CN106433111B - A kind of PA/AS base resin complexes and preparation method thereof - Google Patents
A kind of PA/AS base resin complexes 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
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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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
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention discloses a kind of PA/AS base resin complexes, including 30-70 parts of PA resin, 5-60 parts of AS base resin, 0.1-2 parts of pigment, 2-10 parts of compatilizer, 0.05-0.5 parts of antioxidant, 0.1-0.6 parts of nucleating agent；The pigment is carbon black, and the quality of the metallic element contained in the carbon black accounts for the 0.001-1% of the carbon black mass.The invention also discloses a kind of preparation methods of PA/AS base resin complexes.Compared with prior art, PA/AS base resin complexes of the present invention has good weather resistance, and it will not make appearance color vary widely because carbon black weatherable is precipitated.
Description
Technical field
The present invention relates to polymeric material field, in particular to a kind of PA/AS base resin complexes and preparation method thereof.
Background technique
Polyamide (PA) has excellent mechanical performance, self-lubrication, chemical-resistant, workability, heat oxygen aging resistance
Performance makes them be usually used in the machinery harsher to operating environment requirements, electronic apparatus, motor vehicle industry, but also there are many
Disadvantage, such as the defect that water imbibition is big, poor dimensional stability, dry state and low temperature impact strength are low, and its melt viscosity is big, note
Salivation is easily caused when being moulded into type.And PA and AS base resin are mixed with compound, both obtain PA high heat resistance, high intensity, Gao Gang
Property, with the characteristic of chemicals-resistant, and toughness, the dimensional stability of PA can be improved by AS base resin, this kind of composite materials are suitable
For industries such as machinery, electronic apparatus, electric tool, motor vehicle, buildings.
But currently in order to the weather resistance of enhancing PA/AS base resin complexes, it is common practice to carbon black be added to rise
To shielding ultraviolet rays luminous energy, but this shielding action only plays a protective role to material internal, can not protection materials appearance
It is not influenced by ultraviolet radiation.Meanwhile the concentration of the impurity content and carbon black of carbon black in the material is higher, when material surface is by oxygen
After changing degradation generation dusting, exposed content of carbon black is higher, and the variation of the color change and gray scale of material appearance is got over
Greatly.Such material is not suitable for the demanding material application of appearance, and such as outdoor tool, exposes outdoor build at auto parts
Build material etc..
Summary of the invention
The purpose of the present invention is exactly to solve the above-mentioned problems and provides a kind of PA/AS base resin complexes, this is compound
Object have good weather resistance, and its will not because of carbon black addition and appearance color is varied widely.
Another object of the present invention, which also resides in, provides a kind of preparation method of PA/AS base resin complexes.
To achieve the above object, technical solution of the present invention is implemented as follows:
A kind of PA/AS base resin complexes, including following components and its parts by weight:
The pigment is carbon black, and the quality of the metallic element contained in the carbon black accounts for the 0.001- of the carbon black mass
1%.
Preferably, the metallic element is at least one of aluminium, boron, cobalt, copper, manganese, nickel, tin, zinc and iron.
Preferably, the quality of the metallic element accounts for the 0.001-0.1% of the carbon black mass.
Preferably, the PA resin is PA6 resin；The relative viscosity of the PA6 resin is 2.0-3.0, and the PA6 tree
The molar concentration of amino is higher than the molar concentration of carboxyl in rouge.Viscosity is greater than 3.0, is unfavorable for PA6 and AS base resin is realized well
Dispersion, compatilizer reacts to form PA6 graft copolymer by the end group with PA6, reduces the interface of PA6 and AS base resin
Power realizes having complementary functions for two kinds of resins, therefore the concentration of PA6 end group influences compatible role, therefore selects relatively low viscosity
PA6 be conducive to improve compatible role.
Preferably, the AS base resin is styrene-acrylonitrile copolymer, styrene-acrylonitrile-acrylic ester copolymer
At least one of object and styrene-acrylonitrile-butadiene copolymer.It is furthermore preferred that the AS base resin is styrene-
Acrylonitrile-acrylate copolymer.Wherein, the styrene-acrylonitrile-acrylate copolymer and styrene-acrylonitrile-fourth
Diene copolymers have the rubber phase not less than 10%, it is preferred that rubber-phase content 30-70%.
Preferably, the compatilizer is the styrene-acrylonitrile copolymer AS-g-MAH of maleic anhydride grafting, maleic anhydride
At least one of styrene-acrylonitrile-butadiene ABS-g-MAH and styrene-maleimide copolymer of grafting.
Preferably, the antioxidant is Hinered phenols antioxidant, phosphite ester antioxidant, thioether kind antioxidant and Duo Fang
At least one of fragrant amine antioxidants.
It is furthermore preferred that the hindered phenol be 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane (CAS:
1843-03-4), 1,3,5- tri- (3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid (CAS:27676-62-6), 4,4'- are sub-
Butyl bis- (6- tert-butyl-m-cresol) (CAS:85-60-9), the positive octadecanol of β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid
Ester (CAS:2082-79-3), four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (CAS:6683-19-
8), bis- [1,1- dimethyl -2- [(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyl) propionyloxy] the ethyl] -2,4,8,10- of 3,9-
Four oxaspiros [5.5] hendecane (CAS:90498-90-1) and (3,5- di-t-butyl -4- hydroxyl of 1,3,5- trimethyl -2,4,6- three
At least one of base benzyl) benzene (CAS:1709-70-2)；The phosphite ester is double octadecyl pentaerythrite diphosphites
Ester (CAS:3806-34-6), bis- (2,6- di-t-butyl -4- aminomethyl phenyl) pentaerythritol diphosphate (CAS:80693-00-
1), 2-2 '-di-2-ethylhexylphosphine oxide (4,6- dibutyl-benzyl) -2- ethylhexyl phosphite ester (CAS:126050-54-2), phosphorous acid
Three (2,4- di-tert-butyl-phenyl) esters (CAS:31570-04-4), trisnonyl phenyl phosphite (CAS:26523-78-4) and 4,
At least one of split isopropyl diphenyl base C12-15- alcohol phosphite ester (CAS:96152-48-6) of 4'-；The thioesters is season
Penta tetrol four (3- lauryl thiopropionate) (CAS:29598-76-3)；More aromatic amines are bis- (propyloxy phenyl of 4,4'-
Base) diphenylamines (CAS:10081-67-1).
Preferably, the nucleating agent is at least one in inorganic nucleator and organic nucleating agent of the grain diameter less than 1 μm
Kind；The inorganic nucleator is at least one of talcum powder, montmorillonite and calcium carbonate；The organic nucleating agent is benzoic acid
At least one of sodium, sorbierite dibenzyl ester and carboxylic acid sodium salt.
The present invention also provides a kind of preparation methods of PA/AS base resin complexes, including following preparation step:
Step 1: prepare raw material according to following components and its parts by weight: 30-70 parts of PA resin, 5-60 parts of AS base resin,
0.1-2 parts of pigment, 2-10 parts of compatilizer, 0.05-0.5 parts of antioxidant, 0.1-0.6 parts of nucleating agent；
Step 2: by the dry 0-0.15% for accounting for PA resin quality to the quality of moisture of PA resin in step 1；
Step 3: the PA resin after will be dry in step 2, AS base resin, pigment, compatilizer, nucleating agent in step 1 and
It after antioxidant mixing, puts into double screw extruder, melting extrusion, while through supercooling and granulation, that is, obtaining PA/ of the invention
AS base resin complexes；
The double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Beneficial effects of the present invention are as follows:
PA/AS base resin complexes of the invention, by the way that pigment selection is optimized, compared to conventional carbon black and organic
Mineral black, hence it is evident that improve the weather resistance of PA/AS base resin complexes.First aspect, pigment carbon black of the invention is in dosage
On carried out stringent control, reduce material appearance after dusting occurs for material surface oxidative degradation color change and ash
The variation of degree.The second aspect joined metallic element in pigment carbon black of the invention, and it is multiple that this significantly improves PA/AS base resin
The weather resistance of object is closed, meanwhile, metallic element is also reduced to a certain extent after the generation dusting of material surface oxidative degradation
The variation of the color change and gray scale of material appearance.The present invention has widened the application of PA/AS base resin complexes, can be by it
It is widely used in the application field in the polyamide modified material of tradition, especially automobile, electronic apparatus, construction equipment, outdoor work
The industry fields such as tool.
Specific embodiment
Below in conjunction with embodiment, the invention will be further described.
Comparative example and embodiment see the table below using the manufacturer and model of raw material:
Note: acetylene black, Organic Black in upper table do not contain metallic element, and metal member in the carbon black A of model N330
The quality of element accounts for the 0.001-1% of carbon black A gross mass, and the quality of metallic element accounts for black B in the black B of model Raven M
The 0.001-0.1% of gross mass.The metallic element contains at least one of aluminium, boron, cobalt.
The preparation method of comparative example 1-3 and embodiment 1-3 are as described below, can further illustrate this by these examples
Compared with prior art, the mechanical performance of PA/AS base resin complexes obtained is more excellent for invention.
Comparative example 1
Step 1: according to following components and its parts by weight preparation raw material: 62kgPA6,31kgASA, 0.1kg talcum powder,
0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by PA6, ASA, talcum powder, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) fourth in step 1
It after alkane mixing, puts into double screw extruder, melting extrusion, while through supercooling and granulation, that is, obtaining the product of comparative example 1.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Comparative example 2
Step 1: according to following components and its parts by weight preparation raw material: 83kgPA6,10kgASA, 1kg acetylene black,
0.1kg talcum powder, 0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by PA6, ASA, acetylene black, the talcum powder, (2- methyl -4- hydroxyl -5- tert-butyl of 1,1,3- tri- in step 1
Phenyl) after butane mixing, put into double screw extruder, melting extrusion, while through supercooling and granulation, i.e. acquisition comparative example 2
Product.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Comparative example 3
Step 1: according to following components and its parts by weight preparation raw material: 83kgPA6,10kgASA, 1kg Organic Black,
0.1kg talcum powder, 0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by PA6, ASA, Organic Black, the talcum powder, (2- methyl -4- hydroxyl -5- tert-butyl of 1,1,3- tri- in step 1
Phenyl) after butane mixing, put into double screw extruder, melting extrusion, while through supercooling and granulation, i.e. acquisition comparative example 3
Product.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Embodiment 1
Step 1: preparing raw material: 62kgPA6,31kgASA, 1kg carbon black A, 0.1kg according to following components and its parts by weight
Talcum powder, 0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by the dry 0-0.15% for accounting for PA6 resin quality to the quality of moisture of PA6 resin in step 1；
Step 3: the PA6 after will be dry in step 2, ASA, carbon black A, talcum powder, 1 in step 1,1,3- tri- (2- methyl-
4- hydroxyl -5- tert-butyl-phenyl) after butane mixing, put into double screw extruder, melting extrusion, while through supercooling and making
Grain obtains the product of embodiment 1.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Embodiment 2
Step 1: preparing raw material: 62kgPA6,31kgASA, 1kg black B, 0.1kg according to following components and its parts by weight
Talcum powder, 0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by the dry 0-0.15% for accounting for PA6 resin quality to the quality of moisture of PA6 resin in step 1；
Step 3: the PA6 after will be dry in step 2, ASA, black B, talcum powder, 1 in step 1,1,3- tri- (2- methyl-
4- hydroxyl -5- tert-butyl-phenyl) after butane mixing, put into double screw extruder, melting extrusion, while through supercooling and making
Grain obtains the product of embodiment 2.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Embodiment 3
Step 1: according to following components and its parts by weight preparation raw material: 62kgPA6,31kgASA, 0.5kg carbon black A,
0.5kg black B, 0.1kg talcum powder, 0.05kg1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane；
Step 2: by the dry 0-0.15% for accounting for PA6 resin quality to the quality of moisture of PA6 resin in step 1；
Step 3: the PA6 after will be dry in step 2, ASA, carbon black A, black B, talcum powder, 1 in step 1,1,3- tri-
After the mixing of (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane, put into double screw extruder, melting extrusion, while through being subcooled
But it and is granulated, that is, obtains the product of embodiment 3.
Wherein, double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, and three
230 DEG C of area's temperature, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature
245 DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
Weather resistance assessment:
Material is molded as to the sheet material of 70mm*50mm*3mm, according to American Automobile Association standard SAEJ2527 speeding-up simulation
The weather resistance of outdoor aging test evaluation material, a length of 1900h when always irradiating；The chromatic aberration before and after aging is assessed, is denoted as
ΔE.Δ E value is smaller, and the weather resistance of material is higher.Gray scale is adopted international standards I SO105/A03-1993, basic gray card etc.
Grade amounts to 9 grades of gray cards, at standard sources D65, the gray scale etc. of the sheet material before sheet material and aging after judging aging containing 1-5
Grade, gray scale is smaller, and the variation for representing appearance is more serious.
Above embodiments are used for illustrative purposes only, rather than limitation of the present invention, the technology people in relation to technical field
Member, without departing from the spirit and scope of the present invention, can also make various transformation or modification, therefore all equivalent
Technical solution also should belong to scope of the invention, should be limited by each claim.
Claims (5)
1. a kind of PA/AS base resin complexes, which is characterized in that including following components and its parts by weight:
The pigment is carbon black, and the quality of the metallic element contained in the carbon black accounts for the 0.001-1% of the carbon black mass；
The metallic element is at least one of aluminium, boron, cobalt, copper, manganese, nickel, tin, zinc and iron；
The antioxidant is Hinered phenols antioxidant, phosphite ester antioxidant, thioether kind antioxidant and more aromatic amine antioxygens
At least one of agent；
The Hinered phenols antioxidant is 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyl) butane, 1,3,5- tri-
(3,5- di-tert-butyl-4-hydroxyl benzyl) isocyanuric acid, 4,4' butylidene biss (6- tert-butyl-m-cresol), β-(the tertiary fourth of 3,5- bis-
Base -4- hydroxy phenyl) propionic acid n-octadecyl alcohol ester, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters,
Bis- four oxygen of [1,1- dimethyl -2- [(3- tertiary butyl-4-hydroxy -5- aminomethyl phenyl) propionyloxy] ethyl] -2,4,8,10- of 3,9-
At least one in miscellaneous spiral shell [5.5] hendecane and 1,3,5- trimethyl -2,4,6- three (3,5- di-tert-butyl-4-hydroxyl benzyl) benzene
Kind；The phosphite ester antioxidant is distearyl pentaerythritol diphosphite, bis- (2,6- di-t-butyl -4- methyl
Phenyl) pentaerythritol diphosphate, 2-2 '-di-2-ethylhexylphosphine oxide (4,6- dibutyl-benzyl) -2- ethylhexyl phosphite ester, phosphorous
Sour three (2,4- di-tert-butyl-phenyl) esters, trisnonyl phenyl phosphite and the split isopropyl diphenyl base C12-15- alcohol of 4,4'- are sub-
At least one of phosphate；The sulphur ester antioxidant is pentaerythrite four (3- lauryl thiopropionate)；It is described mostly fragrant
Fragrant amine antioxidants are 4,4'- bis- (propyloxy phenyl base) diphenylamines；
The nucleating agent is at least one of inorganic nucleator of the grain diameter less than 1 μm and organic nucleating agent；It is described inorganic
Nucleating agent is at least one of talcum powder, montmorillonite and calcium carbonate；The organic nucleating agent is carboxylic acid sodium salt and sorbierite two
At least one of benzyl ester.
2. a kind of PA/AS base resin complexes as described in claim 1, which is characterized in that the PA resin is PA6 resin；
The relative viscosity of the PA6 resin is 2.0-3.0, and the molar concentration of amino is higher than the mole dense of carboxyl in the PA6 resin
Degree.
3. a kind of PA/AS base resin complexes as described in claim 1, which is characterized in that the AS base resin is styrene-
In acrylonitrile copolymer, styrene-acrylonitrile-acrylate copolymer and styrene-acrylonitrile-butadiene copolymer extremely
Few one kind.
4. a kind of PA/AS base resin complexes as described in claim 1, which is characterized in that the compatilizer is maleic anhydride
The styrene-acrylonitrile-butadiene ABS-g- that styrene-acrylonitrile copolymer AS-g-MAH, the maleic anhydride of grafting are grafted
At least one of MAH and styrene-maleimide copolymer.
5. a kind of preparation method of PA/AS base resin complexes as described in claim 1, which is characterized in that including following system
Standby step:
Step 1: preparing raw material: 30-70 parts of PA resin, 5-60 parts of AS base resin, pigment according to following components and its parts by weight
0.1-2 parts, 2-10 parts of compatilizer, 0.05-0.5 parts of antioxidant, 0.1-0.6 parts of nucleating agent；
Step 2: by the dry 0-0.15% for accounting for PA resin quality to the quality of moisture of PA resin in step 1；
Step 3: the PA resin after will be dry in step 2, AS base resin, pigment, compatilizer, nucleating agent and antioxygen in step 1
After agent mixing, put into double screw extruder, melting extrusion, while through supercooling and granulation；
The double screw extruder is divided into 9th area, each area's temperature are as follows: 230 DEG C of area's temperature, two 230 DEG C of area's temperature, three area's temperature
230 DEG C of degree, four 230 DEG C of area's temperature, five 230 DEG C of area's temperature, six 240 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature 245
DEG C, nine 250 DEG C of area's temperature；250 revs/min of engine speed.
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| CN103044847A (en) * | 2012-12-30 | 2013-04-17 | 苏州旭光聚合物有限公司 | ABS (Acrylonitrile Butadiene Styrene) composite material and preparation method thereof |
| CN103205112A (en) * | 2013-04-28 | 2013-07-17 | 常熟市筑紫机械有限公司 | ABS (Acrylonitrile Butadiene Styrene) toughened flame-retarded polyamide composite material |
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| CN103044847A (en) * | 2012-12-30 | 2013-04-17 | 苏州旭光聚合物有限公司 | ABS (Acrylonitrile Butadiene Styrene) composite material and preparation method thereof |
| CN103205112A (en) * | 2013-04-28 | 2013-07-17 | 常熟市筑紫机械有限公司 | ABS (Acrylonitrile Butadiene Styrene) toughened flame-retarded polyamide composite material |
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