CN101619168A - Modified polyphenylene sulfide resin and preparation method thereof - Google Patents
Modified polyphenylene sulfide resin and preparation method thereof Download PDFInfo
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Abstract
The invention relates to modified polyphenylene sulfide resin which comprises PPS, PA-66, GF and compatilizer. The modified polyphenylene sulfide resin is characterized in that the compatilizer is 5.0-25.0 percent by weight of compound with at least one group selected from epoxy, amino and isocyanate and at least one of olefine grafts. The invention also discloses a preparation method of the modified polyphenylene sulfide resin, which can ensure that the blended products of PPS and PA-66 have better compatibility and more excellent comprehensively mechanical performance. The preparation method is simple, has proper cost and excellent physical and chemical performances; the heat resistance and the wear resistance of the modified polyphenylene sulfide resin are close to pure PPS single-enhanced and single-toughened materials; and the toughness, the aging resistance, the wear resistance, the tensile strength, the bending strength, the stress resistance, the weather resistance and the like are improved without influencing the original excellent performances. The products of the invention can be widely used in fields of electric products, vehicles, aviation, astronavigation, petroleum, chemical engineering, military projects, household appliances, parts of precise machinery and the like.
Description
Technical field
The present invention relates to engineering plastics, particularly relate to a kind of modified polyphenylene sulfide resin and preparation method thereof.
Background technology
Polyphenylene sulfide, English name: Poly (phenylene sulfide), the abbreviation code name is PPS, has excellent heat-resistant stable, flame retardant resistance and electric property, being widely used in fields such as automobile, electric and electronic and machinery, is the first kind of special engineering plastics.But the PPS impact resistance is relatively poor, and the machine-shaping difficulty.And polyamide 66 (English name: nylon 66, formal name used at school: polyhexamethylene adipamide, the abbreviation code name is PA-66) first place that on production capacity, occupies engineering plastics, be suitable for glass fibre and other materials filling enhancing modified especially, be widely used in various fields such as automobile, electronic apparatus, packing, machinery, daily necessities, and a large amount of modification PA-66 use in a plurality of industries.With PPS and PA-66 blend, can integrate PPS and PA-66 good characteristic separately, remedy defective separately, be beneficial to reduce cost, expand use range.But the two consistency is bad, and the blend product strength is not enough, counter-bending ability, and anti-pressure ability is poor, and weathering resistance is poor, and the environment for use harshness is single, and the processing request height, the cost height.
Summary of the invention
A technical problem to be solved by this invention is to remedy above-mentioned the deficiencies in the prior art, proposes a kind of modified polyphenylene sulfide resin.
Another technical problem to be solved by this invention is to remedy above-mentioned the deficiencies in the prior art, proposes the preparation method of above-mentioned modified polyphenylene sulfide resin.
The technical problem of modified polyphenylene sulfide resin of the present invention is solved by the following technical solutions:
This modified polyphenylene sulfide resin comprises matrix-PPS, PA-66, enhancing body-glass fibre (glass fibre abbreviates GF as) and compatilizer.
The characteristics of this modified polyphenylene sulfide resin are:
Described compatilizer is that weight percent content is 5.0～25.0% the compound with at least a group in the epoxy group(ing) of being selected from, amino, the isocyanate group, and at least a in the olefines grafts.Be used to reduce the interfacial tension between the blend component, improve the interface cohesive force between blend component, improve the consistency of blend.
The technical problem of modified polyphenylene sulfide resin of the present invention adopts following further technical scheme to be solved:
Comprise that also weight percent content is 0.1～1.0% oxidation inhibitor.Be used for effectively preventing that blend is at high temperature because the existence generation thermal-oxidative degradation of minor amount of water and oxygen.
Described oxidation inhibitor is 1,3,5-three (the 4-tertiary butyl-3-alkyl-2, the 6-3,5-dimethylphenyl)-1,3,5-triazine-2,4,6-(1H, 3H, 5H)-triketone (trade(brand)name: oxidation inhibitor cytec1790) with Tyox B (trade(brand)name: oxidation inhibitor DLTDP) composite dose, N, N '-hexa-methylene two (3,5-di-t-butyl-4-alkyl hydrocinnamamide (trade(brand)name: oxidation inhibitor 1098) with two diphosphorous acid two (2, the 4-di-tert-butyl-phenyl) esters of tetramethylolmethane (trade(brand)name: oxidation inhibitor 626) composite dose and 4,4 '-thiobis (2, the 6-tert.-butyl phenol) (trade(brand)name: at least a oxidation inhibitor 4426-S).
Comprise that also weight percent content is 0.1～1.0% coupling agent.Be used for further strengthening the consistency of GF and PPS, PA-66.
Coupling agent Y9669), γ-glycidyl ether oxygen third Trimethoxy silane (trade(brand)name: coupling agent KH-560), γ-(methacryloxy) propyl trimethoxy silicane (trade(brand)name: coupling agent kh-570), γ-An Bingjisanyiyangjiguiwan (trade(brand)name: at least a coupling agent KH-550) and in 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate described coupling agent is an aniline propyl-triethoxysilicane (trade(brand)name:.
Comprise that also weight percent content is 0.1～1.0% lubricant.Have internal lubrication and external lubrication effect concurrently, be used to improve the processing characteristics of blend.
Described lubricant is at least a in pentaerythritol stearate (PETS), ethylene bis-fatty acid amides (TAF), stearic acid, montanic acid, sodium stearate and the PE wax.
Further again technical scheme below the technical problem of modified polyphenylene sulfide resin of the present invention adopts is solved:
Described have an epoxy group(ing) of being selected from, and amino, the compound of more than one groups in the isocyanate group are at least a in bisphenol A type epoxy resin, novolac epoxy and the 3-isocyanate group propyl-triethoxysilicane.
Described olefines grafts is at least a in POE-G-GMA, POE-G-MAH, SEBS-G-GMA, SEBS-G-MAH, SBS-MAH, EPDM-G-GMA, EPDM-g-MAH, EPDM-g-St and the ethylene-methyl methacrylate glycidyl ester copolymer.
The weight percent content of described PPS is 30.0～55.0%.
Preferably, described PPS is that the trade names that Sichuan Deyang Chemistry Co., Ltd. produces are the injection grade PPS of PPS-HB.
The weight percent content of described PA-66 is 5.0～30.0%.
Preferably, described PA-66 is that the trade names that Shanghai Plastic Product No.18 Plant. produces are the PA-66 of M20.
The weight percent content of described GF is 30.0～55.0%.
Preferably, described GF is that the trade names that Taishan glass fiber Ltd produces are the GF of ERS-T635B.
Modified polyphenylene sulfide resin preparation method's of the present invention technical problem is solved by the following technical solutions:
This modified polyphenylene sulfide resin preparation method may further comprise the steps:
1) be that 30.0～55.0% PPS, weight percent content are that 5.0～30.0% PA-66 put into the mixing tank pre-mixing 1～2 minute with weight percent content, adding weight percent content then and be 0.1～1.0% coupling agent and mixed 1～2 minute, is that 5.0～25.0% compatilizer, weight percent content are that 0.1～1.0% lubricant, weight percent content are that 0.1～1.0% oxidation inhibitor is put into the moderate-speed mixers remix again with weight percent content;
2) mixture with step 1) places the twin screw extruder fusion, is 30.0～55.0% GF at glass fibre ingress adding weight percent content;
3) with the traction of the extrudate of twin screw extruder, cross water, deliver to the dicing machine pelletizing after air-cooled;
4) after being inserted the moisture eliminator drying, the pelletizing of dicing machine is goods.
Modified polyphenylene sulfide resin preparation method's of the present invention technical problem adopts following further technical scheme to be solved:
The rotating speed of the moderate-speed mixers of described step 1) is 900 ± 10r/min, and the remix time is 3～6 minutes.
Described step 2) twin screw extruder Zhong Ge district melt temperature is set at: 260～270 ℃ in a district, 270～280 ℃ in two districts, 280～290 ℃ in three districts, 290～300 ℃ in four districts, 290～300 ℃ in five districts, 280～290 ℃ in six districts, 280～290 ℃ of heads.
Described step 2) the residence time of material bar in barrel is 1～2min.
Described step 2) melt pressure is 10～30Mpa.
The drying of described step 4) is to be dry 2～4h in 120 ± 10 ℃ the moisture eliminator of air blast oven dry in temperature.
The beneficial effect that the present invention is compared with the prior art is:
The present invention has changed the shortcoming of single interpolation glass fibre of existing PA-66 blend goods or single interpolation PPS, fundamentally solved the compatibility problem between PPS and the PA-66, make PPS and PA-66 blend goods have better consistency and excellent comprehensive mechanical properties more, to satisfy the service requirements of numerous industries.Preparation method of the present invention is simple, cost is moderate, every physical and chemical performance excellence, the single enhancing of the approaching pure PPS of heat-resisting, wear resistance, single toughening material, promote to some extent at aspects such as toughness, anti-aging, anti-wear, tensile strength, counter-bending ability, anti-pressure ability and weathering resistancies, and do not influence its original excellent properties.PPS of the present invention and PA-66 blend goods can be widely used in electronic apparatus, automobile, aviation, aerospace, oil, fields such as chemical industry, military project, household electrical appliances, precision optical machinery component.
Embodiment
The invention will be further described below in conjunction with five specific embodiments.
Each component of the modified polyphenylene sulfide resin of embodiment 1～5 and the weight percent content of setting thereof see Table 1, and preparation process is as follows:
1) PPS, the PA-66 with the setting weight degree put into the moderate-speed mixers pre-mixing 1～2 minute, the coupling agent that adds the setting weight degree then mixed 1～2 minute, again compatilizer, lubricant, the oxidation inhibitor of setting weight degree was put into the moderate-speed mixers remix 3～6 minutes;
2) mixture with step 1) places the twin screw extruder fusion, the GF that adds the weight percent content of listing by table 1 in the glass fibre ingress, twin screw extruder Zhong Ge district melt temperature is set at: 270 ℃ in a district, 280 ℃ in two districts, 290 ℃ in three districts, 300 ℃ in four districts, 290 ℃ in five districts, 280 ℃ in six districts, 285 ℃ of heads; The material residence time of bar in barrel is 1～2min, and melt pressure is 10-30MPa;
3) with the traction of the extrudate of twin screw extruder, cross water, deliver to the dicing machine pelletizing after air-cooled;
4) pelletizing of dicing machine being inserted temperature is to be goods behind dry 2～4h in 120 ± 10 ℃ the moisture eliminator of air blast oven dry.
Table 1
| Component weight percent content (%) | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| ??PPS | ??30％ | ??33.3％ | ??43.3％ | ??38.3％ | ??55％ |
| ??PA-66 | ??30％ | ??5％ | ??10％ | ??5％ | ??8.3％ |
| ??GF | ??30％ | ??55％ | ??35％ | ??30％ | ??30％ |
| Compatilizer | ??8.3％ | ??5％ | ??10％ | ??25％ | ??5％ |
| Oxidation inhibitor | ??0.6％ | ??0.6％ | ??0.6％ | ??0.6％ | ??0.6％ |
| Coupling agent | ??0.5％ | ??0.5％ | ??0.5％ | ??0.5％ | ??0.5％ |
| Lubricant | ??0.6％ | ??0.6％ | ??0.6％ | ??0.6％ | ??0.6％ |
In the table 1, the compatilizer of embodiment 1～5, oxidation inhibitor, coupling agent and lubricant are as follows respectively:
Compatilizer:
Embodiment 1 is POE-G-MAH;
Embodiment 2 is SEBS-G-MAH;
Embodiment the 3, the 4th, EPDM-G-MAH;
Embodiment 5 is ethylene-methyl methacrylate glycidyl ester copolymer.
Oxidation inhibitor:
Embodiment 1 is that weight percent content is that 0.4% cytec1790 and weight percent content are composite dose of 0.2% DLTDP;
Embodiment 2 is that weight percent content is that 0.3% 4426-S and weight percent content are 0.3% 626 composite dose;
Embodiment 3 be weight percent content be 0.4% 1098 with weight percent content be 0.2% 626 composite dose;
Embodiment 4 weight percent contents are that 0.3% cytec1790 and weight percent content are composite dose of 0.3% DLTDP;
Embodiment 5 be weight percent content be 0.4% cytec1790 with weight percent content be 0.3% 626 composite dose.
Coupling agent:
Embodiment 1 is that weight percent content is that 0.3% KH-560 and weight percent content are composite dose of 0.2% 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate;
Embodiment 2 is that weight percent content is that 0.3% KH-550 and weight percent content are composite dose of 0.2% 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate;
Embodiment 3 is that weight percent content is that 0.3% KH-570 and weight percent content are composite dose of 0.2% 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate;
Embodiment 4 is that weight percent content is that 0.3% Y9669 and weight percent content are composite dose of 0.2% 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate;
Embodiment 5 is that weight percent content is that 0.4% KH-570 and weight percent content are composite dose of 0.1% Y9669.
Lubricant:
Embodiment 1 is that weight percent content is that 0.3% stearic acid and weight percent content are composite dose of 0.3% PETS;
Embodiment 2 is that weight percent content is that 0.3% PE wax and weight percent content are composite dose of 0.3% PETS;
Embodiment 3 is that weight percent content is that 0.3% sodium stearate and weight percent content are composite dose of 0.3% PETS;
Embodiment 4 is that weight percent content is that 0.3% stearic acid and weight percent content are composite dose of 0.3% PE wax;
Embodiment 5 is that weight percent content is that 0.3% PE wax and weight percent content are composite dose of 0.3% TAF.
Embodiment 1～8 product sample is injection molded into the iso standard batten with injection moulding machine, is cooled to the performance perameter of under the ASTM testing standard, testing after the room temperature and is listed in the table below 2:
Table 2
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Testing standard (ASTM) |
| The tall and erect shock strength (J/M) of dust | ??81 | ??92 | ??80 | ??85 | ??75 | ??D/256，1/8″ |
| Tensile strength (Mpa) | ??163 | ??176 | ??164 | ??139 | ??130 | ??D638 |
| Elongation (%) | ??1.2 | ??1.8 | ??2.0 | ??2.3 | ??2.2 | ??D638 |
| Flexural strength (Mpa) | ??229 | ??234 | ??198 | ??188 | ??162 | ??D790 |
| Modulus in flexure (Gpa) | ??10.01 | ??9.16 | ??10.36 | ??12.24 | ??12.4 | ??D790 |
| Heat-drawn wire (℃) | ??277 | ??271 | ??265 | ??254 | ??246 | ??D1525，5Kg/50℃/h |
| Fire-protection rating (UL-94) | ??V0 | ??V0 | ??V0 | ??V1 | ??V1 | ??1/16″ |
Be compared with the prior art the beneficial effect that is had for further specifying the present invention, the goods of four groups of simultaneous tests are provided again, each component and the weight percent content thereof of the goods of Comparative Examples 1～4 see Table 3.
Table 3
In the table 3, the compatilizer of Comparative Examples 1～4, oxidation inhibitor, coupling agent and lubricant are as follows respectively:
Comparative Examples 1～3 no compatilizer, the compatilizer of Comparative Examples 4 is POE-G-MAH;
Oxidation inhibitor all be weight percent content be 0.3% 1098 with weight percent content be 0.3% 626 composite dose;
Coupling agent all is KH560;
Lubricant all is PETS.
Comparative Examples 1～4 product sample is injection molded into the iso standard batten with injection moulding machine, is cooled to the performance perameter of under the ASTM testing standard, testing after the room temperature and is listed in the table below 4:
Table 4
| Performance | Comparative Examples 1 | Comparative Examples 2 | Comparative Examples 3 | Comparative Examples 4 | Testing standard (ASTM) |
| The tall and erect shock strength (J/M) of dust | ??35 | ??52 | ??86 | ??100 | ??D/256，1/8″ |
| Tensile strength (Mpa) | ??67 | ??118 | ??146 | ??169 | ??D638 |
| Elongation (%) | ??1.8 | ??1.6 | ??1.3 | ??0.8 | ??D638 |
| Flexural strength (Mpa) | ??98 | ??130 | ??153 | ??179 | ??D790 |
| Modulus in flexure (Gpa) | ??3.8 | ??6.4 | ??9.16 | ??11.9 | ??D790 |
| Heat-drawn wire (℃) | ??278 | ??273 | ??262 | ??240 | ??D1525，5Kg/50℃/h |
| Fire-protection rating (UL-94) | ??V0 | ??V0 | ??V1 | ??V1 | ??1/16″ |
The performance perameter of embodiment 1～5 and Comparative Examples 1～4 product testing in the contrast table 2,4 has to draw a conclusion:
1) modified polyphenylene sulfide resin excellent combination property of the present invention, especially toughness, stretching, bending, heatproof, wear-resisting, all respects such as anti-aging, processibility, lifting is by a relatively large margin all arranged, and still have good heat-resistant, with the contrast of PPS virgin resin, thermotolerance is significantly improved;
2) adding of GF can improve the mechanical property of PPS, plays the enhanced effect, and mechanical property is improved, and notched Izod impact strength can bring up to 100,3 times nearly from 35;
3) adding of PA66 can improve the toughness of PPS, can also obviously improve the elongation at break of PPS, rises to 2.0 from 1.2, near 1 times;
4) adding of compatilizer can further promote the consistency of PPS and PA-66, and other performances can obviously not reduce.
Above content be in conjunction with concrete preferred implementation to further describing that the present invention did, can not assert that concrete enforcement of the present invention is confined to these explanations.For the general technical staff of the technical field of the invention, make some being equal to without departing from the inventive concept of the premise to substitute or obvious modification, and performance or purposes are identical, all should be considered as belonging to protection scope of the present invention.
Claims (10)
1, a kind of modified polyphenylene sulfide resin comprises PPS, PA-66, GF and compatilizer, it is characterized in that:
Described compatilizer is that weight percent content is 5.0～25.0% the compound with at least a group in the epoxy group(ing) of being selected from, amino, the isocyanate group, and at least a in the olefines grafts.
2, modified polyphenylene sulfide resin as claimed in claim 1 is characterized in that:
Comprise that also weight percent content is 0.1～1.0% oxidation inhibitor, described oxidation inhibitor is 1,3,5-three (the 4-tertiary butyl-3-alkyl-2,6-3,5-dimethylphenyl)-1,3,5-triazine-2,4,6-(1H, 3H, 5H)-composite dose, N of triketone and Tyox B, N '-hexa-methylene two (3, the two diphosphorous acids two (2 of 5-di-t-butyl-4-alkyl hydrocinnamamide and tetramethylolmethane, the 4-di-tert-butyl-phenyl) composite dose and 4 of ester, at least a in 4 '-thiobis (2, the 6-tert.-butyl phenol).
3, modified polyphenylene sulfide resin as claimed in claim 1 or 2, it is characterized in that 3,
Comprise that also weight percent content is 0.1～1.0% coupling agent, described coupling agent is at least a in aniline propyl-triethoxysilicane, γ-glycidyl ether oxygen third Trimethoxy silane, γ-(methacryloxy) propyl trimethoxy silicane, γ-An Bingjisanyiyangjiguiwan and 4-amino phenyl sulfonyl acyl group two (dodecyl benzenesulfonyl) isopropyl titanate.
4, modified polyphenylene sulfide resin as claimed in claim 3 is characterized in that:
Comprise that also weight percent content is 0.1～1.0% lubricant, described lubricant is at least a in PETS, TAF, stearic acid, montanic acid, sodium stearate and the PE wax.
5, modified polyphenylene sulfide resin as claimed in claim 4 is characterized in that:
Described have an epoxy group(ing) of being selected from, and amino, the compound of more than one groups in the isocyanate group are at least a in bisphenol A type epoxy resin, novolac epoxy and the 3-isocyanate group propyl-triethoxysilicane.
6, modified polyphenylene sulfide resin as claimed in claim 5 is characterized in that:
Described olefines grafts is at least a in POE-G-GMA, POE-G-MAH, SEBS-G-GMA, SEBS-G-MAH, SBS-MAH, EPDM-G-GMA, EPDM-g-MAH, EPDM-g-St and the ethylene-methyl methacrylate glycidyl ester copolymer.
7, modified polyphenylene sulfide resin as claimed in claim 6 is characterized in that:
The weight percent content of described PPS is 30.0～55.0%;
The weight percent content of described PA-66 is 5.0～30.0%.
8, modified polyphenylene sulfide resin as claimed in claim 7 is characterized in that:
The weight percent content of described GF is 30.0～55.0%.
9, a kind of modified polyphenylene sulfide resin preparation method is characterized in that:
May further comprise the steps:
1) be that 30.0～55.0% PPS, weight percent content are that 5.0～30.0% PA-66 put into the moderate-speed mixers pre-mixing 1～2 minute with weight percent content, adding weight percent content then and be 0.1～1.0% coupling agent and mixed 1～2 minute, is that 5.0～25.0% compatilizer, weight percent content are that 0.1～1.0% lubricant, weight percent content are that 0.1～1.0% oxidation inhibitor is put into the moderate-speed mixers remix again with weight percent content;
2) mixture with step 1) places the twin screw extruder fusion, is 30.0～55.0% GF at glass fibre ingress adding weight percent content;
3) with the traction of the extrudate of twin screw extruder, cross water, deliver to the dicing machine pelletizing after air-cooled;
4) after being inserted the moisture eliminator drying, the pelletizing of dicing machine is goods.
10, modified polyphenylene sulfide resin preparation method as claimed in claim 9 is characterized in that:
Described step 2) twin screw extruder Zhong Ge district melt temperature is set at: 260～270 ℃ in a district, 270～280 ℃ in two districts, 280～290 ℃ in three districts, 290～300 ℃ in four districts, 290～300 ℃ in five districts, 280～290 ℃ in six districts, 280～290 ℃ of heads.
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