CN104861527A - Flame retardation PTT composite material and preparation method therefore - Google Patents

Abstract

The invention discloses a flame retardation PTT composite material and a preparation method therefore. The PTT composite material comprises the following ingredients, by weight, 65%-85% of PTT, 5%-10% of flame retardant, 5%-10% of nano calcium carbonate, 3%-8% of ethane-octylene copolymers, 2%-5% of polyethylene glycol, 0.1%-1% of carbodiimide, 0.1%-1% of pentaerythritol stearate, 0.1%-0.5% of aluminum titanium composite coupling agents and of 0.1%-0.5% of anti-oxidants. The flame retardant is a composite flame retardant prepared from 60-80wt% of polysulfonyldiphenylene phenyl phosphonate, 20-40wt% of polydimethylsiloxane, 1-5wt% of potassium phenylsulphonyl benzene sulfonate and 1-5wt% of nano polytetrafluoroethylene after uniform mixing. The beneficial effects are that the PTT composite material has excellent flame retardant performance, the limit oxygen index reaches more than 38%, and no-halogen and UL94V-0 level flame retardation requirements are met.

Description

Flame retardant resistance PTT matrix material and preparation method thereof

Technical field

The present invention relates to technical field of polymer materials, specifically a kind of flame retardant resistance PTT matrix material and preparation method thereof.

Background technology

Poly(Trimethylene Terephthalate) (PTT), as a kind of new polyester macromolecular material of excellent combination property, has been widely used in the fields such as fiber, film, engineering plastics at present, but has been used alone the problem that PTT exists poor fire, limits its application.

Summary of the invention

The object of the present invention is to provide a kind of fire-retardant efficient, good impact resistance and the simple flame retardant resistance PTT matrix material of preparation technology and preparation method thereof.

The technical solution adopted for the present invention to solve the technical problems is: flame retardant resistance PTT matrix material, and its component by mass percent proportioning is: PTT 65% ~ 85%, fire retardant 5% ~ 10%, nano-calcium carbonate 5% ~ 10%, ethylene-octene copolymer 3% ~ 8%, polyoxyethylene glycol 2% ~ 5%, carbodiimide 0.1% ~ 1%, pentaerythritol stearate 0.1% ~ 1%, aluminium titanium composite coupler 0.1% ~ 0.5%, oxidation inhibitor 0.1% ~ 0.5%.

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

Described fire retardant mixes obtained compound flame redundant by polyphenylene phosphonic acids sulfobenzide ester 60 ~ 80wt%, polydimethylsiloxane 20 ~ 40wt%, potassium phenylsulphonyl benzene sulfonate 1 ~ 5wt% and nanometer polytetrafluoroethylcomposite 1 ~ 5wt%.

Described oxidation inhibitor is the Hinered phenols antioxidant 1010 or 1076 of mass ratio 1:1 and the compound of phosphite ester kind antioxidant 168.

The preparation method of above-mentioned flame retardant resistance PTT matrix material, comprises the following steps:

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

(2) polyphenylene phosphonic acids sulfobenzide ester 60 ~ 80wt%, polydimethylsiloxane 20 ~ 40wt%, potassium phenylsulphonyl benzene sulfonate 1 ~ 5wt% and nanometer polytetrafluoroethylcomposite 1 ~ 5wt%, is taken by weight ratio, make to mix, obtained composite fire retardant, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by;

(3) take dry nano-calcium carbonate and aluminium titanium composite coupler, 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;

(4), add in high-speed mixer by taking dry PTT by weight ratio, add simultaneously and take the obtained composite fire retardant of step (2) by weight ratio and take the product that step (3) obtains, stir 1 ~ 3 minute, then the ethylene-octene copolymer, polyoxyethylene glycol, carbodiimide, pentaerythritol stearate and the oxidation inhibitor that take by weight ratio is added, make to stir 3 ~ 15 minutes together, evenly rear discharging to be mixed;

(5), the compound of step (4) is added in twin screw extruder, extrudes through melting mixing at 180 DEG C ~ 280 DEG C temperature, cooling granulation, drying, obtain flame retardant resistance PTT matrix material of the present invention.

The invention has the beneficial effects as follows, the present invention has excellent flame retardant properties, and its limiting oxygen index(LOI) reaches more than 38%, and meet Halogen, press down cigarette, environmental protection, efficient and UL94 V-0 level flame-retardancy requirements, there is enhancing, toughness reinforcing and increase firm effect simultaneously; Present invention process is simple to operate, and cost is low, is easy to promote.

Embodiment

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

Embodiment 1:

A kind of flame retardant resistance PTT matrix material, its component by mass percent proportioning is: PTT 66%, fire retardant 10%, nano-calcium carbonate 10%, ethylene-octene copolymer 8%, polyoxyethylene glycol 4%, carbodiimide 0.5%, pentaerythritol stearate 1%, aluminium titanium composite coupler 0.3%, oxidation inhibitor 0.2%, wherein, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described fire retardant is by polyphenylene phosphonic acids sulfobenzide ester 78wt%, polydimethylsiloxane 20wt%, potassium phenylsulphonyl benzene sulfonate 1wt% and nanometer polytetrafluoroethylcomposite 1wt% mixes obtained compound flame redundant, described oxidation inhibitor is the Hinered phenols antioxidant 1010 of mass ratio 1:1 and the compound of phosphite ester kind antioxidant 168.

Preparation method: (1), PTT is placed in forced air circulation baking oven, at 110 DEG C ~ 120 DEG C temperature, drying about 6 ~ 8 hours, stand-by; (2) polyphenylene phosphonic acids sulfobenzide ester 78wt%, polydimethylsiloxane 20wt%, potassium phenylsulphonyl benzene sulfonate 1wt% and nanometer polytetrafluoroethylcomposite 1wt%, is taken by weight ratio, make to mix, obtained composite fire retardant, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by; (3) take dry nano-calcium carbonate and aluminium titanium composite coupler, 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; (4), add in high-speed mixer by taking dry PTT by weight ratio, add simultaneously and take the obtained composite fire retardant of step (2) by weight ratio and take the product that step (3) obtains, stir 1 ~ 3 minute, then the ethylene-octene copolymer, polyoxyethylene glycol, carbodiimide, pentaerythritol stearate and the oxidation inhibitor that take by weight ratio is added, make to stir 3 ~ 15 minutes together, evenly rear discharging to be mixed; (5), the compound of step (4) is added in twin screw extruder, extrudes through melting mixing at 180 DEG C ~ 280 DEG C temperature, cooling granulation, drying, obtain flame retardant resistance PTT matrix material of the present invention.

Embodiment 2:

A kind of flame retardant resistance PTT matrix material, its component by mass percent proportioning is: PTT 80%, fire retardant 8%, nano-calcium carbonate 5%, ethylene-octene copolymer 4%, polyoxyethylene glycol 2%, carbodiimide 0.3%, pentaerythritol stearate 0.5%, aluminium titanium composite coupler 0.1%, oxidation inhibitor 0.1%, wherein, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described fire retardant is by polyphenylene phosphonic acids sulfobenzide ester 70wt%, polydimethylsiloxane 28wt%, potassium phenylsulphonyl benzene sulfonate 1wt% and nanometer polytetrafluoroethylcomposite 1wt% mixes obtained compound flame redundant, described oxidation inhibitor is the Hinered phenols antioxidant 1076 of mass ratio 1:1 and the compound of phosphite ester kind antioxidant 168.

Preparation method: (1), PTT is placed in forced air circulation baking oven, at 110 DEG C ~ 120 DEG C temperature, drying about 6 ~ 8 hours, stand-by; (2) polyphenylene phosphonic acids sulfobenzide ester 70wt%, polydimethylsiloxane 28wt%, potassium phenylsulphonyl benzene sulfonate 1wt% and nanometer polytetrafluoroethylcomposite 1wt%, is taken by weight ratio, make to mix, obtained composite fire retardant, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by; (3) take dry nano-calcium carbonate and aluminium titanium composite coupler, 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; (4), add in high-speed mixer by taking dry PTT by weight ratio, add simultaneously and take the obtained composite fire retardant of step (2) by weight ratio and take the product that step (3) obtains, stir 1 ~ 3 minute, then the ethylene-octene copolymer, polyoxyethylene glycol, carbodiimide, pentaerythritol stearate and the oxidation inhibitor that take by weight ratio is added, make to stir 3 ~ 15 minutes together, evenly rear discharging to be mixed; (5), the compound of step (4) is added in twin screw extruder, extrudes through melting mixing at 180 DEG C ~ 280 DEG C temperature, cooling granulation, drying, obtain flame retardant resistance PTT matrix material of the present invention.

Claims (4)

1. a flame retardant resistance PTT matrix material, it is characterized in that, its component by mass percent proportioning is: PTT 65% ~ 85%, fire retardant 5% ~ 10%, nano-calcium carbonate 5% ~ 10%, ethylene-octene copolymer 3% ~ 8%, polyoxyethylene glycol 2% ~ 5%, carbodiimide 0.1% ~ 1%, pentaerythritol stearate 0.1% ~ 1%, aluminium titanium composite coupler 0.1% ~ 0.5%, oxidation inhibitor 0.1% ~ 0.5%.

2. flame retardant resistance PTT matrix material according to claim 1; it is characterized in that, described fire retardant mixes obtained compound flame redundant by polyphenylene phosphonic acids sulfobenzide ester 60 ~ 80wt%, polydimethylsiloxane 20 ~ 40wt%, potassium phenylsulphonyl benzene sulfonate 1 ~ 5wt% and nanometer polytetrafluoroethylcomposite 1 ~ 5wt%.

3. flame retardant resistance PTT matrix material according to claim 1, is characterized in that, described oxidation inhibitor is the Hinered phenols antioxidant 1010 or 1076 of mass ratio 1:1 and the compound of phosphite ester kind antioxidant 168.

4. the preparation method of flame retardant resistance PTT matrix material according to claim 1, is characterized in that, comprise the following steps:

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

(2) polyphenylene phosphonic acids sulfobenzide ester 60 ~ 80wt%, polydimethylsiloxane 20 ~ 40wt%, potassium phenylsulphonyl benzene sulfonate 1 ~ 5wt% and nanometer polytetrafluoroethylcomposite 1 ~ 5wt%, is taken by weight ratio, make to mix, obtained composite fire retardant, then at 80 DEG C ~ 85 DEG C dry 30 ~ 45 minutes, stand-by;

(3) take dry nano-calcium carbonate and aluminium titanium composite coupler, 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;

(4), add in high-speed mixer by taking dry PTT by weight ratio, add simultaneously and take the obtained composite fire retardant of step (2) by weight ratio and take the product that step (3) obtains, stir 1 ~ 3 minute, then the ethylene-octene copolymer, polyoxyethylene glycol, carbodiimide, pentaerythritol stearate and the oxidation inhibitor that take by weight ratio is added, make to stir 3 ~ 15 minutes together, evenly rear discharging to be mixed;

(5), the compound of step (4) is added in twin screw extruder, extrudes through melting mixing at 180 DEG C ~ 280 DEG C temperature, cooling granulation, drying, obtain flame retardant resistance PTT matrix material of the present invention.