CN101787204A - Low water absorption polyamide composite and preparation method thereof - Google Patents
Low water absorption polyamide composite and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a low water absorption polyamide composite and preparation method thereof. 10-90 parts by weight of polyamide and 3-10 parts by weight of phyllo-silicate clay and less than 2 parts by weight of additive are placed into a high speed mixer to be premixed for 20min and then are added into a double screw extrusion machine, and conveying, melting, cutting, extrusion, cooling and granulation are carried out, thus obtaining polyamide/phyllo-silicate master batch, then the polyamide/phyllo-silicate master batch, 10-60 parts by weight of styrene resin, 2-10 parts by weight of compatilizer and 5-20 parts by weight of short glass fiber are placed into the high speed mixer to be premixed for 20min, temperature is controlled to be 40-60 DEG C, and finally extrusion granulation is carried out in the double screw extrusion machine, thus obtaining the low water absorption polyamide composite. Compared with prior art, the invention has the advantages of solvent resistance, high tenacity and easy processability of polyamide and the advantage of low water absorption of ABS resin; besides, phyllo-silicate clay speeds up crystallization of nylon, degree of crystallization and mechanical strength are improved, extremely low water absorption is obtained, and size stability is greatly improved while impact toughness is maintained.
Description
Technical field
The present invention relates to a kind of composition and method of making the same, especially relate to a kind of low water absorption polyamide composite and preparation method thereof.
Background technology
Polymeric amide (becomes nylon usually, english abbreviation is PA) be output maximum in the five big general engineering plastic, kind at most, the base resin of the widest, the high comprehensive performance of purposes, it has high strength, high tenacity, anti-solvent, wear-resisting, self-lubricating property that melt viscosity is low and good
Polymeric amide is to contain polar-NH-CO-key in the macromolecular chain, and easy and water molecules forms hydrogen bond, and this has just caused the PA water-intake rate bigger, and the dimensional stability of goods is relatively poor.To having done extensive studies in the water-absorbent document of nylon and the patent, and the effective way of improving has been proposed.
Improving its absorptive method by the PA alloying is widely known by the people.As the PA/HDPE alloy organic solvent is had good barrier, a lot of countries make drive-up mailbox with this alloy; The molding shrinkage of PPO is 0.007～0.009, adds a little P PO and can obtain shrinking percentage less than 1.0% alloy material in PA; The PA/ABS alloy has super toughness, high workability and anti-warpage properties, is widely used in automobile, household electrical appliances and sports goods industry.
By fiber reinforcement and mineral-filled nylon is to obtain the valid approach of low water absorbable nylon.In the European patent 07002642.2, the contriver is by filling short cutting or fibrae circulares at PA, the water-intake rate of nylon is reduced to below 1%, but because the fiber addition is 30%～50%, improving the absorptive toughness that greatly reduces material simultaneously, and product surface is coarse, and gloss is relatively poor, has limited use range; Among the Chinese patent CN101314674A, the contriver fills by the preparation talcum powder and has obtained shrinking percentage less than 0.5% nylon composite, but the contriver does not study the mechanical property of material; Among the Te Kaiping JP 150275/01, the contriver is by selecting matrix resin, adding glass fibre in semi-aromatic and fatty polyamide blend strengthens, high-dimensional stability, solvent resistance and the good daiamid composition of anti-steam have been obtained, same because glass fibre addition is up to 50%, and the toughness of material significantly descends.
From the above mentioned, the nylon that exploitation dimensional stability and toughness have both has great importance and vast market prospect, as to the higher automotive upholstery of dimension precision requirement, sports equipment and Communication Equipment shell etc.
Summary of the invention
Purpose of the present invention is exactly to provide low water absorption polyamide composite of a kind of water-absorbent height, good stability and preparation method thereof for the defective that overcomes above-mentioned prior art existence.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of low water absorption polyamide composite is characterized in that, said composition comprises following component and weight part content:
Polymeric amide 40-90;
Styrene resin 10-60;
Compatilizer 2-10;
Layered silicate clay 3-10;
Short glass fiber 5-20;
Additive is less than 2.
The preferred 50-80 of described polymeric amide weight part content, more preferably 65, the preferred 30-50 of styrene resin weight part content, more preferably 35, the preferred 5-10 of weight part content of compatilizer, the preferred 4-8 of weight part content of layered silicate clay, the preferred 10-15 of weight part content of short glass fiber.
Described polymeric amide comprises nylon 6, nylon 66 or nylon 46, and polymeric amide is at 20 ℃, and wt% is that the relative viscosity that records in 2% the meta-cresol solvent is 1.5-3.0, and preferred relative viscosity is the polymeric amide of 1.8-2.5.
Described styrene resin comprises the styrene-acrylonitrile copolymer of styrene-acrylonitrile copolymer or modified rubber, one or more in preferred acrylonitritrile-styrene resin, acrylonitrile-styrene-butadienecopolymer, acrylonitrile-styrene-acrylic rubber multipolymer, the vinyl cyanide-terpolymer EP rubber-styrol copolymer.
The content of rubber is 0-65% (wt%) in the described styrene resin, and melting index is 10-60g/10min, preferred 15-35g/10min.
Described compatilizer contains the group that can carry out chemical reaction with polymeric amide, and this group comprises one or more in maleic anhydride, methyl propenoic acid glycidyl ether, the acrylic or methacrylic acid.
Described compatilizer comprises reactive group and styrene base resin or ethylene propylene diene monomer graft polymer, one or more in optimization styrene-maleic anhydride, acrylonitrile-styrene-methyl propenoic acid glycidyl ether, acrylonitrile-styrene-butadiene-acrylic acid, terpolymer EP rubber-maleic anhydride or the acrylonitrile-styrene-methacrylic acid.
The percentage of grafting of described reactive group is 2-20%, preferred 6-18%.
Described layered silicate clay comprises one or more in polynite, talcum powder, the kaolin, and particle diameter is the 1000-4000 order, preferred 1500-2500 purpose nano imvite.
Described talcum powder is handled through silane coupling agent, and polynite is through the intercalator modification, and intercalator comprises the amino hexadecanoic acid ammonium salt of 14-, the amino hexadecanoic acid ammonium salt of 16-or the amino hexadecanoic acid ammonium salt of 18-.
Described short glass fiber is the alkali-free short glass fiber, and the surface is through silane coupling agent γ-aminopropyl three ethoxy silane treatment, and length-to-diameter ratio is greater than 10.
Described additive comprises oxidation inhibitor, lubricant, described oxidation inhibitor comprises one or more among commercial anti oxygen agent Irganox1010, Irganox 1076, the Irganox 168, and described lubricant comprises one or more in silicone oil, fatty acid amide, barium stearate, Magnesium Stearate, paraffin, polyethylene wax or the ethylene bis stearic acid amide.
A kind of preparation method of low water absorption polyamide composite is characterized in that, this method may further comprise the steps:
(1) according to following component and weight part content batching:
Polymeric amide 40-90;
Styrene resin 10-60;
Compatilizer 2-10;
Layered silicate clay 3-10;
Short glass fiber 5-20;
Additive is less than 2;
(2) polymeric amide, layered silicate clay and additive are placed high-speed mixer premix 20min, temperature is controlled at 40-60 ℃;
(3) raw material that obtains in the step (2) is joined in the twin screw extruder, extrude cooling granulation, obtain the polyamide/laminated silicate master batch by conveying, fusion, shearing;
(4) polyamide/laminated silicate master batch and component styrene resin, compatilizer and the short glass fiber that obtains in the step (3) placed high-speed mixer premix 20min, temperature is controlled at 40-60 ℃, (3) described method adds extruding pelletization in the twin screw extruder more set by step, prepares the daiamid composition of low water absorption.
The length-to-diameter ratio of twin screw extruder is not less than 30 in the described step (3), and temperature regulating device that has and vacuum extractor, material are melted in the twin screw extruder fully, and screw speed is 200-400rpm.
Compared with prior art, the present invention has had both the characteristics of the low water absorbable of polymeric amide solvent resistance, high tenacity, workability and ABS resin; Layered silicate clay has been accelerated the crystallization velocity of nylon in addition, degree of crystallinity and physical strength have been improved, the adding of layered silicate simultaneously makes glass fibre just can make material obtain extremely low water-intake rate at lower loading level, has improved the dimensional stability of material greatly and has kept impelling strength obviously not descend; The present invention can directly process by injection moulding or other forming methods, is applicable to the occasions higher to dimension precision requirement such as making automotive upholstery, Communication Equipment shell, panel board, heat radiation grid, flow deflector or sports equipment.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
Choose the polymeric amide based on nylon 6 (PA6) of Ube, fusing point is 225-230 ℃, and limiting viscosity is 2.52g/dL, water-intake rate 1.8 (23 ℃, 50%RH) and 10.7 (23 ℃, 100%RH), molding shrinkage 1.8%; Styrene butadiene-vinyl cyanide (ABS), commercially available Korea S brocade lake ABS750, melting index 42g/10min, glue content 15%; High glue powder, glue content 60%, melting index 18g/10min; Commercially available compatilizer SMA, the content of maleic anhydride (MAH) is 18%; Layered silicate clay-nano imvite, through the modification of the amino hexadecanoic acid ammonium salt of 16-, particle diameter is 2500 orders, and oxidation inhibitor adopts commercially available oxidation inhibitor Irganox168 and anti-oxidant Irganox 1010, Ciba company refines, and lubricant adopts two ethylene stearylamides (EBS).
Adopt two-step approach to prepare low water absorption polyamide composite:
(1) with the PA6 polymeric amide of 90kg, the EBS of the nano imvite of the amino hexadecanoic acid ammonium salt of the 16-of 8kg intercalation modifying, the anti-oxidant Irganox 168 of 0.8kg and anti-oxidant Irganox 1010,1kg adds premix 20min in the high-speed mixer as additive, temperature is controlled at 50 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200-240 ℃, the rotating speed of forcing machine is controlled at 300rpm, extrude cooling granulation by conveying, fusion, shearing, obtain PA/ nano imvite master batch;
(2) will obtain the high glue powder of ABS, the 23kg of exsiccant PA/ nano imvite master batch 60kg (comprising the PA6 of 55kg and the nano imvite of 5kg), 12kg, the compatilizer SMA of 5kg and the glass fibre of 10kg through above-mentioned steps and be added to premix 20min in the high-speed mixer, temperature is controlled at 50 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200-230 ℃, the rotating speed of forcing machine is controlled at 200rpm, obtains the daiamid composition of low water absorption.
Comparative Examples 1
The lubricant EBS of the anti-oxidant Irganox 168 of compatilizer SMA, the 0.8kg of the high glue powder of ABS, the 23kg of PA6, the 12kg of 60kg, 5kg, 1kg and anti-oxidant Irganox 1010 are added after high-speed mixers mix, by twin screw extruder blend granulation, temperature is controlled at 200-230 ℃, rotating speed is controlled to be 200rpm, obtains comparison 1.
Comparative Examples 2
The glass fibre of the lubricant EBS of the anti-oxidant Irganox 168 of compatilizer SMA, the 0.8kg of the high glue powder of ABS, the 23kg of PA6, the 12kg of 60kg, 5kg, 1kg and anti-oxidant Irganox 1010,10kg is added after high-speed mixer mixes, by twin screw extruder blend granulation, temperature is controlled at 200-230 ℃, rotating speed is controlled to be 200rpm, obtains comparison 2.
Comparative Examples 3
The glass fibre of the lubricant EBS of the anti-oxidant Irganox 168 of compatilizer SMA, the 0.8kg of the high glue powder of ABS, the 23kg of PA6, the 12kg of 60kg, 5kg, 1kg and anti-oxidant Irganox 1010,20kg is added after high-speed mixer mixes, by twin screw extruder blend granulation, temperature is controlled at 200-230 ℃, rotating speed is controlled to be 200rpm, obtains comparison 3.
With the daiamid composition of above-mentioned acquisition and comparison in 90 ℃ of dry 2h, again in 230 ℃ of various test bars of injection moulding, according to following standard and method evaluation:
Tensile strength: ISO527, batten size 150*10*4mm, draw speed 50mm/min;
Shock strength: ISO200, batten size 80*10*4;
Water-intake rate: ISO32, the particle that drying is good and 23 ℃ of storage 48h are in 50%RH and the weightening finish of 100RH% specimen, exosyndrome material water-absorbent; Test result is as shown in table 1:
Table 1 test result
Embodiment 2
A kind of preparation method of low water absorption polyamide composite, this method may further comprise the steps:
(1) with the PA46 of 40kg, fusing point is 225-230 ℃, limiting viscosity is 1.5g/dL, (23 ℃ of water-intake rates 1.8,50%RH) and 10.7 (23 ℃, 100%RH), molding shrinkage 1.8%, the talcum powder of the amino hexadecanoic acid ammonium salt of the 16-of 3kg intercalation modifying, particle diameter is 1000 orders, 0.5kg anti-oxidant Irganox 168,0.5kg silicone oil add premix 20min in the high-speed mixer as additive, temperature is controlled at 40 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200 ℃, the rotating speed of forcing machine is controlled at 300rpm, by carrying, fusion, cooling granulation is extruded in shearing, obtains PA/ talcum powder master batch;
(2) will obtain exsiccant PA/ talcum powder 60kg (comprising the PA66 of 40kg and the talcum powder of 3kg) through above-mentioned steps, vinyl cyanide-terpolymer EP rubber of 60kg-styrol copolymer, rubber content 30% (wt%), melting index is 10g/10min, the compatilizer of 2kg, the percentage of grafting of methyl propenoic acid glycidyl ether is 2%, the glass fibre of 5kg is added to premix 20min in the high-speed mixer, temperature is controlled at 50 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200 ℃, the rotating speed of forcing machine is controlled at 200rpm, obtains the daiamid composition of low water absorption.
Embodiment 3
A kind of preparation method of low water absorption polyamide composite, this method may further comprise the steps:
(1) with the PA6 of 90kg, fusing point is 225-230 ℃, limiting viscosity is 1.5g/dL, the nano imvite of the amino hexadecanoic acid ammonium salt of the 18-of 10kg, particle diameter is 1500 orders, 0.5kg the barium stearate of anti-oxidant Irganox 1010,0.5kg add premix 20min in the high-speed mixer as additive, temperature is controlled at 60 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 240 ℃, the rotating speed of forcing machine is controlled at 300rpm, extrudes cooling granulation by conveying, fusion, shearing, obtains PA/ polynite master batch;
(2) will obtain exsiccant PA/ nano imvite 100kg (comprising the PA6 of 90kg and the nano imvite of 10kg) through above-mentioned steps, acrylonitrile-styrene-butadienecopolymer of 10kg, melting index is 60g/10min, the compatilizer of 10kg, methyl propenoic acid glycidyl ether percentage of grafting be 6% and the glass fibre of 20kg be added to premix 20min in the high-speed mixer, temperature is controlled at 60 ℃, glass fibre is the alkali-free short glass fiber, the surface is through silane coupling agent γ-aminopropyl three ethoxy silane treatment, length-to-diameter ratio is greater than 10, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200 ℃, the rotating speed of forcing machine is controlled at 400rpm, obtain the daiamid composition of low water absorption, the length-to-diameter ratio of twin screw extruder is not less than 30, have accurate temperature regulating device and vacuum extractor, material is melted in the twin screw extruder fully.
Embodiment 4
A kind of preparation method of low water absorption polyamide composite, this method may further comprise the steps:
(1) with the PA66 of 50kg, limiting viscosity is 2.5g/dL, the kaolin of the amino hexadecanoic acid ammonium salt of the 16-of 10kg intercalation modifying, the anti-oxidant Irganox 1076 of 1kg, the paraffin of 0.8kg add premix 20min in the high-speed mixer as additive, temperature is controlled at 60 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 240 ℃, the rotating speed of forcing machine is controlled at 200rpm, extrude cooling granulation by conveying, fusion, shearing, obtain PA/ kaolin master batch;
(2) will obtain exsiccant PA/ kaolin 60kg (comprising the PA66 of 50kg and the kaolin of 10kg) through above-mentioned steps, the acrylonitrile-styrene of 50kg-acrylic rubber multipolymer, rubber content is 65% (wt%), melting index is 35g/10min, the compatilizer of 5kg, the percentage of grafting of maleic anhydride be 18% and the glass fibre of 15kg be added to premix 20min in the high-speed mixer, temperature is controlled at 50 ℃, glass fibre is the alkali-free short glass fiber, the surface is through silane coupling agent γ-aminopropyl three ethoxy silane treatment, length-to-diameter ratio is greater than 10, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200 ℃, the rotating speed of forcing machine is controlled at 400rpm, obtain the daiamid composition of low water absorption, the length-to-diameter ratio of twin screw extruder is not less than 30, has accurate temperature regulating device and vacuum extractor, and material is melted in the twin screw extruder fully.
Embodiment 5
A kind of preparation method of low water absorption polyamide composite, this method may further comprise the steps:
(1) with the PA6 of 65kg, limiting viscosity is 2.0g/dL, the nano imvite of the amino hexadecanoic acid ammonium salt of the 16-of 8kg intercalation modifying, the anti-oxidant Irganox 168 of 0.5kg, the silicone oil of 1.2kg add premix 20min in the high-speed mixer as additive, temperature is controlled at 50 ℃, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 240 ℃, the rotating speed of forcing machine is controlled at 200rpm, extrude cooling granulation by conveying, fusion, shearing, obtain PA/ nano imvite master batch;
(2) will obtain exsiccant PA/ nano imvite 60kg (comprising the PA6 of 65kg and the kaolin of 8kg) through above-mentioned steps, acrylonitrile-styrene-butadienecopolymer of 35kg, melting index is 20g/10min, the compatilizer of 5kg, the percentage of grafting of terpolymer EP rubber-maleic anhydride be 12% and the glass fibre of 10kg be added to premix 20min in the high-speed mixer, temperature is controlled at 50 ℃, glass fibre is the alkali-free short glass fiber, the surface is through silane coupling agent γ-aminopropyl three ethoxy silane treatment, length-to-diameter ratio is greater than 10, then with above-mentioned material through twin screw extruder blend granulation, temperature is controlled at 200 ℃, the rotating speed of forcing machine is controlled at 400rpm, obtain the daiamid composition of low water absorption, the length-to-diameter ratio of twin screw extruder is not less than 30, have accurate temperature regulating device and vacuum extractor, material is melted in the twin screw extruder fully.
Claims (14)
1. a low water absorption polyamide composite is characterized in that, said composition comprises following component and weight part content:
Polymeric amide 40-90;
Styrene resin 10-60;
Compatilizer 2-10;
Layered silicate clay 3-10;
Short glass fiber 5-20;
Additive is less than 2.
2. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, the preferred 50-80 of described polymeric amide weight part content, more preferably 65, the preferred 30-50 of styrene resin weight part content, more preferably 35, the preferred 5-10 of weight part content of compatilizer, the preferred 4-8 of weight part content of layered silicate clay, the preferred 10-15 of weight part content of short glass fiber.
3. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described polymeric amide comprises nylon 6, nylon 66 or nylon 46, polymeric amide is at 20 ℃, wt% is that the relative viscosity that records in 2% the meta-cresol solvent is 1.5-3.0, and preferred relative viscosity is the polymeric amide of 1.8-2.5.
4. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described styrene resin comprises the styrene-acrylonitrile copolymer of styrene-acrylonitrile copolymer or modified rubber, one or more in preferred acrylonitritrile-styrene resin, acrylonitrile-styrene-butadienecopolymer, acrylonitrile-styrene-acrylic rubber multipolymer, the vinyl cyanide-terpolymer EP rubber-styrol copolymer.
5. a kind of low water absorption polyamide composite according to claim 1 is characterized in that, the content of rubber is 0-65% (wt%) in the described styrene resin, and melting index is 10-60g/10min, preferred 15-35g/10min.
6. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described compatilizer contains the group that can carry out chemical reaction with polymeric amide, and this group comprises one or more in maleic anhydride, methyl propenoic acid glycidyl ether, the acrylic or methacrylic acid.
7. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described compatilizer comprises reactive group and styrene base resin or ethylene propylene diene monomer graft polymer, one or more in optimization styrene-maleic anhydride, acrylonitrile-styrene-methyl propenoic acid glycidyl ether, acrylonitrile-styrene-butadiene-acrylic acid, terpolymer EP rubber-maleic anhydride or the acrylonitrile-styrene-methacrylic acid.
8. a kind of low water absorption polyamide composite according to claim 7 is characterized in that, the percentage of grafting of described reactive group is 2-20%, preferred 6-18%.
9. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described layered silicate clay comprises one or more in polynite, talcum powder, the kaolin, and particle diameter is the 1000-4000 order, preferred 1500-2500 purpose nano imvite.
10. a kind of low water absorption polyamide composite according to claim 9, it is characterized in that, described talcum powder is handled through silane coupling agent, and polynite is through the intercalator modification, and intercalator comprises the amino hexadecanoic acid ammonium salt of 14-, the amino hexadecanoic acid ammonium salt of 16-or the amino hexadecanoic acid ammonium salt of 18-.
11. a kind of low water absorption polyamide composite according to claim 1 is characterized in that, described short glass fiber is the alkali-free short glass fiber, and the surface is through silane coupling agent γ-aminopropyl three ethoxy silane treatment, and length-to-diameter ratio is greater than 10.
12. a kind of low water absorption polyamide composite according to claim 1, it is characterized in that, described additive comprises oxidation inhibitor, lubricant, described oxidation inhibitor comprises one or more among commercial anti oxygen agent Irganox 1010, Irganox 1076, the Irganox 168, and described lubricant comprises one or more in silicone oil, fatty acid amide, barium stearate, Magnesium Stearate, paraffin, polyethylene wax or the ethylene bis stearic acid amide.
13. the preparation method of a low water absorption polyamide composite is characterized in that, this method may further comprise the steps:
(1) according to following component and weight part content batching:
Polymeric amide 40-90;
Styrene resin 10-60;
Compatilizer 2-10;
Layered silicate clay 3-10;
Short glass fiber 5-20;
Additive is less than 2;
(2) polymeric amide, layered silicate clay and additive are placed high-speed mixer premix 20min, temperature is controlled at 40-60 ℃;
(3) raw material that obtains in the step (2) is joined in the twin screw extruder, extrude cooling granulation, obtain the polyamide/laminated silicate master batch by conveying, fusion, shearing;
(4) polyamide/laminated silicate master batch and component styrene resin, compatilizer and the short glass fiber that obtains in the step (3) placed high-speed mixer premix 20min, temperature is controlled at 40-60 ℃, (3) described method adds extruding pelletization in the twin screw extruder more set by step, prepares the daiamid composition of low water absorption.
14. a kind of low water absorption polyamide composite according to claim 13 and preparation method thereof, it is characterized in that, the length-to-diameter ratio of twin screw extruder is not less than 30 in the described step (3), temperature regulating device that has and vacuum extractor, material is melted in the twin screw extruder fully, and screw speed is 200-400rpm.
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