CN102127824B - Manufacture method of modified polypropylene flame-retardant fiber - Google Patents
Manufacture method of modified polypropylene flame-retardant fiber Download PDFInfo
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- CN102127824B CN102127824B CN201010606436A CN201010606436A CN102127824B CN 102127824 B CN102127824 B CN 102127824B CN 201010606436 A CN201010606436 A CN 201010606436A CN 201010606436 A CN201010606436 A CN 201010606436A CN 102127824 B CN102127824 B CN 102127824B
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Abstract
The invention relates to a manufacture method of modified polypropylene flame-retardant fiber. Modified polypropylene flame-retardant fiber raw filaments are the copolymer of polypropylene, melamine nitrogen flame retardant, methacrylate and nano titanium dioxide. Through improving and optimizing the related process and the parameters of a raw material preparing step, a stock solution and spinning preparing step and a spinning and post-treatment step, polypropylene fiber has functional characteristic effects which are not owned by the common flame-resistant fiber, such as unique flame resistance, excellent flexibility, static electricity resistance, fuzz avoidance, and the like.
Description
Technical field
The present invention relates to a kind of manufacture method of modified polypropene fire resistance fibre.
Background technology
Polypropylene is a kind of desirable fiber that can be used for clothes, also can be used in carpet, upholster and other goods, as sleeping bag, liner, lid quilt and pillow.Just owing to its resilience with fire resistance is relatively poor that its application is restricted.
Resilience is the measuring of ability that is returned to its original size for fiber after elimination makes the stress of its compression fully,
And how anti-flammability removes to make the heat-proof combustion-resistant fiber of all kinds of yarns as everybody knows.For example: the Work Clothes heat-proof combustion-resistant fiber of hazardous industry, fire-entry suit heat-proof combustion-resistant fiber, military protective clothing heat-proof combustion-resistant fiber all is to make of the fabric that non-synthetic fibre yarn is made, as cotton or wool.These fabrics form through halogen commonly used or the phosphorus base chemicals special disposal of glowing.Yet, limited with its operating period of clothes that this fabric is made, and weight is also heavy than the Work Clothes of making without the processing fabric that glows, and special chemical treatment makes fabric weight increase about 15% to 20%.When this kind fabric burns, form frangible burnt sheet, drop along with moving of fabric.
Summary of the invention
The objective of the invention is polypropylene fibre is carried out that unique anti-flammability is handled and performance such as comfortable is carried out in the relevant modifying process by improving correlation step and the relevant optimal parameter of optimization, it can make polypropylene fibre have concurrently prior art say the fire-retardant and good flexibility of the uniqueness that does not possess, antistatic, resist functional characteristic effect such as fluffing.
For achieving the above object, the present invention is achieved by the following technical solutions:
The manufacture method of a kind of modified polypropene fire resistance fibre of the present invention, modified polypropene fire resistance fibre precursor are the copolymers of polypropylene, melamine class nitrogen flame retardant, methyl acrylate and Nano titanium dioxide; It is characterized in that the manufacture method step of modified polypropene fire resistance fibre comprises:
Step 1, raw material are prepared: adopting polypropylene chip and melamine class nitrogen flame retardant master batch is raw material, at first melamine class nitrogen flame retardant master batch is inserted tackify in the solid-phase tack producing rotary drum equipment, make it become viscosity and reach 1.35 high viscosity melamine class nitrogen flame retardant master batch; The raw material polypropylene chip inserted carry out pre-crystallization in the fluid bed, temperature is 230 ℃, mix with high sticking melamine class nitrogen flame retardant by the polypropylene chip of polypropylene adding machine after pre-crystallization, adjust the addition of meter rotating speed with the control polypropylene chip, the proportion control that makes high polypropylene section and high sticking melamine class nitrogen flame retardant was at 20: 1.
Step 2, stoste and spinning are prepared, with the mixture of the high polypropylene section that obtains in the step 1 and high sticking melamine class nitrogen flame retardant and methyl acrylate as reactant monomer, adopting the oxidation dibenzoyl is initator, potassium rhodanide solution with 65% is solvent, add polymeric kettle, reaction is 5 hours under 90 ℃ temperature; Add Nano titanium dioxide, stabilizing agent and synergist then,, unreacted monomer in the polymer is deviate from, and condensate is stayed in the potassium rhodanide solution, form homogeneous phase macromolecule spinning solution by taking off Dan Ta continuously; With above-mentioned homogeneous phase macromolecule spinning solution at first after filter centrifugal filters, enter vacuum and be deaeration in the deaeration tower of 0.088Mpa, through stoste thermosistor temperature adjustment to 40 ℃, enter centrifugal filter once more and filter then, by the measuring pump metering, enter spinning spinneret assembly spray silk;
Step 3, spinning and post processing: the spinneret orifice diameter in the spinneret component that spinning is adopted is between 0.01-0.09mm, and the spinneret orifice L/D ratio is 12; The stoste thread of ejection is that 30 ℃, density are 1.095g/cm in temperature
3Sodium thiocyanate solution in coagulation forming be as-is fibre, be 60 ℃, 70 ℃, 80 ℃ in temperature again, density 1.24g/cm
3Preliminary draft bathe in 4 times preliminary draft in addition respectively, turn to then and wash in the reflux condensing tube that enters the desalted water that contains 30-40 ℃, again through an insulation slow cooling district and a cooling zone, form spinning; Wherein be incubated the slow cooling district and be positioned at 2-20cm under the spinnerets, be provided with little heater in insulation slow cooling district, the temperature in insulation slow cooling district is controlled at 100-160 ℃; Mainly by being the air-cooled district that cooling media is formed with nitrogen or rare gas, wind-warm syndrome is controlled at 76 ℃ in the cooling zone; Reeling after evenly oiling through cooled fibers then, the speed of spinning silk winding is controlled at 5000m/min, again in drawing machine through the drafting process in 6 roads, the total draft multiplying power is controlled at 8 times, drawing temperature is 60 ℃, and be 150-170 ℃ steam hot-rolling oven dry back rolling by heat setting temperature, take out the cooling back, promptly gets the modified polypropene fire resistance fibre.As optimized technical scheme:
Spinneret orifice diameter in the spinneret component that spinning is adopted in the described step 3 is 0.05mm.
The temperature in insulation slow cooling district is controlled at 120 ℃ in the described step 3.
In the described step 3 in the drawing machine drawing-off multiplying power through the drawing-off in 6 roads successively be respectively 0.9,1.2,0.8,1.6,1.6,1.9.
The specific embodiment
Below in conjunction with the specific embodiment, further set forth the present invention.
Embodiment 1:
Modified polypropene fire resistance fibre precursor is the copolymer of polypropylene, melamine class nitrogen flame retardant, methyl acrylate and Nano titanium dioxide; It is characterized in that the manufacture method step of modified polypropene fire resistance fibre comprises:
Step 1, raw material are prepared: adopting polypropylene chip and melamine class nitrogen flame retardant master batch is raw material, at first melamine class nitrogen flame retardant master batch is inserted tackify in the solid-phase tack producing rotary drum equipment, make it become viscosity and reach 1.35 high viscosity melamine class nitrogen flame retardant master batch; The raw material polypropylene chip inserted carry out pre-crystallization in the fluid bed, temperature is 230 ℃, mix with high sticking melamine class nitrogen flame retardant by the polypropylene chip of polypropylene adding machine after pre-crystallization, adjust the addition of meter rotating speed with the control polypropylene chip, the proportion control that makes high polypropylene section and high sticking melamine class nitrogen flame retardant was at 20: 1.
Step 2, stoste and spinning are prepared, with the mixture of the high polypropylene section that obtains in the step 1 and high sticking melamine class nitrogen flame retardant and methyl acrylate as reactant monomer, adopting the oxidation dibenzoyl is initator, potassium rhodanide solution with 65% is solvent, add polymeric kettle, reaction is 5 hours under 90 ℃ temperature; Add Nano titanium dioxide, stabilizing agent and synergist then,, unreacted monomer in the polymer is deviate from, and condensate is stayed in the potassium rhodanide solution, form homogeneous phase macromolecule spinning solution by taking off Dan Ta continuously; With above-mentioned homogeneous phase macromolecule spinning solution at first after filter centrifugal filters, enter vacuum and be deaeration in the deaeration tower of 0.088Mpa, through stoste thermosistor temperature adjustment to 40 ℃, enter centrifugal filter once more and filter then, by the measuring pump metering, enter spinning spinneret assembly spray silk;
Step 3, spinning and post processing: the spinneret orifice diameter in the spinneret component that spinning is adopted is between 0.01-0.09mm, and the spinneret orifice L/D ratio is 12; The stoste thread of ejection is that 30 ℃, density are 1.095g/cm in temperature
3Sodium thiocyanate solution in coagulation forming be as-is fibre, be 60 ℃, 70 ℃, 80 ℃ in temperature again, density 1.24g/cm
3Preliminary draft bathe in 4 times preliminary draft in addition respectively, turn to then and wash in the reflux condensing tube that enters the desalted water that contains 30-40 ℃, again through an insulation slow cooling district and a cooling zone, form spinning; Wherein be incubated the slow cooling district and be positioned at 2-20cm under the spinnerets, be provided with little heater in insulation slow cooling district, the temperature in insulation slow cooling district is controlled at 100 ℃; Mainly by being the air-cooled district that cooling media is formed with nitrogen or rare gas, wind-warm syndrome is controlled at 76 ℃ in the cooling zone; Reeling after evenly oiling through cooled fibers then, the speed of spinning silk winding is controlled at 5000m/min, again in drawing machine through the drafting process in 6 roads, the total draft multiplying power is controlled at 8 times, drawing temperature is 60 ℃, and be 150 ℃ steam hot-rolling oven dry back rolling by heat setting temperature, take out the cooling back, promptly gets the modified polypropene fire resistance fibre.
Embodiment 2:
Modified polypropene fire resistance fibre precursor is the copolymer of polypropylene, melamine class nitrogen flame retardant, methyl acrylate and Nano titanium dioxide; It is characterized in that the manufacture method step of modified polypropene fire resistance fibre comprises:
Step 1, raw material are prepared: adopting polypropylene chip and melamine class nitrogen flame retardant master batch is raw material, at first melamine class nitrogen flame retardant master batch is inserted tackify in the solid-phase tack producing rotary drum equipment, make it become viscosity and reach 1.35 high viscosity melamine class nitrogen flame retardant master batch; The raw material polypropylene chip inserted carry out pre-crystallization in the fluid bed, temperature is 230 ℃, mix with high sticking melamine class nitrogen flame retardant by the polypropylene chip of polypropylene adding machine after pre-crystallization, adjust the addition of meter rotating speed with the control polypropylene chip, the proportion control that makes high polypropylene section and high sticking melamine class nitrogen flame retardant was at 20: 1.
Step 2, stoste and spinning are prepared, with the mixture of the high polypropylene section that obtains in the step 1 and high sticking melamine class nitrogen flame retardant and methyl acrylate as reactant monomer, adopting the oxidation dibenzoyl is initator, potassium rhodanide solution with 65% is solvent, add polymeric kettle, reaction is 5 hours under 90 ℃ temperature; Add Nano titanium dioxide, stabilizing agent and synergist then,, unreacted monomer in the polymer is deviate from, and condensate is stayed in the potassium rhodanide solution, form homogeneous phase macromolecule spinning solution by taking off Dan Ta continuously; With above-mentioned homogeneous phase macromolecule spinning solution at first after filter centrifugal filters, enter vacuum and be deaeration in the deaeration tower of 0.088Mpa, through stoste thermosistor temperature adjustment to 40 ℃, enter centrifugal filter once more and filter then, by the measuring pump metering, enter spinning spinneret assembly spray silk;
Step 3, spinning and post processing: the spinneret orifice diameter in the spinneret component that spinning is adopted is between 0.01-0.09mm, and the spinneret orifice L/D ratio is 12; The stoste thread of ejection is that 30 ℃, density are 1.095g/cm in temperature
3Sodium thiocyanate solution in coagulation forming be as-is fibre, be 60 ℃, 70 ℃, 80 ℃ in temperature again, density 1.24g/cm
3Preliminary draft bathe in 4 times preliminary draft in addition respectively, turn to then and wash in the reflux condensing tube that enters the desalted water that contains 30-40 ℃, again through an insulation slow cooling district and a cooling zone, form spinning; Wherein be incubated the slow cooling district and be positioned at 2-20cm under the spinnerets, be provided with little heater in insulation slow cooling district, the temperature in insulation slow cooling district is controlled at 130 ℃; Mainly by being the air-cooled district that cooling media is formed with nitrogen or rare gas, wind-warm syndrome is controlled at 76 ℃ in the cooling zone; Reeling after evenly oiling through cooled fibers then, the speed of spinning silk winding is controlled at 5000m/min, again in drawing machine through the drafting process in 6 roads, the total draft multiplying power is controlled at 8 times, drawing temperature is 60 ℃, and be 160 ℃ steam hot-rolling oven dry back rolling by heat setting temperature, take out the cooling back, promptly gets the modified polypropene fire resistance fibre.
Embodiment 1:
Modified polypropene fire resistance fibre precursor is the copolymer of polypropylene, melamine class nitrogen flame retardant, methyl acrylate and Nano titanium dioxide; It is characterized in that the manufacture method step of modified polypropene fire resistance fibre comprises:
Step 1, raw material are prepared: adopting polypropylene chip and melamine class nitrogen flame retardant master batch is raw material, at first melamine class nitrogen flame retardant master batch is inserted tackify in the solid-phase tack producing rotary drum equipment, make it become viscosity and reach 1.35 high viscosity melamine class nitrogen flame retardant master batch; The raw material polypropylene chip inserted carry out pre-crystallization in the fluid bed, temperature is 230 ℃, mix with high sticking melamine class nitrogen flame retardant by the polypropylene chip of polypropylene adding machine after pre-crystallization, adjust the addition of meter rotating speed with the control polypropylene chip, the proportion control that makes high polypropylene section and high sticking melamine class nitrogen flame retardant was at 20: 1.
Step 2, stoste and spinning are prepared, with the mixture of the high polypropylene section that obtains in the step 1 and high sticking melamine class nitrogen flame retardant and methyl acrylate as reactant monomer, adopting the oxidation dibenzoyl is initator, potassium rhodanide solution with 65% is solvent, add polymeric kettle, reaction is 5 hours under 90 ℃ temperature; Add Nano titanium dioxide, stabilizing agent and synergist then,, unreacted monomer in the polymer is deviate from, and condensate is stayed in the potassium rhodanide solution, form homogeneous phase macromolecule spinning solution by taking off Dan Ta continuously; With above-mentioned homogeneous phase macromolecule spinning solution at first after filter centrifugal filters, enter vacuum and be deaeration in the deaeration tower of 0.088Mpa, through stoste thermosistor temperature adjustment to 40 ℃, enter centrifugal filter once more and filter then, by the measuring pump metering, enter spinning spinneret assembly spray silk;
Step 3, spinning and post processing: the spinneret orifice diameter in the spinneret component that spinning is adopted is between 0.01-0.09mm, and the spinneret orifice L/D ratio is 12; The stoste thread of ejection is that 30 ℃, density are 1.095g/cm in temperature
3Sodium thiocyanate solution in coagulation forming be as-is fibre, be 60 ℃, 70 ℃, 80 ℃ in temperature again, density 1.24g/cm
3Preliminary draft bathe in 4 times preliminary draft in addition respectively, turn to then and wash in the reflux condensing tube that enters the desalted water that contains 30-40 ℃, again through an insulation slow cooling district and a cooling zone, form spinning; Wherein be incubated the slow cooling district and be positioned at 2-20cm under the spinnerets, be provided with little heater in insulation slow cooling district, the temperature in insulation slow cooling district is controlled at 160 ℃; Mainly by being the air-cooled district that cooling media is formed with nitrogen or rare gas, wind-warm syndrome is controlled at 76 ℃ in the cooling zone; Reeling after evenly oiling through cooled fibers then, the speed of spinning silk winding is controlled at 5000m/min, again in drawing machine through the drafting process in 6 roads, the total draft multiplying power is controlled at 8 times, drawing temperature is 60 ℃, and be 170 ℃ steam hot-rolling oven dry back rolling by heat setting temperature, take out the cooling back, promptly gets the modified polypropene fire resistance fibre.
Through evidence, a kind of profiled sheeting of the present invention has high tenacity, high-flexural strength and high-wearing feature, corrosion-resistant, anti-oxidant, the level and smooth heat-proof quality that evenly is difficult for producing breach and excellence really; Durable in use, prevent phenomenons such as lousiness, fracture of wire, shorten maintenance time, make winding process more smooth and easy.
Claims (4)
1. the manufacture method of a modified polypropene fire resistance fibre, modified polypropene fire resistance fibre precursor is the copolymer of polypropylene, melamine class nitrogen flame retardant, methyl acrylate and Nano titanium dioxide; It is characterized in that the manufacture method step of modified polypropene fire resistance fibre comprises:
Step 1, raw material are prepared: adopting polypropylene chip and melamine class nitrogen flame retardant master batch is raw material, at first melamine class nitrogen flame retardant master batch is inserted tackify in the solid-phase tack producing rotary drum equipment, make it become viscosity and reach 1.35 high viscosity melamine class nitrogen flame retardant master batch; The raw material polypropylene chip inserted carry out pre-crystallization in the fluid bed, temperature is 230 ℃, mix with high sticking melamine class nitrogen flame retardant by the polypropylene chip of polypropylene adding machine after pre-crystallization, adjust the addition of meter rotating speed with the control polypropylene chip, the proportion control that makes high polypropylene section and high sticking melamine class nitrogen flame retardant was at 20: 1;
Step 2, stoste and spinning are prepared, with the mixture of the high polypropylene section that obtains in the step 1 and high sticking melamine class nitrogen flame retardant and methyl acrylate as reactant monomer, adopting the oxidation dibenzoyl is initator, potassium rhodanide solution with 65% is solvent, add polymeric kettle, reaction is 5 hours under 90 ℃ temperature; Add Nano titanium dioxide, stabilizing agent and synergist then,, unreacted monomer in the polymer is deviate from, and condensate is stayed in the potassium rhodanide solution, form homogeneous phase macromolecule spinning solution by taking off Dan Ta continuously; With above-mentioned homogeneous phase macromolecule spinning solution at first after filter centrifugal filters, enter vacuum and be deaeration in the deaeration tower of 0.088Mpa, through stoste thermosistor temperature adjustment to 40 ℃, enter centrifugal filter once more and filter then, by the measuring pump metering, enter spinning spinneret assembly spray silk;
Step 3, spinning and post processing: the spinneret orifice diameter in the spinneret component that spinning is adopted is between 0.01-0.09mm, and the spinneret orifice L/D ratio is 12; The stoste thread of ejection is that 30 ℃, density are 1.095g/cm in temperature
3Sodium thiocyanate solution in coagulation forming be as-is fibre, be 60 ℃, 70 ℃, 80 ℃ in temperature again, density 1.24g/cm
3Preliminary draft bathe in 4 times preliminary draft in addition respectively, turn to then and wash in the reflux condensing tube that enters the desalted water that contains 30-40 ℃, again through an insulation slow cooling district and a cooling zone, form spinning; Wherein be incubated the slow cooling district and be positioned at 2-20cm under the spinnerets, be provided with little heater in insulation slow cooling district, the temperature in insulation slow cooling district is controlled at 100-160 ℃; Mainly by being the air-cooled district that cooling media is formed with nitrogen or rare gas, wind-warm syndrome is controlled at 76 ℃ in the cooling zone; Reeling after evenly oiling through cooled fibers then, the speed of spinning silk winding is controlled at 5000m/min, again in drawing machine through the drafting process in 6 roads, the total draft multiplying power is controlled at 8 times, drawing temperature is 60 ℃, and be 150-170 ℃ steam hot-rolling oven dry back rolling by heat setting temperature, take out the cooling back, promptly gets the modified polypropene fire resistance fibre.
2. the manufacture method of modified polypropene fire resistance fibre according to claim 1 is characterized in that: the spinneret orifice diameter in the spinneret component that spinning is adopted in the described step 3 is 0.05mm.
3. the manufacture method of modified polypropene fire resistance fibre according to claim 1 is characterized in that: the temperature in insulation slow cooling district is controlled at 120 ℃ in the described step 3.
4. the manufacture method of modified polypropene fire resistance fibre according to claim 1 is characterized in that: in the described step 3 in the drawing machine drawing-off multiplying power through the drawing-off in 6 roads successively be respectively 0.9,1.2,0.8,1.6,1.6,1.9.
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| CN201010606436A CN102127824B (en) | 2010-12-27 | 2010-12-27 | Manufacture method of modified polypropylene flame-retardant fiber |
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| CN103061040B (en) * | 2013-01-06 | 2015-10-28 | 浙江理工大学 | The electrostatic spinning preparation method of fibroin/polyacrylonitrile-radical antibacterial ultraviolet-resistannanofiber nanofiber membrane |
| CN111041568A (en) * | 2019-11-28 | 2020-04-21 | 洪泽联合化纤有限公司 | Preparation method of bi-component fiber |
| CN115216891A (en) * | 2022-06-27 | 2022-10-21 | 广东春夏新材料科技股份有限公司 | Antibacterial polypropylene melt-blown cloth material and preparation process thereof |
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| JPH01207430A (en) * | 1988-02-09 | 1989-08-21 | Benii Toyama Kk | Twisted yarn with high specific gravity for fishing net and fishing net utilizing said twisted yarn |
| CN1103441A (en) * | 1993-12-01 | 1995-06-07 | 北京服装学院 | Method for mfg. lodging resistant polypropylene BCF carpet yarn |
| CN1049260C (en) * | 1995-09-08 | 2000-02-09 | 岳阳石油化工总厂研究院 | Method for manufacturing superfine polypropylene filament |
| CN1176255C (en) * | 2002-02-05 | 2004-11-17 | 东华大学 | Prepn of antiseptic cationic dye capable of dyeing polypropylene fiber |
| CN1184363C (en) * | 2002-04-04 | 2005-01-12 | 中国石化上海石油化工股份有限公司 | Brightened polypropylene fibers |
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