CN115287784B - Spinning oil, self-elasticized spinning fiber and elasticizing method thereof - Google Patents
Spinning oil, self-elasticized spinning fiber and elasticizing method thereof Download PDFInfo
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- 238000009987 spinning Methods 0.000 title claims abstract description 97
- 238000000034 method Methods 0.000 title claims abstract description 38
- 229920001971 elastomer Polymers 0.000 claims abstract description 21
- 239000000806 elastomer Substances 0.000 claims abstract description 21
- 239000003921 oil Substances 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 44
- 239000004697 Polyetherimide Substances 0.000 claims description 38
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- -1 PEI modified graphene Chemical class 0.000 claims description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 20
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims description 14
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 11
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 9
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 9
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims description 6
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- RBNPOMFGQQGHHO-UHFFFAOYSA-N glyceric acid Chemical compound OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 2
- 239000004925 Acrylic resin Substances 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 2
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 2
- 125000005233 alkylalcohol group Chemical group 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000002518 antifoaming agent Substances 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 150000004665 fatty acids Chemical class 0.000 claims description 2
- 229920001921 poly-methyl-phenyl-siloxane Polymers 0.000 claims description 2
- 229920000570 polyether Polymers 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims 1
- 239000002671 adjuvant Substances 0.000 claims 1
- 238000002074 melt spinning Methods 0.000 abstract description 17
- 238000002360 preparation method Methods 0.000 abstract description 10
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 55
- 229920001601 polyetherimide Polymers 0.000 description 37
- 229910021389 graphene Inorganic materials 0.000 description 28
- 238000012360 testing method Methods 0.000 description 26
- 239000004753 textile Substances 0.000 description 24
- 239000000243 solution Substances 0.000 description 23
- 238000003756 stirring Methods 0.000 description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 20
- 230000006399 behavior Effects 0.000 description 16
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- 239000007788 liquid Substances 0.000 description 13
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- 230000007935 neutral effect Effects 0.000 description 10
- 238000002791 soaking Methods 0.000 description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- 238000005507 spraying Methods 0.000 description 9
- 239000012286 potassium permanganate Substances 0.000 description 7
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- 238000007664 blowing Methods 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 239000012153 distilled water Substances 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 238000001704 evaporation Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 229920001778 nylon Polymers 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000007921 spray Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
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- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
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- 229940068041 phytic acid Drugs 0.000 description 2
- 235000002949 phytic acid Nutrition 0.000 description 2
- 239000000467 phytic acid Substances 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920003043 Cellulose fiber Polymers 0.000 description 1
- 229920006052 Chinlon® Polymers 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 230000003542 behavioural effect Effects 0.000 description 1
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- 230000008901 benefit Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 239000008041 oiling agent Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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- 238000004904 shortening Methods 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
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- 230000001360 synchronised effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
- D01D5/096—Humidity control, or oiling, of filaments, threads or the like, leaving the spinnerettes
-
- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02G—CRIMPING OR CURLING FIBRES, FILAMENTS, THREADS, OR YARNS; YARNS OR THREADS
- D02G1/00—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics
- D02G1/02—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist
- D02G1/0206—Producing crimped or curled fibres, filaments, yarns, or threads, giving them latent characteristics by twisting, fixing the twist and backtwisting, i.e. by imparting false twist by false-twisting
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention relates to the technical field of spinning materials, in particular to a spinning oil, an autonomously elasticized spinning fiber and an elasticizing method thereof. The spinning oil comprises a soluble elastomer, the spinning oil is unevenly attached to the surface of a spinning fiber formed by a melt spinning process, so that an unevenly distributed texturing structure is formed on the surface of the spinning fiber, and the spinning fiber has an autonomous texturing behavior through the texturing structure. The spinning oil provided by the invention can be suitable for preparing spinning fibers with autonomous texturing behavior by a one-step method, namely the production efficiency is effectively improved, the preparation process of the spinning fibers is simplified, and the cost is reduced.
Description
Technical Field
The invention relates to the technical field of spinning materials, in particular to a spinning oil, an autonomously elasticized spinning fiber and an elasticizing method thereof.
Background
Textile fibers are the basic units that make up textiles and can be largely divided into two main categories: traditional textile fibers and chemical textile fibers. The quality, structure, function, etc. of textile fibers are key factors in determining the quality of textiles. Meanwhile, because the source, the composition, the shape and the performance of the textile fiber are extremely complex, the textile fiber needs to be processed according to the material preparation in the use process so as to prepare the textile with excellent performance, supply and demand road matching and benefit optimization. Compared with the traditional textile fiber, the chemical textile fiber has the characteristics of smooth surface and single structure. In order to prepare textiles using chemical textile fibers, the chemical textile fibers must be subjected to a specific differential modification treatment. Ziyang Chang, xianhui An et al prepared a compact coating of phytic acid doped polyaniline by chelation of zirconium ions with phytic acid. The prepared fiber composite material has controllable polyaniline loading capacity, and can remarkably improve the conductivity, flame retardance and electrochemical stability of the composite material (High mass loading polyaniline layer anchored cellulose fibers:Enhanced interface junction for high conductivity and flame retardancy,DOI：10.1016/j.carbpol.2019.115660).
In recent years, the chemical industry is developing at a high speed, chemical textile fibers are also in high water-rise, the use amount of the chemical textile fibers is far more than that of the traditional textile fibers, and the chemical textile fiber textiles gradually replace the traditional textile fibers in many aspects. The efficient and high-quality differentiation treatment leads to an increasingly wide application field of chemical fibers.
The texturing treatment of the existing chemical spinning fiber is usually carried out after spinning is finished, and the processing mode is difficult to meet the requirement of efficient production. Therefore, a method for effectively shortening the process is needed.
Disclosure of Invention
In order to overcome the defects in the prior art, the technical problems to be solved by the invention are as follows: a spin finish which is suitable for the preparation of textile fibers having texturing behavior by the one-step process, a texturing process suitable for the spin finish, and the spun fibers prepared by the texturing process are provided.
In order to solve the technical problems, the invention provides a spinning oil, which comprises a soluble elastomer.
Further provided is a texturing method of spun fibers, comprising using the spinning oil, and spraying the spinning oil on the surface of the spun fibers formed simultaneously in a non-uniform manner.
Further provided is an autonomously texturing spun fiber prepared by the foregoing texturing process.
The invention has the beneficial effects that: the spinning oil provided by the invention can be suitable for preparing spinning fibers with autonomous elasticizing behaviors by a one-step method, effectively improves the production efficiency, simplifies the spinning fiber preparation process and reduces the cost.
Drawings
FIG. 1 is a photograph of a spun fiber with autonomous texturing behavior prepared in accordance with the present invention during winding;
FIG. 2 is a photograph of a natural state of a spun fiber with autonomous texturing behavior prepared in accordance with the present invention after unreeling;
FIG. 3 is a schematic structural view of a spun fiber with autonomous texturing behavior prepared in accordance with the present invention;
FIG. 4 shows an infrared spectrum of PEI-modified graphene oxide in a specific embodiment of the present invention.
Description of the reference numerals: 1. spinning the fiber; 2. and (5) a spring adding structure.
Detailed Description
In order to describe the technical contents, the achieved objects and effects of the present invention in detail, the following description will be made with reference to the embodiments in conjunction with the accompanying drawings.
In this context, the melt spinning (MELT SPINNING) is a process in which a polymer melt or solution is extruded from a spinneret at a certain flow rate, and is subjected to oiling, drawing, winding, etc. to obtain a fiber having a certain fineness.
In this context, the oil (Oiling Agent) is an important auxiliary in the melt spinning process. The oiling can increase the cohesion of the fibers, reduce the friction coefficient among the fibers, ensure that the fibers have certain hygroscopicity and antistatic property, and improve the spinnability of the fibers. Common oils include span 60, tween 60, etc.
In this context, textured yarn (DTY) is a finished yarn obtained by improving the spinnability of fibers, and further processing after the yarn formation. Namely, the chemical textile fiber is shaped in a false twisting mode to generate certain bending. The chemical textile fiber treated by the false twisting is opened and generates certain elongation when the external force is applied, and the false twisting is recovered when the external force is removed, even if the chemical textile fiber has certain rebound resilience.
In this context, the self-texturing behavior is that the spun fibers after oiling have a certain elasticity after drawing and winding, have a durable bending form in a state of no external force stretching, and still have the elasticity capability after external force stretching and external force withdrawal.
A spin finish comprising a soluble elastomer. The spinning oil agent is unevenly attached to the surface of the spinning fiber formed by the melt spinning process through the elastomer, so that an unevenly distributed texturing structure is formed on the surface of the spinning fiber, and the spinning fiber has an autonomous texturing behavior through the texturing structure.
Referring specifically to fig. 3, since the texturing structures 2 are unevenly distributed on the spun fibers 1, the spun fibers can be formed into a curved structure by the stress generated by the elastic body after it has been plastic even though the spun fibers have an autonomous texturing behavior.
In this context, the "one-step process" is achieved by attaching the elastomer mixed in the spin finish to the spun fiber and by synchronizing the two actions of the spun fiber formation. When the spinning fiber is formed based on a melt spinning process, the formed spinning fiber surface is uniformly sprayed or elastomer is unevenly attached to the formed spinning fiber surface in other modes, so that the formed spinning fiber has self-elastic action during spinning, and the elastic processing is not required to be further performed after the spinning, namely, the process of spinning fiber is simplified, and the production efficiency is improved.
Preferably, the elastomer is selected from Thermoplastic Polyurethane (TPU) or Waterborne Polyurethane (WPU).
In experiments, although the elastic body can realize synchronous formation of the self-elastic action, the adhesive force of the elastic body on the spinning fiber is poor, so that the spinning fiber is easy to fall off in a long-time use process, and the self-elastic action of the spinning fiber is lost, so that the adsorption force of the elastic body on the spinning fiber needs to be enhanced. In experiments, the applicant finds that the PEI (polyetherimide) modified graphene oxide can be mixed into the spinning oil to effectively improve the adhesive force of the elastomer to the spinning fiber, and the PEI modification can effectively improve the dispersibility of the graphene oxide in the spinning oil. Wherein, the graphene oxide is preferably prepared by adopting a Hummers method, and more preferably, the graphene oxide is prepared by adopting the following method: and increasing the consumption of potassium permanganate (taking 3g of graphene powder as a base and 8-12 g of potassium permanganate) in the ice bath stage, and simultaneously increasing the ice bath time (prolonging the traditional 0.5h ice bath time to 1-3 h) so as to obtain graphene oxide with higher oxidation degree. For the grafting method of PEI, any existing grafting method can be used for grafting PEI on the surface of graphene oxide, for example, a chemical synthesis method is used for grafting PEI on the surface of graphene oxide in a covalent bond mode.
The dispersibility of graphene oxide in the spinning oil can be optimized by changing the particle size of the graphene oxide. Specifically, it was found in experiments that PEI modified graphene oxide prepared from the graphene powder has excellent dispersibility in a spin finish when the particle size of the graphene powder used is between 2000 mesh and 5000 mesh.
Of course, the spin finish should contain a solvent and an auxiliary for improving the quality of the spin finish; wherein the solvent is used to dissolve the elastomer or to distribute the elastomer in the solvent in the form of emulsion droplets; the auxiliary agent is at least one selected from defoamer, flatting agent and finishing agent.
Wherein the solvent is at least one selected from Dimethylformamide (DMF), N-methylformamide (NMF) and water. The solvent may be selected according to the actual needs. In one embodiment, when the elastomer is TPU, the solvent is preferably Dimethylformamide (DMF).
The defoaming agent is at least one selected from emulsified silicone oil, higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene alcohol amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether and polydimethylsiloxane.
The leveling agent is at least one selected from polydimethylsiloxane, polymethylphenylsiloxane, acrylic resin, urea resin and melamine formaldehyde resin.
The finishing agent is at least one selected from span 80, polyether, nonylphenol polyoxyethylene ether, alkyl alcohol polyoxyethylene ether, polyethylene glycol ester and fatty acid polyoxyethylene addition product.
In one embodiment, the preparation method of the spinning oil comprises the following steps:
s1, preparing PEI modified graphene oxide;
s2, adding the elastomer into a solvent to dissolve or disperse the elastomer in the solvent in a emulsion droplet manner;
s3, further adding PEI modified graphene oxide and an auxiliary agent into the solvent, and uniformly stirring to obtain the spinning oil.
The spun fibers should have a certain fineness to ensure the realization of autonomous texturing behavior. Preferably, the spun fibers are between 2.2 and 3.3 dtex. The spinning fiber can be any fiber formed by the prior melt spinning process, such as terylene, chinlon and the like.
A texturing method for spinning fiber includes using the spinning oil and spraying the spinning oil on the surface of the spinning fiber formed synchronously in a non-uniform manner.
The spraying may be achieved by a spray head/nozzle and by adjusting the spray frequency of the spray head/nozzle to achieve non-uniform spray. At the same time, since the spinning dope uses an organic solvent, there is a risk of corroding the relevant parts (all parts from the dope tank to the nozzle) such as the nozzle, and therefore, it is preferable to optimize the materials of these parts. Preferably, these components are made of stainless steel or polytetrafluoroethylene.
In the actual production process, the spinning fiber after texturing (after spraying the spinning oil) is also required to be drawn, so as to further maintain and stabilize the autonomous texturing behavior of the spinning fiber. In one embodiment, the drawing is carried out by means of a segmented drawing with four heated rolls having different rotational speeds, wherein the rotational speed of the second roll and the third roll is generally greater than that of the first roll and the rotational speed of the fourth roll is generally less than that of the second roll and the third roll, but is generally expressed in terms of frequency during the actual production process. In a more specific embodiment, the first roll frequency is set to 60Hz, the second roll frequency is set to 75Hz, the third roll frequency is set to 78Hz, the fourth roll frequency is set to 70Hz, and the winding frequency is set to 65Hz.
A spun fiber having autonomous texturing behavior prepared by the foregoing texturing method.
Example 1
The preparation method of the spinning oil comprises the following steps:
S1, taking 3g of 2000-mesh graphite (purchased from Allatin), adding 3.1g of sodium nitrate (NaNO 3, purity is more than or equal to 99.0%) and 145mL of concentrated sulfuric acid (H 2SO4, 98%) into a 500mL three-necked flask in sequence, and setting the stirring speed to be 350r/min. After stirring for 1.5h in an ice bath environment, 10g of potassium permanganate (KMnO 4, 98%) was added in small portions, and then the temperature was raised to 50℃for 2h. Distilled water is dropwise added, and the temperature of the system is controlled to be lower than 75 ℃. After the dripping is finished, the temperature is raised to 98 ℃, and after the temperature is kept for 15min, the mixture is poured into 600mL of stirred aqueous solution of hydrogen peroxide (H 2O2, 30 percent) (the volume ratio of water to hydrogen peroxide is 2:1). Continuously stirring until no bubbles are generated, and washing with deionized water to neutrality successively to obtain a neutral graphene oxide aqueous solution with high oxidation degree;
S2, sucking 2g of PEI by using a dropper, dripping the PEI into the neutral graphene oxide aqueous solution containing 1g of graphene oxide, and magnetically stirring the solution at 60 ℃ for 8 hours to obtain PEI modified graphene oxide; carrying out infrared spectrum detection on the obtained PEI modified graphene oxide, wherein the result is shown in a figure 4, namely, the PEI is grafted on the surface of the graphene oxide;
S3, dispersing 1g of PEI modified graphene oxide in 1000mL of water by ultrasonic, adding 1000mL of dimethylformamide (purchased from Chinese medicine), and completely evaporating out the water by a distillation method to obtain a base solution a1; then, 100g of thermoplastic polyurethane (1170A, commercially available from Basoff, germany) was added to the base liquid a1, and stirred with a magnetic stirrer until the thermoplastic polyurethane was completely dissolved, to obtain a base liquid a2;
s4, adding 0.5g of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3g of polydimethylsiloxane into the base solution a2 to obtain a spinning oil A1.
And spraying the spinning oil A1 on the surface of nylon fiber (2.2 dtex) formed by a melt spinning process by using an oil nozzle. Drawing (wherein the frequency of the first roll is set to 60Hz, the frequency of the second roll is set to 75Hz, the frequency of the third roll is set to 78Hz, the frequency of the fourth roll is set to 70Hz, the winding frequency is set to 65 Hz), winding to obtain the spinning fiber A2 with the self-texturing behavior, the picture after winding is shown in figure 1, and the state of the spinning fiber A2 in a natural state after unreeling is shown in figure 2.
Wherein the melt spinning machine is selected from FCF-9 spinning machines produced by a master batch plant of the Bobo Linzi Fang Chen, and the specific parameters are as follows:
The set temperature of the five sections of heating zones of the screw is 280 ℃, 290 ℃, 280 ℃, the die head temperature 280 ℃, the temperatures of the first roller, the second roller, the third roller and the fourth roller are 65 ℃, 95 ℃ and the measured blowing temperature is 10 ℃.
Adhesion test
10M long spinning fiber A2 is taken and put into 100ml pure water with the absorbance of 0.237/m when being illuminated by 600nm wavelength, and soaked and placed for 48 hours at room temperature (25 ℃). Then, a proper amount of soaking solution is taken, and the absorbance of the soaking solution is tested to be 0.2548/m by using a compatible projection reflection spectrocolorimeter CS-820 and 600nm wavelength light, which shows that the adhesion of the PEI modified graphene oxide elastomer on the fiber is good.
The main principle of the adhesive force test is as follows: when the spinning oil on the surface of the spinning fiber is soaked in water, a part of spinning oil (solid after drying) falls off, namely, some particles formed by falling off of the spinning oil exist in soaked water, so that the adhesive force of the spinning oil can be indirectly represented by measuring the change of absorbance in water, and the larger the change of absorbance value of the water is, the worse the adhesive force of the spinning oil is indicated.
Elongation test
The spun fiber A2 was twisted to a tension of 0.1cN/dtex from 0.05cN/dtex, and the twisted spun fiber was subjected to a stretching ratio test on an Instron (model-11127) electronic universal tester, which gave a stretching ratio of 4.3% at a tensile strength of 1 cN/dtex.
Tensile Property test
Spun fiber A2 was sampled according to GB/T14344-2003 standard. The above-mentioned test specimen was tested under room temperature conditions using an Instron (model-11127) electronic universal tester, and the breaking strength of the spun fiber A2 was measured to be 5.02.+ -. 0.5cN/dtex.
Example 2
The preparation method of the spinning oil comprises the following steps:
S1, taking 3g of 2000-mesh graphite (purchased from Allatin), adding 3.1g of sodium nitrate (NaNO 3, purity is more than or equal to 99.0%) and 145mL of concentrated sulfuric acid (H 2SO4, 98%) into a 500mL three-necked flask in sequence, and setting the stirring speed to be 350r/min. After stirring for 1.5h in an ice bath environment, 10g of potassium permanganate (KMnO 4, 98%) was added in small portions, and then the temperature was raised to 50℃for 2h. Distilled water is dropwise added, and the temperature of the system is controlled to be lower than 75 ℃. After the dripping is finished, the temperature is raised to 98 ℃, and after the temperature is kept for 15min, the mixture is poured into 600mL of stirred aqueous solution of hydrogen peroxide (H 2O2, 30 percent) (the volume ratio of water to hydrogen peroxide is 2:1). Continuously stirring until no bubbles are generated, and washing with deionized water to neutrality successively to obtain a neutral graphene oxide aqueous solution with high oxidation degree;
s2, sucking 2g of PEI by using a dropper, dripping the PEI into the neutral graphene oxide aqueous solution containing 1g of graphene oxide, and magnetically stirring the solution at 60 ℃ for 8 hours to obtain PEI modified graphene oxide;
s3, dispersing 1g of PEI modified graphene oxide in 1000mL of water by ultrasonic, adding 1000mL of dimethylformamide (purchased from Chinese medicine), and completely evaporating out the water by a distillation method to obtain a base solution b1; then 200g of thermoplastic polyurethane (1170A, purchased from Basoff, germany) was added to the base liquid b1, and stirred with a magnetic stirrer until the thermoplastic polyurethane was completely dissolved, to obtain a base liquid b2;
S4, adding 0.5g of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3g of polydimethylsiloxane into the base liquid B2 to obtain a spinning oil B1.
And spraying the spinning oil B1 on the surface of nylon (2.2 dtex) formed by a melt spinning process by using an oil nozzle. The spun fiber B2 having an autonomous texturing behavior was obtained by drawing (wherein the frequency of the first roll was set to 60Hz, the frequency of the second roll was set to 75Hz, the frequency of the third roll was set to 78Hz, the frequency of the fourth roll was set to 70Hz, and the winding frequency was set to 65 Hz).
Wherein the melt spinning machine is selected from FCF-9 spinning machines produced by a master batch plant of the Bobo Linzi Fang Chen, and the specific parameters are as follows:
The set temperature of the five sections of heating zones of the screw is 280 ℃, 290 ℃, 280 ℃, the die head temperature 280 ℃, the temperatures of the first roller, the second roller, the third roller and the fourth roller are 65 ℃, 95 ℃ and the measured blowing temperature is 10 ℃.
Adhesion test
10M long spinning fiber B2 is taken and put into 100ml pure water with the absorbance of 0.237/m when being illuminated by 600nm wavelength, and soaked and placed for 48 hours at room temperature (25 ℃). Then, a proper amount of soaking solution is taken, and the absorbance of the soaking solution is 0.2628/m by using a compatible projection reflection spectrocolorimeter CS-820 and using 600nm wavelength light, which shows that the adhesion of the PEI modified graphene oxide elastomer on the fiber is good.
Elongation test
The spun fiber B2 was twisted to a tension of 0.1cN/dtex from 0.05cN/dtex, and the twisted spun fiber was subjected to a stretching ratio test on an Instron (model-11127) electronic universal tester, which gave a stretching ratio of 6.3% at a tensile strength of 1 cN/dtex.
Tensile Property test
Spun fiber B2 was sampled according to GB/T14344-2003 standard. The above-mentioned test specimen was tested under room temperature conditions using an Instron (model-11127) electronic universal tester, and the breaking strength of the spun fiber B2 was measured to be 6.8.+ -. 0.5cN/dtex.
Example 3
The preparation method of the spinning oil comprises the following steps:
s1, taking 3g of 2000-mesh graphite (purchased from Allatin), adding 3.1g of sodium nitrate (NaNO 3, purity is more than or equal to 99.0%) and 145mL of concentrated sulfuric acid (H 2SO4, 98%) into a 500mL three-necked flask in sequence, and setting the stirring speed to be 350r/min. After stirring for 1.5h in an ice bath environment, 12g of potassium permanganate (KMnO 4, 98%) was added a small number of times, and then the temperature was raised to 50℃for 3h. Distilled water is dropwise added, and the temperature of the system is controlled to be lower than 75 ℃. After the dripping is finished, the temperature is raised to 98 ℃, and after the temperature is kept for 15min, the mixture is poured into 600mL of stirred aqueous solution of hydrogen peroxide (H 2O2, 30 percent) (the volume ratio of water to hydrogen peroxide is 2:1). Continuously stirring until no bubbles are generated, and washing with deionized water to neutrality successively to obtain a neutral graphene oxide aqueous solution with high oxidation degree;
s2, sucking 2g of PEI by using a dropper, dripping the PEI into the neutral graphene oxide aqueous solution containing 1g of graphene oxide, and magnetically stirring the solution at 60 ℃ for 8 hours to obtain PEI modified graphene oxide;
S3, dispersing 1g of PEI modified graphene oxide in 1000mL of water by ultrasonic, adding 1000mL of dimethylformamide (purchased from Chinese medicine), and completely evaporating out the water by a distillation method to obtain a base solution c1; then, 100g of thermoplastic polyurethane (1170A, commercially available from Basoff, germany) was added to the base liquid c1, and stirred with a magnetic stirrer until the thermoplastic polyurethane was completely dissolved, to obtain a base liquid c2;
S4, adding 0.5g of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3g of polydimethylsiloxane into the base liquid C2 to obtain a spinning oil C1.
And spraying the spinning oil C1 on the surface of nylon (3.3 dtex) formed by a melt spinning process by using an oil nozzle. The spun fiber C2 having an autonomous texturing behavior was obtained by drawing (wherein the frequency of the first roll was set to 60Hz, the frequency of the second roll was set to 75Hz, the frequency of the third roll was set to 78Hz, the frequency of the fourth roll was set to 70Hz, and the winding frequency was set to 65 Hz).
Wherein the melt spinning machine is selected from FCF-9 spinning machines produced by a master batch plant of the Bobo Linzi Fang Chen, and the specific parameters are as follows:
The set temperature of the five sections of heating zones of the screw is 280 ℃, 290 ℃, 280 ℃, the die head temperature 280 ℃, the temperatures of the first roller, the second roller, the third roller and the fourth roller are 65 ℃, 95 ℃ and the measured blowing temperature is 10 ℃.
Adhesion test
10M long spinning fiber C2 is taken and put into 100ml pure water with the absorbance of 0.237/m when being illuminated by 600nm wavelength, and soaked and placed for 48 hours at room temperature (25 ℃). Then, a proper amount of soaking solution is taken, and the absorbance of the soaking solution is 0.2435/m by using a compatible projection reflection spectrocolorimeter CS-820 and using 600nm wavelength light, which shows that the adhesion of the PEI modified graphene oxide elastomer on the fiber is good.
Elongation test
The spun fiber C2 was twisted to a tension of 0.1cN/dtex from 0.05cN/dtex, and the twisted spun fiber was subjected to a stretching ratio test on an Instron (model-11127) electronic universal tester, which gave a stretching ratio of 4.1% at a tensile strength of 1 cN/dtex.
Tensile Property test
Spun fiber C2 was sampled according to GB/T14344-2003 standard. The above-mentioned test specimen was tested under room temperature conditions using an Instron (model-11127) electronic universal tester, and the breaking strength of the spun fiber C2 was measured to be 5.5.+ -. 0.3cN/dtex.
Example 4
The preparation method of the spinning oil comprises the following steps:
S1, taking 3g of 2000-mesh graphite (purchased from Allatin), adding 3.1g of sodium nitrate (NaNO 3, purity is more than or equal to 99.0%) and 145mL of concentrated sulfuric acid (H 2SO4, 98%) into a 500mL three-necked flask in sequence, and setting the stirring speed to be 350r/min. After stirring for 1.5h in an ice bath environment, 10g of potassium permanganate (KMnO 4, 98%) was added in small portions, and then the temperature was raised to 50℃for 2h. Distilled water is dropwise added, and the temperature of the system is controlled to be lower than 75 ℃. After the dripping is finished, the temperature is raised to 98 ℃, and after the temperature is kept for 15min, the mixture is poured into 600mL of stirred aqueous solution of hydrogen peroxide (H 2O2, 30 percent) (the volume ratio of water to hydrogen peroxide is 2:1). Continuously stirring until no bubbles are generated, and washing with deionized water to neutrality successively to obtain a neutral graphene oxide aqueous solution with high oxidation degree;
S2, sucking 0.5g of PEI by a dropper, dripping the PEI into the neutral graphene oxide aqueous solution containing 1g of graphene oxide, and magnetically stirring the solution for 8 hours at 60 ℃ to obtain PEI modified graphene oxide;
s3, dispersing 1g of PEI modified graphene oxide in 1000mL of water by ultrasonic, adding 1000mL of dimethylformamide (purchased from Chinese medicine), and completely evaporating out the water by a distillation method to obtain a base solution d1; then, 100g of thermoplastic polyurethane (1170A, purchased from Basoff, germany) was added to the base liquid d1, and stirred with a magnetic stirrer until the thermoplastic polyurethane was completely dissolved, to obtain a base liquid d2;
s4, adding 0.5g of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3g of polydimethylsiloxane into the base liquid D2 to obtain a spinning oil D1.
And spraying the spinning oil D1 on the surface of nylon fiber (2.2 dtex) formed by a melt spinning process by using an oil nozzle. The spun fiber D2 having an autonomous texturing behavior was obtained by drawing (in which the frequency of the first roll was set to 60Hz, the frequency of the second roll was set to 75Hz, the frequency of the third roll was set to 78Hz, the frequency of the fourth roll was set to 70Hz, and the winding frequency was set to 65 Hz).
Wherein the melt spinning machine is selected from FCF-9 spinning machines produced by a master batch plant of the Bobo Linzi Fang Chen, and the specific parameters are as follows:
The set temperature of the five sections of heating zones of the screw is 280 ℃, 290 ℃, 280 ℃, the die head temperature 280 ℃, the temperatures of the first roller, the second roller, the third roller and the fourth roller are 65 ℃, 95 ℃ and the measured blowing temperature is 10 ℃.
Adhesion test
10M long spinning fiber D2 is taken and put into 100ml pure water with the absorbance of 0.237/m when being illuminated by 600nm wavelength, and soaked and placed for 48 hours at room temperature (25 ℃). Then, a proper amount of soaking solution is taken, and the absorbance of the soaking solution is 0.2761/m by using a compatible projection reflection spectrocolorimeter CS-820 and using 600nm wavelength light, which shows that the adhesion of the PEI modified graphene oxide elastomer on the fiber is good.
Elongation test
The spun fiber D2 was twisted to a tension of 0.1cN/dtex from 0.05cN/dtex, and the twisted spun fiber was subjected to a stretching ratio test on an Instron (model-11127) electronic universal tester, which gave a stretching ratio of 4.5% at a tensile strength of 1 cN/dtex.
Tensile Property test
Spun fiber D2 was sampled according to GB/T14344-2003 standard. The above-mentioned test specimen was tested under room temperature conditions using an Instron (model-11127) electronic universal tester, and the breaking strength of the spun fiber D2 was measured to be 4.8.+ -. 0.6cN/dtex.
Example 5
The preparation method of the spinning oil comprises the following steps:
S1, taking 3g of 2000-mesh graphite (purchased from Allatin), adding 3.1g of sodium nitrate (NaNO 3, purity is more than or equal to 99.0%) and 145mL of concentrated sulfuric acid (H 2SO4, 98%) into a 500mL three-necked flask in sequence, and setting the stirring speed to be 350r/min. After stirring for 1.5h in an ice bath environment, 10g of potassium permanganate (KMnO 4, 98%) was added in small portions, and then the temperature was raised to 50℃for 2h. Distilled water is dropwise added, and the temperature of the system is controlled to be lower than 75 ℃. After the dripping is finished, the temperature is raised to 98 ℃, and after the temperature is kept for 15min, the mixture is poured into 600mL of stirred aqueous solution of hydrogen peroxide (H 2O2, 30 percent) (the volume ratio of water to hydrogen peroxide is 2:1). Continuously stirring until no bubbles are generated, and washing with deionized water to neutrality successively to obtain a neutral graphene oxide aqueous solution with high oxidation degree;
s2, sucking 2g of PEI by using a dropper, dripping the PEI into the neutral graphene oxide aqueous solution containing 1g of graphene oxide, and magnetically stirring the solution at 60 ℃ for 8 hours to obtain PEI modified graphene oxide;
s3, dispersing 2g of PEI modified graphene oxide in 1000mL of water by ultrasonic, adding 1000mL of dimethylformamide (purchased from Chinese medicine), and completely evaporating out the water by a distillation method to obtain a base solution e1; then, 100g of thermoplastic polyurethane (1170A, purchased from Basoff, germany) was added to the base liquid e1, and stirred with a magnetic stirrer until the thermoplastic polyurethane was completely dissolved, to obtain a base liquid e2;
s4, adding 0.5g of polyoxyethylene polyoxypropylene pentaerythritol ether and 0.3g of polydimethylsiloxane into the base solution E2 to obtain a spinning oil E1.
And spraying the spinning oil E1 on the surface of nylon fiber (2.2 dtex) formed by a melt spinning process by using an oil nozzle. The spun fiber E2 having an autonomous texturing behavior was obtained by drawing (wherein the frequency of the first roll was set to 60Hz, the frequency of the second roll was set to 75Hz, the frequency of the third roll was set to 78Hz, the frequency of the fourth roll was set to 70Hz, and the winding frequency was set to 65 Hz).
Wherein the melt spinning machine is selected from FCF-9 spinning machines produced by a master batch plant of the Bobo Linzi Fang Chen, and the specific parameters are as follows:
The set temperature of the five sections of heating zones of the screw is 280 ℃, 290 ℃, 280 ℃, the die head temperature 280 ℃, the temperatures of the first roller, the second roller, the third roller and the fourth roller are 65 ℃, 95 ℃ and the measured blowing temperature is 10 ℃.
Adhesion test
10 M long spinning fiber E2 is taken and put into 100ml pure water with the absorbance of 0.237/m when being illuminated by 600nm wavelength, and is soaked and placed for 48 hours at room temperature. Then, a proper amount of soaking solution is taken, and the absorbance of the soaking solution is 0.3143/m by using a compatible projection reflection spectrocolorimeter CS-820 and using 600nm wavelength light, which shows that the adhesion of the PEI modified graphene oxide elastomer on the fiber is good.
Elongation test
The spun fiber E2 was twisted to a tension of 0.1cN/dtex from 0.05cN/dtex, and the twisted spun fiber was subjected to a elongation test on an Instron (model-11127) electronic universal tester, which gave a elongation of 3.9% at a tensile strength of 1 cN/dtex.
Tensile Property test
Spun fiber E2 was sampled according to GB/T14344-2003 standard. The above-mentioned test specimen was tested under room temperature conditions using an Instron (model-11127) electronic universal tester, and the breaking strength of the spun fiber E2 was measured to be 6.3.+ -. 0.5cN/dtex.
In conclusion, the spinning oil provided by the invention can be suitable for preparing spinning fibers with the autonomous texturing action by a one-step method, so that the yarn manufacturing process can be effectively reduced, the cost is reduced, and the production efficiency is improved; the addition of PEI modified graphene oxide ensures that the graphene has excellent dispersion performance in the spinning oil, so that the adhesion of the elastomer on the fiber surface is stronger, and the spinnability of the self-elasticized behavioural fiber is higher.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent changes made by the specification and drawings of the present invention, or direct or indirect application in the relevant art, are included in the scope of the present invention.
Claims (7)
1. A texturing method of spinning fibers, characterized in that a spinning oil is sprayed on the surface of the spinning fibers formed simultaneously in a non-uniform manner, wherein the spinning oil comprises a soluble elastomer and PEI modified graphene oxide, and the elastomer is selected from thermoplastic polyurethane or aqueous polyurethane.
2. The method of texturing a spun fiber of claim 1 wherein the spin finish further comprises a solvent and an adjuvant;
the auxiliary agent is at least one selected from defoamer, flatting agent and finishing agent.
3. The method of texturing a spun fiber of claim 2 wherein the solvent is selected from at least one of dimethylformamide, N-methylformamide, and water.
4. The texturing method of a spun fiber according to claim 2, wherein the antifoaming agent is at least one selected from the group consisting of emulsified silicone oil, higher alcohol fatty acid ester complex, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene alcohol amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether, and polydimethylsiloxane.
5. The texturing method of a spun fiber according to claim 2, wherein the leveling agent is at least one selected from the group consisting of polydimethylsiloxane, polymethylphenylsiloxane, acrylic resin, urea resin and melamine formaldehyde resin.
6. The method for texturing spun fibers of claim 2 wherein the finish is selected from at least one of span 80, polyether, polyoxyethylene nonylphenol ether, polyoxyethylene alkyl alcohol ether, polyethylene glycol ester, polyoxyethylene fatty acid adducts.
7. An autonomous texturing spun fiber made by the texturing process of any one of claims 1-6.
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