CN106544746A - Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre - Google Patents
Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre Download PDFInfo
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Abstract
Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre, the mixed solution for possessing intrinsic viscosity formed by polyvinyl resin with super-high molecular weight and spinning good solvent, auxiliary agent and additives of pigments, the ultra-high molecular weight polyethylene colored fibers of excellent quality, preparation method are prepared by dry spinning device：1st, uniformly possesses the preparation of the spinning material mixed solution of intrinsic viscosity；2nd, the preparation of the precursor of frozen glue containing pigment；3rd, ring blow, upper boundling, the preparation of the nascent colored fibre of high power jet stretch；4th, the recycling and process of spinning good solvent, pigment and system dry gas；5th, high power first break draft prepares ultra-high molecular weight polyethylene colored fibers.Dye-free technique of the present invention, thus fiber cost it is low, pollute little, product aberration it is little, fiber quality is excellent to can be widely used for the fields such as netting, military project, composite.
Description
Technical field
The invention belongs to chemical fiber field, is related to a kind of ultra-high molecular weight polyethylene mixed solution dry spinning and prepares the method for colored fibre using the ultra-high molecular weight polyethylene colored fibers for possessing excellent properties prepared by this method.
Background technology
Ultra-high molecular weight polyethylene (UHMWPE) fiber, it is also called high-strength high-modulus polyethylene fiber, it is high-tech, the high-performance fiber for occurring the beginning of the nineties, it is one of three big tec fibers of world today (carbon fiber, aramid fiber, high-strength high-modulus polyethylene fiber), as the dilute fiber of superhigh molecular weight polyethylene has high-crystallinity and height-oriented extended-chain configuration, compared with carbon fiber, aramid fiber, the intensity of the dilute fiber of superhigh molecular weight polyethylene is higher；Quality is lighter, and chemical stability is more preferable；With very strong chemical inertness, resistance to strong acid, strong base solution and organic solvent；With good weatherability, Jing after 1500h Exposures to Sunlight, fibre strength conservation rate is still up to 80%, and UV resistance is very superior；Lower temperature resistance is good, can as little as -150 DEG C using temperature；Outside, the wear-resisting resistance to bend(ing) energy of the dilute fiber of superhigh molecular weight polyethylene, fatigue tension performance, it is cutting resistance can be also most strong in existing high-performance fiber.Very important effect is played in safety, protection, Aeronautics and Astronautics, defence equipment, vehicle manufacture, shipbuilding industry, sporting world.It is widely used in the fields such as rope, fishing net, setline, composite.In addition, the dilute fiber of superhigh molecular weight polyethylene is also had broad application prospects as shock resistance, vibration-absorptive material and high performance light composite material in civilian industry field.
High-strength high-modulus polyethylene fiber is high due to molecular weight, main chain is combined, the degree of orientation, degree of crystallinity are high, therefore its specific strength be current all fibres most. polyethylene has the chemical constitution of the connected macromolecular chain of methylene (- CH2-CH2-), the crystal structure of the dilute amorphous area and folded chain that there are a large amount of random coils of superhigh molecular weight polyethylene.In super times of drawing-off, its macromolecular chain it is height-oriented, be fully extended crystalline region and the macromole of amorphous area, define the extended chain supramolecular structure of highly crystalline.Such supramolecular structure determines the superior function of high-tenacity polyethylene fibre.Its molecule is nonpolarity and crystallization regularity makes dye molecule be difficult to incision wherein simultaneously, and stock-dye is difficult, and the mostly of production are brown stocks at present.If inorganic pigment additive is directly mixed with ultra-high molecular weight polyethylene powder, pigment easily reunion bad dispersibility easily causes uneven dyeing, is dyeed again as the chemical inertness light fastness of polyethylene is not high after making product.
The content of the invention
The present invention innovative approach be：The measuring rheological property data base of the ultra-high molecular weight polyethylene mixed solution determined using torque rheometer（The data base contains 1, the different polyvinyl resin concentration without pigment, different shear rate, the measuring rheological property data of the ultra-high molecular weight polyethylene starting material liquid mixture of different mixing temperatures；2nd, different type, the at different conditions pigment of variable concentrations, measuring rheological property data of mixed solution etc. are added under same polyvinyl resin concentration）, by polyvinyl resin with super-high molecular weight and spinning good solvent, auxiliary agent, the optimal proportion that specific complex antioxidant and the special pigment nontoxic containing nanoscale are empirically determined, solution in injection special raw material configuration system twines swelling in kettle, high shear in a solvent makes appropriate solution between ultra-high molecular weight polyethylene macromole twine to form the homogeneous mixture solotion for possessing particular fluid rheological property, twine after the regular hour by the swelling solution of concentration proportioning, injected by the delivery pump that flows back and further sheared in homogenizing kettle, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards, the spinning equipment extruding spinning such as static mixer.
The present invention is achieved like this：Ultra-high molecular weight polyethylene mixed solution dry spinning prepares the method and fiber of colored fibre, the fiber is the mixed solution for possessing particular fluid rheological property formed by polyvinyl resin with super-high molecular weight and spinning good solvent, auxiliary agent and additives of pigments, trial assembly is expanded by existing spinning and puts the ultra-high molecular weight polyethylene colored fibers for preparing excellent quality, preparation method is embodied as comprising the following steps：（1）Uniformly possesses the preparation of the spinning material mixed solution of particular fluid rheological characteristic；（2）The preparation of the precursor of frozen glue containing pigment；（3）Ring blows, upper boundling, the preparation of the nascent colored fibre of high power jet stretch；（4）The recycling and process of spinning good solvent, pigment and system dry gas；（5）High power first break draft prepares ultra-high molecular weight polyethylene colored fibers.
Usually, the spinning material mixed solution for possessing particular fluid rheological characteristic refers to the homogeneous emulsus mixed solution that the raw material mixed solution for preparing colored fibre of the present invention is formed after appropriate solution is twined in raw material configuration system, which passes through the rheological characteristic test test result of torque rheometer, its peak torque L is 4 ~ 30Nm, preferably 8 ~ 15 Nm；
The spinning material mixed solution for possessing particular fluid rheological characteristic refers to the homogeneous emulsus mixed solution that the raw material mixed solution for preparing colored fibre of the present invention is formed after appropriate solution is twined in raw material configuration system, which passes through the rheological characteristic test of torque rheometer, test result, its plasticizing moment of torsion F is 2 ~ 15Nm, preferably 5 ~ 10 Nm；
In the spinning material mixed solution for possessing particular fluid rheological characteristic, additives of pigments is not limited to one kind of inorganic pigment or its similar combination such as red normal perylene, quinoline promise furan phthalein, azo organic pigment and carbon black, bismuth vanadate yellow.
The addition of additives of pigments for mixed solution 0.005% ~ 0.250% in the spinning material mixed solution for uniformly possessing particular fluid rheological characteristic, preferably 0.010% ~ 0.150%；
The auxiliary agent added in the spinning material mixed solution for uniformly possessing particular fluid rheological characteristic, it is not limited to conventional use of antioxidant and magnesium stearate plasticizer etc., the composite antioxidant composite assistants HTB-7630 used to the colored fibre that the present invention is obtained by preferred pin, can make the color fastness of finished product colored fibre improve more than 1 grade using the compound antioxidant composite assistants.
The process for preparing nascent colored fibre is contained, go out the frozen glue precursor of spinneret by ring blow equipment by which in after most of good solvent for including reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtain high power jet stretch.
The recycling of the spinning good solvent, pigment and system dry gas and processing procedure contain one or several special efficient unitized exchangers, and comprising being not limited to the dry spinning equipment such as conventional compressor, blower fan and membrane separator.
Recycling and the processing procedure of the spinning good solvent, pigment and system dry gas, the response rate of its good solvent reach more than 99%, and in good solvent, pigment concentration is less than 50ppm.
Nascent colored fibre, the finished fiber of Jing high power first break draft are prepared using the inventive method, its intensity is 10 ~ 35g/d, and modulus is 300 ~ 1600g/d.
The present invention is on the basis of existing spinning technique is optimized, the setting and regulation of spinning process equipment and technological parameter are targetedly instructed by the sign to spinning material liquid, the especially preparation of colour system fiber, significantly reduce production cost, the colored fibre for being obtained under controllable process conditions, excellent quality, the technical process after improvement, pollution problem of the pigment to environment is also overcomed, the production process of environmental protection is realized.
Dye-free technique of the present invention, thus fiber cost it is low, pollute little, product aberration it is little, fiber quality is excellent, can be widely used for the fields such as netting, military project, composite.
Description of the drawings
Fig. 1 is embodiment of the present invention UHMWPE mixed resin solution rheological characteristic test result.
Specific embodiment
The present invention is expanded on further below by way of instantiation.It should be understood that, cited example is only used for the narration present invention rather than limits the scope of the present invention, and general spinning equipment such as double screw extruder, dosing pump, spinneret etc. are not defined in illustrated example, but do not affect the preparation of the colored fibre for being obtained of the invention.In addition, it is to be understood that after the content that the present invention is lectured is read, those skilled in the art can make various changes or modification to the present invention, these equivalent form of values also fall within the scope that the claim appended by the application is limited.
Example 1
By the UHMWPE resins of 15KG（Relative average molecular weight is 4,500,000）, 190 liters of good solvents（It is preferred that decahydronaphthalenes）, antioxidant composite assistants HTB-7630 addition for UHMWPE weight resins 0.7% by coppers mix homogeneously, inject special raw material configuration system in solution twine swelling 3.5 hours in kettle, injected by the delivery pump that flows back and further sheared in homogenizing kettle, now sampling carries out the fluid rheology test of the mixed solution, in its data result as Fig. 1 shown in A lines, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards（Shear rate is 80rpm）, static mixer, the spinning equipment extruding spinning such as spinneret, the frozen glue precursor for obtaining by ring blow equipment by which in after the most of good solvent that includes reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtains high power jet stretch, obtain nascent colored fibre prepared by UHMWPE mixed resin solutions dry spinning, the multistage first break draft of Jing high powers obtains finished product ultra-high molecular weight polyethylene colored fibers, characteristic test is carried out to finished fiber sampling, its intensity, modulus, fiber number, the characteristic index part such as color fastness is shown in Table 1.
Example 2
By the UHMWPE resins of 13KG（Relative average molecular weight is 5,000,000）, 190 liters of good solvents（It is preferred that decahydronaphthalenes）, antioxidant composite assistants HTB-7630 addition for UHMWPE weight resins 0.7%, the red K-4180 pigment of 0.1KG perylenes, twined swelling 3.5 hours in kettle by the solution in coppers mix homogeneously, injection special raw material configuration system, injected by the delivery pump that flows back and further sheared in homogenizing kettle, now sampling carries out the fluid rheology test of the mixed solution, in its data result as Fig. 1 shown in B lines, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards（Shear rate is 70rpm）, static mixer, the spinning equipment extruding spinning such as spinneret, the frozen glue precursor for obtaining by ring blow equipment by which in after the most of good solvent that includes reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtains high power jet stretch, obtain nascent colored fibre prepared by UHMWPE mixed resin solutions dry spinning, the multistage first break draft of Jing high powers obtains finished product ultra-high molecular weight polyethylene colored fibers, characteristic test is carried out to finished fiber sampling, its intensity, modulus, fiber number, the characteristic index part such as color fastness is shown in Table 1.
Example 3
By the UHMWPE resins of 14KG（Relative average molecular weight is 5,000,000）, 190 liters of good solvents（It is preferred that decahydronaphthalenes）, antioxidant composite assistants HTB-7630 addition for UHMWPE weight resins 0.7%, 0.125KG quinoline promise furan phthalein phthalocyanine blue K-7090 pigment, twined swelling 3.5 hours in kettle by the solution in coppers mix homogeneously, injection special raw material configuration system, injected by the delivery pump that flows back and further sheared in homogenizing kettle, now sampling carries out the fluid rheology test of the mixed solution, in its data result as Fig. 1 shown in C lines, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards（Shear rate is 75rpm）, static mixer, the spinning equipment extruding spinning such as spinneret, the frozen glue precursor for obtaining by ring blow equipment by which in after the most of good solvent that includes reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtains high power jet stretch, obtain nascent colored fibre prepared by UHMWPE mixed resin solutions dry spinning, the multistage first break draft of Jing high powers obtains finished product ultra-high molecular weight polyethylene colored fibers, characteristic test is carried out to finished fiber sampling, its intensity, modulus, fiber number, the characteristic index part such as color fastness is shown in Table 1.
Example 4
By the UHMWPE resins of 15KG（Relative average molecular weight is 6,000,000）, 190 liters of good solvents（It is preferred that decahydronaphthalenes）, antioxidant composite assistants HTB-7630 addition for UHMWPE weight resins 0.7%, 0.186KG bismuth vanadate yellow K-1160FG pigment, twined swelling 3.5 hours in kettle by the solution in coppers mix homogeneously, injection special raw material configuration system, injected by the delivery pump that flows back and further sheared in homogenizing kettle, now sampling carries out the fluid rheology test of the mixed solution, in its data result as Fig. 1 shown in D lines, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards（Shear rate is 90rpm）, static mixer, the spinning equipment extruding spinning such as spinneret, the frozen glue precursor for obtaining by ring blow equipment by which in after the most of good solvent that includes reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtains high power jet stretch, obtain nascent colored fibre prepared by UHMWPE mixed resin solutions dry spinning, the multistage first break draft of Jing high powers obtains finished product ultra-high molecular weight polyethylene colored fibers, characteristic test is carried out to finished fiber sampling, its intensity, modulus, fiber number, the characteristic index part such as color fastness is shown in Table 1.
Example 5
By the UHMWPE resins of 16KG（Relative average molecular weight is 6,000,000）, 190 liters of good solvents（It is preferred that decahydronaphthalenes）, antioxidant composite assistants HTB-7630 addition for UHMWPE weight resins 0.7%, 0.250KG carbon black BP5560 pigment, twined swelling 3.5 hours in kettle by the solution in coppers mix homogeneously, injection special raw material configuration system, injected by the delivery pump that flows back and further sheared in homogenizing kettle, now sampling carries out the fluid rheology test of the mixed solution, in its data result as Fig. 1 shown in E lines, mixed solution quantitatively enters double screw extruder by the storage tank with stirring afterwards（Shear rate is 100rpm）, static mixer, the spinning equipment extruding spinning such as spinneret, the frozen glue precursor for obtaining by ring blow equipment by which in after the most of good solvent that includes reclaims, winding apparatus of optimized improved upper cluster tool and the outlet of connection path positioned at path entrance again, precursor obtains high power jet stretch, obtain nascent colored fibre prepared by UHMWPE mixed resin solutions dry spinning, the multistage first break draft of Jing high powers obtains finished product ultra-high molecular weight polyethylene colored fibers, characteristic test is carried out to finished fiber sampling, its intensity, modulus, fiber number, the characteristic index part such as color fastness is shown in Table 1.
Table 1 --- UHMWPE resin colored fibre embodiment sample property lists
。
Claims (10)
1. a kind of method that ultra-high molecular weight polyethylene mixed solution dry spinning prepares colored fibre, it is characterized in that colored fibre is using the spinning material mixed solution for possessing particular fluid rheological property formed by polyvinyl resin with super-high molecular weight and spinning good solvent, auxiliary agent and additives of pigments, ultra-high molecular weight polyethylene colored fibers are prepared by device for spinning, preparation method is comprised the following steps：（1）Uniformly possesses the preparation of the spinning material mixed solution of particular fluid rheological characteristic；（2）The preparation of the precursor of frozen glue containing pigment；（3）Ring blows, upper boundling, the preparation of the nascent colored fibre of high power jet stretch；（4）The recycling and process of spinning good solvent, pigment and system dry gas；（5）High power first break draft prepares ultra-high molecular weight polyethylene colored fibers.
2. method according to claim 1, it is characterised in that：The spinning material mixed solution for possessing particular fluid rheological characteristic is the homogeneous emulsus mixed solution that appropriate solution is formed after twining in raw material configuration system, and which passes through the rheological characteristic test of torque rheometer：Peak torque L is 4 ~ 30Nm, and plasticizing moment of torsion F is 2 ~ 15Nm.
3. method according to claim 1, it is characterised in that：In spinning material mixed solution, additives of pigments bag includes red perylene, quinoline promise furan phthalein, azo organic pigment and carbon black, one kind of bismuth vanadate yellow inorganic pigment or its similar combination.
4. method according to claim 1, it is characterised in that：The addition of additives of pigments for mixed solution 0.005% ~ 0.250% in spinning material mixed solution.
5. method according to claim 1, it is characterised in that：Auxiliary agent in spinning material mixed solution, including composite antioxidant and magnesium stearate plasticizer.
6. method according to claim 6, it is characterised in that：Composite antioxidant is HTB-7630 composite assistants.
7. method according to claim 1, it is characterised in that：The process for preparing nascent colored fibre is contained, go out the frozen glue precursor of spinneret by ring blow equipment by which in after most of good solvent for including reclaims, Jing is located at the upper cluster tool of path entrance and the winding apparatus of connection path outlet again, and precursor obtains high power jet stretch.
8. method according to claim 1, it is characterised in that：Spinning good solvent, the recycling of pigment and system dry gas and processing procedure contain one or several efficient combined-type heat exchangers, compressor, blower fan and membrane separator.
9. method according to claim 1, it is characterised in that：The response rate more than 99% of spinning good solvent, in spinning good solvent, pigment concentration is less than 50ppm.
10. the fiber that according to claim 1 prepared by method, it is characterised in that：The nascent colored fibre for preparing, the finished product colored fibre of Jing high power first break draft, its intensity are 10 ~ 35g/d, and modulus is 300 ~ 1600g/d.
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| CN109680351A (en) * | 2017-10-19 | 2019-04-26 | 中国石油化工股份有限公司 | Ultra-high molecular weight polyethylene colored fibers and preparation method thereof |
| CN110629315A (en) * | 2019-09-12 | 2019-12-31 | 中国石油化工股份有限公司 | Cut-resistant colored fiber and preparation method thereof |
| CN112144138A (en) * | 2019-06-26 | 2020-12-29 | 中石化南京化工研究院有限公司 | Method for improving performance of ultra-high molecular weight polyethylene colored fiber and fiber |
| CN114481372A (en) * | 2020-10-23 | 2022-05-13 | 中国石油化工股份有限公司 | Method for recovering solvent in fiber spinning process and fiber spinning system |
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