CN115467042B - PBT stretch fiber yarn with high scratch resistance and preparation method thereof - Google Patents
PBT stretch fiber yarn with high scratch resistance and preparation method thereof Download PDFInfo
- Publication number
- CN115467042B CN115467042B CN202211117316.XA CN202211117316A CN115467042B CN 115467042 B CN115467042 B CN 115467042B CN 202211117316 A CN202211117316 A CN 202211117316A CN 115467042 B CN115467042 B CN 115467042B
- Authority
- CN
- China
- Prior art keywords
- pbt
- slag
- slag micropowder
- micropowder
- mass
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000000835 fiber Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 143
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims abstract description 35
- 235000013539 calcium stearate Nutrition 0.000 claims abstract description 35
- 239000008116 calcium stearate Substances 0.000 claims abstract description 35
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 29
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 29
- 229920000915 polyvinyl chloride Polymers 0.000 claims abstract description 29
- 239000004800 polyvinyl chloride Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 11
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 44
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 29
- 229910052787 antimony Inorganic materials 0.000 claims description 29
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 29
- 229910052748 manganese Inorganic materials 0.000 claims description 29
- 239000011572 manganese Substances 0.000 claims description 29
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical group [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 claims description 22
- 239000010436 fluorite Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 10
- 238000002074 melt spinning Methods 0.000 claims description 9
- 238000012986 modification Methods 0.000 claims description 9
- 230000004048 modification Effects 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 230000003678 scratch resistant effect Effects 0.000 claims description 4
- 229920002334 Spandex Polymers 0.000 claims description 2
- 239000004759 spandex Substances 0.000 claims description 2
- 210000004177 elastic tissue Anatomy 0.000 abstract description 26
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000155 melt Substances 0.000 abstract 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 71
- 239000000843 powder Substances 0.000 description 34
- 238000009987 spinning Methods 0.000 description 14
- 239000000203 mixture Substances 0.000 description 11
- 229920000728 polyester Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000007790 scraping Methods 0.000 description 5
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 229920001634 Copolyester Polymers 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 229920006351 engineering plastic Polymers 0.000 description 2
- 239000002657 fibrous material Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 241000203475 Neopanax arboreus Species 0.000 description 1
- -1 Polybutylene terephthalate Polymers 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003158 alcohol group Chemical group 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004595 color masterbatch Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to the technical field of fiber manufacture, in particular to a PBT elastic fiber yarn with high scratch resistance and a preparation method thereof, which is prepared by introducing slag micropowder into PBT, mixing with high-speed substances under the conditions of polyvinyl chloride, polyvinyl alcohol and calcium stearate, heating in nitrogen atmosphere, and preparing the PBT elastic fiber yarn by a melt spinning-stretching-heat treatment process, so that the scratch resistance of the PBT elastic fiber yarn is greatly improved, the breaking strength reaches 3.6-4.1cN/dex, and the breaking elongation reaches 30-50%.
Description
Technical Field
The invention relates to the technical field of fiber manufacturing, in particular to a PBT stretch fiber yarn with high scratch resistance and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) is crystalline linear saturated polyester, has the characteristics of high temperature resistance, moisture resistance, excellent electrical insulation, oil resistance, chemical corrosion resistance and the like, has quick crystallization molding, has irreplaceable superiority in industrial application, becomes the fifth most common engineering plastic at present, and is widely applied to a plurality of fields of automobile industry, electronic and electric appliance industry, food and medical equipment, packaging materials, environmental engineering and the like. With the ongoing intensive research into the structure and performance of PBT, for example: engineering plastics with high impact property, heat resistance, flame retardance and the like are widely applied to synthetic fibers, and PBT fibers are prepared, so that the obtained fiber yarns have the advantages of terylene, acrylon, spandex and the like, and are soft in hand feeling and convenient to dye.
However, with continuous research on properties of PBT fiber materials, not only good properties of PBT fibers are explored, but also the applicable range of PBT fibers is found to be limited, and thus modification treatment of PBT is needed to achieve functional characteristics imparting differentiation to PBT, for example: antistatic, high-strength wear-resistant, anti-fouling, super-hydrophobic and other performances.
For example: the patent number 201310447203.0 discloses fluorine-containing random copolyester DTY fibers, the patent number 201310445643.2 discloses fluorine-containing PET-PBT copolyester DTY fibers, the patent number 201310445114.2 discloses fluorine-containing PBT polyester DTY fibers and the like, and by introducing fluorine atoms, the performances of the fibers in the aspects of superhydrophobicity, hydrophobicity, oleophobicity, pollution resistance and the like are greatly improved, so that the fluorine-containing random copolyester DTY fibers can be widely applied to the preparation of waterproof clothing, pollution-resistant working clothing and the like.
For another example: the patent number 201610780369.8 discloses that in order to facilitate the entering of micro particles such as dyeing into the inside of the PBT polyester, the dyeing rate is improved, meanwhile, the solution viscosity, the processing temperature and the degradation rate of the PBT fiber are reduced, the excellent performance of the PBT fiber is ensured, and the branched chain-containing dihydric alcohol chain forging is introduced into the molecular chain of the modified PBT polyester.
For another example: for surface decolorization, the color fastness is high, and patent number 201810698304.8 discloses ultra-soft high-elasticity color yarn fiber, and a special color master batch (containing PBT) is matched with polyester fiber, so that the coloring rate of the polyester fiber is effectively improved, and the phenomena of decolorization, fading and the like are avoided.
Therefore, the prior art has adopted modification treatment to PBT, so that fibers with different properties are obtained, meanwhile, how to improve the scratch resistance of the PBT stretch fiber yarn and enhance the wear resistance is also focused by those skilled in the art.
Based on the above, the researcher is based on long-term study of PBT fiber materials, introduces the technical idea of changing waste into valuable, and provides a new idea for the production of PBT stretch fiber yarns.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides a PBT stretch yarn with high scratch resistance and a preparation method thereof.
The method is realized by the following technical scheme:
the invention aims to provide a PBT stretch yarn with high scratch resistance, which comprises, by mass, 10-20 parts of PBT, 3-8 parts of polyvinyl chloride, 0.1-0.5 part of polyvinyl alcohol, 0.1-0.5 part of calcium stearate and 0.1-1 part of slag micropowder.
By introducing slag micropowder and adding the slag micropowder into the PBT base material under specific conditions, the scratch resistance of the PBT elastic fiber yarn is improved, and the breaking strength and the breaking elongation are improved.
In order to make the scratch resistance more excellent, it is preferable that the raw materials include, by mass, 15 parts of PBT, 5 parts of polyvinyl chloride, 0.2 part of polyvinyl alcohol, 0.4 part of calcium stearate, and 0.3 part of slag micropowder. More preferably, the raw materials comprise 14 parts by mass of PBT, 7 parts by mass of polyvinyl chloride, 0.4 part by mass of polyvinyl alcohol, 0.3 part by mass of calcium stearate and 0.8 part by mass of slag micropowder.
Preferably, the slag micropowder is a sieve bottom material obtained by calcining slag at 800-1000 ℃ for at least 30min, then sending the slag micropowder into a ball mill for ball milling and sieving the slag micropowder with a 1000-mesh sieve. Can make the filling and stacking effect of slag micropowder more excellent.
More preferably, the slag micropowder is a sieve bottom material obtained by calcining slag at 900 ℃ for at least 30min, then sending the slag micropowder into a ball mill for ball milling and sieving the slag micropowder with a 1000-mesh sieve.
The slag micropowder is one or more selected from fluorite tailing slag micropowder, electrolytic manganese slag micropowder and antimony tailing micropowder.
The second object of the invention is to provide a preparation method of the PBT elastic fiber yarn with high scratch resistance, which comprises the following steps:
(1) Preparing slag micropowder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for carrying out a physical mixing step;
(3) A modification treatment step of modifying the material obtained in the material mixing step in a nitrogen atmosphere;
(4) And (3) preparing the PBT stretch fiber yarn with high scratch resistance by melt spinning, stretching and heat treatment of the material obtained in the modification treatment step.
In order to enable the materials to be mixed more uniformly and enable slag micropowder to be filled in gaps among the materials, preferably, the step (2) is to sequentially add the slag micropowder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into the PBT, and stir the materials at a stirring speed of at least 1000r/min in the adding process until the calcium stearate is added, and continuously stirring for at least 30min.
Preferably, the step (3) is to heat the material treated in the step (2) to 100 ℃ for at least 20min under the nitrogen atmosphere and the vacuum degree of 0.1-0.3 MPa.
Compared with the prior art, the invention has the technical effects that:
the PBT elastic fiber yarn is prepared by introducing slag micropowder, mixing at high speed under the conditions of polyvinyl chloride, polyvinyl alcohol and calcium stearate, heating in nitrogen atmosphere, and then preparing the PBT elastic fiber yarn by a melt spinning, stretching and heat treatment process, so that the scratch resistance of the PBT elastic fiber yarn is greatly improved, the breaking strength reaches 3.6-4.1cN/dex, and the breaking elongation reaches 30-50%.
Detailed Description
The technical scheme of the present invention is further defined below in conjunction with the specific embodiments, but the scope of the claimed invention is not limited to the description.
In some embodiments, the high scratch resistance PBT stretch yarn comprises, by mass, 10-20 parts of PBT, 3-8 parts of polyvinyl chloride, 0.1-0.5 part of polyvinyl alcohol, 0.1-0.5 part of calcium stearate and 0.1-1 part of slag micropowder; for example: the raw materials comprise 15 parts by mass of PBT, 5 parts by mass of polyvinyl chloride, 0.2 part by mass of polyvinyl alcohol, 0.4 part by mass of calcium stearate and 0.3 part by mass of slag micropowder. Or the raw materials comprise 14 parts by mass of PBT, 7 parts by mass of polyvinyl chloride, 0.4 part by mass of polyvinyl alcohol, 0.3 part by mass of calcium stearate and 0.8 part by mass of slag micropowder. Or 10 parts of PBT, 3 parts of polyvinyl chloride, 0.1 part of polyvinyl alcohol, 0.1 part of calcium stearate and 0.1 part of slag micropowder. Or, the raw materials comprise 20 parts of PBT, 8 parts of polyvinyl chloride, 0.5 part of polyvinyl alcohol, 0.5 part of calcium stearate, 1 part of slag micropowder and the like in parts by mass, and slag micropowder with lower cost is introduced through reasonable selection of raw material proportion and raw material components, so that the PBT stretch fiber yarn is prepared after the PBT is modified under the action of the polyvinyl alcohol, the calcium stearate and the polyvinyl chloride, the scratch resistance of the fiber yarn is improved, and the breaking strength and the breaking elongation of the stretch fiber yarn are enhanced.
In certain embodiments, the slag micropowder is produced by calcining slag at 800-1000 ℃ for at least 30 minutes, for example: calcining at 800deg.C for 30min, calcining at 900deg.C for 30min, and calcining at 1000deg.C for 30min. And (5) feeding the mixture into a ball mill for ball milling and sieving the mixture with a 1000-mesh sieve to obtain the sieve bottom material. The slag micropowder is selected from fluorite tailing slag micropowder, electrolytic manganese slag micropowder and/or antimony tailing micropowder, wherein in order to better promote ductility of formed elastic fibers and improve tensile elongation at break, the electrolytic manganese slag micropowder and the antimony tailing micropowder are added as slag micropowder after being uniformly mixed according to mass ratios of 1:2, 1:3, 1:4, 1:5, 1:6 and the like. And through experimental trial, after the electrolytic manganese slag micro powder and the antimony tailings micro powder are added according to the mass ratio of 1:5, the stretch-breaking elongation resistance of the formed elastic fiber yarn is better, and compared with the pure addition of the electrolytic manganese slag micro powder or the antimony tailings micro powder, the stretch-breaking elongation resistance of the elastic fiber yarn is improved by about 10%.
The invention provides a preparation method of PBT stretch yarn with high scratch resistance in certain embodiments, which comprises the following steps:
(1) Preparing slag micropowder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for carrying out a physical mixing step;
(3) A modification treatment step of modifying the material obtained in the material mixing step in a nitrogen atmosphere;
(4) And (3) preparing the PBT stretch fiber yarn with high scratch resistance by melt spinning, stretching and heat treatment of the material obtained in the modification treatment step.
Adding slag micropowder, sequentially adding polyvinyl chloride, polyvinyl alcohol, calcium stearate and the like, and uniformly mixing, so that the contact time of the slag micropowder and the PBT is longer in the mixing process, improving the environment of the PBT and the slag micropowder by adding the subsequent polyvinyl chloride, the polyvinyl alcohol and the calcium stearate, modifying the environment by using nitrogen atmosphere, and further ensuring that the properties of scratch resistance, strength, tensile elongation at break and the like of the PBT stretch fiber yarn prepared by melt spinning-stretching-heat treatment are modified.
In certain embodiments, the step (2) is to sequentially add the slag micropowder, polyvinyl chloride, polyvinyl alcohol and calcium stearate to the PBT, and stir at a stirring speed of at least 1000r/min during the adding process until the calcium stearate is added, and continuously stirring for at least 30min. So that the mixture is more uniform.
In certain embodiments, the step (3) is to heat the material treated in the step (2) to 100 ℃ for at least 20min under nitrogen atmosphere and vacuum of 0.1-0.3 MPa.
In order to better verify the technical effects brought by the technical scheme, the researchers develop the preparation of the following products in the research process, and the products are used for detecting the performances such as scratch resistance, breaking strength, breaking elongation and the like.
The fluorite tailing slag micropowder, electrolytic manganese slag micropowder and antimony tailing micropowder used in the following examples were prepared in the following manner.
Fluorite tailing slag micropowder: calcining fluorite tailing slag at 800 ℃ for 30min, and then sending the fluorite tailing slag into a ball mill for ball milling and sieving the fluorite tailing slag with a 1000-mesh sieve.
Electrolytic manganese slag micropowder: and (3) calcining the electrolytic manganese slag at 800 ℃ for 30min, and then sending the electrolytic manganese slag into a ball mill for ball milling and sieving the electrolytic manganese slag with a 1000-mesh sieve.
Antimony tailing micropowder: calcining the antimony tailings at 800 ℃ for 30min, and then sending the antimony tailings into a ball mill for ball milling and sieving the antimony tailings with a 1000-mesh sieve.
Experiment one, single slag micropowder addition experiment study
Example 1
The raw materials comprise 15 parts by mass (kg) of PBT, 5 parts by mass of polyvinyl chloride, 0.2 part by mass of polyvinyl alcohol, 0.4 part by mass of calcium stearate and 0.3 part by mass of slag micropowder.
The preparation method comprises the following steps:
sequentially adding slag micropowder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into the PBT, and stirring at a stirring speed of 1000r/min in the adding process until the calcium stearate is added, and continuously stirring for 30min to obtain the mixture.
Heating the mixture to 100 ℃ in nitrogen atmosphere with the vacuum degree between 0.1 and 0.3MPa for 20min to obtain the modified material.
Feeding the modified material into a double-screw extruder for melt spinning to obtain a spinning melt, wherein the melt spinning temperature is 280 ℃; and (3) sending the obtained spinning melt into a spinning box for spinning, spraying out the spinning melt through a spinning plate, and stretching the spinning melt through a stretching roller and performing heat treatment to obtain the scratch-resistant PBT elastic fiber yarn.
The slag micropowder adopts fluorite tailing slag micropowder.
Example 2
Based on the example 1, the raw materials comprise 14 parts by mass (kg) of PBT, 7 parts by mass of polyvinyl chloride, 0.4 part by mass of polyvinyl alcohol, 0.3 part by mass of calcium stearate and 0.8 part by mass of slag micropowder. The slag micropowder is electrolytic manganese slag micropowder, and the other components are the same as in example 1.
Example 3
Based on the example 1, the raw materials comprise 10 parts by mass of PBT, 3 parts by mass of polyvinyl chloride, 0.1 part by mass of polyvinyl alcohol, 0.1 part by mass of calcium stearate and 0.1 part by mass of slag micropowder. The slag micropowder was antimony tailing micropowder, and the other examples were the same as in example 1.
Example 4
On the basis of the example 1, the raw materials comprise, by mass, 20 parts of PBT, 8 parts of polyvinyl chloride, 0.5 part of polyvinyl alcohol, 0.5 part of calcium stearate and 1 part of slag micropowder, and the other materials are the same as in the example 1.
Example 5
The slag fine powder in example 1 was replaced with equal mass of calcium stearate based on example 1, and the same as in example 1 was repeated.
Example 6
Based on example 1, the slag micropowder of example 1 was SiO 2 The same mass substitution as in example 1 was carried out on the silicon micropowder with a content of > 99%.
The sample elastic fiber yarn prepared in the examples 1 to 6 was randomly sampled 5 groups each, and the measured data of the 5 groups were averaged to obtain the measured results of the corresponding indexes, wherein the measured indexes are: scratch resistance, breaking strength, elongation at break.
Scratch resistance: firstly, measuring the diameter of the PBT elastic fiber yarn, then scraping the surface of the PBT elastic fiber yarn by using a five-finger scraping method, controlling the scraping speed to be 100mm/s, and measuring the diameter loss rate (delta L) of the scraped position of the PBT elastic fiber yarn after scraping for 10 s.
The breaking strength was obtained by taking the breaking strength required when the obtained sample elastic fiber was broken, and the elongation at break was recorded as compared with the elongation at the start of stretching, and the breaking elongation was recorded as shown in the following table 1.
TABLE 1 Single slag micropowder addition test
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Scratch resistance (delta L) | 0.09 | 0.11 | 0.09 | 0.08 | 2.89 | 2.45 |
| Tensile Strength (cn/dex) | 3.6 | 3.8 | 3.6 | 3.7 | 2.4 | 2.7 |
| Tensile elongation about (%) | 35 | 31 | 34 | 33 | 33 | 26 |
As can be seen from Table 1, the addition of fluorite tailing slag micropowder, electrolytic manganese slag micropowder and antimony tailing micropowder to the PBT elastic fiber raw material alone can better maintain the tensile elongation of the PBT elastic fiber yarn containing the raw materials such as PBT, polyvinyl chloride, polyvinyl alcohol and calcium stearate, and can improve the scratch resistance and enhance the tensile strength of the PBT elastic fiber yarn.
Experiment two, composite slag micropowder addition test study
Example 7
Based on the embodiment 1, the slag micropowder adopts a mixture formed by mixing fluorite tailing slag micropowder and electrolytic manganese slag micropowder according to a mass ratio of 1:2.
The preparation method comprises the following steps:
sequentially adding slag micropowder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into the PBT, and stirring at a stirring speed of 2000r/min in the adding process until the calcium stearate is added, and continuously stirring for 30min to obtain the mixture.
Heating the mixture to 100 ℃ in nitrogen atmosphere with the vacuum degree between 0.1 and 0.3MPa for 30min to obtain the modified material.
Feeding the modified material into a double-screw extruder for melt spinning to obtain a spinning melt, wherein the melt spinning temperature is 280 ℃; and (3) sending the obtained spinning melt into a spinning box for spinning, spraying out the spinning melt through a spinning plate, and stretching the spinning melt through a stretching roller and performing heat treatment to obtain the scratch-resistant PBT elastic fiber yarn.
The procedure is as in example 1.
Example 8
Based on the embodiment 7, the slag micropowder adopts a mixture formed by mixing fluorite tailing slag micropowder and antimony tailing micropowder according to a mass ratio of 1:2, and the other materials are the same as the embodiment 7.
Example 9
On the basis of the embodiment 7, the slag micropowder adopts a mixture formed by mixing electrolytic manganese slag micropowder and antimony tailing micropowder according to the mass ratio of 1:2, and the other materials are the same as the embodiment 7.
Example 10
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tail slag micro powder are mixed according to the mass ratio of 1:3, and the other materials are the same as the embodiment 9.
Example 11
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tail slag micro powder are mixed according to the mass ratio of 1:4, and the other materials are the same as the embodiment 9.
Example 12
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tail slag micro powder are mixed according to the mass ratio of 1:5, and the other materials are the same as the embodiment 9.
Example 13
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tail slag micro powder are mixed according to the mass ratio of 1:6, and the other materials are the same as the embodiment 9.
Example 14
On the basis of the embodiment 7, the slag micropowder adopts a mixture formed by mixing fluorite tailing slag micropowder and antimony tailing micropowder with electrolytic manganese slag micropowder according to the mass ratio of 1:2:1, and the other materials are the same as the embodiment 7.
Example 15
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1:3:1, and the other materials are the same as the embodiment 14.
Example 16
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1:4:1, and the other materials are the same as the embodiment 14.
Example 17
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1:5:1, and the other materials are the same as the embodiment 14.
Example 18
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1:6:1, and the other materials are the same as the embodiment 14.
Example 19
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.5:5:1, and the other materials are the same as the embodiment 14.
Example 20
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.1:5:1, and the other materials are the same as the embodiment 14.
Example 21
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing slag micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.1:6:1, and the other materials are the same as the embodiment 14.
The sample elastic fiber filaments obtained in examples 7 to 21 were tested for scratch resistance, tensile breaking strength and tensile elongation according to the test method of test one, and the results are shown in table 2 below.
Table 2 study of composite slag micropowder addition test
| Scratch resistance (delta L) | Tensile Strength (cn/dex) | Tensile elongation about (%) | |
| Example 7 | 0.07 | 3.7 | 38 |
| Example 8 | 0.08 | 3.6 | 33 |
| Example 9 | 0.05 | 3.9 | 37 |
| Example 10 | 0.05 | 3.8 | 36 |
| Example 11 | 0.04 | 3.9 | 39 |
| Example 12 | 0.03 | 4.0 | 42 |
| Example 13 | 0.06 | 3.2 | 31 |
| Example 14 | 0.06 | 3.5 | 37 |
| Example 15 | 0.05 | 3.7 | 39 |
| Example 16 | 0.05 | 3.9 | 39 |
| Example 17 | 0.04 | 4.1 | 40 |
| Example 18 | 0.05 | 3.1 | 38 |
| Example 19 | 0.08 | 4.1 | 33 |
| Example 20 | 0.02 | 4.0 | 49 |
| Example 21 | 0.09 | 3.4 | 36 |
As can be seen from Table 2, when slag micropowder is added in a compounding manner, the selected slag micropowder is emphasized, and the proper compounding ratio is adopted, so that the scraping resistance of the PBT elastic fiber yarn is improved, the tensile strength is ensured, the tensile length is prolonged, and the friction resistance, the strength and the flexibility of the PBT elastic fiber yarn after being prepared into products are improved.
Study on test III and slag micropowder treatment process
On the basis of the first test, raw materials are selected according to the production process and the raw material proportion of the embodiment 1, slag micropowder is prepared by adopting different processes, and then the process adjustment shows that the scratch resistance of the PBT stretch yarn is influenced, as shown in the table 3.
TABLE 3 study of slag micropowder treatment Process
As is clear from tables 1 and 3, when the slag micropowder is calcined at a temperature higher than 800 ℃, the influence on the scratch resistance is not remarkable, but when the process of directly drying to constant weight and ball milling and sieving with a 1000-mesh sieve is carried out, when the treatment temperature is far lower than 800 ℃, the antimony tailing micropowder is adopted as the slag micropowder, the influence on the scratch resistance is also small, and when the electrolytic manganese slag and fluorite tailing slag are adopted as the slag micropowder raw materials for preparation, the influence on the scratch resistance is large, so that the scratch resistance of the PBT elastic fiber after the slag micropowder is added is improved, and meanwhile, the requirements of improving the scratch resistance of various slag (electrolytic manganese slag, fluorite tailing slag and antimony tailing slag) on the PBT elastic fiber can be met.
The invention is realized by referring to the prior art or common general knowledge and conventional technical means which are well known to the person skilled in the art, for example: the processes of melt spinning, stretching, heat treatment and the like mentioned in the creation of the invention are produced by referring to the processes described in the prior art, such as the color yarn fiber production process disclosed in the patent number 201810698304.8.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The PBT stretch yarn with high scratch resistance is characterized by comprising, by mass, 10-20 parts of PBT, 3-8 parts of polyvinyl chloride, 0.1-0.5 part of polyvinyl alcohol, 0.1-0.5 part of calcium stearate and 0.1-1 part of slag micropowder;
the slag micropowder is fluorite tailing slag micropowder, electrolytic manganese slag micropowder and/or antimony tailing micropowder.
2. The high scratch resistance PBT stretch yarn as claimed in claim 1, wherein the raw materials comprise 15 parts by mass of PBT, 5 parts by mass of polyvinyl chloride, 0.2 part by mass of polyvinyl alcohol, 0.4 part by mass of calcium stearate and 0.3 part by mass of slag micropowder.
3. The high scratch resistance PBT stretch yarn as claimed in claim 1, wherein the raw materials comprise, by mass, 14 parts of PBT, 7 parts of polyvinyl chloride, 0.4 part of polyvinyl alcohol, 0.3 part of calcium stearate and 0.8 part of slag micropowder.
4. A high scratch resistant PBT stretch yarn according to claim 1, 2 or 3, wherein the slag micropowder is a sieve base material obtained by calcining slag at 800-1000 ℃ for at least 30min, ball milling in a ball mill and sieving with a 1000 mesh sieve.
5. The high scratch resistant PBT stretch yarn as claimed in claim 4, wherein the slag micropowder is a sieve base material obtained by calcining slag at 900 ℃ for at least 30min, feeding the slag into a ball mill, ball milling and sieving with a 1000-mesh sieve.
6. A method of making high scratch resistance PBT spandex filament according to any one of claims 1 to 5, comprising the steps of:
(1) Preparing slag micropowder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for carrying out a physical mixing step;
(3) A modification treatment step of modifying the material obtained in the material mixing step in a nitrogen atmosphere;
(4) Preparing the PBT stretch fiber yarn with high scratch resistance by melt spinning, stretching and heat treatment of the material obtained in the modification treatment step;
the step (1) is to calcine the slag for at least 30min at 800-1000 ℃, send the slag into a ball mill for ball milling and pass through a sieve with 1000 meshes to obtain a sieve bottom material;
and (3) heating the material treated in the step (2) to 100 ℃ for at least 20min under the nitrogen atmosphere and the vacuum degree of 0.1-0.3 MPa.
7. The method for preparing the PBT stretch yarn with high scratch resistance according to claim 6, wherein the step (2) is to sequentially add slag micropowder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into the PBT, and stir at a stirring speed of at least 1000r/min during the adding process until the calcium stearate is added, and continuously stirring for at least 30min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211117316.XA CN115467042B (en) | 2022-09-14 | 2022-09-14 | PBT stretch fiber yarn with high scratch resistance and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211117316.XA CN115467042B (en) | 2022-09-14 | 2022-09-14 | PBT stretch fiber yarn with high scratch resistance and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115467042A CN115467042A (en) | 2022-12-13 |
| CN115467042B true CN115467042B (en) | 2023-11-03 |
Family
ID=84333563
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211117316.XA Active CN115467042B (en) | 2022-09-14 | 2022-09-14 | PBT stretch fiber yarn with high scratch resistance and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115467042B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117248295A (en) * | 2023-10-19 | 2023-12-19 | 无锡市兴盛新材料科技有限公司 | A kind of PBT elastic fiber yarn with scratch-resistant and stain-resistant properties and its preparation process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464868A (en) * | 2010-11-05 | 2012-05-23 | 合肥杰事杰新材料股份有限公司 | Scratch-resistant polybutylene terephthalate composition and preparation method thereof |
| CN107400343A (en) * | 2017-09-15 | 2017-11-28 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant scratch-resistant PBT composite and preparation method thereof |
| CN114015209A (en) * | 2021-11-26 | 2022-02-08 | 凉山瑞禾新材料有限公司 | Slag micro powder enhanced PET plastic steel binding belt and preparation method thereof |
-
2022
- 2022-09-14 CN CN202211117316.XA patent/CN115467042B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102464868A (en) * | 2010-11-05 | 2012-05-23 | 合肥杰事杰新材料股份有限公司 | Scratch-resistant polybutylene terephthalate composition and preparation method thereof |
| CN107400343A (en) * | 2017-09-15 | 2017-11-28 | 安徽江淮汽车集团股份有限公司 | A kind of fire-retardant scratch-resistant PBT composite and preparation method thereof |
| CN114015209A (en) * | 2021-11-26 | 2022-02-08 | 凉山瑞禾新材料有限公司 | Slag micro powder enhanced PET plastic steel binding belt and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 玻璃纤维增强PBT复合材料刮擦行为研究;程前;蒋晗;李永华;洪志豪;乔亮;陈迪;张亮亮;;塑料工业(08);第79-82页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115467042A (en) | 2022-12-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN115467042B (en) | PBT stretch fiber yarn with high scratch resistance and preparation method thereof | |
| EP1383716A1 (en) | Sized reinforcements, and materials reinforced with such reinforcements | |
| CN105176023A (en) | Sound-absorbing and heat-preserving composite environment-friendly material for automotive upholstery and preparing method of sound-absorbing and heat-preserving composite environment-friendly material | |
| CN115044135A (en) | Antistatic polypropylene composition and preparation method thereof | |
| CN109575535B (en) | Self-lubricating PET fiber composite material and preparation method thereof | |
| Yang et al. | Preparation and characterization of novel super-artificial hair fiber based on biomass materials | |
| Dastjerdi et al. | Investigating the effect of various blend ratios of prepared masterbatch containing Ag/TiO2 nanocomposite on the properties of bioactive continuous filament yarns | |
| CN115928291A (en) | Antibacterial flame-retardant suede, preparation method and application thereof in automotive interior | |
| CN113045872A (en) | High-heat-resistance and high-toughness biodegradable PLA modified material and preparation method thereof | |
| CN110699799B (en) | High-elastic polyester yarn and preparation method thereof | |
| CN112647146B (en) | Preparation method and application of waterproof polyester fiber | |
| CN110204897A (en) | A kind of flame-retardant and anti-static type polyamide compoiste material and preparation method thereof | |
| CN111519278A (en) | Biodegradable antibacterial polyester fiber material and preparation method thereof | |
| CN120401057A (en) | ES special-shaped fiber and its manufacturing method | |
| KR20020077525A (en) | Bulky polyester multifilament composite yarn and process for producing the same | |
| Nedjma et al. | Effect of chemical treatment on newspaper fibers reinforced polymer poly (vinyl chloride) composites | |
| CN1238419C (en) | Composition of delustered styrene acrylonitrile copolymer containing gel powder acrylonitrile butadiene rubber | |
| CN116732630A (en) | Multifunctional graphene low-molecular-weight polyethylene fiber and preparation method thereof | |
| CN110424066A (en) | A kind of composite enhanced polyester fiber of luggage and preparation method thereof | |
| DE60130931D1 (en) | POLYOLEFINBASING SYNTHESIS FIBERS AND METHOD FOR THE PRODUCTION THEREOF | |
| CN115536971B (en) | Heat aging-resistant ASA/PBT composition and preparation method thereof | |
| CN105176026A (en) | Scratching-proof polylactic acid composite automotive upholstery material and preparing method thereof | |
| KR930007830B1 (en) | Process for producing high strength polyester monofilament with excellent processability | |
| EP3660207A1 (en) | Non-woven artificial leather using dope-dyed polyester sea-island type composite yarn and method for producing same | |
| CN103804910B (en) | A kind of glass, SiO2Strengthen Polyphenylene Sulfide Toughened material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |