阅读说明：本技术 玻璃纤维填充的阻燃性聚丙烯组合物 (Glass fiber filled flame retardant polypropylene composition ) 是由 温亮 于 2019-09-24 设计创作，主要内容包括：本发明涉及玻璃纤维填充的阻燃性聚丙烯组合物,其包含：(A)基于聚丙烯的聚合物,(B)总组合物的15至40重量％的量的第一阻燃剂,其中所述第一阻燃剂为包含聚磷酸铵和至少一种选自以下的磷酸酯/盐的颗粒的形式：磷酸三聚氰胺、聚磷酸三聚氰胺、焦磷酸三聚氰胺、磷酸哌嗪、聚磷酸哌嗪、焦磷酸哌嗪、单磷酸2-甲基哌嗪、磷酸三甲酚酯、磷酸烷基酯、磷酸卤代烷基酯、焦磷酸四苯酯、聚(2-羟基丙烯螺环季戊四醇双磷酸酯),和聚(2,2-二甲基丙烯螺环季戊四醇双膦酸酯),和(C)总组合物的0.1至15重量％的量的第二阻燃剂,其中所述第二阻燃剂包含芳族磷酸酯,和(D)总组合物的5至40重量％的量的玻璃纤维。(The present invention relates to a glass fiber filled flame retardant polypropylene composition comprising: (A) a polypropylene-based polymer, (B) a first flame retardant in an amount of 15 to 40 wt.% of the total composition, wherein the first flame retardant is in the form of particles comprising ammonium polyphosphate and at least one phosphate selected from the group consisting of: melamine phosphate, melamine polyphosphate, melamine pyrophosphate, piperazine phosphate, piperazine polyphosphate, piperazine pyrophosphate, 2-methylpiperazine monophosphate, tricresyl phosphate, alkyl phosphate, haloalkyl phosphate, tetraphenyl pyrophosphate, poly (2-hydroxypropylspiropentaerythritol diphosphonate), and poly (2, 2-dimethylpropylenespiropentaerythritol diphosphonate), and (C) a second flame retardant in an amount of 0.1 to 15% by weight of the total composition, wherein the second flame retardant comprises an aromatic phosphate ester, and (D) glass fibers in an amount of 5 to 40% by weight of the total composition.)

1. Glass fiber filled flame retardant polypropylene composition comprising

(A) A propylene-based polymer which is a propylene-based polymer,

(B) a first flame retardant in an amount of 15 to 40 wt% of the total composition, wherein the first flame retardant is in the form of particles comprising ammonium polyphosphate and at least one phosphate ester selected from

Melamine phosphate,

Polyphosphoric acid melamine,

Melamine pyrophosphate,

Piperazine phosphate,

Polyphosphoric acid piperazine,

Piperazine pyrophosphate,

2-methylpiperazine monophosphate,

Tricresyl phosphate, a salt thereof, a process for preparing the same and a use of the same,

An alkyl phosphate ester,

A halogenated alkyl phosphate,

Tetraphenyl pyrophosphate,

Poly (2-hydroxypropylspirocyclic pentaerythritol diphosphate), and

poly (2, 2-dimethylpropylene spiropentaerythritol diphosphonate), and

(C) a second flame retardant in an amount of 0.1 to 15 wt% of the total composition, wherein the second flame retardant comprises an aromatic phosphate ester, and

(D) glass fibers in an amount of 5 to 40 wt.% of the total composition.

2. The composition of claim 1, wherein the polypropylene-based polymer comprises a propylene homopolymer or a propylene-a-olefin copolymer consisting of at least 70 wt% propylene and up to 30 wt% a-olefin, based on the total weight of the copolymer, wherein the a-olefin is selected from a-olefins having 2 or 4-10 carbon atoms.

3. Composition according to any one of the preceding claims, in which the polypropylene-based polymer comprises a heterophasic propylene copolymer consisting of

(a) A matrix based on propylene, the matrix being,

wherein the propylene-based matrix consists of a propylene homopolymer and/or a propylene copolymer consisting of at least 70 wt% propylene monomer units and up to 30 wt% ethylene and/or alpha-olefin monomer units, based on the total weight of the propylene-based matrix, and

wherein the propylene-based matrix is present in an amount of from 60 to 95 wt. -%, based on the total heterophasic propylene copolymer, and

(b) a dispersed ethylene-alpha-olefin copolymer,

wherein the dispersed ethylene-alpha-olefin copolymer is present in an amount of from 40 to 5 wt. -%, based on the total heterophasic propylene copolymer, and

wherein the sum of the total amount of propylene-based matrix and the total amount of dispersed ethylene-alpha-olefin copolymer in the heterophasic propylene copolymer is 100 wt%,

preferably, the propylene copolymer of the matrix consists of propylene monomer units and ethylene and/or alpha-olefin monomer units, wherein the alpha-olefin is selected from alpha-olefins having 2 or 4 to 10 carbon atoms, and

preferably, the dispersed ethylene-a-olefin copolymer consists of ethylene and an a-olefin selected from a-olefins having from 3 to 8 carbon atoms.

4. The composition of any preceding claim, wherein the first flame retardant has a normal particle size distribution (D50) of at least 8 microns as determined by a Mastersizer 2000 available from Malvern.

5. The composition of any preceding claim, wherein the amount of phosphate ester/salt in the first flame retardant is 40-75 wt%, as measured using an ICP-OES spectrometer (iCAP 6300Duo, available from Thermo Fisher) after treatment with nitric acid.

6. The composition of any of the preceding claims, wherein the first flame retardant comprises melamine phosphate.

7. The composition of any of the preceding claims, the first flame retardant further comprising zinc oxide.

8. The composition of any preceding claim, wherein the amount of ammonium polyphosphate in the first flame retardant is from 5 to 15 weight percent.

9. The composition according to any one of the preceding claims, wherein

The amount of the ammonium polyphosphate in the first flame retardant is 5-15 wt%,

the amount of melamine phosphate in the first flame retardant is 50 to 80 wt%,

the amount of piperazine phosphate in the first flame retardant is 10-25 wt%, and

the amount of zinc oxide in the first flame retardant is 1-10 wt%.

10. The composition of any of the preceding claims, wherein the aromatic phosphate is selected from the group consisting of resorcinol bis (diphenyl phosphate);

tetraphenylresorcinol bis (diphenyl phosphate);

bisphenol a bis (diphenyl phosphate);

bisphenol a diphosphate;

resorcinol bis (di-2, 6-xylyl phosphate),

mixed esters of phosphoric acid with [1,1'-biphenyl ] -4-4' -diol and phenol;

resorcinol bis (diphenyl phosphate);

1, 3-phenylene-tetrakis (2, 6-dimethylphenyl) diphosphate;

isopropenylphenyl diphenyl phosphate;

4-phenylphenol formaldehyde phenylphosphonate;

tris (2, 6-xylyl) phosphate;

resorcinol bis (di-2, 6-xylyl phosphate);

bisphenol S bis (diphenyl phosphate);

resorcinol-bisphenol a phenyl phosphate.

11. Composition according to any one of the preceding claims, wherein the amount of (A) is from 50 to 90% by weight, such as from 55 to 85% by weight or from 60 to 80% by weight, relative to the total composition.

12. The composition of any of the preceding claims wherein the total amount of (A), (B), (C) and (D) is at least 90% by weight of the total composition.

13. Composition according to any one of the preceding claims, the composition according to the invention having at least 4.0kJ/m²According to ISO 179-1:2010 at 23 ℃ (test geometry: 80 x 10 x 4mm) notched simple beam impact strength.

14. A process for preparing the composition of any preceding claim, comprising melt mixing (a), (B), (C), and (D), and optional components.

15. An article comprising the composition according to any one of claims 1 to 13, preferably wherein the article is selected from the group consisting of battery racks and covers in electric vehicles, housings, lids and closures for (micro) circuit breakers, batteries, tubs, containers, exterior and interior parts in appliances, such as printed circuit board holders, breaker covers, liquid trays in refrigerators, deflection coils for televisions, stadium seats, exterior parts of automobiles, such as bumpers, interior parts of automobiles, such as instrument panels, and automotive parts under the hood.

Examples

The materials shown in table 1 were used in the experiments.

TABLE 1

The polypropylene is premixed with the additives and the mixture is extruded using a twin-screw extruder to obtain pellets. The pellets were dried at 100 ℃ for 3h and injection molded using a FANUC injection molding machine (S-2000i) to prepare test specimens.

The MFI of the compositions was measured according to ISO1133-1:2011(2.16kg/230 ℃).

Flame retardancy was measured according to UL94 test standards at sample thicknesses of 3mm, 1.5mm, and 0.8 mm. The samples were aged for 48 hours at 23 ℃ and 50% relative humidity or 168 hours at 70 ℃ and 50% relative humidity prior to testing. The sample bars were burned at the gated end to evaluate Vx.

The Impact strength of the simply-supported beam was measured at 23 ℃ according to ISO 179-1:2010 by a Toyoseiki Digital Impact DG-UB equipped with a 2J pendulum (test geometry: 80 × 10 × 4 mm).

Flexural modulus was measured according to ISO 178:2010 (parallel; test geometry: 80 x 10 x 4 mm).

Tensile testing was performed at room temperature according to ISO527-1: 2012.

The results are summarized in tables 2 and 3. In table 2, the propylene-based polymer is a propylene homopolymer and the glass fibers are long glass fibers. In table 3, the propylene-based polymer is a mixture of propylene homopolymer and heterophasic propylene copolymer and the glass fibers are short glass fibers.

TABLE 2

From a comparison of CE1 with the same amount of flame retardant compared to Ex2, it can be understood that the use of a combination of FR1 and FR2 (Ex2) results in better flame retardancy in a glass fiber filled composition than FR1(CE1) alone.

From the comparison of CE3 with CE4, it can be understood that also in non-glass fiber filled compositions, the use of a combination of FR1 and FR2 (CE4) results in better flame retardancy than the use of FR1 alone (CE 3). However, from the comparison of CE4 with Ex5, Ex6 and Ex7, in which the amount of glass fiber was varied, it is understood that the presence of glass fiber resulted in better flame retardancy. Thus, very good flame retardancy was achieved using a combination of FR1 and FR2 in a glass fiber filled composition.

From the comparison of CE5 with Ex7, it can be seen that Ex7 balances higher melt flow (compared to CE 5) with good impact, flexural modulus, and flame retardancy.

TABLE 3

It is understood from the comparison of Ex8-10 that higher amounts of FR1 in combination with FR 1B lead to better flame retardancy.

As can be understood from the comparison of Ex 11 with Ex12, higher amounts of glass fiber resulted in better flame retardancy.