CN104861503A - Red phosphorus master batch flame retardation PTT polyester and preparation method therefor - Google Patents

Abstract

The invention discloses a red phosphorus master batch flame retardation PTT polyester and a preparation method therefor. The red phosphorus master batch flame retardation PTT polyester comprises the following ingredients, by weight, 60%-80% of PTT, 10%-15% of red phosphorus master batch, 8%-15% of glass fibers, 2%-8% of POE, 1%-4% of calcium oxide, 0.1%-0.5% of aluminum titanium composite coupling agents, 0.1%-0.5% of anti-oxidants and 0.1%-1% of lubricants. The calcium oxide is calcium oxide particles with a particle size of being less than 5 micrometers. The beneficial effects are that the red phosphorus master batch is employed as a flame retardant, the flame retardation of PTT is raised, and the tensile strength, the bending strength and the CTI value of PTT are also raised obviously; a proper amount of calcium oxide is added for strengthening, a proper amount of POE is added for toughening, calcium oxide and the red phosphorus master batch has good flame retardant synergism effects, and the cost is lowered.

Description

Red phosphor masterbatch flame-retarding PTT polyester and preparation method thereof

Technical field

The present invention relates to technical field of polymer materials, specifically a kind of red phosphor masterbatch flame-retarding PTT polyester and preparation method thereof.

Background technology

Poly(Trimethylene Terephthalate) (PTT) is a kind of by terephthalic acid and 1, the aromatic polyester that ammediol synthesizes through esterification and polycondensation, since the nineties in last century suitability for industrialized production, the fields such as fiber, film, engineering plastics are widely used in.Especially in engineering plastics field, PTT has the high-performance of PET and the workability of PBT simultaneously, and its price is much lower compared with PBT, thus has important using value.But PTT itself can not fire-retardant (limiting oxygen index(LOI) be about 21), thus limits the range of application of PTT.

Summary of the invention

The object of the present invention is to provide a kind of red phosphor masterbatch flame-retarding PTT polyester and preparation method thereof.

The technical solution adopted for the present invention to solve the technical problems is: red phosphor masterbatch flame-retarding PTT polyester, and its component by mass percent proportioning is: PTT 60% ~ 80%, red phosphor masterbatch 10% ~ 15%, glass fibre 8% ~ 15%, POE 2% ~ 8%, calcium oxide 1% ~ 4%, aluminium titanium composite coupler 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 red phosphor masterbatch is commercially available RPM-540B red phosphor masterbatch.

Described glass fibre is that surface is through silane coupler modified process and the alkali-free short glass fiber of diameter within the scope of 4 ~ 17 μm.

Described POE is ethylene-octene copolymer elastomer.

Described calcium oxide is the calcium oxide particulate that particle diameter is less than 5 μm.

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 modification ethylene bis-fatty acid amides.

The preparation method of above-mentioned red phosphor masterbatch flame-retarding PTT polyester, comprises the following steps:

(1) forced air circulation baking oven, by PTT is placed at 110 DEG C ~ 120 DEG C temperature dry 6 ~ 8 hours, by red phosphor masterbatch, glass fibre and calcium oxide separately respectively at 60 DEG C ~ 100 DEG C temperature dry 1 ~ 2 hour, stand-by;

(2), take dry calcium oxide by weight ratio and add barrel temperature in the high-speed mixer of 80 DEG C ~ 120 DEG C, add aluminium titanium composite coupler by weight ratio simultaneously, make, after rotating speed 3000 ~ 4500r/min stirs 10 ~ 45 minutes, to be cooled to lower than 40 DEG C of dischargings stand-by;

(3) PTT and the red phosphor masterbatch that, take drying by weight ratio add in high-speed mixer, add the POE, oxidation inhibitor and the lubricant that take by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 5 minutes together, discharging after fully mixing;

(4), the compound of step (3) is added the main spout of twin screw extruder, add from the side spout of twin screw extruder simultaneously and take dry glass fibre by weight ratio, by twin screw extruder melting mixing 1 ~ 2 minute, screw speed controls at 120 ~ 500r/min, processing temperature is 180 DEG C ~ 260 DEG C scopes, then extruding pelletization, obtains red phosphor masterbatch flame-retarding PTT polyester of the present invention.

The invention has the beneficial effects as follows, the present invention take red phosphor masterbatch as fire retardant, not only increase the flame retardant resistance of PTT, but also obviously improve its tensile strength, flexural strength and CTI value, add simultaneously appropriate calcium oxide strengthen and POE toughness reinforcing, also there is between calcium oxide and red phosphor masterbatch good cooperative flame retardant effect, and reduce cost.

Embodiment

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

Embodiment 1:

A kind of red phosphor masterbatch flame-retarding PTT polyester, its component by mass percent proportioning is: PTT 64%, red phosphor masterbatch 12%, glass fibre 15%, POE 5%, calcium oxide 3%, aluminium titanium composite coupler 0.1%, antioxidant 1010 0.2%, modification ethylene bis-fatty acid amides 0.7%, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described red phosphor masterbatch is commercially available RPM-540B red phosphor masterbatch, described glass fibre is that surface is through silane coupler modified process, and the alkali-free short glass fiber of diameter within the scope of 4 ~ 17 μm, described POE is ethylene-octene copolymer elastomer, described calcium oxide is the calcium oxide particulate that particle diameter is less than 5 μm.

Preparation method: (1), PTT is placed in forced air circulation baking oven at 110 DEG C ~ 120 DEG C temperature dry 6 ~ 8 hours, by red phosphor masterbatch, glass fibre and calcium oxide separately respectively at 60 DEG C ~ 100 DEG C temperature dry 1 ~ 2 hour, stand-by; (2), take dry calcium oxide by weight ratio and add barrel temperature in the high-speed mixer of 80 DEG C ~ 120 DEG C, add aluminium titanium composite coupler by weight ratio simultaneously, make, after rotating speed 3000 ~ 4500r/min stirs 10 ~ 45 minutes, to be cooled to lower than 40 DEG C of dischargings stand-by; (3) PTT and the red phosphor masterbatch that, take drying by weight ratio add in high-speed mixer, add the POE, antioxidant 1010, the modification ethylene bis-fatty acid amides that take by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 5 minutes together, discharging after fully mixing; (4), the compound of step (3) is added the main spout of twin screw extruder, add from the side spout of twin screw extruder simultaneously and take dry glass fibre by weight ratio, by twin screw extruder melting mixing 1 ~ 2 minute, screw speed controls at 120 ~ 500r/min, processing temperature is 180 DEG C ~ 260 DEG C scopes, then extruding pelletization, obtains red phosphor masterbatch flame-retarding PTT polyester of the present invention.

Embodiment 2:

A kind of red phosphor masterbatch flame-retarding PTT polyester, its component by mass percent proportioning is: PTT 70%, red phosphor masterbatch 14%, glass fibre 10%, POE 3.5%, calcium oxide 2%, aluminium titanium composite coupler 0.1%, the compound 0.1% of antioxidant 1076 and irgasfos 168, modification ethylene bis-fatty acid amides 0.3%, described PTT is the Poly(Trimethylene Terephthalate) of limiting viscosity 0.7 ~ 1.2dL/g, described red phosphor masterbatch is commercially available RPM-540B red phosphor masterbatch, described glass fibre is that surface is through silane coupler modified process, and the alkali-free short glass fiber of diameter within the scope of 4 ~ 17 μm, described POE is ethylene-octene copolymer elastomer, described calcium oxide is the calcium oxide particulate that particle diameter is less than 5 μm.

Preparation method: (1), PTT is placed in forced air circulation baking oven at 110 DEG C ~ 120 DEG C temperature dry 6 ~ 8 hours, by red phosphor masterbatch, glass fibre and calcium oxide separately respectively at 60 DEG C ~ 100 DEG C temperature dry 1 ~ 2 hour, stand-by; (2), take dry calcium oxide by weight ratio and add barrel temperature in the high-speed mixer of 80 DEG C ~ 120 DEG C, add aluminium titanium composite coupler by weight ratio simultaneously, make, after rotating speed 3000 ~ 4500r/min stirs 10 ~ 45 minutes, to be cooled to lower than 40 DEG C of dischargings stand-by; (3) PTT and the red phosphor masterbatch that, take drying by weight ratio add in high-speed mixer, add the compound of POE, antioxidant 1076 and the irgasfos 168 taken by weight ratio, modification ethylene bis-fatty acid amides simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 5 minutes together, discharging after fully mixing; (4), the compound of step (3) is added the main spout of twin screw extruder, add from the side spout of twin screw extruder simultaneously and take dry glass fibre by weight ratio, by twin screw extruder melting mixing 1 ~ 2 minute, screw speed controls at 120 ~ 500r/min, processing temperature is 180 DEG C ~ 260 DEG C scopes, then extruding pelletization, obtains red phosphor masterbatch flame-retarding PTT polyester of the present invention.

Claims (6)

1. a red phosphor masterbatch flame-retarding PTT polyester, it is characterized in that, its component by mass percent proportioning is: PTT 60% ~ 80%, red phosphor masterbatch 10% ~ 15%, glass fibre 8% ~ 15%, POE 2% ~ 8%, calcium oxide 1% ~ 4%, aluminium titanium composite coupler 0.1% ~ 0.5%, oxidation inhibitor 0.1% ~ 0.5%, lubricant 0.1% ~ 1%.

2. red phosphor masterbatch flame-retarding PTT polyester according to claim 1, is characterized in that, described glass fibre is that surface is through silane coupler modified process and the alkali-free short glass fiber of diameter within the scope of 4 ~ 17 μm.

3. red phosphor masterbatch flame-retarding PTT polyester according to claim 1, is characterized in that, described calcium oxide is the calcium oxide particulate that particle diameter is less than 5 μm.

4. red phosphor masterbatch flame-retarding PTT polyester 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.

5. red phosphor masterbatch flame-retarding PTT polyester according to claim 1, is characterized in that, described lubricant is modification ethylene bis-fatty acid amides.

6. the preparation method of red phosphor masterbatch flame-retarding PTT polyester according to claim 1, is characterized in that, comprise the following steps:

(1) forced air circulation baking oven, by PTT is placed at 110 DEG C ~ 120 DEG C temperature dry 6 ~ 8 hours, by red phosphor masterbatch, glass fibre and calcium oxide separately respectively at 60 DEG C ~ 100 DEG C temperature dry 1 ~ 2 hour, stand-by;

(2), take dry calcium oxide by weight ratio and add barrel temperature in the high-speed mixer of 80 DEG C ~ 120 DEG C, add aluminium titanium composite coupler by weight ratio simultaneously, make, after rotating speed 3000 ~ 4500r/min stirs 10 ~ 45 minutes, to be cooled to lower than 40 DEG C of dischargings stand-by;

(3) PTT and the red phosphor masterbatch that, take drying by weight ratio add in high-speed mixer, add the POE, oxidation inhibitor and the lubricant that take by weight ratio simultaneously, and add the product that step (2) obtains, make to stir 3 ~ 5 minutes together, discharging after fully mixing;

(4), the compound of step (3) is added the main spout of twin screw extruder, add from the side spout of twin screw extruder simultaneously and take dry glass fibre by weight ratio, by twin screw extruder melting mixing 1 ~ 2 minute, screw speed controls at 120 ~ 500r/min, processing temperature is 180 DEG C ~ 260 DEG C scopes, then extruding pelletization, obtains red phosphor masterbatch flame-retarding PTT polyester of the present invention.