropwise into the culture dish of experimental group and blank control group9/
ML), cultivated 5 days in 28 DEG C, measurement experiment group and blank colony diameter are converted into bacteriostasis rate.
Bacteriostasis rate=(blank colony diameter-sample colony diameter)/blank colony diameter × 100%
Its bacteriostasis rate test result is as shown in table 2:
Table 2
According to table 2, the inhibiting rate that embodiment 1-6 grows Penicillium notatum reaches 50% or more, with comparative example 1-4 phase
Than, embodiment 1-6 there is apparent bacteriostasis to Penicillium notatum, it was demonstrated that rotomoulding polyethylene grade of the invention is filling-modified compound
Material has apparent fungistatic effect.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. a kind of filling-modified composite material of rotomoulding polyethylene grade, it is characterised in that: in parts by weight, including following component:
LLDPE1:25~90 part；
LLDPE2:0~40 part；
Inorganic filler: 10~50 parts；
Compatilizer: 1~6 part；
Toughener: 0.5~10 part；
Antioxidant: 0.1~1 part；
Lubricant: 0.2~0.6 part；
Wherein, the LLDPE1 and LLDPE2 is the LLDPE material of two kinds of different performances；
The inorganic filler contains glass microballoon；
The compatilizer is PE grafted maleic anhydride.
2. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the LLDPE1's
Melt index >=5g/10min, tensile yield strength >=12MPa, simply supported beam notch impact strength >=70kJ/m2；The LLDPE2
Melt index >=20g/10min, tensile yield strength >=9MPa, simply supported beam notch impact strength >=60kJ/m2。
3. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the inorganic filler
It further include at least one of modified superfine barium sulfate, talcum powder, calcium carbonate.
4. the filling-modified composite material of rotomoulding polyethylene grade according to claim 3, it is characterised in that: the inorganic filler
It in parts by weight include: 10~50 parts of glass microballoons, 10~50 parts of modified superfine barium sulfate, 10~50 parts of talcum powder, 10~50
Part calcium carbonate.
5. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the inorganic filler
For powder, powder diameter is more than 800 mesh.
6. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the antioxidant is
At least one of irgasfos 168, antioxidant 1010, antioxidant 1098.
7. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the lubricant is
Lubricate EBS-SF.
8. the filling-modified composite material of rotomoulding polyethylene grade according to claim 1, it is characterised in that: the toughener is
At least one of POE plastics grafted maleic anhydride and glycidyl methacrylate graft ethylene-octene copolymer.
9. a kind of preparation method of such as filling-modified composite material of the described in any item rotomoulding polyethylene grades of claim 1-8,
It is characterized in that: the following steps are included:
Step 1, to weigh LLDPE, inorganic filler, compatilizer, toughener, antioxidant, lubricant according to the weight ratio mixed in low speed
It is uniformly mixed in conjunction machine, then puts into extruding pelletization in double screw extruder, drying for standby；
Step 2, plastic pellet obtained in step 1 is worn into flour mill the powder of 30-40 mesh to get polyethylene filling change
Property rotational moulding PP Pipe Compound.
10. the preparation method of the filling-modified composite material of rotomoulding polyethylene grade according to claim 9, it is characterised in that:
The technological parameter that low speed mixer mixes in step 1 are as follows: 10~50rpm of revolving speed, 5~15min of incorporation time.
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| CN113929998A (en) * | 2021-09-13 | 2022-01-14 | 神华(北京)新材料科技有限公司 | Polyolefin composition for rotational molding, polyolefin powder for rotational molding, and preparation method and application thereof |
| US11746220B2 (en) | 2020-06-12 | 2023-09-05 | Braskem S.A. | High flow rotomolding compositions, processes thereof, and articles therefrom |
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Application publication date: 20190507 |