Flame Retardant-Stabilizer Combination for Thermoplastic Polymers
20190225772 · 2019-07-25
Assignee
Inventors
Cpc classification
C08L77/02
CHEMISTRY; METALLURGY
C08K5/34924
CHEMISTRY; METALLURGY
C08K13/04
CHEMISTRY; METALLURGY
C08K2201/005
CHEMISTRY; METALLURGY
C08L77/06
CHEMISTRY; METALLURGY
International classification
Abstract
The invention relates to a novel flame retardant-stabilizer combination for thermoplastic polymers, comprising, as component A, from 25 to 99.9% by weight of a phosphinic acid salt of the formula (I) wherein R.sup.1, R.sup.2 are the same or different and are each C.sub.1-C.sub.8-alkyl, linear or branched, C.sub.6-C.sub.18-aryl, C.sub.7-C.sub.18-arylalkyl or C.sub.7-C.sub.18-alkylaryl, or R.sup.1 and R.sub.2 form one or more rings with each other, M is Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr, Ce, Bi, Sr, Mn, Li, Na, K and/or a protonated nitrogen base; m is from 1 to 4; as component B, from 0 to 75% by weight of a synergist or of a phosphorus/nitrogen flame retardant and, as component C, from 0.1 to 30% by weight of telomeric phosphinic acid salts as component D, from 0 to 20% by weight of organo phosphonic acid salt, as component E, from 0 to 5% by weight of phosphonic acid salt, the sum of the components always being 100% by weight, and wherein the angle of repose of said flame retardant-stabilizer combination is between 5 and 45.
##STR00001##
Claims
1. A flame retardant-stabilizer combination for thermoplastic polymers, comprising, as component A, from 25 to 99.9% by weight of a phosphinic acid salt of the formula (I) ##STR00007## wherein R.sup.1, R.sup.2 are the same or different and are each C.sub.1-C.sub.18-alkyl, linear or branched, C.sub.6-C.sub.18-aryl, C.sub.7-C.sub.18-arylalkyl or C.sub.7-C.sub.18-alkylaryl, or R.sup.1 and R.sup.2 form one or more rings with each other, M is Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr, Ce, Bi, Sr, Mn, Li, Na, K and/or a protonated nitrogen base; m is from 1 to 4; as component B, from 0 to 75% by weight of a synergist or of a phosphorus/nitrogen flame retardant, as component C, from 0.1 to 30% by weight of telomeric phosphinic acid salts, as component D, from 0 to 20% by weight of organo phosphonic acid salt, and as component E, from 0 to 5% by weight of phosphonic acid salt, the sum of the components always being 100% by weight, and wherein the angle of repose of said flame retardant-stabilizer combination is between 5 and 45.
2. A flame retardant-stabilizer combination as claimed in claim 1, wherein the angle of repose of said flame retardant-stabilizer combination is between 20 and 400.
3. A flame retardant-stabilizer combination as claimed in claim 1, wherein R.sup.1, R.sup.2 are the same or different and are each methyl, ethyl, n-propyl, isopropyl, n-butyl, tert-butyl, n-pentyl, 2-pentyl, 3-pentyl, 2-methylbutyl, 3-methylbutyl (iso-mentyl), 3-methylbut-2-yl, 2-methylbut-2-yl, 2,2-dimethylpropyl (neopentyl), hexyl, heptyl, octyl, nonyl, decyl, cyclopentyl, cyclopentylethyl, cyclohexyl, cyclohexylethyl, phenyl, phenylethyl, methylphenyl und/oder methylphenylethyl
4. A flame retardant-stabilizer combination as claimed in claim 1, wherein M is a calcium, aluminum, zinc, titanium or iron ion.
5. A flame retardant-stabilizer combination as claimed in claim 1, wherein component B comprises one or more of groups a)-e) a) condensation products of melamine, b) reaction products of melamine with polyphosphoric acid and/or reaction products of condensation products of melamine with polyphosphoric acid or mixtures thereof, c) phosphates of the formulae (NH.sub.4).sub.y H.sub.3-y PO.sub.4 or (NH.sub.4 PO.sub.3).sub.z, where y is from 1 to 3 and z is from 1 to 10 000, d) N-synergists of the formulae (III) to (VIII) or mixtures thereof ##STR00008## where R.sup.5 to R.sup.7 are each hydrogen, C.sub.1-C.sub.8-alkyl, C.sub.5-C.sub.16-cycloalkyl or -alkylcycloalkyl, possibly substituted by a hydroxyl or a C.sub.1-C.sub.4-hydroxyalkyl function, C.sub.2-C.sub.8-alkenyl, C.sub.1-C.sub.8-alkoxy, -acyl, -acyloxy, C.sub.6-C.sub.12-aryl or -arylalkyl, OR.sup.8 and N(R.sup.8)R.sup.9, N-alicyclic or N-aromatic, R.sup.8 is hydrogen, C.sub.1-C.sub.8-alkyl, C.sub.5-C.sub.16-cycloalkyl or -alkylcycloalkyl, possibly substituted by a hydroxyl or a C.sub.1-C.sub.4-hydroxyalkyl function, C.sub.2-C.sub.8-alkenyl, C.sub.1-C.sub.8-alkoxy, -acyl, -acyloxy or C.sub.6-C.sub.12-aryl or -arylalkyl, R.sup.9 to R.sup.13 are each the same groups as R.sup.8 and also OR.sup.8, m and n are each independently of 1, 2, 3 or 4, X is an acid which can form adducts with triazine compounds (III); or oligomeric esters of tris(hydroxyethyl) isocyanurate with aromatic polycarboxylic acids, e) aluminium phosphites.
6. A flame retardant-stabilizer combination as claimed in claim 5, wherein the condensation products a) of melamine are melem, melam, melon and/or more highly condensed compounds thereof; the reaction products of melamine b) are dimelamine pyrophosphate, melamine polyphosphate, melem polyphosphate, melam polyphosphate, melon polyphosphate and/or mixed polysalts of this type; the phosphates c) are ammonium hydrogenphosphate, ammonium dihydrogenphosphate and/or ammonium polyphosphate; the N-synergists d) are benzoguanamine, tris(hydroxyethyl) isocyanurate, allantoin, glycouril, melamine, melamine cyanurate, dicyandiamide and/or guanidine; the aluminium phosphites e) are of the formula (X), (XI) and/or (XII)
Al.sub.2(HPO.sub.3).sub.3(H.sub.2O).sub.q(X) where q is 0 to 4
Al.sub.2.00M.sub.z(HPO.sub.3).sub.y(OH).sub.v(H.sub.2O).sub.w(XI) where M are Alkali metal ions z 0.01 to 1.5 y 2.63 to 3.5 v 0 to 2 and w 0 to 4,
Al.sub.2.00(HPO.sub.3).sub.u(H.sub.2PO.sub.3).sub.t(H.sub.2O).sub.s(XII) where u is 2 to 2.99 t 2 to 0.01 and s 0 to 4 and/or mixtures of aluminium phosphite of formula (X) with aluminium salt of limited solubility and nitrogen free ions, mixtures of aluminium phosphite of formula (XII) with aluminium salts, aluminium phosphite [Al(H2PO.sub.3).sub.3], secondary aluminium phosphite [Al.sub.2(HPO.sub.3).sub.3], basic aluminium phosphite [Al(OH)(H.sub.2PO.sub.3).sub.2*2aq], aluminium phosphite tetrahydrate [Al.sub.2(HPO.sub.3).sub.3*4aq], aluminium phosphonate, Al.sub.7(HPO.sub.3).sub.9(OH).sub.6(1,6-hexandiamine).sub.1.5*12H.sub.2O, Al.sub.2(HPO.sub.3).sub.3*Al.sub.2O.sub.3*nH.sub.2O with x=2.27-1, Al.sub.4H.sub.6P.sub.16O.sub.18 and/or mixtures of 0-99.9 wt.-% Al.sub.2(HPO.sub.3).sub.3*nH.sub.2O with 0.1-100 Gew.-% sodium aluminium phosphite.
7. A flame retardant-stabilizer combination as claimed in claim 1, wherein the aluminium phosphite is a mixture of 50-99 wt.-% Al.sub.2(HPO.sub.3).sub.3(H.sub.2O).sub.q where q is 0 to 4 with 1-50 wt.-% sodium aluminium phosphite.
8. A flame retardant-stabilizer combination as claimed in claim 1, wherein the aluminium phosphite is a mixture of 50-99 wt.-% Al.sub.2(HPO.sub.3).sub.3(H.sub.2O).sub.q where q is 0 to 4 with 1-50 wt.-% Al.sub.2.00M.sub.z(HPO.sub.3).sub.y(OH).sub.v(H.sub.2O).sub.w (II) where M is sodium, z is 0.005 to 0.15, y is 2.8 to 3.1, v is 0 to 0.4 and w is 0 to 4.
9. A flame retardant-stabilizer combination as claimed in claim 1, wherein component B is melamine polyphosphate.
10. A flame retardant-stabilizer combination as claimed in claim 1, wherein component C is a telomeric phosphinic acid salt of formula (XIII)
H(C.sub.wH.sub.2w).sub.kP(O)(OMe)(C.sub.xH.sub.2x).sub.lH(XIII) where, in formula (XIII), independently from each other, k is from 1 to 9, l is from 1 to 9, w is from 2 to 9, x is from 2 to 9, Me is minimum one of the cations of the group Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na and/or K.
11. A flame retardant-stabilizer combination as claimed in claim 10, wherein in formula (XIII) w and x are from 2 to 4 and k and l are from 1 to 4.
12. A flame retardant-stabilizer combination as claimed in claim 10, wherein in formula (XIII) w and x are from 2 or 3 and k and l are from 1 to 3.
13. A flame retardant-stabilizer combination as claimed in claim 10, wherein Me is a cation of the group Al, Ti, Fe and/or Zn.
14. A flame retardant-stabilizer combination as claimed in claim 1, wherein the telomeric phosphinic acid salts are metal salts of ethyl butyl phosphinic acid, dibutyl phosphinic acid, ethyl hexyl phosphinic acid, butyl hexyl phosphinic acid, ethyl octyl phosphinic acid, sec-butyl ethyl phosphinic acid, 1-ethylbutyl-butyl-phosphinic acid, ethyl-1-methylpentyl-phosphinic acid, di-sec-butyl phosphinic acid (di-1-methyl-propyl phosphinic acid), propyl-hexyl phosphinic acid, dihexyl phosphinic acid, hexyl-nonyl phosphinic acid, propyl-nonyl phosphinic acid, dinonyl phosphinic acid, dipropyl phosphinic acid, butyl-octyl phosphinic acid, hexyl-octyl phosphinic acid, dioctyl phosphinic acid, ethyl cyclopentylethyl phosphinic acid, butyl cyclopentylethyl phosphinic acid, ethyl cyclohexylethyl phosphinic acid, butyl cyclohexylethyl phosphinic acid, ethyl phenylethyl phosphinic acid, butyl phenylethyl phosphinic acid, ethyl 4-methylphenylethyl phosphinic acid, butyl 4-methylphenylethyl phosphinic acid, butyl cyclopentyl phosphinic acid, butyl cyclohexylethyl phosphinic acid, butylphenyl phosphinic acid, ethyl 4-methylphenyl phosphinic acid and/or butyl 4-methylphenyl phosphinic acid and wherein the metal is minimum one of the group Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na and/or K.
15. A flame retardant-stabilizer combination as claimed in claim 1, comprising as component A, from 70 to 99.99% by weight of a phosphinic acid salt of the formula (I) ##STR00009## wherein R.sup.1, R.sup.2 are the same or different and are each C.sub.1-C.sub.18-alkyl, linear or branched, C.sub.6-C.sub.18-aryl, C.sub.7-C.sub.18-arylalkyl or C.sub.7-C.sub.18-alkylaryl, or R.sup.1 and R.sup.2 form one or more rings with each other, M is Mg, Ca, Al, Sb, Sn, Ge, Ti, Zn, Fe, Zr, Ce, Bi, Sr, Mn, Li, Na, K and/or a protonated nitrogen base; m is from 1 to 4 and, as component C, from 0.01 to 30% by weight of at least one telomeric phosphinic acid salt of the type ethyl butyl phosphinic acid, dibutyl phosphinic acid, ethyl hexyl phosphinic acid, butyl hexyl phosphinic acid, ethyl octyl phosphinic acid, sec-butyl ethyl phosphinic acid, 1 ethylbutyl-butyl-phosphinic acid, ethyl-1-methylpentyl-phosphinic acid, di-sec-butyl phosphinic acid (di-1-methyl-propyl phosphinic acid), propyl-hexyl phosphinic acid, dihexyl phosphinic acid, hexyl-nonyl phosphinic acid, propyl-nonyl phosphinic acid, dinonyl phosphinic acid, dipropyl phosphinic acid, butyl-octyl phosphinic acid, hexyl-octyl phosphinic acid, dioctyl phosphinic acid, ethyl cyclopentylethyl phosphinic acid, butyl cyclopentylethyl phosphinic acid, ethyl cyclohexylethyl phosphinic acid, butyl cyclohexylethyl phosphinic acid, ethyl phenylethyl phosphinic acid, butyl phenylethyl phosphinic acid, ethyl 4-methylphenylethyl phosphinic acid, butyl 4-methylphenylethyl phosphinic acid, butyl cyclopentyl phosphinic acid, butyl cyclohexylethyl phosphinic acid, butylphenyl phosphinic acid, ethyl 4-methylphenyl phosphinic acid and/or butyl 4-methylphenyl phosphinic acid, where the metal of said salt is minimum one of the group Mg, Ca, Al, Sb, Sn, Ge, Ti, Fe, Zr, Zn, Ce, Bi, Sr, Mn, Li, Na and/or K; wherein the component B is different to component A; and wherein the angle of repose of said high-flow mixture is between 5 and 45.
16. A flame retardant-stabilizer combination as claimed in claim 1, wherein component D is alkyl phosphonate according to formula (II) ##STR00010## wherein R.sup.3 is an ethyl, propyl and/or butyl group, M is Mg, Ca, Al, Zn or Fe and m is from 1 to 4.
17. A flame retardant-stabilizer combination as claimed in claim 1, wherein component D is a phosphite according to formula (IX); ##STR00011## wherein R.sup.3 is H, M is Mg, Ca, Al, Zn or Fe and m is from 1 to 4.
18. A flame retardant-stabilizer combination as claimed in claim 1, wherein from 25 to 99.9% by weight of component A, from 0 to 75% by weight of component B, from 0.1 to 15% by weight of component C, from 0 to 10% by weight of component D and from 0 to 2% by weight of component E are present.
19. A flame retardant-stabilizer combination as claimed in claim 1, wherein from 25 to 99.8% by weight of component A, from 0 to 75% by weight of component B, from 0.1 to 10% by weight of component C, from 0.1 to 5% by weight of component D and from 0 to 2% by weight of component E are present.
20. A flame retardant-stabilizer combination as claimed in claim 1, wherein from 25 to 99.7% by weight of component A, from 0.1 to 75% by weight of component B, from 0.1 to 10% by weight of component C, from 0.1 to 5% by weight of component D and from 0 to 1% by weight of component E are present.
21. A flame retardant-stabilizer combination as claimed in claim 1, wherein the residual moisture content of said flame retardant-stabilizer combination is between 0.01 wt.-% and 10 wt.-%.
22. A flame retardant-stabilizer combination as claimed in claim 1, wherein the residual moisture content of said flame retardant-stabilizer combination is between 0.1 wt.-% and 1 wt.-%.
23. A flame retardant-stabilizer combination as claimed in claim 1, wherein the particle size of said flame retardant-stabilizer combination is between 1 m and 100 m.
24. A flame retardant-stabilizer combination as claimed in claim 1, wherein the bulk density of said flame retardant-stabilizer combination is between 100 g/L and 1000 g/L.
25. A flame retardant-stabilizer combination as claimed in claim 1, wherein the tap density of said flame retardant-stabilizer combination is between 200 g/L and 1100 g/L.
26. The use of the flame retardant-stabilizer combination as claimed in claim 1, as a flame retardant or as an intermediate for preparation of flame retardants for thermoplastic polymers, for thermoset polymers, for clearcoats, for intumescent coatings, for wood and other cellulosic products, for polymer shaped body, film, thread or fiber, for production of flame-retardant polymer molding compositions, for production of flame-retardant polymer moldings and/or for rendering pure and blended polyester and cellulose fabrics flame-retardant by impregnation.
27. The use as claimed in claim 26, wherein the thermoplastic polymers are polyester, polystyrene and/or polyamide, and the thermoset polymers are unsaturated polyester resins, epoxy resins, polyurethanes and/or acrylates.
28. A flame-retardant plastics molding composition, polymer shaped body, film, thread or fiber comprising the flame retardant-stabilizer combination as claimed in claim 1.
29. A flame-retardant plastics molding composition, polymer shaped body, film, thread or fiber, as claimed in claim 28, wherein the plastics used are thermoplastic polymers of the type high-impact polystyrene, polyphenylene ether, polyamides, polyesters, polycarbonates, thermoplastic polyurethanes and blends or polymer blends of the type ABS (acrylonitrile-butadiene-styrene) or PC/ABS (polycarbonate/acrylonitrile-butadiene-styrene) or PPE/HIPS (polyphenylene ether/HI polystyrene) plastics.
30. A flame-retardant plastics molding composition, polymer shaped body, film, thread or fiber as claimed in claim 28, which comprises the flame retardant-stabilizer combination in an amount of from 2 to 50% by weight, based on the plastics molding composition.
31. A flame-retardant plastics molding composition, polymer shaped body, film, thread or fiber as claimed in claim 28, which comprises the flame retardant-stabilizer combination in an amount of from 10 to 30% by weight, based on the plastics molding composition.
32. A flame-retardant plastics molding composition, polymer shaped body, film, thread or fiber as claimed in claim 28 for the use in or for connectors, power wetted parts in current distributors (RCCB), boards, potting compounds, power connectors, circuit breakers, lamp housing, LED housing, condenser housing, bobbins and fans, protection contacts, connectors, in/on circuit boards, casings for connectors, cables, flexible circuit boards, charger for mobile phones, engine covers, textile coatings, moldings in the form of components for the electrical/electronics sector, in particular for parts of printed circuit boards, housings, films, cables, switches, distribution boards, relays, resistors, capacitors, coils, lamps, diodes, LEDs, transistors, connectors, controllers, memories and sensors, in the form of large-area components.
Description
EXAMPLES
1. Component s Used
Standard Commercial Polymers (Granules):
[0119] PA 6,6 GF: Durethan AKV 30 (Bayer AG, D), contains 30% glass fibers.
PBT GF: Celanex 2300 GV1/30 (Ticona, D), contains 30% glass fibers.
PA 6: Ultramid B 27 E
PA 6,6: Ultramid A 27 E (BASF)
[0120] Glass fiber: PPG Glass fiber HP 3610 EC 10 4.5 mm
Flame Retardant Components (Pulverulent):
[0121] Component A: Aluminum salts of diethylphosphinic acid, referred to hereinbelow as DEPAL. [0122] Component B: Melapur 200 (melamine polyphosphate, MPP), from BASF [0123] Component B: Aluminiumphosphite (AP) according to DE-A-102014001222 [0124] Component C1: Butylethyl phosphinic acid, aluminium salt [0125] Component C2: Dibutyl phosphinic acid, aluminium salt [0126] Component C3: Ethyl-phenylethyl phosphinic acid, aluminium salt [0127] Component D1: Ethyl phosphonic acid, aluminium salt [0128] Component D2: Butyl phosphonic acid, aluminium salt [0129] Component E1: Phosphonic acid, aluminium salt
2. Production, Processing and Testing of Flame-Retardant Plastics Molding Compositions
[0130] The flame-retardant component s were mixed with the polymer granules, lubricants and stabilizers in the ratio specified in the tables and incorporated in a Leistritz LSM 30/34 double-screw extruder at temperatures of from 260 to 310 C. (GFR PA-6,6) or from 240 to 280 C. (GFR PBT). The homogenized polymer strand was drawn off, cooled in a water bath and then granulated.
[0131] After sufficient drying, the molding compositions were processed to give test specimens on a Arburg 320 C Allrounder injection molding machine at temperatures of from 270 to 320 C. (GFR PA-6,6) or from 260 to 280 C. (GFR PBT) and, with the aid of the UL 94 test (Underwriter Laboratories), were tested for flame resistance and classified.
[0132] The flowability of the molding composition was determined by determining the melt volume index (MVR) at 275 C./2.16 kg. A sharp rise in the MVR value indicated polymer degradation.
[0133] The processing properties in polyester were assessed with reference to the specific viscosity (SV). After sufficient drying, the plastics molding composition granules were used to prepare a 1.0% solution in dichloroacetic acid and the SV value was determined. The higher the SV value is, the lower was the polymer degradation during the incorporation of the flame retardant.
[0134] Unless stated otherwise, all experiments of a particular series were carried out under identical conditions (temperature program, screw geometries, injection molding parameters, etc.) for the purpose of comparability.
[0135] Thus, for the inventive flame retardant-stabilizer combinations of components A, B, C, D and E an improvement in the angle of repose can be detected.
[0136] One can obtain an improvement in the angle of repose if only components A and C are used in the inventive flame retardant-stabilizer combination.
[0137] Unless stated otherwise, the amounts quoted are always in percent by weight.
[0138] In the present invention, angle of repose were used to evaluate the flowability of said dialkylphosphinate. For example, to measure the angle of repose, the powder sample was poured through a funnel and dropped down to a round plate with a radius of r. The powder was continuously poured into the funnel and accumulated into a cone-shaped pile growing up until the height of the pile did not increase. The height of the pile, h, was measured and the angle of repose, a, was calculated according to formula (1)
tg=h/r(1)
[0139] The smaller is, the better the flowability of the powder is. Generally, when is smaller than 30, the powder can flow freely; when is between 30 and 40, the powder can meet the processing requirements; when is greater than 40, the powder cannot meet the processing requirements.
Example 1 (Comparison)
[0140] A sample produced according to CN-A-104059101 was tested for its angle of repose. The result is listed in table 1.
Example 2
[0141] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component C1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 3
[0142] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component C1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 4
[0143] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component D1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 5
[0144] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component D1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 6
[0145] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 7
[0146] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and component E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 8
[0147] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C1 and D1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 9
[0148] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C2 and D2 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 10
[0149] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C1 and E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 11
[0150] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C2 and E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 12
[0151] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C1, D1 and E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 13
[0152] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate and components C3, D2 and E1 in types and amounts according to table 1. It was tested for its angle of repose, the result is listed in table 1 and is better than comparative example 1.
Example 14
[0153] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B and component C1 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
Example 14a (Comparison)
[0154] A flame retardant-stabilizer combination was mixed from 66.5 wt.-% aluminiumdiethylphosphinate and 33.8 wt.-% component B. It was tested for its angle of repose of 35 degrees, which was worse than pure aluminiumdiethylphosphinate.
Example 15
[0155] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B and component C1 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
Example 16
[0156] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B, component C1, component D1 and component E1 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
Example 17
[0157] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B, component C1, component D2 and component E1 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
Example 18
[0158] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B, component C1 and component D1 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
Example 18a (Comparison)
[0159] A flame retardant-stabilizer combination was mixed from 82.1 wt.-% aluminiumdiethylphosphinate and 17.9 wt.-% component B. It was tested for its angle of repose of 30 degrees, which was worse than pure aluminiumdiethylphosphinate.
Example 19
[0160] A flame retardant-stabilizer combination according to the invention was mixed from aluminiumdiethylphosphinate, component B, component C1 and component D2 in types and amounts according to table 1. It was tested for its angle of repose, the very good result is listed in table 1.
TABLE-US-00001 TABLE 1 Compositions of flame retardant-stabilizer combinations and angles of repose Alu- Angle minium- phos- component of pinate B C D E repose Example [wt.-%] [wt.-%] [wt.-%] [wt.-%] [wt.-%] [] 1 (Com) 100 25 2 99.9 C1 0.1 23 3 80 C1 20 24.9 4 99.99 D1 0.01 22.9 5 95 D1 5 24 6 99.99 E1 0.01 23.2 7 95 E1 5 24.5 8 99.69 C1 0.3 D1 0.01 24.1 9 93 C2 5 D2 2 24.7 10 99.69 C1 0.3 E1 0.01 24.2 11 94.7 C2 5 E1 0.3 24.5 12 99.68 C1 0.3 D1 0.01 E1 0.01 24.3 13 97.75 C3 2 D2 0.05 E1 0.2 24.5 14 66.2 MPP 32.6 C1 1.2 27 15 63.7 MPP 31.4 C1 5 30 16 66.2 MPP 32.6 C1 1.2 D1 0.03 E1 0.01 26 17 62.5 MPP 30.9 C1 5 D2 1.5 E1 0.2 27 18 81.5 AP 17.9 C1 0.6 D1 0.05 26 19 80.0 AP 17.6 C1 1.4 D2 1 26
Example 20
[0161] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component B, component C1 and zinc borate in glass fiber-reinforced PA-6 was produced in the composition according to table using a melt temperature on injection molding of 290 C.
Example 21
[0162] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component C3, component D2, component E1 and zinc borate in glass fiber-reinforced PA-6,6 was produced in the composition according to table using a melt temperature on injection molding of 300 C.
Example 22
[0163] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component B, component C1, component D1, component E1 in glass fiber-reinforced PA-6,6 was produced in the composition according to table using a melt temperature on injection molding of 300 C.
Example 23
[0164] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component B, component C1, component D1, component E1 in glass fiber-reinforced PA-6,6 was produced in the composition according to table using a melt temperature on injection molding of 300 C.
Example 24
[0165] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component B, component C1, component D1, component E1 in glass fiber-reinforced PA-6,6 was produced in the composition according to table using a melt temperature on injection molding of 300 C.
Example 25
[0166] An inventive flame-retardant molding composition comprising the combination of aluminiumdiethylphosphinate, component B and component C in glass fiber-reinforced PBT was produced in the composition according to table using a melt temperature on injection molding of 275 C.
TABLE-US-00002 TABLE 2 Compositions of flame-retardant molding compositions and test results Glas fiber Zinc Flame retard.-stab. UL 94 class Polymer (calc.) borate comb (0.8 mm) Example Type [wt.-%] [wt.-%] [wt.-%] acc. to exp. [wt.-%] [-] 20 PA 6 52 30 0.72 14 18 V-0 21 PA 6, 6 80 0 0.8 13 20 V-0 22 PA 6, 6 72 10 16 18 V-0 23 PA 6, 6 GF 82 (24.6) 18 18 V-0 24 PA 6, 6 42 40 16 18 V-0 25 PBT GF 82 (24.6) 16 18 V-0
[0167] In general the angle of repose of aluminiumdiethylphosphinate plus components C and/or D and/or E are better than of pure aluminiumdiethylphosphinate (comparison example).
[0168] The angle of repose of aluminiumdiethylphosphinate plus components B and C and/or D and/or E are better than of aluminiumdiethylphosphinate plus components B (comparison example 14a, 18a).