CN104862814A - Preparation method for polytrimethylene terephthalate flame-retardation fibers - Google Patents
Preparation method for polytrimethylene terephthalate flame-retardation fibers Download PDFInfo
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- CN104862814A CN104862814A CN201410533628.8A CN201410533628A CN104862814A CN 104862814 A CN104862814 A CN 104862814A CN 201410533628 A CN201410533628 A CN 201410533628A CN 104862814 A CN104862814 A CN 104862814A
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Abstract
The invention discloses a preparation method for polytrimethylene terephthalate flame-retardation fibers. The preparation method is characterized in that the method comprises the following steps: first, a flame retardant 2-hydroxyethyl (phenyl) phosphinic acid slurry is prepared; second, a catalyst zinc acetate is added in an esterification kettle and an esterification reaction is carried out; third, the ester obtained in the second step is transferred to a polymerization kettle, anti-oxidants, lubricants, stabilizing agents, aging resistant agents, core-shell copolymers MBS and organo-silicone PDMS are added and a condensation polymerization is carried out; fourth, the product obtained in the third step is dried, added into a screw extruder, melt and subjected to spinning. The beneficial effects are that the flame retardant 2-hydroxyethyl (phenyl) phosphinic acid is subjected to copolymerization fusion and is embedded into polytrimethylene terephthalate, thus the product prepared after spinning achieves high-efficiency and permanent flame retardation effects, and the flexibility, resilience, anti-pollution performance and aging resistance of the fibers are raised.
Description
Technical field
The present invention relates to technical field of polymer materials, specifically a kind of preparation method of polytrimethylene terephthalate fire resistance fibre.
Background technology
Polytrimethylene 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 be used alone the problem that PTT exists poor fire, limit applying of its.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of polytrimethylene terephthalate fire resistance fibre.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of polytrimethylene terephthalate fire resistance fibre, is characterized in that comprising the following steps:
(1), with 1, ammediol is solvent, in esterifying kettle, fire retardant 2-ethoxy (phenyl) phosphinic acids are made into the slurries that mass percent concentration is 20 ~ 40wt%, add catalyst acetic acid zinc again, make when temperature 140 DEG C ~ 165 DEG C, normal pressure and stirring carry out esterification 2 ~ 6h, then discharging, to filter;
(2) the raw material terephthalic acid (TPA) and 1 of polytrimethylene terephthalate, is got, ammediol adds in esterifying kettle by quality 1.5 ~ 2:1, still adds catalyst acetic acid zinc, at temperature 165 DEG C ~ 200 DEG C and condition of normal pressure, carry out esterification 1 ~ 4h, when no longer distillating water, esterification terminates and generates carboxylate;
(3), the carboxylate of step (2) is proceeded in polymeric kettle, add step (1) gained filtrate simultaneously, and add antioxidant, lubricant, stabilizing agent, antiager, core-shell copolymerized thing MBS, organosiloxane PDMS, then polycondensation catalyst butyl titanate is added, temperature 265 DEG C ~ 270 DEG C, pressure carries out polycondensation reaction 2 ~ 4h under being less than 100Pa, after the inherent viscosity of product reaches 0.7 ~ 0.9dL/g, section is made in discharging, described antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 2921, antioxidant 245, one or more in irgasfos 168, described lubricant is pentaerythritol stearate or soap, described stabilizing agent is trimethyl phosphate or triphenyl phosphate, described antiager is the tertiary octyl phenyl of 2-(2-hydroxyl-5-) benzotriazole, 2-hydroxyl-4 n-octyloxies-benzophenone, 2, one in 4-dihydroxy benaophenonel,
(4), the section that step (3) obtains is placed in vacuum drum drying machine dry, baking temperature heats up from 60 DEG C, heating rate controls at 10 ~ 15 DEG C/h, until after temperature reaches 150 DEG C ~ 160 DEG C, carry out insulation 3 ~ 5h, after making section crystallization, moisture content is less than 0.003%, then adds screw extruder melting and carries out spinning, to complete the present invention.
The consumption of step (1) described 2-ethoxy (phenyl) phosphinic acids is 10 ~ 20wt% of the weight of polytrimethylene terephthalate.
The consumption of step (1) and the described catalyst acetic acid zinc of step (2) is 0.01 ~ 0.05wt% of the weight of polytrimethylene terephthalate.
The consumption of step (3) described oxidant is 0.1 ~ 1wt% of the weight of polytrimethylene terephthalate.
The consumption of step (3) described lubricant is 0.1 ~ 1wt% of the weight of polytrimethylene terephthalate.
The consumption of step (3) described stabilizing agent is 0.1 ~ 1wt% of the weight of polytrimethylene terephthalate.
The consumption of step (3) described antiager is 0.5 ~ 2wt% of the weight of polytrimethylene terephthalate.
The consumption of the described core-shell copolymerized thing MBS of step (3) is 1 ~ 5wt% of the weight of polytrimethylene terephthalate.
The consumption of the described organosiloxane PDMS of step (3) is 1 ~ 5wt% of the weight of polytrimethylene terephthalate.
Step (4) described spinning technology parameter is: spinning melt temperature controls between 240 DEG C ~ 280 DEG C, and winding speed controls at 500 ~ 3000m/min, and heat setting temperature is 80 DEG C ~ 150 DEG C, and drafting multiple controls between 2 ~ 4 times.
The invention has the beneficial effects as follows, the present invention is embedded in polytrimethylene terephthalate with fire retardant 2-ethoxy (phenyl) phosphinic acids through copolymerization melting, the obtained product of spinning is made to reach efficient, permanent flame retardant effect, but also improve the flexibility of fiber, resilience, resistance tocrocking and ageing-resistant performance, make the use field of PTT fiber more extensive.
Detailed description of the invention
Technical scheme of the present invention is further illustrated below in conjunction with concrete preferred embodiment.
A preparation method for polytrimethylene terephthalate fire resistance fibre, is characterized in that comprising the following steps:
(1), with 1, ammediol is solvent, in esterifying kettle, fire retardant 2-ethoxy (phenyl) phosphinic acids are made into the slurries that mass percent concentration is 20 ~ 40wt%, the consumption of 2-ethoxy (phenyl) phosphinic acids accounts for 10 ~ 20wt% of the weight of polytrimethylene terephthalate, and then add catalyst acetic acid zinc, make when temperature 140 DEG C ~ 165 DEG C, normal pressure and stirring carry out esterification 2 ~ 6h, then discharging, filter, the consumption of described zinc acetate accounts for 0.01 ~ 0.05wt% of the weight of polytrimethylene terephthalate;
(2) the raw material terephthalic acid (TPA) and 1 of polytrimethylene terephthalate, is got, ammediol adds in esterifying kettle by quality 1.5 ~ 2:1, add catalyst acetic acid zinc, the consumption of zinc acetate accounts for 0.01 ~ 0.05wt% of the weight of polytrimethylene terephthalate, then at temperature 165 DEG C ~ 200 DEG C and condition of normal pressure, carry out esterification 1 ~ 4h, when no longer distillating water, esterification terminates and generates carboxylate;
(3), the carboxylate of step (2) is proceeded in polymeric kettle, add step (1) gained filtrate simultaneously, and add antioxidant, lubricant, stabilizing agent, antiager, core-shell copolymerized thing MBS, organosiloxane PDMS, then polycondensation catalyst butyl titanate is added, temperature 265 DEG C ~ 270 DEG C, pressure carries out polycondensation reaction 2 ~ 4h under being less than 100Pa, after the inherent viscosity of product reaches 0.7 ~ 0.9dL/g, section is made in discharging, described antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 2921, antioxidant 245, one or more in irgasfos 168, the consumption of oxidant is 0.1 ~ 1wt% of the weight of polytrimethylene terephthalate, described lubricant is pentaerythritol stearate or soap, described stabilizing agent is trimethyl phosphate or triphenyl phosphate, described antiager is the tertiary octyl phenyl of 2-(2-hydroxyl-5-) benzotriazole, 2-hydroxyl-4 n-octyloxies-benzophenone, 2, one in 4-dihydroxy benaophenonel, and the consumption of described antioxidant, lubricant, stabilizing agent, antiager, core-shell copolymerized thing MBS and organosiloxane PDMS accounts for 0.1 ~ 1wt%, 0.1 ~ 1wt%, 0.1 ~ 1wt%, 0.5 ~ 2wt%, 1 ~ 5wt%, the 1 ~ 5wt% of the weight of polytrimethylene terephthalate respectively,
(4), the section that step (3) obtains is placed in vacuum drum drying machine dry, baking temperature heats up from 60 DEG C, heating rate controls at 10 ~ 15 DEG C/h, until after temperature reaches 150 DEG C ~ 160 DEG C, carry out insulation 3 ~ 5h, after making section crystallization, moisture content is less than 0.003%, then add screw extruder melting and carry out spinning, spinning melt temperature controls between 240 DEG C ~ 280 DEG C, winding speed controls at 500 ~ 3000m/min, heat setting temperature is 80 DEG C ~ 150 DEG C, and drafting multiple controls between 2 ~ 4 times.
Claims (5)
1. a preparation method for polytrimethylene terephthalate fire resistance fibre, is characterized in that, comprises the following steps:
(1), with 1, ammediol is solvent, in esterifying kettle, fire retardant 2-ethoxy (phenyl) phosphinic acids are made into the slurries that mass percent concentration is 20 ~ 40wt%, add catalyst acetic acid zinc again, make when temperature 140 DEG C ~ 165 DEG C, normal pressure and stirring carry out esterification 2 ~ 6h, then discharging, to filter;
(2) the raw material terephthalic acid (TPA) and 1 of polytrimethylene terephthalate, is got, ammediol adds in esterifying kettle by quality 1.5 ~ 2:1, add catalyst acetic acid zinc, at temperature 165 DEG C ~ 200 DEG C and condition of normal pressure, carry out esterification 1 ~ 4h, when no longer distillating water, esterification terminates and generates carboxylate;
(3), the carboxylate of step (2) is proceeded in polymeric kettle, add step (1) gained filtrate simultaneously, and add antioxidant, lubricant, stabilizing agent, antiager, core-shell copolymerized thing MBS, organosiloxane PDMS, then polycondensation catalyst butyl titanate is added, temperature 265 DEG C ~ 270 DEG C, pressure carries out polycondensation reaction 2 ~ 4h under being less than 100Pa, after the inherent viscosity of product reaches 0.7 ~ 0.9dL/g, section is made in discharging, described antioxidant is antioxidant 1010, antioxidant 1076, antioxidant 2921, antioxidant 245, one or more in irgasfos 168, described lubricant is pentaerythritol stearate or soap, described stabilizing agent is trimethyl phosphate or triphenyl phosphate, described antiager is the tertiary octyl phenyl of 2-(2-hydroxyl-5-) benzotriazole, 2-hydroxyl-4 n-octyloxies-benzophenone, 2, one in 4-dihydroxy benaophenonel,
(4), the section that step (3) obtains is placed in vacuum drum drying machine dry, baking temperature heats up from 60 DEG C, heating rate controls at 10 ~ 15 DEG C/h, until after temperature reaches 150 DEG C ~ 160 DEG C, carry out insulation 3 ~ 5h, after making section crystallization, moisture content is less than 0.003%, then adds screw extruder melting and carries out spinning, to complete the present invention.
2. the preparation method of a kind of polytrimethylene terephthalate fire resistance fibre according to claim 1, is characterized in that, the consumption of step (1) described 2-ethoxy (phenyl) phosphinic acids is 10 ~ 20wt% of the weight of polytrimethylene terephthalate.
3. the preparation method of a kind of polytrimethylene terephthalate fire resistance fibre according to claim 1, it is characterized in that, the consumption of step (1) and the described catalyst acetic acid zinc of step (2) is 0.01 ~ 0.05wt% of the weight of polytrimethylene terephthalate.
4. the preparation method of a kind of polytrimethylene terephthalate fire resistance fibre according to claim 1, it is characterized in that, the consumption of step (3) described oxidant, lubricant, stabilizing agent, antiager, core-shell copolymerized thing MBS and organosiloxane PDMS is respectively 0.1 ~ 1wt%, 0.1 ~ 1wt%, 0.1 ~ 1wt%, 0.5 ~ 2wt%, 1 ~ 5wt%, the 1 ~ 5wt% of the weight of polytrimethylene terephthalate.
5. the preparation method of a kind of polytrimethylene terephthalate fire resistance fibre according to claim 1, it is characterized in that, step (4) described spinning technology parameter is: spinning melt temperature controls between 240 DEG C ~ 280 DEG C, winding speed controls at 500 ~ 3000m/min, heat setting temperature is 80 DEG C ~ 150 DEG C, and drafting multiple controls between 2 ~ 4 times.
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| CN201410533628.8A CN104862814A (en) | 2014-10-11 | 2014-10-11 | Preparation method for polytrimethylene terephthalate flame-retardation fibers |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117265694A (en) * | 2023-11-21 | 2023-12-22 | 上海华灏化学有限公司 | Method for preparing bio-based PTT fiber by recycling waste fabric |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117265694A (en) * | 2023-11-21 | 2023-12-22 | 上海华灏化学有限公司 | Method for preparing bio-based PTT fiber by recycling waste fabric |
| CN117265694B (en) * | 2023-11-21 | 2024-01-30 | 上海华灏化学有限公司 | Method for preparing bio-based PTT fiber by recycling waste fabric |
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Application publication date: 20150826 |