CN104861513A - Halogen-free flame retardation reinforcing polytrimethylene terephthalate composition - Google Patents

Abstract

The invention discloses a halogen-free flame retardation reinforcing polytrimethylene terephthalate composition. The composition comprises the following ingredients, by weight, 70%-90% of PTT, 5%-15% of inorganic filling material, 3%-10% of halogen-free flame retardants, 2%-4% of plasticizers, 0.5%-1% of anti-hydrolysis agents, 0.1%-0.5% of coupling agents, 0.1%-0.5% of anti-oxidants and 0.1%-1% of lubricants. The inorganic filling material is one selected from wollastonite, talcum, mica, kaolin and calcium carbonate. The halogen-free flame retardants halogen-free flame retardants are a mixture of 60-70wt% of polysulfonyldiphenylene phenyl phosphonate, 30-35wt% of polydimethylsiloxane and 1-5 wt% of polytetrafluoroethylene after uniform mixing. The beneficial effects are that the composition has characteristics of high intensity, good flame retardation, excellent heat resistance and the like, and the halogen-free, smoke inhibition, no droplet and UL94V-0 level flame retardation effects are achieved.

Description

Halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition

Technical field

The present invention relates to technical field of polymer materials, specifically a kind of halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition.

Background technology

Poly(Trimethylene Terephthalate) (PTT) is as a kind of new polyester macromolecular material of excellent combination property, the fields such as fiber, film, engineering plastics are widely used at present, but PTT is used alone exists that its intensity is not high, thermotolerance is bad, the problem of poor fire, limit its application.

Summary of the invention

The object of the present invention is to provide a kind of halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition.

The technical solution adopted for the present invention to solve the technical problems is: halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition, and its component by mass percent proportioning is: PTT 70% ~ 90%, mineral filler 5% ~ 15%, halogen-free flame retardants 3% ~ 10%, softening agent 2% ~ 4%, hydrolysis-resisting agent 0.5% ~ 1%, coupling agent 0.1% ~ 0.5%, oxidation inhibitor 0.1% ~ 0.5%, lubricant 0.1% ~ 1%.

Described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g.

Described mineral filler is the one in wollastonite, talcum, mica, kaolin, calcium carbonate.

Described halogen-free flame retardants is mixed by polyphenylene phosphonic acids sulfobenzide ester 60 ~ 70wt%, polydimethylsiloxane 30 ~ 35wt% and tetrafluoroethylene 1 ~ 5wt% three and obtained compound.

Described softening agent is phthalic acid two (2-ethylhexyl ester) or dibutyl phthalate.

Described hydrolysis-resisting agent is carbodiimide.

Described coupling agent is the one in γ-aminopropyltrimethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidoxypropyltrime,hoxysilane, β-(1,1-epoxy group(ing) cyclohexyl) ethyl trimethoxy silane.

Described oxidation inhibitor is the one in the compound of antioxidant 1010, antioxidant 1076, antioxidant 1010 or antioxidant 1076 and irgasfos 168.

Described lubricant is the one in sodium stearate, calcium stearate, ethylene bis stearamide, pentaerythritol stearate.

The preparation method of above-mentioned halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition, comprises the following steps:

(1) drying about 6 ~ 8 hours at 110 DEG C ~ 120 DEG C temperature of forced air circulation baking oven, by PTT is placed in, stand-by;

(2) take mineral filler and coupling agent, by weight ratio, add a material temperature degree in the high-speed mixer of 80 DEG C ~ 120 DEG C, after rotating speed 3000 ~ 4500 revs/min stirs 10 ~ 45 minutes, be cooled to lower than 40 DEG C of dischargings stand-by;

(3) polyphenylene phosphonic acids sulfobenzide ester 60 ~ 70wt%, polydimethylsiloxane 30 ~ 35wt% and tetrafluoroethylene 1 ~ 5wt%, is taken by weight ratio, make to mix, with obtained described halogen-free flame retardants, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by;

(4) dry PTT, is taken by weight ratio and the obtained halogen-free flame retardants of step (3) adds in high-speed mixer, add the softening agent, hydrolysis-resisting agent, oxidation inhibitor and the lubricant that take by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 15 minutes together, discharging after fully mixing;

(5), the compound of step (4) is added in twin screw extruder, extrudes after melt blending at 180 DEG C ~ 260 DEG C, cooling granulation, then dry, obtain halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition of the present invention.

The invention has the beneficial effects as follows, the present invention has the features such as intensity is high, good flame resistance, excellent heat resistance, and meet Halogen, press down cigarette, without molten drop and UL94 V-0 level flame retardant effect.

Embodiment

Technical scheme of the present invention is further illustrated below in conjunction with concrete preferred embodiment.

Embodiment 1:

A kind of halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition, its component by mass percent proportioning is: PTT 70%, wollastonite 15%, halogen-free flame retardants 10%, phthalic acid two (2-ethylhexyl ester) 3%, carbodiimide 1%, γ-aminopropyltrimethoxysilane 0.2%, antioxidant 1010 0.2%, sodium stearate 0.6%, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described halogen-free flame retardants is by polyphenylene phosphonic acids sulfobenzide ester 65wt%, polydimethylsiloxane 30wt% and tetrafluoroethylene 5wt% three mix and obtained compound.

Preparation method: (1), PTT is placed in the drying about 6 ~ 8 hours at 110 DEG C ~ 120 DEG C temperature of forced air circulation baking oven, stand-by; (2) take wollastonite and γ-aminopropyltrimethoxysilane, by weight ratio, add a material temperature degree in the high-speed mixer of 80 DEG C ~ 120 DEG C, after rotating speed 3000 ~ 4500 revs/min stirs 10 ~ 45 minutes, be cooled to lower than 40 DEG C of dischargings stand-by; (3) take polyphenylene phosphonic acids sulfobenzide ester 65wt%, polydimethylsiloxane 30wt% and tetrafluoroethylene 5wt%, by weight ratio, make to mix, with obtained described halogen-free flame retardants, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by; (4) dry PTT, is taken by weight ratio and the obtained halogen-free flame retardants of step (3) adds in high-speed mixer, add simultaneously take by weight ratio phthalic acid two (2-ethylhexyl ester), carbodiimide, antioxidant 1010, sodium stearate, and add the product that step (2) obtains, make to stir 3 ~ 15 minutes together, discharging after fully mixing; (5), the compound of step (4) is added in twin screw extruder, extrudes after melt blending at 180 DEG C ~ 260 DEG C, cooling granulation, then dry, obtain halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition of the present invention.

Embodiment 2:

A kind of halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition, its component by mass percent proportioning is: PTT 80%, calcium carbonate 10%, halogen-free flame retardants 6%, dibutyl phthalate 3%, carbodiimide 0.5%, γ-glycidoxypropyltrime,hoxysilane 0.1%, the compound 0.1% of antioxidant 1076 and irgasfos 168, pentaerythritol stearate 0.3%, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described halogen-free flame retardants is by polyphenylene phosphonic acids sulfobenzide ester 64wt%, polydimethylsiloxane 32wt% and tetrafluoroethylene 4wt% three mix and obtained compound.

Preparation method: (1), PTT is placed in the drying about 6 ~ 8 hours at 110 DEG C ~ 120 DEG C temperature of forced air circulation baking oven, stand-by; (2) calcium carbonate and γ-glycidoxypropyltrime,hoxysilane, is taken by weight ratio, add a material temperature degree in the high-speed mixer of 80 DEG C ~ 120 DEG C, after rotating speed 3000 ~ 4500 revs/min stirs 10 ~ 45 minutes, be cooled to lower than 40 DEG C of dischargings stand-by; (3) take polyphenylene phosphonic acids sulfobenzide ester 64wt%, polydimethylsiloxane 32wt% and tetrafluoroethylene 4wt%, by weight ratio, make to mix, with obtained described halogen-free flame retardants, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by; (4) dry PTT, is taken by weight ratio and the obtained halogen-free flame retardants of step (3) adds in high-speed mixer, add compound, the pentaerythritol stearate of dibutyl phthalate, carbodiimide, antioxidant 1076 and the irgasfos 168 taken by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 15 minutes together, discharging after fully mixing; (5), the compound of step (4) is added in twin screw extruder, extrudes after melt blending at 180 DEG C ~ 260 DEG C, cooling granulation, then dry, obtain halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition of the present invention.

Claims (9)

1. a halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition, it is characterized in that, its component by mass percent proportioning is: PTT 70% ~ 90%, mineral filler 5% ~ 15%, halogen-free flame retardants 3% ~ 10%, softening agent 2% ~ 4%, hydrolysis-resisting agent 0.5% ~ 1%, coupling agent 0.1% ~ 0.5%, oxidation inhibitor 0.1% ~ 0.5%, lubricant 0.1% ~ 1%.

2. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, described mineral filler is the one in wollastonite, talcum, mica, kaolin, calcium carbonate.

3. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, it is characterized in that, described halogen-free flame retardants is mixed by polyphenylene phosphonic acids sulfobenzide ester 60 ~ 70wt%, polydimethylsiloxane 30 ~ 35wt% and tetrafluoroethylene 1 ~ 5wt% three and obtained compound.

4. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, described softening agent is phthalic acid two (2-ethylhexyl ester) or dibutyl phthalate.

5. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, described hydrolysis-resisting agent is carbodiimide.

6. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, it is characterized in that, described coupling agent is the one in γ-aminopropyltrimethoxysilane, N-β-(aminoethyl)-γ-aminopropyltrimethoxysilane, γ-glycidoxypropyltrime,hoxysilane, β-(1,1-epoxy group(ing) cyclohexyl) ethyl trimethoxy silane.

7. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, described oxidation inhibitor is the one in the compound of antioxidant 1010, antioxidant 1076, antioxidant 1010 or antioxidant 1076 and irgasfos 168.

8. halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, described lubricant is the one in sodium stearate, calcium stearate, ethylene bis stearamide, pentaerythritol stearate.

9. the preparation method of halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition according to claim 1, is characterized in that, comprise the following steps:

(1) drying about 6 ~ 8 hours at 110 DEG C ~ 120 DEG C temperature of forced air circulation baking oven, by PTT is placed in, stand-by;

(2) take mineral filler and coupling agent, by weight ratio, add a material temperature degree in the high-speed mixer of 80 DEG C ~ 120 DEG C, after rotating speed 3000 ~ 4500 revs/min stirs 10 ~ 45 minutes, be cooled to lower than 40 DEG C of dischargings stand-by;

(3) polyphenylene phosphonic acids sulfobenzide ester 60 ~ 70wt%, polydimethylsiloxane 30 ~ 35wt% and tetrafluoroethylene 1 ~ 5wt%, is taken by weight ratio, make to mix, with obtained described halogen-free flame retardants, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by;

(4) dry PTT, is taken by weight ratio and the obtained halogen-free flame retardants of step (3) adds in high-speed mixer, add the softening agent, hydrolysis-resisting agent, oxidation inhibitor and the lubricant that take by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 15 minutes together, discharging after fully mixing;

(5), the compound of step (4) is added in twin screw extruder, extrudes after melt blending at 180 DEG C ~ 260 DEG C, cooling granulation, then dry, obtain halogen-free flame-proof reinforced poly propylene glycol ester terephthalate composition of the present invention.