CH672495A5 - - Google Patents

Description

DESCRIPTION There is an extensive state of the art for the production of polyamide moldings with good impact properties and high rigidity.

According to DAS 1241606 / GB 998439, high impact strength is achieved by incorporating copolyolefins, which are inherently poorly compatible with the polyamide matrix, into rigid polyamides after they have been grafted with unsaturated carboxylic acids.

Patent specification CH 649566 describes polyamide mixtures in which, for the same purpose, polyolefins from ethylene, propylene and hexadiene (1.4) or norbornadiene (2.5), which are activated with α, β-unsaturated dicarboxylic acids, anhydrides or esters, various known polyamides -Types of high flexural modulus have been added.

Shaped articles produced by this process have very good impact and notch impact properties and high ductility, but are generally not sufficiently rigid and dimensionally stable, i.e. they have a high tendency to creep, which is why they are out of the question for many applications.

US Patents 4,410,661 and 4,536,541 deal with impact resistance adjustment of rigid amorphous copolyamides by admixing core-shell polymers or grafted copolyolefins. These intrinsically highly viscous and stiff polymer mixtures experience considerable shrinkage even after brief exposure to higher temperatures.

Moldings made from it are therefore unsuitable for many areas of application, such as thermally stressed workpieces.

DE 3 436 362 modifies the impact resistance of rigid polyamides from terephthalic acid, isophthalic acid and alkanediamines by adding copolymers of ethylene and / or acrylates which, after grafting, have carboxyl groups. EP 0 027 198 describes impact-resistant polyamide compositions in which the impact modifier is a core-shell polymer in which grafted onto a polybutadiene or butadiene / styrene core acyl acid derivatives. The loss of stiffness is compensated for by adding glass fibers.

U.S. Patent 4,180,494 describes impact modifiers used in the present invention. In DE 3 339 000, similar core-shell polymers are used in polyamides.

Molding compositions of this type are generally unsatisfactory with regard to their dimensional stability because they also tend to creep and exhibit high heat shrinkage.

GB 1,069,176 attempted to achieve a higher melt strength and better dimensional stability of moldings by admixing the polypolymer melts with crosslinking diepoxides.

In GB 1 376 537 and DOS 2 144 687, stiffness and dimensional stability are obtained by adding epoxy resins to plastomeric compositions which are largely dimensionally stable and stiff, but are not sufficiently impact-resistant; in addition, these products achieve a high density due to the high proportion of packing and reinforcing additives, which in many cases has an unfavorable effect.

However, there is an increasing demand for polymeric materials from which impact-resistant, rigid and dimensionally stable workpieces can be produced by simple injection molding, e.g. for formwork and protective parts in machine, apparatus and body construction.

It was therefore the task to provide polyamide molding compositions which are impact-resistant and at the same time have a high degree of rigidity and dimensional stability, and should also be low in creep and shrinkage without being associated with an excessive increase in the specific weight.

This invention therefore relates to molding compositions based on thermoplastically processable polyamide alloys with high impact strength, rigidity and dimensional stability, which contain at least one elastomeric polymer and at least one epoxy compound with more than one epoxy group and at the same time are characterized by low creep and Mark inclination.

It has surprisingly been found that polyamide moldings which have the combinations of properties mentioned above can be obtained if, in addition to the impact-modifying polymers, polyamide molding compositions are also used to add epoxy compounds having more than one epoxy group.

A particular and unexpected advantage of this invention is given by the fact that in the presence of epoxy compound and impact modifier in the polyamide

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672 495

the amount of the latter can be reduced without reducing the impact properties. This synergistic effect enables a much more favorable ratio of toughness and stiffness to be achieved. In addition, cost savings can be realized. Another advantage is that moldings made from these products are particularly dimensionally stable and low creep.

The polyamide molding compositions according to the invention include known polyamides such as polyamide 6, polyamide 6.6, polyamide 6.10, polyamide 11, polyamide 12, polyamide 6.12, crystalline and amorphous copolyamides, but also polyamide elastomers such as polyether amides, polyether ester amides in amounts of at least 40% by weight of the molding compositions.

The polyamide molding compositions according to the invention contain the impact-increasing polymers in amounts of at least 3% by weight, preferably 5 to 30% by weight, based on the total molding composition. Weight fractions of 10 to 20% are particularly preferred.

Known elastomeric copolymers are used as impact strength-increasing components, e.g. the copolyolefins activated with unsaturated dicarboxylic acids, based on ethylene, propylene, 1-butene or else so-called core-shell homo- or copolymers, e.g. those whose butadiene-containing or acyl-containing copolyolefin core has a vinyl grafted-on compound, e.g. Have acrylic compounds formed coat.

Suitable epoxy compounds according to the invention are considered to be those which have more than one epoxy group, preferably a terminally arranged epoxy group, in particular more than one glycidyl ether group in the molecule. Diglycid compounds are used in amounts of at least 0.001% by weight, based on the total molding composition. Amounts of 0.01 to 15% by weight are preferred, particularly preferably 0.1 to 5% by weight. However, it is also possible to use polymeric epoxy compounds which should likewise contain at least 2 epoxy groups or glycidether groups per molecule.

The preferred diglycid ethers of the general formula

Y-O-X-O-Y

with Y = epoxy group, X = divalent alkyl radical (C2-C10) or aralkyl radical (C7-C2o)

are those based on neopenlyl glycol and / or bisphenol A.

The polyamide molding compositions according to the invention are premixed in known mixing apparatus, such as in tumble mixers, agitating mixers, kneaders, wave mixers, etc., in screw machines such as extruders, plastic orders or the like. processed in the melt to molding compounds or granules, strands, etc. and then z. B. deformed on injection molding machines or extruders.

The molding compositions mentioned may contain further additives, such as e.g. Stabilizers, pigments, lubricants, emulsifiers, mold release agents, dyes, flame retardants, mineral or metallic fillers, reinforcing agents.

The polyamide molding compositions according to the invention are illustrated by the following examples.

Production of the polyamide molding compounds

The polyamide was successively mixed with the impact modifier and the epoxy compound and the mixture was used on a 2-shaft extruder of the type e.g. Werner Pfleiderer ZSK 30 homogenized at temperatures of 220-290 0 C, extruded into a strand and crushed into uniform granules. After drying it under nitrogen blanketing at 80-90 ° C. and then vacuuming at 30-50 mbar, test specimens were produced with the aid of an Arburg extruder, type 320-210-250, on which the mechanical properties were measured.

The following 5 tables contain examples listed in comparison to samples which do not contain any diepoxide compounds.

In these 5 tables, the sample numbers of the test products are in column 0, the weight fraction of the polyamide used in column 1, and the weight fraction of the notched impact strength modifier of the type of a copolyolefin modified with maleic hydride from ethylene, propylene, 1-butene in column 2 (Tables I-IV ) or of the core-shell polymer type (Table V), in column 3 the weight fraction of neopentyl glycol diglycidyl ether and in column 4 the melt viscosity in Pa-s at 270 ° C and 122.6 N).

The following columns show certain mechanical properties which were measured on test specimens:

In columns 5 and 6 the impact strength or notched impact strength according to DIN 53453 (measured dry at 23 ° C.), in column 7 the flexural modulus and in column 8 the limit bending stress, both according to DIN standard 53452; Columns 9, 10, 11 and 12 show the values of yield stress, tensile strength and elongation at break in accordance with DIN standard 53455 (measured dry at 23 ° C).

Column 13 lists longitudinal shrinkage values on DIN tensile bars 53445/3, which were measured at 100% after storage for 24 hours in a forced-air oven, and those of tensile bars in column 14 after storage for 1 hour at 140 ° C. in the same oven . Column 15 (Tables I and II) contains spray shrinkage values measured using DIN tensile bars 53445/3 after 24 hours of dry storage after spraying. The values are given in percent.

The polyamides used in Tables I-V are of the following types:

in Table I around polyamide 6 with mp. 221 ° C,

in Table II an amorphous copolyamide based on hexamethylene diamine / isophthalic acid with a glass transition point of 140 ° C.

In Table III an amorphous copolyamide of the type Grila-mid TR5 5 with a TG of 15 5 ° C.

in Table IV for a polyamide 12 with a melting point of 178 ° C. in Table V for a polyamide 6 with a melting point of 221 ° C.

The epoxy compound used with preference in the experiments in Tables I-V is the neopentyl diglycidyl ether with the chemical name 2,2 '- (2,2-dimethyl-1,3-propanedyl) bis (oxymethylene) bis oxirane.

In Table II, experiment (1) (E 5867) 1,4-butane diglycid ether was used.

Table IV shows results using diglycidyl ether of bisphenol A:

G 1302 from Ems-Chemie AG in CH 7013 Domat / Ems with molecular weight 385, G 1203.5 from Ems-Chemie AG with molecular weight 1500.

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Table I «Polyamide 6 - molding compositions with impact modifier based on copolyolefins grafted with dicarboxylic acids

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r

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ether Ikositat Ihigkeit Izahigl. since 5w. * 11270V122. ENI 123'C / tro I £ 3'C / tro! lkJ / «2 IkJ / n2

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Elongation at yield stress t

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t Longitudinal * I <Long-Schrcppf Ischruapf according to Inach £ 4h / I00 * C 11 h / 140 * Cl24 l

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350

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I 55 I 10 I!

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I 26 * 5 I 109 1 I

1 -I

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I (cl I I E 5179 I

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I cE I 35.4 I I

I 1203 I 84 I I

I 42 J

I 17.2 1

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1 <d) 1 I E 5178 I

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I 1550 I 83 I I

I 65.3 1 264 I 1

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I cB I 44.7 I I

1 1940 I 79.fi! I.

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I 53.3 I

I 1870! I 1

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I 2160 1 90! I.

1 53.3 1 144 I I

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I 1243 I 91.3 I I

I (il! I E 4796 1

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3 I 10000 1

I 2625 I 104 1!

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Table XI ■ amorphous copolyamide (type E 3038) based on hexamethylenediamine / isophthalic acid with impact modifier (impact modifier as in Table X)

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Table III = Amorphous copolyamide TR55 (impact zemodifier as in Table I)

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Table IV = polyamide 12 with impact modifier (impact modifier as in Table I)

I 0 I

1 I

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I 7 I

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I 9

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I Sample No. Polyolyid I Impact Resistant

IDiglycidyl-Melting Vis

Ichlagzä-I impact impact

I-Bend E-I Limit Bend-I Stretch -

I stretch

I hot

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I * longitudinal

I * longitudinal I * spray I

I IGew. Isodifier ether etherity

Yourself

Toughness

I module voltage

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I I

IGew- <

IGew. * 1 (270 '/ 122.6N) I23 "C / tro 123'C / tro

123'C / tro IN / naS

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Table V = polyamide 6 with impact modifier based on core-shell polymers

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14 I 15 I

I Sample No. IPolyaHid I

IDiglycidyl

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ScMagzä

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Limit Bending

Stretch

I stretch

I hot

I hot

I * longitudinal

I * longitudinal IÏ Spritz-I

I IBew.X Identifier etherity ability

Toughness

Ilfedtil

I tension tension I at stretch

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I I

IGeH- *

IGew. #

270V122.6M

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Table VI = various polyamides with impact modifier (type elastomeric copolyolef; and diglycidyl ether

I 0

I 1

1

2nd

I 3

I 4

I.

5

I.

S

I 7 I

8th

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10th

I 11

I.

12

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IProben-NrlPolyardd

I impact strength

IDiglycidyl

ISrimslzvis-

Ichlagzä-IKsrbschlag-

IBiege E- IGrenzbieoe-IStreck-Iehrurg

I hot

I hot

I.

I.

IGew.X

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Icosity

Yourself

Toughness

I module voltage

I voltage Ibe

Stretch

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Stretching

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I.

I.

IGew-! I

IGeH.Ü

I (270- / 122.5M) 123'C / tro I £ 3 ° C / tro

123'C / tro IN / rariP

123'C / tro tension

Ikeit

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I.

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I.

lkJ / t «2

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I 80X Pfl 6

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62

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78

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69

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7

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135

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Diglycid ether, type bisphenol A from Ems-Chemie AG

G 1302 low molecular weight G 1203.5 high molecular weight

Claims (9)

672 495 1. Molding compositions based on thermoplastically processable polyamide alloys with high impact strength, rigidity and dimensional stability, characterized in that that they contain at least one elastomeric polymer and at least one epoxy compound with more than one epoxy group. 2. Molding compositions according to claim 1, characterized in that the polyamide is a homo-polyamide, an amorphous or partially crystalline copolyamide, a polyether amide or a mixture of said polyamides and makes up at least 40% by weight of the total organic polymer mass. 2nd PATENT CLAIMS 3. Molding compositions according to claim 1, characterized in that the elastomeric polymer is an impact modifier made from modified polyolefins based on activated homobenz. Copolyolefins or mixtures thereof and is contained in an amount of at least 3 wt .-% in the molding composition, preferably 5-30 wt .-%, particularly preferably 10-20 wt .-%. 4. Molding compositions according to claim 1, characterized in that the elastomeric polymer is an impact modifier of the core-shell polymer type with a core of homo- or copolymers which contain butadiene or acyl compounds and grafted vinyl or acyl compounds own as a coat. 5. Molding compositions according to claim 1, characterized in that the elastomeric polymer is a mixture of modified copolyolefins according to claim 3 with core-shell polymers according to claim 4. 6. Molding compositions according to claim 1, characterized in that the epoxy compound contains at least 2 epoxy or glycidyl ether groups and in an amount of at least 0.001% by weight, preferably 0.01 to 15% by weight, particularly preferably 0 , 1 to 5 wt .-%, based on the molding composition, is contained therein. 7. Molding compositions according to claim 1, characterized in that they contain additives such as stabilizers, lubricants, plasticizers, pigments, dyes, anti-hammers, mineral or metallic fillers and reinforcing agents. 8. Molding compositions according to claim 6, characterized in that they have glycidyl ethers of the general formula Y-O-X-Y with Y = epoxy group, X = divalent alkyl radical (C2-C20) or aralkyl radical (C7-C20). 9. Molding compositions according to claim 8, characterized in that they contain diglycidyl ether based on neopenyl glycol and / or bisphenol A.