CN85102042B - With glass fiber-reinforced polypropene composition - Google Patents
With glass fiber-reinforced polypropene composition Download PDFInfo
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- CN85102042B CN85102042B CN85102042A CN85102042A CN85102042B CN 85102042 B CN85102042 B CN 85102042B CN 85102042 A CN85102042 A CN 85102042A CN 85102042 A CN85102042 A CN 85102042A CN 85102042 B CN85102042 B CN 85102042B
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Abstract
A polypropylene composition reinforced with glass fiber and excellent in mechanical properties, rigidity and appearance, is a mixture obtained by melting and kneading a specific amount a), b), c), wherein a) is passed through an unsaturated carboxylic acid A modified polypropylene resin by acid or its anhydride or 5 parts by weight or more by weight of a polypropylene resin modified by an unsaturated carboxylic acid or its anhydride, b) by polycondensation of m-xylene diamine and adipic acid The resulting polyamide resin, c) glass fiber.
Description
The present invention is about the polypropene composition with glass fiber-reinforced.In more detail, the present invention is about in mechanical property, hardness with have in appearance the glass fiber-reinforced polypropene composition of use of superiority.
Recently, greatly increase for the requirement of the thermoplastic resin starting material (this material can be used for manufacturing auto parts, appliances and various other mechanicals) of high rigidity and high mechanical strength.For meeting this requirement, with regard to polypropylene, (claim that hereinafter polypropylene is PP), use energetically the development of glass fiber-reinforced polypropylene (hereinafter referred to as FR-PP).
But because PP is non-polar resin, therefore on fiberglass surfacing, PP and glass fibre avidity are very weak.Even when glass fibre is added to PP simply, be also difficult to find out the effect of improving of physical strength (as tensile strength, transverse strength or similar intensity).
Therefore, will with unsaturated carboxylic acid or its acid anhydride (hereinafter, be called unsaturated carboxylic acid base) improvement PP (hereinafter referred to as improvement PP) be added in PP and glass fibre, use for the activated silane coupling agent of unsaturated carboxylic acid tool their surface is processed, their application can be used as one and improves the method for wettability (being the adhesivity between PP and glass fibre).
On the other hand, along with the enhancing of degree of adhesion between PP and glass fibre, occurred that moulded product outward appearance becomes worse trend.
Say, can improve hardness although increase the add-on of glass fibre, there will be so again a problem, i.e. the increase meeting of the glass fibre add-on just outward appearance of moulded product becomes poorer.And if the add-on of glass fibre increases, except above-mentioned mentioned outward appearance degenerates, the proportion of moulded product also can increase, thereby makes product lose the advantage of lightweight, therefore, the increase of glass fibre add-on is conditional.
So, it would be desirable and add a small amount of glass fibre, just can obtain beautiful outward appearance, can obtain again high rigidity, high mechanical strength.
Therefore, existing method is in PP, to add polyamide resin, especially nylon 6 or nylon 66 and glass fibre.In the case, in order to improve the consistency of PP and polyamide resin, in PP, add MODIFIED PP.But, in the case of containing PP, MODIFIED PP, common polyamide resin as the composition of nylon 6, nylon 66 and glass fibre, in the time making moulded product by said composition, because nylon 6 and nylon 66 have moisture-absorption characteristics, result can produce the problem that physical strength and hardness obviously reduce due to moisture absorption.
Say again, in this system, in the time carrying out heating and melting and mix, between the carboxylate radical that above-mentioned MODIFIED PP is derivative and polyamide resin, can there is strong reaction, the moulded product forming not only its color can become extremely light yellow, and can obviously lose original gloss.Thereby problem can be summed up as a bit, if outward appearance shows its condition of surface be: tarnished and utmost point unfairness, result just can not obtain glossiness aesthetic appearances.
In order to solve the problem of above mentioned FR-PP, inventor of the present invention has done a large amount of research.They have adopted a kind of specific polyamide resin obtaining by the polycondensation of m-xylene diamine and hexanodioic acid, use it as a kind of polyamide resin, this polyamide resin and MODIFIED PP or the PP that comprises MODIFIED PP and glass fibre are mixed, melting subsequently and stirring, found that, prepared glass fiber-reinforced polypropene composition, physical strength, the hardness of its moulded product all improve, and present good outward appearance.Like this, they have completed the present invention.
Can find out significantly from above-mentioned explanation, the object of the invention is in order to provide a kind of use glass fiber-reinforced polypropene composition, the moulded product of making by said composition has good physical strength and hardness, and has fabulous outward appearance.
Employing has the composition of the present invention of following component, can realize object of the present invention.
The mixture that contains following component by melting and stirring, can make with glass fiber-reinforced polypropene composition, and each group is respectively:
A): the acrylic resin that 60～95 parts (by weight, lower with) improved by unsaturated carboxylic acid or its acid anhydride, or containing 5 parts or the more parts of acrylic resins with the acrylic resins of unsaturated carboxylic acid or the improvement of its acid anhydride.
B): 40～5 parts of polyamide resins that obtain by the polycondensation of m-xylene diamine and hexanodioic acid.
C): the glass fibre of 50～100 parts.(refer to that every 100 parts of above-mentioned A add B total amount.
The polyamide resin that the present invention is used, to obtain by the polycondensation of m-xylene diamine and hexanodioic acid, it is a kind of specific polyamide resin, it has following molecular formula, in molecular chain, comprise an aryl rings (phenyl ring), be commonly referred to nylon MXD 6 (hereinafter referred to as nylon MXD 6).
In the molecular chain of this nylon, have a phenyl ring, it presents large rigidity, with other polyamide resin, and as nylon 6, nylon 66 etc. are compared, being characterized as of nylon MXD 6: have high physical strength and higher hardness.Nylon MXD 6 also has an obvious feature, and, compared with above-mentioned other nylon 6, nylon 66, its water absorbability is minimum.
So in composition of the present invention, make polyamide resin with nylon MXD 6, by utilizing the above-mentioned feature of nylon MXD 6, can see the improvement of characteristic in my innocent life.
In the present invention, except using separately above mentioned nylon MXD 6 (as polyamide resin), also can be by other polyamide resin, for example nylon 6, nylon 66, nylon 11, nylon 12, NYLON610, nylon 612 and the nylon MXD 6 as main ingredient mix use.
The MODIFIED PP that the present invention is used is the material obtaining by adopt improvement PP with unsaturated carboxylic acid base.The unsaturated carboxylic acid base using has: vinylformic acid, methacrylic acid, maleic acid, propylenedicarboxylic acid, anti-(formula) butene dioic acid, methyl are along (formula) butene dioic acid, MALEIC ANHYDRIDE, methyl-maleic acid acid anhydride, propylenedicarboxylic acid acid anhydride and analogue.
The PP starting material of using in MODIFIED PP are had no particular limits.Common homopolymer polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymers, propylene-ethylene-butene multipolymer, propylene-ethylene-hexene copolymer all can be used.
Conventionally by various known method production MODIFIED PP.But, very easy by above mentioned any one unsaturated carboxylic acid base by following method, common radical generates agent if organo-peroxide is (as two-tert-butyl peroxide, dicumyl peroxide, benzoyl peroxide, 2,5-dimethyl-2,5-bis-(tert-butyl hydroperoxide) hexane, 1, two (t-butyl peroxy sec.-propyl) benzene of 3-is added in polypropylene powder, carries out melting and the stirring of mixture, thereby can make MODIFIED PP with extrusion machine.
As production MODIFIED PP PP starting material used, the unmodified PP of the use in the present invention has no particular limits, thereby can use above mentioned various PP.When the MODIFIED PP of 60～95% (weighing scales) is mixed use with PP, as long as MODIFIED PP accounts for 5 parts (by weight) or more (below claiming that this mixture is MODIFIED PP base) of amount of the mixture, their any ratio of mixture is all allowed so, even allows whole use MODIFIED PP.Nylon MXD 6 and MODIFIED PP or comprise 5 parts (by weight) or that PP of more MODIFIED PP, its ratio of mixture is the nylon MXD 6 of 5～50 parts (by weight) preferably, MODIFIED PP or any one MODIFIED PP base with 95～50 parts (by weight), exactly, the preferably nylon MXD 6 of 10～40 parts (by weight) and the MODIFIED PP of 90～60 parts (by weight) or any one MODIFIED PP base of their ratio of mixture.In the time that nylon MXD 6 is less than 5 parts (weight), can not reach the effect of improving of expection.
The glass fibre that used is in the present invention preferably with the glass fibre of strengthening ordinary resin, as glass roving, the glass rope of chopping off, the glass fibre grinding and analogue.
If MODIFIED PP or arbitrarily MODIFIED PP base and nylon MXD 6 total amount are as 100 parts (by weight), the glass fibre amount that added is 5～100 parts (by weight), and 20～90 parts better, and 30～80 parts best.In the time that the add-on of glass fibre is less than 5 parts (by weight), can not obtain gratifying strengthening effect.But, if the add-on of glass fibre exceedes 100 parts (by weight), be also unfavorable, because the melting of mixture and stirring can become very difficulty, and the reduction of fused solution mobility can affect the processing characteristics of goods.
In addition, in the method for the invention, conventionally can add multiple additives simultaneously, as antioxidant, thermo-stabilizer, UV light absorber, metal-salt, lubricant, tinting material and the mineral filler of the acid of high ester fat.
In the time producing composition of the present invention, can adopt various method, these methods are exemplified below:
(1), the method is first by MODIFIED PP or any one MODIFIED PP base, nylon MXD 6 and glass fibre amount is in accordance with regulations mixed, and then mixture is carried out to melting and stirring.
(2), the method first, by MODIFIED PP or any one MODIFIED PP base and nylon MXD 6 melting, stirs and granulates, then add glass fibre, and again carry out melting and stirring.
3, an extrusion machine for the method, this extrusion machine is except having a conventional feed orifice, on its cylinder part, also there is a feed orifice, can add MODIFIED PP or any one MODIFIED PP base and nylon MXD 6 by conventional feed orifice, and by being positioned at the feed orifice on cylinder part, add glass fibre, then carry out melting and stirring.
(4), in the method, not only from conventional feed orifice, add MODIFIED PP or any one MODIFIED PP base, also add nylon MXD 6 and glass fibre from the feed orifice being arranged in cylinder part simultaneously.And also carry out melting and stirring.
Whipping appts used is preferably: if Henschel agitator (trade name) (this is a kind of high speed agitator with splash bar), general mixer are as ribbon blender, drum-type agitator and similar agitator.Common list or double-screw extrusion machine can be used for melting and the stirring of mixture.The temperature of melting and stirring is 200～300 DEG C, and 200～280 DEG C better, and 240～280 DEG C best.
The glass fiber-reinforced polypropylene GRANULES of use obtaining with aforesaid method, is molded as the test sample of specified dimension, and measures its physical strength, hardness and outward appearance.These samples absorb water after processing through forcing, then in order to measure its physical strength, hardness and outward appearance.
The result of comparing with control sample shows, all its physical strength of composition, hardness and the outward appearances (as the unevenness of glossiness, color, gloss, condition of surface) of the present invention all have clear improvement, and can be effectively for needing the appliances of high mechanical strength, high rigidity and good appearance.In auto parts and various mechanicals.
The present invention will do explanation more fully to the present invention with embodiment and comparative example.In the present invention, estimate physical strength by the mensuration of tensile strength and transverse strength, calculate hardness with flexural modulus, evaluate outward appearance by the ununiformity of observation surface gloss, color and gloss.In embodiment and comparative example, measure based on following testing method.
Mandatory water suction processing and water-intake rate are measured
The dip treating that sample is stood three days in the boiling water of 100 DEG C, then calculates water-intake rate according to the percentage ratio of processing forward and backward sample weight increase.
The observation of outward appearance
With a block length 150mm, wide 150mm, thick be the flat board of 2mm as sample, their condition of surface of detecting by an unaided eye, color and lustre lacking uniformity to sample are made an appraisal.
Tensile strength: measure by the method for JIS K 7113.
Transverse strength: measure by the method for JIS K 7203.
Flexural modulus: measure by the method for JIS K 7203.
Glossiness: press ASTMD523, with the inclination angle of 60 °, the mirror surface luster of the plane plate specimen that mensuration thickness is 2mm.
embodiment 1～3, comparative example 1～3
By 98.15 parts (by weight, homopolymer polypropylene down together), its smelt flow speed (is 230 DEG C in temperature, in the time applying the load of a 2.16kg, the extrusion capacity of molten resin in 10 minutes) be 4.5g/10min, 1 part of MALEIC ANHYDRIDE, 0.1 part 2, 6-bis--tertiary butyl-p-Cresol, 0.1 part of calcium stearate, 0.05 part 1, two (t-butyl peroxy sec.-propyl) benzene of 3-and 0.6 part of magnesium hydroxide, in Hens-chel agitator, mix 3 minutes, the double-screw extrusion machine that is 45mm with an internal diameter, its the raw material supply hole of several L/D=30 above, at the temperature of 200 DEG C, mixture is carried out to melting, stir and extruding, to obtain the MODIFIED PP particle of smelt flow speed as 130g/10min.
Then by above-mentioned MODIFIED PP and nylon MXD 6 (RENY-6001, produced by gas company limited of Mitsubishi Chemical) deliver in drum-type agitator by the listed specified amount of table 1, stir 10 minutes, but join wherein by the conventional feed orifice of above-mentioned extrusion machine, add glass fibre to measure feeding quantity from the feed orifice being positioned at cylinder part simultaneously.At the temperature of 250 DEG C, in carrying out melting, stir and extruding, granulate.
And in comparative example 1, by the method for embodiment 1～3, (except not using nylon MXD 6) under the same conditions, makes MODIFIED PP, glass fibre melting, stirs and extrude, to granulate.
And in comparative example 2, adopting the method for embodiment 1～3, (except nylon 6 is used as polyamide resin) under the same conditions, makes mixture carry out melting, stir and extrude, and then granulates.
And in comparative example 3, its method identical with embodiment 1～3 (except doing polyamide resin with nylon 66), at 270 DEG C of temperature, by mixture melting, stir and extrude, to granulate, its service temperature is 270 DEG C.
Obtained particle is sent in an injection moulding machine, is 250 DEG C at resin temperature, and molding temperature is under the working conditions of 80 DEG C, is molded as the sample of specified dimension, for various tests.But the in the situation that of containing nylon 66 in particle, while carrying out injection-molded, resin temperature is that 275 DEG C, molding temperature are 80 DEG C, to be molded into the test sample of specified dimension, this sample is for various tests.Test result is listed in table 1.
embodiment 4～5, comparative example 4～5
The effect simultaneously using in order to test MODIFIED PP and common unmodified PP, press the blending ratio of the listed each component of table 2, mix various MODIFIED PP, unmodified PP, nylon MXD 6 and glass fibre, in this example, mix, melting, to stir and extrude then the method for granulating all identical with embodiment 1～3.And comparative example 4～5 mixing, melting, stir identical with embodiment 1～3 with mixture ratio example and the method extruding to granulate.
Utilize these particles, can be molded into the sample (the same with the sample in embodiment 1～3) of specified dimension, for various tests.
Test result is as shown in table 2.
embodiment 6～8, comparative example 6～10
In order to test the impact of glass fibre add-on, by the listed blending ratio of table 3, mix various MODIFIED PP.Nylon MXD 6 and glass fibre, by the method for embodiment 1～3, mix, melting, stir and extrude, and granulate.
In comparative example 6～10, mix each component by the listed blending ratio of table 3, by the method for embodiment 1～3, mix, melting, stir and extrude, then in order to granulate.
By prepared particle, be added to the sample with molded specified dimension in injection moulding machine (as embodiment 1～3), for various tests.
Test result is as shown in table 3.
Table 1 illustrates, the product that embodiment 1～3 provides, and its physical strength (as tensile strength, transverse strength (flexural modulus)) is although be better than the product (this product does not use polyamide resin) that comparative example 1 provides.But although unexpectedly used polyamide resin, and the Optimality of the outward appearance of present composition goods is confirmed, the outward appearance of the product of embodiment 1～3 with do not use the product of polyamide resin the same.
And, in the time that embodiment 1～3 compares as the comparative example 2～3 of polyamide resin with employing nylon 6, nylon 66, confirming that the product of embodiment 1～3 is forward and backward in water suction processing, its physical strength, hardness and outward appearance are all better than the product of comparative example 2～3.
In addition, embodiment 2 has confirmed that composition of the present invention has surprising premium properties.In other words, although the consumption of nylon MXD 6 is only 10 parts (by weight), but in embodiment 2, the physical strength of composition and hardness are all better than comparative example 2～3 composition (having used nylon 6 and nylon 66 in comparative example 2～3).
Test result shows, the water absorbing properties of composition of the present invention is more much smaller than using the composition of nylon 6 and nylon 66.
In addition, test-results also shows, absorbs water after processing through pressure, and the physical strength of the present composition and the reduction of hardness are less than using the composition of nylon 6 and nylon 66.
Table 2 illustrates, in the time that the MODIFIED PP amount of mixing with unmodified PP is 5 parts or more (by weight), the consistency aspect of nylon MXD 6 and unmodified PP is no problem, and can obtain gratifying physical strength, hardness and outward appearance.
In comparative example 4, because used MODIFIED PP amount is less, the consistency of unmodified PP and nylon MXD 6 is reduced, and do not demonstrate the effect that adds nylon MXD8.In comparative example 5, because the add-on of nylon MXD 6 is 3 parts (by weight), a bit do not see and change general effect.
Table 3 illustrates, if increase the add-on of glass fibre, physical strength and hardness also must increase so, but its appearance characteristics but declines thereupon, but in embodiment 6～8, the outward appearance of its product is better than comparative example 6～8 product.Test-results also shows, its mechanical property and hardness ratio are used the comparative example's 9～10 of nylon 6 product to have clear improvement.
Thereby, can proved inventive composition in physical strength, hardness with have clear improvement in appearance, and composition water-absorbent of the present invention is less.
Claims (9)
1. with glass fiber-reinforced polypropene composition, by melting and stir A), B), C) mixture make.Wherein A), B), C) composition as follows:
A): the acrylic resin with unsaturated carboxylic acid or its anhydride modification of 60～95 parts (by weight), or containing 5 parts (by weight) or more with the acrylic resin of the acrylic resin of unsaturated carboxylic acid or its anhydride modification.
B): the polyamide resin that 40～5 parts (by weight) makes by the polycondensation of m-xylene diamine and hexanodioic acid.
C): the glass fibre (with the total of every 100 parts of above-mentioned A and B component) of 5～100 parts (by weight).
Claim 1 by glass fiber-reinforced polypropene composition, A): 70 parts (by weight) is by the acrylic resin of unsaturated carboxylic acid or its anhydride modification, B): the polyamide resin that 30 parts (by weight) makes by the polycondensation of m-xylene diamine and hexanodioic acid.C): 50 parts of (by weight) glass fibre, based on A) and B) total amount of component is 100 parts, by this mixture melting and stir.
Claim 1 by glass fiber-reinforced polypropene composition, A): 80 parts (by weight) is by the acrylic resin of unsaturated carboxylic acid or its anhydride modification.B) polyamide resin: 20 parts (by weight)) making by the polycondensation of two phenylenediamine and hexanodioic acid.C): 55 parts of (by weight) glass fibre, the total amount of (based on above-mentioned A) and B) component is 100 parts), mixture is carried out to melting and stirring.
Claim 1 by glass fiber-reinforced polypropene composition, this unsaturated carboxylic acid or its acid anhydride are at least selected following a kind of composition, comprise vinylformic acid, methacrylic acid, maleic acid, propylenedicarboxylic acid, instead (formula) butene dioic acid, methyl are along (formula) butene dioic acid, MALEIC ANHYDRIDE, methyl-maleic acid acid anhydride, propylenedicarboxylic acid acid anhydride.
Claim 1 by glass fiber-reinforced polypropene composition, above-mentioned acrylic resin is at least selected from following a kind of composition, comprise: homopolymer polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymers, propylene-ethylene-butene multipolymer and propylene-ethylene-hexene copolymer.
Claim 2 by glass fiber-reinforced polypropene composition, above-mentioned unsaturated carboxylic acid or its acid anhydride are at least selected from following-kind of composition, comprise: vinylformic acid, methacrylic acid, maleic acid, propylenedicarboxylic acid, instead (formula) butene dioic acid, methyl is along (formula) butene dioic acid, MALEIC ANHYDRIDE, methyl-maleic acid acid anhydride, propylenedicarboxylic acid.
Claim 3 by glass fiber-reinforced polypropene composition, above-mentioned unsaturated carboxylic acid or its acid anhydride are to be at least selected from following a kind of composition, comprise: vinylformic acid, methacrylic acid, maleic acid, propylenedicarboxylic acid, instead (formula) butene dioic acid, methyl is along (formula) butene dioic acid, MALEIC ANHYDRIDE, methyl-maleic acid acid anhydride, propylenedicarboxylic acid acid anhydride.
Claim 2 by glass fiber-reinforced polypropene composition, above-mentioned acrylic resin is to be at least selected from following a kind of composition, comprise: homopolymer polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymers, propylene-ethylene-butene multipolymer and propylene-ethylene-hexene copolymer.
Claim 3 by glass fiber-reinforced polypropene composition, above-mentioned acrylic resin is at least selected from following a kind of composition, comprises, homopolymer polypropylene, propylene-ethylene block copolymer, propylene-ethylene random copolymers, propylene-ethylene-butene multipolymer and propylene-ethylene-hexene copolymer
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85102042A CN85102042B (en) | 1984-03-28 | 1985-04-01 | With glass fiber-reinforced polypropene composition |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59060379A JPH0618929B2 (en) | 1984-03-28 | 1984-03-28 | Glass fiber reinforced polypropylene composition |
| CN85102042A CN85102042B (en) | 1984-03-28 | 1985-04-01 | With glass fiber-reinforced polypropene composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85102042A CN85102042A (en) | 1987-01-31 |
| CN85102042B true CN85102042B (en) | 1988-10-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85102042A Expired CN85102042B (en) | 1984-03-28 | 1985-04-01 | With glass fiber-reinforced polypropene composition |
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| Country | Link |
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| CN (1) | CN85102042B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558681A (en) * | 2011-12-30 | 2012-07-11 | 福建晟扬管道科技有限公司 | Trenchless corrugated pipe special for electric power and preparation method thereof |
-
1985
- 1985-04-01 CN CN85102042A patent/CN85102042B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102558681A (en) * | 2011-12-30 | 2012-07-11 | 福建晟扬管道科技有限公司 | Trenchless corrugated pipe special for electric power and preparation method thereof |
| CN102558681B (en) * | 2011-12-30 | 2013-09-18 | 福建晟扬管道科技有限公司 | Trenchless corrugated pipe special for electric power and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN85102042A (en) | 1987-01-31 |
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