CN103572396B - Preparation method of blended modified ultra-high molecular weight polyethylene fiber - Google Patents
Preparation method of blended modified ultra-high molecular weight polyethylene fiber Download PDFInfo
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Abstract
The invention relates to an ultra-high molecular weight polyethylene fiber and particularly relates to a preparation method of a blended modified ultra-high molecular weight polyethylene fiber, which is used for preparing the ultra-high molecular weight polyethylene fiber. The preparation method comprises the following steps of: preparing swelling suspension liquid, preparing modified mixed suspension liquid, blending the swelling suspension liquid with the modified mixed suspension liquid, and preparing grey-series ultra-high molecular weight polyethylene fibers. According to the preparation method of the blended modified ultra-high molecular weight polyethylene fiber disclosed by the invention, the ultra-high molecular weight polyethylene fiber is enabled to be modified fiber with good impact resistance, wear resistance and creeping deformation resistance.
Description
Technical field
The present invention relates to a kind of superhigh molecular weight polyethylene fibers, particularly relate to a kind of preparation method of blending and modifying superhigh molecular weight polyethylene fibers, for the preparation of superhigh molecular weight polyethylene fibers.
Background technology
Superhigh molecular weight polyethylene fibers has excellent mechanical property, impact resistance and resistance to chemical corrosion, also there is fabulous bending property and UV resistant performance simultaneously, at high-technology field, the important application especially in hawser and high-strength composite material Material Field is subject to people and pays close attention to greatly.
By analyzing the molecular structure of superhigh molecular weight polyethylene fibers, the supramolecular structure of known fiber is quite simple, and high-sequential.Non-polar group on fiber macromolecular chain, without chemism, and surface energy is lower.Therefore, fiber is being that impact resistance, ABRASION RESISTANCE and creep-resistant property are inadequate as bullet resistant material, hawser, protective materials use.Above-mentioned drawbacks limit fiber applying in high-grade, precision and advanced industry, therefore, improves fiber inherent shortcoming targetedly, and it is necessary for improving resistant fiber impact, ABRASION RESISTANCE and creep resistance.
Summary of the invention
The present invention mainly solves the deficiencies in the prior art, provides a kind of by adding a certain proportion of Single Walled Carbon Nanotube, Graphene powder, Nano-meter SiO_2 in spinning solution
2be prepared into modification mixing suspension, obtain grey colour system modified ultra-high molecular weight polyethylene frozen glue precursor through spinning screw and filament spinning component after mixing, the preparation method of blending and modifying superhigh molecular weight polyethylene fibers of modified fibre of excellent impact resistance, ABRASION RESISTANCE and creep resistance can be had through extraction-drying-hot-stretch.
Above-mentioned technical problem of the present invention is mainly solved by following technical proposals:
A preparation method for blending and modifying superhigh molecular weight polyethylene fibers, carries out according to the following steps:
(1), swelling suspension is prepared:
Ultra-high molecular weight polyethylene raw material is dissolved in C
16~ C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, under constantly stirring in swelling still, the temperature in swelling still, with ramp to 120 ~ 125 DEG C of 1.2 DEG C/min, after insulation 0.5h, obtains swelling suspension;
The addition of ultra-high molecular weight polyethylene raw material is C
16~ C
31isoparaffin mixed solvent 10.788%, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 9.738%;
C
16~ C
31isoparaffin mixed solvent be the special white oil of 70#HPE spinning.
The model of emulsifying agent is LW90.
The model of antioxidant is B225 type.
(2), modification mixing suspension is prepared:
By Single Walled Carbon Nanotube and Nano-meter SiO_2
2put into mulser to disperse, the time of dispersion is 30min, and point adds Graphene powder 3 times, and obtain modification mixing suspension after emulsification, in modification mixing suspension, solid content is 5.264%;
The mass percentage concentration of Single Walled Carbon Nanotube is 1.724%;
Nano-meter SiO_2
2mass percentage concentration is 2.699%;
The mass percentage concentration of Graphene powder is 0.841%;
The model of Single Walled Carbon Nanotube comprises following several: JCST-95-11-10, TNST, CNT400, SWCNT.
(3), swelling suspension and modification mixing suspension blended:
Modification mixing suspension is mixed in swelling still with the mass ratio of swelling suspension according to 1:39.92 ~ 1:69.54, then constantly stir, stir and be warming up to 150 DEG C, after insulation 0.5h, form spin fluid, wherein the mass percent of ultra-high molecular weight polyethylene is 9.5% ~ 9.6%; Spin fluid injects double screw extruder by blanking still;
Spin fluid temperature rises to 275 ~ 290 DEG C by 110 ~ 115 DEG C, twines effect through screw rod solution, lasts 12.5 ~ 13min and enters spinning pack, is with certain flow slivering under the prerequisite of 293 ~ 295 DEG C in temperature, the grey frozen glue precursor obtained;
(4), grey colour system superhigh molecular weight polyethylene fibers is prepared:
After frozen glue precursor shrinks 48h in advance after stress equilibrium, agent for carbon hydrogen detergent is used to extract frozen glue precursor, and complete extractant removal technique at the baking oven of 40 DEG C, form superhigh molecular weight polyethylene fibers semi-finished product, superhigh molecular weight polyethylene fibers semi-finished product are that the seven roller drawing machines of 130 DEG C carry out ultra-drawing in temperature, make the macromolecular orientation in fiber, in the macromolecular degree of crystallinity of stress induced lower raising polyethylene, ultra-high molecular weight polyethylene molecule changes extended-chain configuration into by folded-chain structure, fall obtained grey colour system superhigh molecular weight polyethylene fibers after a rolling, wherein Single Walled Carbon Nanotube, Nano-meter SiO_2
2, Graphene is 0.255 ~ 0.443%, 0.399 ~ 0.694%, 0.124 ~ 0.216% relative to the weight ratio of ultra-high molecular weight polyethylene.
As preferably, in step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 550 ~ 6,000,000, the mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.003 ~ 0.0035%, the mass percentage concentration that antioxidant accounts for ultra-high molecular weight polyethylene is 0.2 ~ 0.5%, the mixing speed of swelling still is 65 ~ 70 turns/min, and the mixing time of swelling still is 2.0 ~ 2.5h;
In step (2), the rate of dispersion of mulser is 3000 turns/min, and the jitter time of mulser is 15 ~ 30min, and each interval time of adding Graphene powder is 5 ~ 10min;
In step (3), the ratio of modification mixing suspension and swelling suspension is 1:39.92, and the speed of stirring is 65 ~ 70 turns/min, and the time of stirring is 1.9 ~ 2.2h, and the speed of flow is 16 ~ 16.26kg/h.
Therefore, the preparation method of blending and modifying superhigh molecular weight polyethylene fibers of the present invention, makes superhigh molecular weight polyethylene fibers have the modified fibre of excellent impact resistance, ABRASION RESISTANCE and creep resistance.
Detailed description of the invention
Below by embodiment, technical scheme of the present invention is described in further detail.
Embodiment 1: a kind of preparation method of blending and modifying superhigh molecular weight polyethylene fibers, carry out according to the following steps:
(1), swelling suspension is prepared:
Ultra-high molecular weight polyethylene raw material is dissolved in C
16isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, under constantly stirring in swelling still, the temperature in swelling still, with the ramp to 120 DEG C of 1.2 DEG C/min, after insulation 0.5h, obtains swelling suspension;
The addition of ultra-high molecular weight polyethylene raw material is C
16isoparaffin mixed solvent 10.788%, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 9.738%;
(2), modification mixing suspension is prepared:
By Single Walled Carbon Nanotube and Nano-meter SiO_2
2put into mulser to disperse, the time of dispersion is 30min, and point adds Graphene powder 3 times, and obtain modification mixing suspension after emulsification, in modification mixing suspension, solid content is 5.264%;
The mass percentage concentration of Single Walled Carbon Nanotube is 1.724%;
Nano-meter SiO_2
2mass percentage concentration is 2.699%;
The mass percentage concentration of Graphene powder is 0.841%;
(3), swelling suspension and modification mixing suspension blended:
Modification mixing suspension is mixed in swelling still with the mass ratio of swelling suspension according to 1:39.92, then constantly stir, stir and be warming up to 150 DEG C, after insulation 0.5h, form spin fluid, wherein the mass percent of ultra-high molecular weight polyethylene is 9.5%; Spin fluid injects double screw extruder by blanking still;
Spin fluid temperature rises to 275 DEG C by 110 DEG C, twines effect through screw rod solution, lasts 12.5min and enters spinning pack, is the prerequisite down-off slivering of 293 DEG C in temperature, the grey frozen glue precursor obtained;
(4), grey colour system superhigh molecular weight polyethylene fibers is prepared:
After frozen glue precursor shrinks 48h in advance after stress equilibrium, agent for carbon hydrogen detergent is used to extract frozen glue precursor, and complete extractant removal technique at the baking oven of 40 DEG C, form superhigh molecular weight polyethylene fibers semi-finished product, superhigh molecular weight polyethylene fibers semi-finished product are that the seven roller drawing machines of 130 DEG C carry out ultra-drawing in temperature, make the macromolecular orientation in fiber, in the macromolecular degree of crystallinity of stress induced lower raising polyethylene, ultra-high molecular weight polyethylene molecule changes extended-chain configuration into by folded-chain structure, fall obtained grey colour system superhigh molecular weight polyethylene fibers after a rolling, wherein Single Walled Carbon Nanotube, Nano-meter SiO_2
2, Graphene is 0.255%, 0.399%, 0.124% relative to the weight ratio of ultra-high molecular weight polyethylene.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 5,500,000, the mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.003%, the mass percentage concentration that antioxidant accounts for ultra-high molecular weight polyethylene is 0.2%, the mixing speed of swelling still is 65 turns/min, and the mixing time of swelling still is 2.0h;
In step (2), the rate of dispersion of mulser is 3000 turns/min, and the jitter time of mulser is 15min, and each interval time of adding Graphene powder is 5min;
In step (3), the ratio of modification mixing suspension and swelling suspension is 1:39.92, and the speed of stirring is 65 turns/min, and the time of stirring is 1.9h, and the speed of flow is 16kg/h.
Embodiment 2: a kind of preparation method of blending and modifying superhigh molecular weight polyethylene fibers, carry out according to the following steps:
(1), swelling suspension is prepared:
Ultra-high molecular weight polyethylene raw material is dissolved in C
20isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, under constantly stirring in swelling still, the temperature in swelling still, with the ramp to 122 DEG C of 1.2 DEG C/min, after insulation 0.5h, obtains swelling suspension;
The addition of ultra-high molecular weight polyethylene raw material is C
20isoparaffin mixed solvent 10.788%, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 9.738%;
(2), modification mixing suspension is prepared:
By Single Walled Carbon Nanotube and Nano-meter SiO_2
2put into mulser to disperse, the time of dispersion is 30min, and point adds Graphene powder 3 times, and obtain modification mixing suspension after emulsification, in modification mixing suspension, solid content is 5.264%;
The mass percentage concentration of Single Walled Carbon Nanotube is 1.724%;
Nano-meter SiO_2
2mass percentage concentration is 2.699%;
The mass percentage concentration of Graphene powder is 0.841%;
(3), swelling suspension and modification mixing suspension blended:
Modification mixing suspension is mixed in swelling still with the mass ratio of swelling suspension according to 1:40, then constantly stir, stir and be warming up to 150 DEG C, after insulation 0.5h, form spin fluid, wherein the mass percent of ultra-high molecular weight polyethylene is 9.55%; Spin fluid injects double screw extruder by blanking still;
Spin fluid temperature rises to 280 DEG C by 112 DEG C, twines effect through screw rod solution, lasts 12.7min and enters spinning pack, is the prerequisite down-off slivering of 294 DEG C in temperature, the grey frozen glue precursor obtained;
(4), grey colour system superhigh molecular weight polyethylene fibers is prepared:
After frozen glue precursor shrinks 48h in advance after stress equilibrium, agent for carbon hydrogen detergent is used to extract frozen glue precursor, and complete extractant removal technique at the baking oven of 40 DEG C, form superhigh molecular weight polyethylene fibers semi-finished product, superhigh molecular weight polyethylene fibers semi-finished product are that the seven roller drawing machines of 130 DEG C carry out ultra-drawing in temperature, make the macromolecular orientation in fiber, in the macromolecular degree of crystallinity of stress induced lower raising polyethylene, ultra-high molecular weight polyethylene molecule changes extended-chain configuration into by folded-chain structure, fall obtained grey colour system superhigh molecular weight polyethylene fibers after a rolling, wherein Single Walled Carbon Nanotube, Nano-meter SiO_2
2, Graphene is 0.3%, 0.5%, 0.2% relative to the weight ratio of ultra-high molecular weight polyethylene.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 5,800,000, the mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.0032%, the mass percentage concentration that antioxidant accounts for ultra-high molecular weight polyethylene is 0.4%, the mixing speed of swelling still is 68 turns/min, and the mixing time of swelling still is 2.2h;
In step (2), the rate of dispersion of mulser is 3000 turns/min, and the jitter time of mulser is 25min, and each interval time of adding Graphene powder is 7min;
In step (3), the ratio of modification mixing suspension and swelling suspension is 1:50, and the speed of stirring is 68 turns/min, and the time of stirring is 2.0h, and the speed of flow is 16.1kg/h.
Embodiment 3: a kind of preparation method of blending and modifying superhigh molecular weight polyethylene fibers, carry out according to the following steps:
(1), swelling suspension is prepared:
Ultra-high molecular weight polyethylene raw material is dissolved in C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, under constantly stirring in swelling still, the temperature in swelling still, with the ramp to 125 DEG C of 1.2 DEG C/min, after insulation 0.5h, obtains swelling suspension;
The addition of ultra-high molecular weight polyethylene raw material is C
31isoparaffin mixed solvent 10.788%, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 9.738%;
(2), modification mixing suspension is prepared:
By Single Walled Carbon Nanotube and Nano-meter SiO_2
2put into mulser to disperse, the time of dispersion is 30min, and point adds Graphene powder 3 times, and obtain modification mixing suspension after emulsification, in modification mixing suspension, solid content is 5.264%;
The mass percentage concentration of Single Walled Carbon Nanotube is 1.724%;
Nano-meter SiO_2
2mass percentage concentration is 2.699%;
The mass percentage concentration of Graphene powder is 0.841%;
(3), swelling suspension and modification mixing suspension blended:
Modification mixing suspension is mixed in swelling still with the mass ratio of swelling suspension according to 1:69.54, then constantly stir, stir and be warming up to 150 DEG C, after insulation 0.5h, form spin fluid, wherein the mass percent of ultra-high molecular weight polyethylene is 9.6%; Spin fluid injects double screw extruder by blanking still;
Spin fluid temperature rises to 290 DEG C by 115 DEG C, twines effect through screw rod solution, lasts 13min and enters spinning pack, is with certain flow slivering under the prerequisite of 295 DEG C in temperature, the grey frozen glue precursor obtained;
(4), grey colour system superhigh molecular weight polyethylene fibers is prepared:
After frozen glue precursor shrinks 48h in advance after stress equilibrium, agent for carbon hydrogen detergent is used to extract frozen glue precursor, and complete extractant removal technique at the baking oven of 40 DEG C, form superhigh molecular weight polyethylene fibers semi-finished product, superhigh molecular weight polyethylene fibers semi-finished product are that the seven roller drawing machines of 130 DEG C carry out ultra-drawing in temperature, make the macromolecular orientation in fiber, in the macromolecular degree of crystallinity of stress induced lower raising polyethylene, ultra-high molecular weight polyethylene molecule changes extended-chain configuration into by folded-chain structure, fall obtained grey colour system superhigh molecular weight polyethylene fibers after a rolling, wherein Single Walled Carbon Nanotube, Nano-meter SiO_2
2, Graphene is 0.443%, 0.694%, 0.216% relative to the weight ratio of ultra-high molecular weight polyethylene.
In step (1), the viscosity average molecular weigh of ultra-high molecular weight polyethylene raw material is 6,000,000, the mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.0035%, the mass percentage concentration that antioxidant accounts for ultra-high molecular weight polyethylene is 0.5%, the mixing speed of swelling still is 70 turns/min, and the mixing time of swelling still is 2.5h;
In step (2), the rate of dispersion of mulser is 3000 turns/min, and the jitter time of mulser is 15 ~ 30min, and each interval time of adding Graphene powder is 10min;
In step (3), the ratio of modification mixing suspension and swelling suspension is 1:69.54, and the speed of stirring is 70 turns/min, and the time of stirring is 2.2h, and the speed of flow is 16.26kg/h.
Claims (2)
1. a preparation method for blending and modifying superhigh molecular weight polyethylene fibers, is characterized in that carrying out according to the following steps:
(1), swelling suspension is prepared:
Ultra-high molecular weight polyethylene raw material is dissolved in C
16~ C
31isoparaffin mixed solvent in, and add emulsifying agent and antioxidant, under constantly stirring in swelling still, the temperature in swelling still, with ramp to 120 ~ 125 DEG C of 1.2 DEG C/min, after insulation 0.5h, obtains swelling suspension;
The addition of ultra-high molecular weight polyethylene raw material is C
16~ C
31isoparaffin mixed solvent 10.788%, the mass percentage concentration of ultra-high molecular weight polyethylene raw material is 9.738%;
(2), modification mixing suspension is prepared:
By Single Walled Carbon Nanotube and Nano-meter SiO_2
2put into mulser to disperse, the time of dispersion is 30min, and point adds Graphene powder 3 times, and obtain modification mixing suspension after emulsification, in modification mixing suspension, solid content is 5.264%;
The mass percentage concentration of Single Walled Carbon Nanotube is 1.724%;
Nano-meter SiO_2
2mass percentage concentration is 2.699%;
The mass percentage concentration of Graphene powder is 0.841%;
(3), swelling suspension and modification mixing suspension blended:
Modification mixing suspension is mixed in swelling still with the mass ratio of swelling suspension according to 1:39.92 ~ 1:69.54, then constantly stir, stir and be warming up to 150 DEG C, after insulation 0.5h, form spin fluid, wherein the mass percent of ultra-high molecular weight polyethylene is 9.5% ~ 9.6%; Spin fluid injects double screw extruder by blanking still;
Spin fluid temperature rises to 275 ~ 290 DEG C by 110 ~ 115 DEG C, twines effect through screw rod solution, lasts 12.5 ~ 13min and enters spinning pack, is the prerequisite down-off slivering of 293 ~ 295 DEG C in temperature, the grey frozen glue precursor obtained;
(4), grey colour system superhigh molecular weight polyethylene fibers is prepared:
After frozen glue precursor shrinks 48h in advance after stress equilibrium, agent for carbon hydrogen detergent is used to extract frozen glue precursor, and complete extractant removal technique at the baking oven of 40 DEG C, form superhigh molecular weight polyethylene fibers semi-finished product, superhigh molecular weight polyethylene fibers semi-finished product are that the seven roller drawing machines of 130 DEG C carry out ultra-drawing in temperature, make the macromolecular orientation in fiber, in the macromolecular degree of crystallinity of stress induced lower raising polyethylene, ultra-high molecular weight polyethylene molecule changes extended-chain configuration into by folded-chain structure, fall obtained grey colour system superhigh molecular weight polyethylene fibers after a rolling, wherein Single Walled Carbon Nanotube, Nano-meter SiO_2
2, Graphene is 0.255 ~ 0.443%, 0.399 ~ 0.694%, 0.124 ~ 0.216% relative to the weight ratio of ultra-high molecular weight polyethylene.
2. the preparation method of blending and modifying superhigh molecular weight polyethylene fibers 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 550 ~ 6,000,000, the mass percentage concentration that emulsifying agent accounts for ultra-high molecular weight polyethylene is 0.003 ~ 0.0035%, the mass percentage concentration that antioxidant accounts for ultra-high molecular weight polyethylene is 0.2 ~ 0.5%, the mixing speed of swelling still is 65 ~ 70 turns/min, and the mixing time of swelling still is 2.0 ~ 2.5h;
In step (2), the rate of dispersion of mulser is 3000 turns/min, and the jitter time of mulser is 15 ~ 30min, and each interval time of adding Graphene powder is 5 ~ 10min;
In step (3), the ratio of modification mixing suspension and swelling suspension is 1:39.92 ~ 1:69.54, and the speed of stirring is 65 ~ 70 turns/min, and the time of stirring is 1.9 ~ 2.2h, and the speed of flow is 16 ~ 16.26kg/h.
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| PT3072998T (en) * | 2014-09-17 | 2020-04-30 | Jiangsu Jonnyma New Mat Co Ltd | Preparation method for and application of ultra-high molecular weight polyethylene fiber with high cut resistance |
| CN104762683A (en) * | 2015-04-09 | 2015-07-08 | 江苏九九久科技股份有限公司 | Graphene composite modified high-strength polyethylene fiber and preparation method thereof |
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