CN103590130A - Method for improving fluidity of ultra-high molecular weight polyethylene fiber spinning solution - Google Patents
Method for improving fluidity of ultra-high molecular weight polyethylene fiber spinning solution Download PDFInfo
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Abstract
The invention relates to a method for improving fluidity of a spinning solution, and particularly relates to a method for improving fluidity of an ultra-high molecular weight polyethylene fiber spinning solution, which is used for preparation of ultra-high molecular weight polyethylene fibers. The method comprises the following steps: preparing a fluid jelly-like dissolution material, preparing a swelling suspension, and preparing ultra-high molecular weight polyethylene fibers. The method for improving fluidity of an ultra-high molecular weight polyethylene fiber spinning solution increases the fluidity of ultra-high molecular weight polyethylene fibers and increases the spinning concentration.
Description
Technical field
The present invention relates to a kind of method of improving spinning solution mobility, relate in particular to a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility, for the preparation of superhigh molecular weight polyethylene fibers.
Background technology
The superhigh molecular weight polyethylene fibers of currently available technology and aramid fiber, carbon fiber also claim three large high-performance fibers.This fiber, with performances such as its good intensity, modulus, degree of crystallinity, ABRASION RESISTANCE, cutting resistance, resistances to tearing, is widely used in fields such as maritime affairs hawser, high strength fishing net, bullet resistant material, anti-cutting appliances for labor protection, sports equipment, medical elements.
Along with superhigh molecular weight polyethylene fibers industry development, fibre manufacturing technique is ripe gradually, and every profession and trade has proposed higher requirement of strength to superhigh molecular weight polyethylene fibers.And improve fibre strength, the most significant method is for improving spinning material molecular weight, and molecular weight, by original 100～3,000,000, is increased to 500～6,000,000.The molecular weight of ultra-high molecular weight polyethylene raw material is higher, and its mobility in screw rod and filament spinning component is poorer, and the concentration of spinning solution should suitably reduce, and can meet the requirement of existing processing conditions, makes solution smooth solution in screw rod twine and export.
Summary of the invention
The present invention solves the deficiencies in the prior art, provide under the existing process conditions of a kind of solution spinning solution to flow poor, the problem that spinning concentration is lower, flow aid is mixed with ultra-high molecular weight polyethylene weak solution, obtain mobility gel and dissolve material, again it is fully mixed in mixing kettle with swelling suspension, make a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility of the spinning solution of higher concentration.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
Improve a method for superhigh molecular weight polyethylene fibers spinning solution mobility, carry out according to the following steps:
(1), preparation mobility gel dissolves material:
Ultra-high molecular weight polyethylene raw material is dissolved in to C
16～C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, emulsion process adds olefin homo;
The ultra-high molecular weight polyethylene raw material of 8kg is at C
16～C
31isoparaffin mixed solvent in dissolve, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 0.08%; The mass percentage concentration of olefin homo is 0.449%～0.748%;
Temperature in dissolution kettle is heated to 133 ℃～137 ℃, and is incubated 2～2.3h, after insulation finishes, be contained in and dissolve in bucket, and it is 25 degrees Celsius in temperature, humidity is that under 65% condition, standing 48～72h, to gel, obtains mobility gel and dissolves material, stand-by after placing;
C
16～C
31isoparaffin mixed solvent be the special-purpose white oil of 70#HPE spinning.
The model of emulsifying agent is LW90.
The model of antioxidant is B225.
(2), preparation swelling suspension:
Ultra-high molecular weight polyethylene raw material and olefin homo are at C
16～C
31isoparaffin mixed solvent in carry out emulsification and mix dispersion treatment, wherein, the mass percentage concentration of ultra-high molecular weight polyethylene is 25%, under constantly stirring, the temperature in swelling still is warming up to 120 ℃ with the speed of 1.2 ℃/min, after insulation 0.5h, obtain swelling suspension, stand-by after placing;
(3), prepare superhigh molecular weight polyethylene fibers:
Mobility gel is dissolved to material and in mixing kettle, mix with the weight ratio of 1:1.4 with swelling suspension, then constantly stir, the spinning solution that formation concentration is 15%;
Spinning solution is warming up to 150 ℃, enter in screw extruder, the temperature of spinning head is 297 ℃, form frozen glue precursor, frozen glue precursor obtains superhigh molecular weight polyethylene fibers after extraction → dry → drawing-off, and wherein the mass percentage concentration of olefin homo is ultra-high molecular weight polyethylene 1.2%～2.0%.
As preferably, in step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 500～5,500,000, the additional proportion of emulsifying agent is 0.003～0.0035% of ultra-high molecular weight polyethylene quality percentage, the additional proportion of antioxidant is 0.2～0.5% of ultra-high molecular weight polyethylene raw material, the emulsification times of emulsion process is 15～20min, the speed of heating of dissolution kettle is 1.2 ℃/min, emulsifying agent is FLUFDOLW90, antioxidant is the mixture of antioxidant 1010 and Irgafos-168, and the viscosity average molecular weigh of olefin homo divides 3,500 ten thousand;
In step (2), the mixing time in swelling still is 19～2.2h, and mixing speed is 65～70 turn/min;
In step (3), mixing time is 25～40min, and mixing speed is 65～70 turn/min, and the speed of intensification is 0.75～1.2 ℃;
Screw extruder has 16 warm areas, and the total time that warm area passes through is 12～13min;
The temperature of the first warm area is 108～109 ℃, the temperature of the second warm area is 175～176 ℃, the temperature of three-temperature-zone is 214～215 ℃, the temperature of four-temperature region is 237～238 ℃, the temperature of the 5th warm area is 244～245 ℃, the temperature of the 6th warm area is 248～249 ℃, the temperature of the 7th warm area is 250～251 ℃, the temperature of the 8th warm area is 250～251 ℃, the temperature of the 9th warm area is 255～256 ℃, the temperature of the tenth warm area is 258～260 ℃, the temperature of the 11 warm area is 269～270 ℃, the temperature of the 12 warm area is 274～275 ℃, the temperature of the tenth three-temperature-zone is 274～275 ℃, the temperature of the tenth four-temperature region is 274～275 ℃, the temperature of the 15 warm area is 273～274 ℃, the temperature of the 16 warm area is 272～273 ℃.
Therefore, a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility of the present invention, improves superhigh molecular weight polyethylene fibers mobility, improves spinning concentration.
The specific embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility, carry out according to the following steps:
(1), preparation mobility gel dissolves material:
Ultra-high molecular weight polyethylene raw material is dissolved in to C
16isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, emulsion process adds olefin homo;
The ultra-high molecular weight polyethylene raw material of 8kg is at C
16isoparaffin mixed solvent in dissolve, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 0.08%; The mass percentage concentration of olefin homo is 0.449%;
Temperature in dissolution kettle is heated to 133 ℃, and is incubated 2h, be contained in and dissolve in bucket, and be 25 degrees Celsius in temperature after insulation finishes, under the condition that humidity is 65%, standing 48h, to gel, obtains mobility gel and dissolves material, stand-by after placing;
(2), preparation swelling suspension:
Ultra-high molecular weight polyethylene raw material and olefin homo are at C
16isoparaffin mixed solvent in carry out emulsification and mix dispersion treatment, wherein, the mass percentage concentration of ultra-high molecular weight polyethylene is 25%, under constantly stirring, the temperature in swelling still is warming up to 120 ℃ with the speed of 1.2 ℃/min, after insulation 0.5h, obtain swelling suspension, stand-by after placing;
(3), prepare superhigh molecular weight polyethylene fibers:
Mobility gel is dissolved to material and in mixing kettle, mix with the weight ratio of 1:1.4 with swelling suspension, then constantly stir, the spinning solution that formation concentration is 15%;
Spinning solution is warming up to 150 ℃, enter in screw extruder, the temperature of spinning head is 297 ℃, forms frozen glue precursor, frozen glue precursor obtains superhigh molecular weight polyethylene fibers after extraction → dry → drawing-off, and wherein the mass percentage concentration of olefin homo is ultra-high molecular weight polyethylene 1.2%.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 5,000,000, the additional proportion of emulsifying agent is 0.003% of ultra-high molecular weight polyethylene quality percentage, the additional proportion of antioxidant is 0.2% of ultra-high molecular weight polyethylene raw material, the emulsification times of emulsion process is 15min, and the speed of heating of dissolution kettle is 1.2 ℃/min, and emulsifying agent is FLUFDOLW90, antioxidant is the mixture of antioxidant 1010 and Irgafos-168, and the viscosity average molecular weigh of olefin homo divides 3,500 ten thousand;
In step (2), the mixing time in swelling still is 19h, and mixing speed is 65 turn/min;
In step (3), mixing time is 25min, and mixing speed is 65 turn/min, and the speed of intensification is 0.75 ℃;
Screw extruder has 16 warm areas, and the total time that warm area passes through is 12min;
The temperature of the first warm area is 108 ℃, the temperature of the second warm area is 175 ℃, the temperature of three-temperature-zone is 214 ℃, the temperature of four-temperature region is 237 ℃, the temperature of the 5th warm area is 244 ℃, the temperature of the 6th warm area is 248 ℃, the temperature of the 7th warm area is 250 ℃, the temperature of the 8th warm area is 250 ℃, the temperature of the 9th warm area is 255 ℃, the temperature of the tenth warm area is 258 ℃, the temperature of the 11 warm area is 269 ℃, the temperature of the 12 warm area is 274 ℃, the temperature of the tenth three-temperature-zone is 274 ℃, the temperature of the tenth four-temperature region is 274 ℃, the temperature of the 15 warm area is 273 ℃, the temperature of the 16 warm area is 272 ℃.
Embodiment 2: a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility, carry out according to the following steps:
(1), preparation mobility gel dissolves material:
Ultra-high molecular weight polyethylene raw material is dissolved in to C
20isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, emulsion process adds olefin homo;
The ultra-high molecular weight polyethylene raw material of 8kg is at C
20isoparaffin mixed solvent in dissolve, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 0.08%; The mass percentage concentration of olefin homo is 0.521%;
Temperature in dissolution kettle is heated to 135 ℃, and is incubated 2.2h, be contained in and dissolve in bucket, and be 25 degrees Celsius in temperature after insulation finishes, under the condition that humidity is 65%, standing 60h, to gel, obtains mobility gel and dissolves material, stand-by after placing;
(2), preparation swelling suspension:
Ultra-high molecular weight polyethylene raw material and olefin homo are at C
20isoparaffin mixed solvent in carry out emulsification and mix dispersion treatment, wherein, the mass percentage concentration of ultra-high molecular weight polyethylene is 25%, under constantly stirring, the temperature in swelling still is warming up to 120 ℃ with the speed of 1.2 ℃/min, after insulation 0.5h, obtain swelling suspension, stand-by after placing;
(3), prepare superhigh molecular weight polyethylene fibers:
Mobility gel is dissolved to material and in mixing kettle, mix with the weight ratio of 1:1.4 with swelling suspension, then constantly stir, the spinning solution that formation concentration is 15%;
Spinning solution is warming up to 150 ℃, enter in screw extruder, the temperature of spinning head is 297 ℃, forms frozen glue precursor, frozen glue precursor obtains superhigh molecular weight polyethylene fibers after extraction → dry → drawing-off, and wherein the mass percentage concentration of olefin homo is ultra-high molecular weight polyethylene 1.8%.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 5,200,000, the additional proportion of emulsifying agent is 0.0032% of ultra-high molecular weight polyethylene quality percentage, the additional proportion of antioxidant is 0.4% of ultra-high molecular weight polyethylene raw material, the emulsification times of emulsion process is 18min, and the speed of heating of dissolution kettle is 1.2 ℃/min, and emulsifying agent is FLUFDOLW90, antioxidant is the mixture of antioxidant 1010 and Irgafos-168, and the viscosity average molecular weigh of olefin homo divides 3,500 ten thousand;
In step (2), the mixing time in swelling still is 2.0h, and mixing speed is 67 turn/min;
In step (3), mixing time is 35min, and mixing speed is 68 turn/min, and the speed of intensification is 1.02 ℃;
Screw extruder has 16 warm areas, and the total time that warm area passes through is 12.5min;
The temperature of the first warm area is 108.5 ℃, the temperature of the second warm area is 175.5 ℃, the temperature of three-temperature-zone is 214.5 ℃, the temperature of four-temperature region is 237.5 ℃, the temperature of the 5th warm area is 244.5 ℃, the temperature of the 6th warm area is 248.5 ℃, the temperature of the 7th warm area is 250.5 ℃, the temperature of the 8th warm area is 250.5 ℃, the temperature of the 9th warm area is 255.5 ℃, the temperature of the tenth warm area is 259 ℃, the temperature of the 11 warm area is 269.5 ℃, the temperature of the 12 warm area is 27.5 ℃, the temperature of the tenth three-temperature-zone is 274.5 ℃, the temperature of the tenth four-temperature region is 274.5 ℃, the temperature of the 15 warm area is 273.5 ℃, the temperature of the 16 warm area is 272.5 ℃.
Embodiment 3: a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility, carry out according to the following steps:
(1), preparation mobility gel dissolves material:
Ultra-high molecular weight polyethylene raw material is dissolved in to C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, emulsion process adds olefin homo;
The ultra-high molecular weight polyethylene raw material of 8kg is at C
31isoparaffin mixed solvent in dissolve, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 0.08%; The mass percentage concentration of olefin homo is 0.748%;
Temperature in dissolution kettle is heated to 137 ℃, and is incubated 2.3h, be contained in and dissolve in bucket, and be 25 degrees Celsius in temperature after insulation finishes, under the condition that humidity is 65%, standing 72h, to gel, obtains mobility gel and dissolves material, stand-by after placing;
(2), preparation swelling suspension:
Ultra-high molecular weight polyethylene raw material and olefin homo are at C
31isoparaffin mixed solvent in carry out emulsification and mix dispersion treatment, wherein, the mass percentage concentration of ultra-high molecular weight polyethylene is 25%, under constantly stirring, the temperature in swelling still is warming up to 120 ℃ with the speed of 1.2 ℃/min, after insulation 0.5h, obtain swelling suspension, stand-by after placing;
(3), prepare superhigh molecular weight polyethylene fibers:
Mobility gel is dissolved to material and in mixing kettle, mix with the weight ratio of 1:1.4 with swelling suspension, then constantly stir, the spinning solution that formation concentration is 15%;
Spinning solution is warming up to 150 ℃, enter in screw extruder, the temperature of spinning head is 297 ℃, forms frozen glue precursor, frozen glue precursor obtains superhigh molecular weight polyethylene fibers after extraction → dry → drawing-off, and wherein the mass percentage concentration of olefin homo is ultra-high molecular weight polyethylene 2.0%.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 5,500,000, the additional proportion of emulsifying agent is 0.0035% of ultra-high molecular weight polyethylene quality percentage, the additional proportion of antioxidant is 0.5% of ultra-high molecular weight polyethylene raw material, the emulsification times of emulsion process is 20min, and the speed of heating of dissolution kettle is 1.2 ℃/min, and emulsifying agent is FLUFDOLW90, antioxidant is the mixture of antioxidant 1010 and Irgafos-168, and the viscosity average molecular weigh of olefin homo divides 3,500 ten thousand;
In step (2), the mixing time in swelling still is 2.2h, and mixing speed is 70 turn/min;
In step (3), mixing time is 40min, and mixing speed is 70 turn/min, and the speed of intensification is 1.2 ℃;
Screw extruder has 16 warm areas, and the total time that warm area passes through is 13min;
The temperature of the first warm area is 109 ℃, the temperature of the second warm area is 176 ℃, the temperature of three-temperature-zone is 215 ℃, the temperature of four-temperature region is 238 ℃, the temperature of the 5th warm area is 245 ℃, the temperature of the 6th warm area is 249 ℃, the temperature of the 7th warm area is 251 ℃, the temperature of the 8th warm area is 251 ℃, the temperature of the 9th warm area is 256 ℃, the temperature of the tenth warm area is 260 ℃, the temperature of the 11 warm area is 270 ℃, the temperature of the 12 warm area is 275 ℃, the temperature of the tenth three-temperature-zone is 275 ℃, the temperature of the tenth four-temperature region is 275 ℃, the temperature of the 15 warm area is 274 ℃, the temperature of the 16 warm area is 273 ℃.
Claims (2)
1. improve a method for superhigh molecular weight polyethylene fibers spinning solution mobility, it is characterized in that carrying out according to the following steps:
(1), preparation mobility gel dissolves material:
Ultra-high molecular weight polyethylene raw material is dissolved in to C
16～C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, emulsion process adds olefin homo;
The ultra-high molecular weight polyethylene raw material of 8kg is at C
16～C
31isoparaffin mixed solvent in dissolve, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 0.08%; The mass percentage concentration of olefin homo is 0.449%～0.748%;
Temperature in dissolution kettle is heated to 133 ℃～137 ℃, and is incubated 2～2.3h, after insulation finishes, be contained in and dissolve in bucket, and it is 25 degrees Celsius in temperature, humidity is that under 65% condition, standing 48～72h, to gel, obtains mobility gel and dissolves material, stand-by after placing;
(2), preparation swelling suspension:
Ultra-high molecular weight polyethylene raw material and olefin homo are at C
16～C
31isoparaffin mixed solvent in carry out emulsification and mix dispersion treatment, wherein, the mass percentage concentration of ultra-high molecular weight polyethylene is 25%, under constantly stirring, the temperature in swelling still is warming up to 120 ℃ with the speed of 1.2 ℃/min, after insulation 0.5h, obtain swelling suspension, stand-by after placing;
(3), prepare superhigh molecular weight polyethylene fibers:
Mobility gel is dissolved to material and in mixing kettle, mix with the weight ratio of 1:1.4 with swelling suspension, then constantly stir, the spinning solution that formation concentration is 15%;
Spinning solution is warming up to 150 ℃, enter in screw extruder, the temperature of spinning head is 297 ℃, form frozen glue precursor, frozen glue precursor obtains superhigh molecular weight polyethylene fibers after extraction → dry → drawing-off, and wherein the mass percentage concentration of olefin homo is ultra-high molecular weight polyethylene 1.2%～2.0%.
2. a kind of method of improving superhigh molecular weight polyethylene fibers spinning solution mobility according to claim 1, is characterized in that:
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 500～5,500,000, the additional proportion of emulsifying agent is 0.003～0.0035% of ultra-high molecular weight polyethylene quality percentage, the additional proportion of antioxidant is 0.2～0.5% of ultra-high molecular weight polyethylene raw material, the emulsification times of emulsion process is 15～20min, the speed of heating of dissolution kettle is 1.2 ℃/min, emulsifying agent is FLUFDOLW90, B225 type antioxidant is the mixture of antioxidant 1010 and Irgafos-168, and the viscosity average molecular weigh of olefin homo divides 3,500 ten thousand;
In step (2), the mixing time in swelling still is 19～2.2h, and mixing speed is 65～70 turn/min;
In step (3), mixing time is 25～40min, and mixing speed is 65～70 turn/min, and the speed of intensification is 0.75～1.2 ℃;
Screw extruder has 16 warm areas, and the total time that warm area passes through is 12～13min;
The temperature of the first warm area is 108～109 ℃, the temperature of the second warm area is 175～176 ℃, the temperature of three-temperature-zone is 214～215 ℃, the temperature of four-temperature region is 237～238 ℃, the temperature of the 5th warm area is 244～245 ℃, the temperature of the 6th warm area is 248～249 ℃, the temperature of the 7th warm area is 250～251 ℃, the temperature of the 8th warm area is 250～251 ℃, the temperature of the 9th warm area is 255～256 ℃, the temperature of the tenth warm area is 258～260 ℃, the temperature of the 11 warm area is 269～270 ℃, the temperature of the 12 warm area is 274～275 ℃, the temperature of the tenth three-temperature-zone is 274～275 ℃, the temperature of the tenth four-temperature region is 274～275 ℃, the temperature of the 15 warm area is 273～274 ℃, the temperature of the 16 warm area is 272～273 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179494A (en) * | 2018-01-18 | 2018-06-19 | 上海斯瑞科技有限公司 | A kind of superhigh molecular weight polyethylene fibers and preparation method thereof |
| CN110318116A (en) * | 2019-05-29 | 2019-10-11 | 长青藤高性能纤维材料有限公司 | A kind of preparation method of extra-high strong ultra high molecular weight polyethylene fiber |
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| CN102020738A (en) * | 2009-09-09 | 2011-04-20 | 赞南科技(上海)有限公司 | Olefin polymer and blend fiber and preparation methods and applications thereof |
| CN103305954A (en) * | 2013-07-01 | 2013-09-18 | 浙江大学 | Method for preparing ultra-high molecular weight polyethylene fiber |
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| US4413110A (en) * | 1981-04-30 | 1983-11-01 | Allied Corporation | High tenacity, high modulus polyethylene and polypropylene fibers and intermediates therefore |
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| CN102020738A (en) * | 2009-09-09 | 2011-04-20 | 赞南科技(上海)有限公司 | Olefin polymer and blend fiber and preparation methods and applications thereof |
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| CN108179494A (en) * | 2018-01-18 | 2018-06-19 | 上海斯瑞科技有限公司 | A kind of superhigh molecular weight polyethylene fibers and preparation method thereof |
| CN108179494B (en) * | 2018-01-18 | 2020-05-29 | 上海斯瑞科技有限公司 | Ultra-high molecular weight polyethylene fiber and preparation method thereof |
| CN110318116A (en) * | 2019-05-29 | 2019-10-11 | 长青藤高性能纤维材料有限公司 | A kind of preparation method of extra-high strong ultra high molecular weight polyethylene fiber |
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Application publication date: 20140219 |