CN112095168B - Colored ultrahigh molecular weight polyethylene fiber and preparation method thereof - Google Patents
Colored ultrahigh molecular weight polyethylene fiber and preparation method thereof Download PDFInfo
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- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
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Abstract
The invention provides a colored ultrahigh molecular weight polyethylene fiber and a preparation method thereof, which comprises the steps of uniformly mixing single or compound organic pigment and solvent white oil according to a certain proportion, heating to a certain temperature to prepare colored oily color paste, injecting the color paste into a multistage single-stage soft mixing mill, fully mixing an ultrahigh molecular weight polyethylene melt base material and the colored oily color paste by the single-stage soft mixing mill to prepare a colored melt, filtering the colored melt by a melt filter, feeding the filtered colored melt into a spinning box, and spinning by a spinneret plate under the action of a metering pump to form a colored ultrahigh molecular weight polyethylene fiber gel yarn so as to prepare the colored ultrahigh molecular weight polyethylene fiber. The method eliminates the limitation of the temperature resistance of the pigment, especially the green and fluorescent pigments, solves the problem of color distortion caused by poor temperature resistance of the pigment or the problem of low color fastness caused by coating and coloring, has simple process and lower input cost, and is suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the field of ultra-high molecular weight polyethylene fibers, and particularly relates to a colored ultra-high molecular weight polyethylene fiber and a preparation method thereof.
Background
The fishing line is a commonly used silk thread in the fishery, can be used for sea fishing and weaving fishing nets, plays an indispensable role in the fishery, and most of the components of the fishing line seen in daily life are nylon 6 and 66, which are formed by melting nylon resin slices and drawing, but the fishing line or the fishing net formed by nylon yarns is often required to be added with other components to improve the appearance and the performance in the practical marine fishery application due to the defects of low strength, easy decomposition and aging, no ultraviolet resistance, no wear resistance and the like. The high-strength PE fiber has the advantages of high strength, corrosion resistance, ultraviolet resistance and the like, makes up for the defects of nylon threads, has the advantages of self-lubricating property, easy knotting, no fishing vessel memory, small expansion ratio and the like, and is suitable for the high-end market of marine fishery.
Under the premise, with the development of fishery, customers have strict requirements on diversified high-end fishing lines, colored fishing lines are produced at the same time, and the method for coloring fibers in the world at present can be roughly divided into two methods of blending coloring and surface coating coloring. Generally, the color fastness of the colored ultra-high molecular weight polyethylene fiber is lower than that of the colored ultra-high molecular weight polyethylene fiber blended for coloring only by coating, and particularly relates to a green ultra-high molecular weight polyethylene fiber fishing line series which can be solved only by the coating coloring process in Japan.
In the published patents of blended coloring, for example: the patent ZL 200810014184.1 published in 7/30.2008, adopts the method that inorganic pigment is directly added into polyethylene and white spirit solvent for mixing, and the method requires that the diameter of inorganic pigment particles is below 1um, so that the equipment pigment is easily polluted, the coloring capability of the inorganic pigment to high-viscosity polyethylene base materials is low, the pigment is easily decomposed at the spinning temperature, and the like. The invention patent ZL 201410233026.0 published in 2017, 8, 18 and the preparation method of the ultra-high molecular weight polyethylene colored fiber adopts the steps that the organic pigment is injected into a double-screw extruder and is fully mixed under the action of high temperature and high shear in the screw extruder, the problem of uniform coloring of the pigment is solved by the method, but the organic pigment needs to be subjected to high temperature of the screw, so that higher requirements on temperature resistance are met, most of the existing pigment color systems are decomposed at the temperature of more than 260 ℃, so that the color of the finished ultra-high molecular weight polyethylene fiber is distorted, and the injection and addition of the organic pigment into the screw can increase the difficulty of the decoloring and cleaning work inside the double-screw extruder.
Disclosure of Invention
The invention aims to provide a preparation method of colored ultrahigh molecular weight polyethylene fibers, which solves the problem of color distortion caused by poor temperature resistance of pigments or the problem of low color fastness caused by coating and coloring.
The invention also aims to provide the colored ultrahigh molecular weight polyethylene fiber, the color fastness of which reaches more than five levels, the modulus of which is not less than 1200cN/dtex, and the strength of which is not less than 31cN/dtex.
The specific technical scheme of the invention is as follows:
a preparation method of colored ultra-high molecular weight polyethylene fibers comprises the following steps:
1) Heating the pigment and the solvent and uniformly stirring to obtain oily color paste;
2) Mixing the oily color paste obtained in the step 1) and the ultrahigh molecular weight polyethylene melt base material in a multistage single-stage soft mixing roll, and processing to obtain the colored ultrahigh molecular weight polyethylene fiber.
Further, the preparation method of the oily color paste in the step 1) comprises the following steps: adding the organic pigment into a solvent stirred at the speed of 60-80r/min, heating the obtained mixed solution to 150-180 ℃, continuously stirring for 20-30min, simultaneously performing ultrasonic emulsification and dispersion in the stirring process, and obtaining the oily color paste with moderate pigment concentration and uniform color after dispersion.
Further, the mass ratio of the organic pigment to the solvent is 1.
The ultrasonic emulsification and dispersion power is 3-5KW/m 2 And the frequency is 25-59HZ.
The solvent is kerosene, decalin, mineral oil or white oil which can be used for spinning the ultra-high molecular weight polyethylene fiber, and the white oil is preferred.
The organic pigment includes, but is not limited to, a green organic pigment, a yellow organic pigment, or a fluorescent organic pigment;
the green organic pigment, the yellow organic pigment or the fluorescent organic pigment has poor temperature resistance.
Further, the organic pigment further comprises: phthalocyanine blue, carbon black, green phase blue, fluorescein green, red phase yellow, phthalocyanine green, blue phase red, middle phase red, pink, and the like.
Preferably, the green organic pigment is selected from: one or more than two of phthalocyanine green G, phthalocyanine green GW and phthalocyanine green GH;
the yellow organic pigment is selected from one or two or more of H2R yellow, H4G yellow, HG yellow, HGR yellow, HR02 yellow, HR yellow, H3R yellow, H10G yellow, GR yellow, H2R yellow, G180 yellow, G151 yellow, permanent yellow 2G, permanent yellow GR, fast yellow G, pigment yellow 151, fast yellow 10G, permanent yellow 5GX, 138 yellow, 168 yellow, permanent yellow HR, permanent yellow 2GS, benzidine yellow G, permanent yellow SD-BRL, permanent yellow G, permanent yellow SD-GTL, permanent yellow SD-TRP, permanent yellow HRZ, permanent yellow-03 HR, permanent yellow SD-FGL, permanent yellow SD-GRP, newly linked aniline yellow SD-GRX, permanent yellow SD-3 and permanent yellow SD-2;
the fluorescent color organic pigment is selected from one or two of 10G yellow or 8G yellow.
Preferably, the green organic pigment and the yellow organic pigment are mixed with white oil to prepare green oily color paste, the green oily color paste can be used for spinning the green ultra-high molecular weight polyethylene fiber by the method, and the green ultra-high molecular weight polyethylene fiber can be characterized by No. 372-375 and No. 2285-2287 colors by using a pantone color card, and more preferably is green by No. 375 and No. 2284-2286 colors.
More preferably, the preparation method of the green oily color paste comprises the following steps: mixing a green organic pigment and a yellow organic pigment according to a mass ratio of 0.12-0.3 to obtain an organic pigment, adding the obtained organic pigment into white oil stirred at the speed of 60-80r/min to obtain a mixed solution, wherein the mass ratio of the organic pigment to the white oil is 1 2 And ultrasonic emulsification dispersion with the frequency of 25-59HZ can obtain the green oily color paste with moderate pigment concentration and uniform color after dispersion.
The preparation of the oily color paste in the step 1) is carried out in an oily color paste stirring kettle, and the oily color paste is injected into an oily color paste storage kettle through a centrifugal pump and stored for later use.
Further, in the step 2), the ratio of the ultra-high molecular weight polyethylene melt base stock to the oily color paste is 1: 0.0001-0.01.
In the step 2), the preparation method of the ultrahigh molecular weight polyethylene melt base stock comprises the following steps: the weight ratio of polyethylene to white oil is 1:8.2 to 15.7, and then extruding the mixture by a double-screw extruder. As the oily color paste in the subsequent process contains white oil, the solid content of the prepared solution base material is higher in order to control the ratio of the white oil to the PE powder under the condition of meeting the normal spinning condition.
Preferably, the length-diameter ratio of the twin-screw extruder is 65-85.
The polyethylene has a relative molecular weight of 4-8 × 10 6 。
Preferably, the high molecular weight polyethylene melt base comprises the following raw materials: the ultra-high molecular weight polyethylene powder is prepared from raw materials of Taikona, white oil as solvent, and antioxidant (B225 type), titanium dioxide and emulsifier (EL-12) as small materials. The mixture ratio of each material is as follows: ultra-high molecular weight polyethylene powder: white oil: antioxidant: titanium dioxide: the emulsifier is 1:8.2-15.7:0.0001-0.0005:0.000025-0.000075: 0.000001-0.000005.
Preferably, the preparation method of the high molecular weight polyethylene melt base stock comprises the following steps: firstly, adding white oil into a blending kettle, then adding PE powder, starting stirring, after stirring, uniformly mixing an antioxidant, titanium dioxide, an emulsifier and the white oil, adding the mixture into the blending kettle, wherein the mass ratio of the white oil added in the two times is 2000-5000.
Further, in order to melt the slurry, the temperature of an extruder of the double-screw extruder is 130-283 ℃, the rotating speed is 190-220r/min, and the material stays in the screw for 12-15 minutes.
The prepared high molecular weight polyethylene melt base stock is cooled by a cooling pipeline, the temperature is reduced to 180-200 ℃, and the base stock and oily color paste can be injected into a multistage single-stage soft mixing mill together for preparing colored ultrahigh molecular weight polyethylene fibers.
In the step 2), the multistage single-stage soft mixing mill fully mixes the ultra-high molecular weight polyethylene melt base stock with the colored oily color paste to prepare colored melt, the colored melt is filtered by a melt filter, enters a spinning manifold under the action of a metering pump, and is spun by a spinneret plate to form the colored ultra-high molecular weight polyethylene fiber gel yarn. The colored gel silk is processed by the procedures of extraction, drying and drafting which are well known in the industry to prepare the colored ultra-high molecular weight polyethylene fiber.
Preferably, the step 2) is specifically: injecting the oily color paste into a multistage single-stage soft mixing mill through a slurry booster pump, mixing the oily color paste with an ultrahigh molecular weight polyethylene melt base material extruded from a double-screw extruder in the multistage single-stage soft mixing mill, wherein the speed difference ratio of a differential meshing rotor is 3-4:5, preparing a colored melt at the temperature of 180-200 ℃, and then preparing colored fibers.
Further, the pressure of the slurry booster pump is 3-10MPa; preferably 8-10MPa;
further, the temperature in the multistage single-stage mild mixing mill is 182-195 ℃.
Furthermore, a booster pump is started in the preparation process to ensure that the colored melt flows normally, so that the front pressure and the rear pressure of the melt filter are consistent.
The single-stage gentle mixing machine in the step 2) is a first-stage dissolver part of a double-stage gentle mixing machine applied to the ultra-high molecular weight polyethylene fibers, which is disclosed in the patent number ZL 201822041771.1.
In the step 2), the multistage single-stage softening mixing mill is at least 3 stages, namely at least 3 single-stage softening mixing mills are connected in series.
Further, in the step 2), the feeding hole of the multistage single-stage soft mixing mill is connected with the discharging hole of the double-screw extruder through a cooling pipeline, the discharging hole of the multistage single-stage soft mixing mill is connected with the feeding hole of the solution filter, one side of the feeding hole of the multistage single-stage soft mixing mill is connected with the outlet of the slurry booster pump, and the inlet of the slurry booster pump is connected with the discharging hole of the oily color paste storage kettle.
Further, a feed inlet of the oily color paste storage kettle is connected with a discharge outlet of the oily color paste stirring kettle.
Further, the prepared colored ultra-high molecular weight polyethylene fiber gel yarn enters an extraction process after being balanced for 72 hours, and the extractant is selected from a hydrocarbon cleaning agent, but not limited to the hydrocarbon cleaning agent, and can also be dichloromethane, tetrachloroethylene, tetrahydrofuran, N-Dimethylformamide (DMF) and the like which are used for extraction steps in the preparation process of the ultra-high molecular weight polyethylene fiber.
And after the extraction process, drying and super-drawing, and winding to obtain the colored ultrahigh molecular weight polyethylene fiber, wherein the drying temperature is 45 ℃, the temperature of a drawing hot box is 160 ℃, and the super-drawing draw ratio is 25.
The colored ultrahigh molecular weight polyethylene fiber provided by the invention is prepared by adopting the method.
The existing industry adopts a stock solution coloring method to prepare a colored solution by mixing pigment, PE powder, a solvent and a small material auxiliary agent through the high-temperature shearing action of an extruder, but the temperature resistance of the pigment has certain limitation, and the existing known pigment has the common temperature resistance of 260 ℃ and a few pigments with poor temperature resistance within 200 ℃, such as green pigment, fluorescent pigment and the like. Because of the poor temperature resistance of green pigments and fluorescent pigments, the fibers of green or fluorescent colors produced at present are severely distorted and cannot meet the requirements.
Compared with the prior art, the preparation method of the colored ultra-high molecular weight polyethylene fiber is produced by a stock solution coloring method, and the method is a process route designed for eliminating the limitation of the temperature resistance of pigments, particularly green and fluorescent pigments. The color ultrahigh molecular weight polyethylene fiber produced by the method, especially the green ultrahigh molecular weight polyethylene fiber, has undistorted color and high color fastness and can meet the requirements.
Drawings
FIG. 1 is a schematic view of the structure of a process apparatus according to the present invention; 1-a double-screw extruder, 2-a cooling pipeline, 3-a five-stage single-stage soft mixing mill, 4-a melt filter, 5-a metering pump, 6-a spinning box, 7-a slurry booster pump, 8-a centrifugal pump, 9-an oily color paste storage kettle, 10-an oily color paste stirring kettle and 11-a booster pump;
FIG. 2 shows the flow of oily color paste and ultrahigh molecular weight polyethylene melt base material in a five-stage single-stage mild mixing mill and the flow of cooling water in a cooling pipe, wherein the arrows in FIG. 2 indicate the material flow direction, and in the figure, 2-cooling pipe and 3-five-stage single-stage mild mixing mill are provided.
Detailed Description
Example 1
A preparation method of colored ultra-high molecular weight polyethylene fibers is used for preparing 400D green ultra-high molecular weight polyethylene fibers and comprises the following steps:
1) Firstly, respectively weighing phthalocyanine green G and phthalocyanine green GW according to the mass ratio: permanent yellow HR 0.18:0.005 2 Continuously stirring for 20min under the ultrasonic condition with the frequency of 33HZ to prepare green oily color paste, and pumping the prepared green oily color paste into an oily color paste storage kettle 9 from an oily color paste stirring kettle 10 under the action of a centrifugal pump 8 for standby.
2) Preparing an ultra-high molecular weight polyethylene melt base stock: the viscosity average molecular weight of the ultra-high molecular weight polyethylene raw material produced by the American taconide reaches 5 x 10 6 The PE powder has white oil as solvent, and antioxidant B225, titanium white powder and emulsifier EL-12 as small material. The mixture ratio of the materials is as follows: ultra-high molecular weight polyethylene powder: white oil: antioxidant: titanium dioxide: the emulsifier is 1:10.003:0.0001:0.000025:0.000001.
the preparation method comprises the following steps: firstly, 600kg of white oil is put into a batching kettle, 60kg of PE powder is added, stirring is started, the rotating speed is set to be 75r/min and is stirred for 10min, 6g of antioxidant, 1.5g of titanium dioxide and 0.06g of emulsifier are added into a beaker, about 0.2kg of white oil is added, after stirring is carried out for 5min by a small-sized homogeneous stirrer, the batching kettle is added and is continuously stirred for 15min, then the mixed solution in the batching kettle is put into a swelling kettle, the temperature of the swelling kettle is controlled to be 110 ℃, the rotating speed is set to be 75r/min, after stirring is carried out for 2 h, the mixture is injected into a double-screw extruder 1 with the length-diameter ratio of 85, the extruder comprises 17 zones, in order to ensure that the slurry is completely melted, the rotating speed of the double-screw extruder is 200r/min, the material stays in a screw for 12 min, and the temperature of each zone of the double-screw extruder 1 is as shown in the following table 1:
TABLE 1 temperatures of the blocks of the twin-screw extruder
| |
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 |
| Temperature (. Degree. C.) | 130 | 194 | 204 | 212 | 225 | 233 | 242 | 246 | 251 | 255 | 260 | 267 | 271 | 276 | 280 | 283 | 271 |
3) Injecting the green oily slurry prepared in the step 1) into a five-stage single-stage soft mixing mill 3 from an oily slurry storage kettle 9 through a 9.2MPa slurry booster pump 7, cooling the prepared high molecular weight polyethylene melt base material through a cooling pipeline 2, and reducing the temperature to 190 ℃; the green oily slurry in the gentle mixing mill and the ultra-high molecular weight polyethylene melt base material of the cooling pipeline 2 extruded from the double-screw extruder 1 are fully mixed under the condition that the differential speed ratio is 4.3 and the temperature is set to be 182 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, wherein each stage of the five-stage single-stage gentle mixing mill is divided into four blocks, the temperature of each block in the same stage is set to be the same, so that a green melt with uniform color can be prepared, the green melt is filtered by the melt filter 4 and subjected to heat preservation, is uniformly dispersed by the pressurization of the booster pump 11, is metered by the metering pump 5, enters the spinning box 6, is sprayed into a cooling water tank by a spinneret plate for quenching, and is finally prepared into green gel silk by a silk spreader falling barrel, wherein the temperature of the melt filter 4 is set to be 200 ℃, the pressure of the booster pump 11 is stabilized at 5.5MPa, the frequency of the metering pump 5 is 25HZ, and the temperature of each zone of the spinning box 6 is set to be 195 ℃ in sequence in an increasing mode. The five-stage single-stage soft mixing machine 3 is positioned between the double-screw extruder 1 and the melt filter 4, a feed inlet of the five-stage single-stage soft mixing machine 3 is connected with a discharge outlet of the double-screw extruder 1 through a cooling pipeline 2, circulating cooling water is introduced to the surface of the cooling pipeline 2 to achieve the purpose of cooling, a discharge outlet of the five-stage single-stage soft mixing machine 3 is connected with a feed inlet of the solution filter 4, an outlet of a slurry booster pump 7 is connected to one side of the feed inlet of the five-stage single-stage soft mixing machine 3, an inlet of the slurry booster pump 7 is connected with a discharge outlet of an oily color paste storage kettle 9, and a feed inlet of the oily color paste storage kettle 9 is connected with an outlet of an oily color paste stirring kettle 10. The preparation of the oily color paste is carried out in an oily color paste stirring kettle 10, and the oily color paste is injected into an oily color paste storage kettle through a centrifugal pump 8 and stored for later use 9.
The green oily slurry and the ultra-high molecular weight polyethylene slurry enter a five-stage single-stage soft mixing mill according to the following material mass ratio: 0.00059:1.
4) After balancing for 72 hours, the green gel silk enters an extraction process, an extractant selects a hydrocarbon cleaning agent extraction process, then drying and super-drawing are carried out, winding is carried out, wherein the drying temperature is selected to be 45 ℃, the temperature of a drawing hot box is 160 ℃, and the super-drawing draw ratio is 25, and finally the green ultra-high molecular weight polyethylene fiber is obtained, and the green fiber is the No. 375 color of the international Pantong color card.
5) The performance test results of the prepared green ultra-high molecular weight polyethylene fibers are shown in the following table 2:
table 2 example 1 sample performance test data
As can be seen from the table above, the color fastness of the colored fiber sample silk is over five grades, the modulus is not lower than 1230 cN/dtex, and the strength is not lower than 33cN/dtex.
Example 2
A preparation method of colored ultra-high molecular weight polyethylene fiber is used for preparing 200D green ultra-high molecular weight polyethylene fiber, and comprises the following steps:
1) Firstly, phthalocyanine green G is weighed according to the mass ratio: HG yellow is 0.25 2 Continuously stirring for 20min under the ultrasonic condition with the frequency of 33HZ to prepare green oily color paste, and pumping the prepared green oily color paste into an oily color paste storage kettle 9 from an oily color paste stirring kettle 10 under the action of a centrifugal pump 8 for standby.
2) Preparing ultra-high molecular weight polyethylene slurry, wherein the viscosity average molecular weight of the ultra-high molecular weight polyethylene raw material produced by Tacrona is 5 to 10 6 The PE powder has white oil as solvent, and antioxidant B225, titanium white powder and emulsifier EL-12 as small material. The mixture ratio of each material is as follows: ultra-high molecular weight polyethylene powder: white oil: antioxidant: titanium dioxide: the emulsifier is 1:10:0.0001:0.000025:0.000001;
the preparation method comprises the following steps: firstly, 600kg of white oil is put into a batching kettle, 60kg of PE powder is added, stirring is started, the rotating speed is set to be 75r/min, and stirring is carried out for 10min; adding 6g of antioxidant, 1.5g of titanium dioxide and 0.06g of emulsifier into a beaker, adding about 0.2kg of white oil, stirring for 5min by using a small-sized homogenizing stirrer, adding into a batching kettle, continuously stirring for 15min by using the batching kettle, then pumping a mixed solution in the batching kettle into a swelling kettle, setting the temperature of the swelling kettle to be 110 ℃, setting the revolution number to be 75r/min, stirring for 2 h, and then injecting into a double-screw extruder 1 with the length-diameter ratio of 85, wherein the double-screw extruder comprises 17 zones, and in order to thoroughly melt slurry, the rotating speed of the extruder is 200r/min, the material stays in a screw for 12 min, and the temperature of each zone of the double-screw extruder 1 is shown in the following table 3:
TABLE 3 temperatures of the blocks of the twin-screw extruder
| |
1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 | 10 | 11 | 12 | 13 | 14 | 15 | 16 | 17 |
| Temperature (. Degree. C.) | 130 | 194 | 204 | 212 | 225 | 233 | 242 | 246 | 251 | 255 | 260 | 267 | 271 | 276 | 280 | 283 | 271 |
3) Injecting the green oily slurry prepared in the step 1) into a five-stage single-stage soft mixing mill 3 from an oily slurry storage kettle 9 through a slurry booster pump 7 at 8.7MPa, cooling the prepared high molecular weight polyethylene melt base material through a cooling pipeline 2, and reducing the temperature to 190 ℃; the green oily slurry in the gentle mixing mill and the ultra-high molecular weight polyethylene melt base material of the cooling pipeline 2 extruded from the double-screw extruder 1 are fully mixed under the condition that the differential speed ratio is 4.3 and the temperature is set to be 182 ℃, 185 ℃, 190 ℃ and 195 ℃ in sequence, wherein each stage of a five-stage single-section gentle mixing mill is divided into four blocks, the temperature of each block in the same stage is set to be the same, so that a green melt with uniform color can be prepared, the green melt is filtered by a melt filter 4 and subjected to heat preservation, is uniformly dispersed by the pressurization of a booster pump 11, is metered by a metering pump 5, enters a spinning box 6, is sprayed into a cooling water tank by a spinneret plate for quenching, and is finally prepared into green gel silk by a silk spreader falling barrel, wherein the temperature of the melt filter 4 is set to be 200 ℃, the pressure of the booster pump 11 is stabilized to be 5.5MPa, the frequency of the metering pump 5 is 25HZ, and the temperature of each zone of the spinning box 6 is gradually increased and set to be 195-200 ℃. The five-stage single-stage soft mixing machine 3 is located between the double-screw extruder 1 and the melt filter 4, a feed port of the five-stage single-stage soft mixing machine 3 is connected with a discharge port of the double-screw extruder 1 through a cooling pipeline 2, circulating cooling water is introduced to the surface of the cooling pipeline 2 to achieve the purpose of cooling, a discharge port of the five-stage single-stage soft mixing machine 3 is connected with a feed port of the solution filter 4, an outlet of a slurry booster pump 7 is connected to one side of the feed port of the five-stage single-stage soft mixing machine 3, an inlet of the slurry booster pump 7 is connected with a discharge port of an oily color paste storage kettle 9, and a feed port of the oily color paste storage kettle 9 is connected with an outlet of an oily color paste stirring kettle 10. The preparation of the oily color paste is carried out in an oily color paste stirring kettle 10, and the oily color paste is injected into an oily color paste storage kettle through a centrifugal pump 8 and stored for later use 9.
The green oily slurry and the ultrahigh molecular weight polyethylene slurry enter a multistage single-stage soft mixing mill according to the mass ratio of the materials: 0.00059:1.
4) After balancing for 72 hours, the green gel silk enters an extraction process, the extracting agent selects a hydrocarbon cleaning agent, drying and super-drawing are carried out after the extraction process, and the preparation of the green ultra-high molecular weight polyethylene fiber is finished after winding, wherein the drying temperature is selected to be 45 ℃, the temperature of a drawing hot box is 160 ℃, and the super-drawing draft ratio is 25. Finally, the green ultra-high molecular weight polyethylene fiber is prepared, and the color of the green ultra-high molecular weight polyethylene fiber is the international Pantong color card with the number of 2285.
5) The performance of the prepared green ultra-high molecular weight polyethylene fiber was tested, and the results are shown in table 4 below:
table 4 example 2 sample performance test data
The obtained product has the color fastness of more than five grades, the modulus of not less than 1200cN/dtex and the strength of not less than 31cN/dtex.
Claims (6)
1. A preparation method of colored ultra-high molecular weight polyethylene fibers is characterized by comprising the following steps:
1) Heating the pigment and the solvent and uniformly stirring to obtain oily color paste;
2) Mixing the oily color paste obtained in the step 1) and the ultrahigh molecular weight polyethylene melt base stock in a multistage single-stage soft mixing mill, and processing to obtain colored ultrahigh molecular weight polyethylene fibers;
the preparation method of the oily color paste in the step 1) comprises the following steps: adding organic pigment into white oil solvent stirred at the speed of 60-80r/min, heating the obtained mixed solution to 150-180 ℃, continuously stirring for 20-30min, and simultaneously performing ultrasonic emulsification and dispersion during stirring to obtain oily color paste;
the mass ratio of the organic pigment to the solvent is 1;
the organic pigment is selected from green organic pigment, yellow organic pigment or fluorescent organic pigment;
the step 2) is specifically as follows: injecting the oily color paste into a multistage single-stage soft mixing mill through a paste booster pump, mixing the oily color paste with an ultrahigh molecular weight polyethylene melt base material extruded from a double-screw extruder in the multistage single-stage soft mixing mill, and performing differential meshing rotor speed difference mixing at a speed ratio of 3-4:5, fully mixing the ultra-high molecular weight polyethylene melt base stock with the oily color paste at the temperature of 180-200 ℃ to prepare a colored melt, and processing to obtain colored ultra-high molecular weight polyethylene fibers; the single-stage mixing roll is a first-stage dissolver part in a double-stage mixing roll;
in the step 2), the mass ratio of the ultrahigh molecular weight polyethylene melt base material to the oily color paste is 1:0.0001-0.01;
the multistage single-stage mixing roll is at least 3 stages;
the modulus of the colored ultrahigh molecular weight polyethylene fiber is not lower than 1200cN/dtex, and the strength is not lower than 31cN/dtex.
2. The method according to claim 1, wherein the green organic pigment is selected from the group consisting of: one or more than two of phthalocyanine green G, phthalocyanine green GW and phthalocyanine green GH;
the yellow organic pigment is selected from one or two or more of H2R yellow, H4G yellow, HG yellow, HGR yellow, HR02 yellow, HR yellow, H3R yellow, H10G yellow, GR yellow, H2R yellow, G180 yellow, G151 yellow, permanent yellow 2G, permanent yellow GR, fast yellow G, pigment yellow 151, fast yellow 10G, permanent yellow 5GX, 138 yellow, 168 yellow, permanent yellow HR, permanent yellow 2GS, benzidine yellow G, permanent yellow SD-BRL, permanent yellow G, permanent yellow SD-GTL, permanent yellow SD-TRP, permanent yellow HRZ, permanent yellow HR-03, permanent yellow SD-FGL, permanent yellow SD-GRP, newly linked aniline yellow SD-GRX, permanent yellow SD-3 and permanent yellow SD-2 RP;
the fluorescent organic pigment is selected from one or two of 10G yellow or 8G yellow.
3. The preparation method of claim 2, wherein the green organic pigment and the yellow organic pigment are mixed with white oil to prepare a green oily color paste, and the green oily color paste is used for preparing the green ultra-high molecular weight polyethylene fiber, wherein the colors of the green ultra-high molecular weight polyethylene fiber can be represented by Pantong color card numbers 372-375 and 2285-2287.
4. The production method according to claim 3, characterized in that the mass ratio of the green organic pigment to the yellow organic pigment is 0.12 to 0.3.
5. The method according to claim 1 or 4, wherein the molten base stock of the ultra-high molecular weight polyethylene in step 2) is prepared by: the weight ratio of polyethylene to white oil is 1:8.2-15.7, and then extruding the mixture by a double-screw extruder;
the temperature of the extruder of the double-screw extruder is 130-283 ℃, the rotating speed is 190-220r/min, and the materials stay in the screw for 12-15 minutes.
6. A colored ultra high molecular weight polyethylene fiber prepared by the method of any one of claims 1 to 5.
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