CN108047712A - Fire-retardant Nylon 66 composite material and preparation method thereof - Google Patents
Fire-retardant Nylon 66 composite material and preparation method thereof Download PDFInfo
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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
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention proposes a kind of fire-retardant Nylon 66 composite material and preparation method thereof, is calculated according to weight percent, including following raw material:PA6630~45%, bromide fire retardant 15~20%, antimony oxide 2~6%, nanoscale mineral filler 0~10%, toughening compatilizer 2~5%, silane coupling agent 0.3~1.0%, PET resin 0~10%, antioxidant 0.5~1.0%, lubricant 0.5~1.0% and glass fibre 25~30%.Preparation method:1) first PA66 resins, PET resin, nanoscale mineral filler are dried, it is for use to obtain drying composite in below 0.03wt% for control moisture content;2) drying composite with other raw materials in addition to glass fibre is uniformly mixed, obtains mixture A;3) mixture A is added in double screw extruder, glass fibre is added in the exhaust outlet of double screw extruder, through frit reaction, extruding pelletization.Not only mechanical property is good for the composite material, also with low warping characteristic, the dimensional stability and planarization of maintenance PA66 composite materials.
Description
Technical field
The invention belongs to polyamide resin material technical fields, and in particular to a kind of fire-retardant Nylon 66 composite material and its system
Preparation Method.
Background technology
Polyamide, English name polyamide, abbreviation PA.Nylon (Nylon) is commonly called as, it is macromolecular main chain
The general name of high polymer containing amide group in repetitive unit.Polyamide has high-tensile;It is resistance to it is tough, impact resistance is special excellent;From
Lubricant nature, wearability are good, resistance to chemical reagents is excellent;Low-temperature characteristics is good;Has self-extinguishment.Since nylon PA plastic materials have many spies
Therefore property, is widely used in machinery, instrument and meter, automobile component, electric, railway, household electrical appliances, communication, frame, physical culture are stopped
Not busy articles for use, oil pipe, fuel tank and some precision engineering products.Polyamide is and low temperature resistant also because hygroscopic, poor dimensional stability
The shortcomings of scarce capacity, limits its application field.
PA66 (poly- oxalyl diamines is commonly called as nylon double six, and abridge nylon 66) is a kind of translucent or opaque breast
White crystals type polymer extensively should with the performances such as its excellent mechanics, heat-resisting, wear-resisting, self-lubricating, low temperature resistant, fire-retardant
For fields such as machinery, electronics, automobile, chemical industry, weavings.With economic growth and improvement of living standard, PA66 becomes Buddhist nun
Yield is maximum in imperial series of products, one of most widely used kind.Wherein, flame-retardant PA 66 composite material is because with high mechanicalness
Can, heat resistance, lower temperature resistance are good, are mainly used on electronic apparatus.However, with the development of electronic enterprises, common
Flame-retardant PA 66 composite material cannot meet existing electrical and electronic component requirement.Some component structures are special, to other of material
Performance requires higher, such as present our company client longer, common flame-retardant PA 66 composite material injection system that is molded electronic component
After part, a period of time is placed, angularity becomes higher so that electronic component can not be assembled, so it is steady to develop low warpage size
The PA66 composite materials of fixed fire-retardant high-mechanical property are met customer need, and have good actual application value.
The content of the invention
The present invention proposes a kind of fire-retardant Nylon 66 composite material, and not only mechanical property is good for the composite material, is also stuck up with low
Bent characteristic maintains the dimensional stability and planarization of PA66 composite materials.
The technical proposal of the invention is realized in this way:
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6630~45%, bromide fire retardant 15~20%, antimony oxide 2~6%, nanoscale mineral filler 0~
10%th, toughening compatilizer 2~5%, silane coupling agent 0.3~1.0%, PET resin 0~10%, antioxidant 0.5~1.0%, profit
Lubrication prescription 0.5~1.0% and glass fibre 25~30%.
Preferably, calculated according to weight percent, including following raw material:
PA6632%, bromide fire retardant 18%, antimony oxide 2%, nanoscale mineral filler 5%, toughening compatilizer
3%th, silane coupling agent 0.5%, PET resin 10%, antioxidant 0.5%, lubricant 1.0% and glass fibre 28%.
Preferably, the viscosity of the PA66 is 2.4~2.8dl/g, as Huafeng Group Corp., Ltd. produces PA66EP1107;
The viscosity of PET resin is 0.68~1.30dl/g, the SB500 produced such as Yizheng petrochemical industry.
Preferably, the bromide fire retardant is selected from brominated Polystyrene, decabromodiphenylethane and high molecular weight brominated epoxy
One or more in resin, the nanoscale mineral filler are nanoscale talcum powder, nano mica powder and nanoscale glass
One or more in glass microballon.
Preferably, the bromide fire retardant is high molecular weight brominated epoxy resin, and the nanoscale mineral filler is nanometer
Grade mica powder.
Preferably, the toughening compatilizer is selected from POE grafted maleic anhydrides, Research of Grafting Malaic Anhydride Onto Polyethylene, ethylene, propylene
One or more in acid butyl ester, ethylene acrylic acid co polymer, maleic anhydride-g-SBS.
Preferably, the silane coupling agent is gamma-aminopropyl-triethoxy-silane, such as KH550.
Preferably, the antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythrites
Ester and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preferably, the lubricant is the one or more in polysiloxanes and ethylene bis stearamide, as domestic
Silicone powder and TAF.
Preferably, the glass fibre is fine for alkali-free length, 10~14 μm of diameter, such as Chongqing Polycomp International Co., Ltd
ECT-4300A.
It is a further object to provide a kind of preparation method of fire-retardant Nylon 66 composite material, including following step
Suddenly:
1) raw material for standby is weighed according to proportioning, wherein first doing PA66 resins, PET resin, nanoscale mineral filler
Dry, it is for use to obtain drying composite in below 0.03wt% for control moisture content;
2) drying composite of step 1) with other raw materials in addition to glass fibre is uniformly mixed, is mixed
Object A;
3) the mixture A of step 2) is added in double screw extruder, while melting extrusion, in double screw extruder
Exhaust outlet adds in glass fibre, through frit reaction, extruding pelletization.
Preferably, when the drying means of the step 1) is that drying 3~5 is small at 110~130 DEG C;Double screw extruder
Process conditions be:One area's temperature:180~200 DEG C, two area's temperature:250~260 DEG C, three area's temperature:240~250 DEG C, 4th area
Temperature:230~240 DEG C, five area's temperature:210~220 DEG C, six area's temperature:210~220 DEG C, seven area's temperature:200~210 DEG C,
Eight area's temperature:200~210 DEG C, nine area's temperature:220~230 DEG C, head temperature:240~260 DEG C;Vacuum degree 0.05~
0.15MP, screw speed:300~500r/min;Feeding rotating speed:10~30r/min.
Beneficial effects of the present invention:
The fire-retardant Nylon 66 composite material of the present invention adds nanoscale mineral filler in the feed, and uses PA and PET
Alloy modification technology, composite material obtained have low warpage, dimensionally stable, and anti-flammability is high, good mechanical performance, at low cost etc.
Feature can be widely applied on electronic apparatus and auto industry field.
Specific embodiment
Embodiment 1
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6638%, high molecular weight brominated epoxy resin 21%, antimony oxide 6%, POE grafted maleic anhydrides 3%,
Gamma-aminopropyl-triethoxy-silane 0.5%, antioxidant 0.5%, ethylene bis stearamide 1.0% and glass fibre 30%.Antioxygen
Agent is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] pentaerythritol esters and three (2,4- di-tert-butyls
Base) phosphite ester by weight 1:1 mixes.
Preparation method:
1) raw material for standby is weighed according to proportioning, wherein when first drying 3 is small at 130 DEG C by PA66 resins, controls moisture content
In below 0.03wt%, it is for use to obtain drying composite;
2) drying composite of step 1) with other raw materials in addition to glass fibre is uniformly mixed, is mixed
Object A;
3) the mixture A of step 2) is added in double screw extruder, while melting extrusion, in double screw extruder
Exhaust outlet adds in glass fibre, through frit reaction, extruding pelletization.
Wherein, the process conditions of double screw extruder are:One area's temperature:180 DEG C, two area's temperature:250 DEG C, three area's temperature:
240 DEG C, four area's temperature:230 DEG C, five area's temperature:210 DEG C, six area's temperature:210 DEG C, seven area's temperature:200 DEG C, eight area's temperature:
200 DEG C, nine area's temperature:220 DEG C, head temperature:240℃;Vacuum degree 0.05MP, screw speed:300r/min;Feeding rotating speed:
10r/min。
Embodiment 2
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642%, high molecular weight brominated epoxy resin 18%, antimony oxide 2%, nanoscale talcum powder 5%, poly- second
Alkene grafted maleic anhydride 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, ethylene are double hard
Acyl amine 1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic esters]
Pentaerythritol ester and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method:
1) raw material for standby is weighed according to proportioning, wherein first by PA66 resins, PET resin, nanoscale talcum powder at 110 DEG C
It is dry 5 it is small when, it is for use to obtain drying composite in below 0.03wt% for control moisture content;
2) drying composite of step 1) with other raw materials in addition to glass fibre is uniformly mixed, is mixed
Object A;
3) the mixture A of step 2) is added in double screw extruder, while melting extrusion, in double screw extruder
Exhaust outlet adds in glass fibre, through frit reaction, extruding pelletization.
Wherein, the process conditions of double screw extruder are:One area's temperature:200 DEG C, two area's temperature:260 DEG C, three area's temperature:
250 DEG C, four area's temperature:240 DEG C, five area's temperature:220 DEG C, six area's temperature:220 DEG C, seven area's temperature:210 DEG C, eight area's temperature:
210 DEG C, nine area's temperature:230 DEG C, head temperature:260℃;Vacuum degree 0.15MP, screw speed:500r/min;Feeding rotating speed:
30r/min。
Embodiment 3
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642%, brominated Polystyrene 18%, antimony oxide 2%, nanoscale talcum powder 5%, maleic anhydride grafting
SEBS 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, polysiloxanes 1.0% and glass
Glass fiber 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] pentaerythritol esters and three
(2,4- di-tert-butyl-phenyls) phosphite ester is by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 1, the difference is that raw material and content are different.
Embodiment 4
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642%, decabromodiphenylethane 18%, antimony oxide 2%, nanoscale talcum powder 5%, maleic anhydride grafting
SEBS 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, ethylene bis stearamide
1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] Ji Wusi
Alcohol ester and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 2, the difference is that raw material and content are different.
Embodiment 5
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642%, high molecular weight brominated epoxy resin 18%, antimony oxide 2%, nano mica powder 5%, Malaysia
Acid anhydrides Maleated SEBS 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, ethylene are double stearic
Amide 1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] seasons
Doutrate and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 1, the difference is that raw material and content are different.
Embodiment 6
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642%, high molecular weight brominated epoxy resin 18%, antimony oxide 2%, nanometer glass microballon 5%, horse
Maleic anhydride grafted SEBS 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, ethylene are double hard
Acyl amine 1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic esters]
Pentaerythritol ester and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 1, the difference is that raw material and content are different.
Embodiment 7
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6642.5%, high molecular weight brominated epoxy resin 18%, antimony oxide 1.5%, nano mica powder 10%,
Maleic anhydride-g-SBS 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 0%, antioxidant 0.5%, ethylene are double
Stearmide 1.0% and glass fibre 23%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic acid
Ester] pentaerythritol ester and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 2, the difference is that raw material and content are different.
Embodiment 8
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6637%, high molecular weight brominated epoxy resin 18%, antimony oxide 2%, nano mica powder 5%, POE connect
Branch maleic anhydride 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 5%, antioxidant 0.5%, ethylene stearic bicine diester
Amine 1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] seasons penta
Four alcohol esters and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 2, the difference is that raw material and content are different.
Embodiment 9
A kind of fire-retardant Nylon 66 composite material, calculates according to weight percent, including following raw material:
PA6632%, high molecular weight brominated epoxy resin 18%, antimony oxide 2%, nano mica powder 5%, POE connect
Branch maleic anhydride 3%, gamma-aminopropyl-triethoxy-silane 0.5%, PET resin 10%, antioxidant 0.5%, ethylene stearic bicine diester
Amine 1.0% and glass fibre 28%.Antioxidant is by four [methyl-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] seasons penta
Four alcohol esters and three (2,4- di-tert-butyl-phenyls) phosphite esters are by weight 1:1 mixes.
Preparation method is substantially the same manner as Example 2, the difference is that raw material and content are different.
Test example
When by the particle for completing to be granulated in embodiment 1-9, drying 3~4 is small in 110~120 DEG C of convection oven, then will
Dried particle is molded sample preparation in 80T injection grades, and injection temperature and injection pressure are consistent in sample making course, and mould temperature is kept to exist
Between 80~100 DEG C, the batten non-trimming of making carries out performance measurement, the results are shown in Table 1.
Wherein, tensile strength and elongation at break are tested by 1040 standards of GB/T.Specimen types be I types, batten ruler
Very little (mm):165 (length) × (13 ± 0.2) (end portion width) × (3.2 ± 0.2) (thickness), tensile speed 50mm/min.Bending is strong
Degree and bending modulus are tested by 9341 standards of GB/T.Specimen size (mm):(64±2)×(12.7±0.2)×(3.2±
0.2) rate of bending is 2mm/min.Notch impact strength is tested by 1043 standards of GB/T, sample be I types, specimen size
(mm):(64±2)×(12.7±0.2)×(3.2±0.2);Notch type is A classes.Flame retardant property presses UL94 standard testings.It sticks up
Song deformation determination method:Disk is molded by DIN16901, specification is 100mm × 100mm × 3.2mm, and 3.2mm thickness disks are placed in
In horizontal table top, place 24H after visually its buckling deformation degree and place 15 days after see buckling deformation.
The measurement result of the fire-retardant Nylon 66 composite material of 1 embodiment 1-9 of table
Continued 1
From 1 test data of table, using filling-modified and alloy modification, flame-retardant PA 66 composite material can be reduced
Buckling deformation keeps good dimensional stability, but can lower the mechanical property of material for a long time.The present invention uses macromolecule
It measures brominated epoxy, proper amount of nano grade mica powder and suitable PET to be modified, solves the buckling deformation of flame-retardant PA 66 composite material
While, ensure that the mechanical properties such as material notch impact strength, tensile strength, bending strength meet the requirement of client, cost performance
It is high.Preferable additionally, due to the high molecular weight brominated epoxy resin mobility used, so during Injection moulded part, material flowability is good,
It is easily molded, production efficiency can be improved, there is higher competitive advantage on the market.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
With within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention god.
Claims (10)
1. a kind of fire-retardant Nylon 66 composite material, which is characterized in that calculated according to weight percent, including following raw material:
PA66 30~45%, bromide fire retardant 15~20%, antimony oxide 2~6%, nanoscale mineral filler 0~10%,
Toughening compatilizer 2~5%, silane coupling agent 0.3~1.0%, PET resin 0~10%, antioxidant 0.5~1.0%, lubricant
0.5~1.0% and glass fibre 25~30%.
2. fire-retardant Nylon 66 composite material according to claim 1, which is characterized in that calculate, wrap according to weight percent
Include following raw material:
PA66 32%, bromide fire retardant 18%, antimony oxide 2%, nanoscale mineral filler 5%, toughening compatilizer 3%, silicon
Alkane coupling agent 0.5%, PET resin 10%, antioxidant 0.5%, lubricant 1.0% and glass fibre 28%.
3. fire-retardant Nylon 66 composite material according to claim 1 or 2, which is characterized in that the viscosity of the PA66 is 2.4
~2.8dl/g, the viscosity of PET resin is 0.68~1.30dl/g.
4. fire-retardant Nylon 66 composite material according to claim 1 or 2, which is characterized in that the bromide fire retardant is selected from
One or more in brominated Polystyrene, decabromodiphenylethane and high molecular weight brominated epoxy resin, the nanoscale ore deposit
Object filler is the one or more in nanoscale talcum powder, nano mica powder and nanometer glass microballon.
5. fire-retardant Nylon 66 composite material according to claim 4, which is characterized in that the bromide fire retardant is macromolecule
Brominated epoxy resin is measured, the nanoscale mineral filler is nano mica powder.
6. fire-retardant Nylon 66 composite material according to claim 1 or 2, which is characterized in that the toughening compatilizer is selected from
POE grafted maleic anhydrides, Research of Grafting Malaic Anhydride Onto Polyethylene, ethylene butyl acrylate, ethylene acrylic acid co polymer, maleic anhydride connect
One or more in branch SEBS.
7. fire-retardant Nylon 66 composite material according to claim 1 or 2, which is characterized in that the antioxidant is by four [first
Base-b- (3,5- di-tert-butyl-hydroxy phenyls) propionic ester] pentaerythritol ester and three (2,4- di-tert-butyl-phenyls) phosphite esters
By weight 1:1 mixes.
8. fire-retardant Nylon 66 composite material according to claim 1 or 2, which is characterized in that the lubricant is poly- silica
One or more in alkane and ethylene bis stearamide.
9. the preparation method of the fire-retardant Nylon 66 composite material as described in claim 1 to 8 any one, which is characterized in that bag
Include following steps:
1) raw material for standby is weighed according to proportioning, wherein first PA66 resins, PET resin, nanoscale mineral filler are dried, controlled
It is for use to obtain drying composite in below 0.03wt% for moisture content processed;
2) drying composite of step 1) with other raw materials in addition to glass fibre is uniformly mixed, obtains mixture A;
3) the mixture A of step 2) is added in double screw extruder, while melting extrusion, in the exhaust of double screw extruder
Mouth adds in glass fibre, through frit reaction, extruding pelletization.
10. the preparation method of fire-retardant Nylon 66 composite material according to claim 9, which is characterized in that the step 1)
Drying means be at 110~130 DEG C it is dry 3~5 it is small when;The process conditions of double screw extruder are:One area's temperature:180
~200 DEG C, two area's temperature:250~260 DEG C, three area's temperature:240~250 DEG C, four area's temperature:230~240 DEG C, five area's temperature:
210~220 DEG C, six area's temperature:210~220 DEG C, seven area's temperature:200~210 DEG C, eight area's temperature:200~210 DEG C, nine area's temperature
Degree:220~230 DEG C, head temperature:240~260 DEG C;0.05~0.15MP of vacuum degree, screw speed:300~500r/min;
Feeding rotating speed:10~30r/min.
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