CN115467042A - High-scratch-resistance PBT (polybutylene terephthalate) elastic fiber yarn and preparation method thereof - Google Patents
High-scratch-resistance PBT (polybutylene terephthalate) elastic fiber yarn and preparation method thereof Download PDFInfo
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- CN115467042A CN115467042A CN202211117316.XA CN202211117316A CN115467042A CN 115467042 A CN115467042 A CN 115467042A CN 202211117316 A CN202211117316 A CN 202211117316A CN 115467042 A CN115467042 A CN 115467042A
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- pbt
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- elastic fiber
- scratch resistance
- fiber yarn
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- 210000004177 elastic tissue Anatomy 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229920001707 polybutylene terephthalate Polymers 0.000 title description 73
- -1 polybutylene terephthalate Polymers 0.000 title description 3
- 239000002893 slag Substances 0.000 claims abstract description 128
- 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
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 105
- 229910052787 antimony Inorganic materials 0.000 claims description 28
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 28
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 27
- 229910052748 manganese Inorganic materials 0.000 claims description 27
- 239000011572 manganese Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 23
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [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 20
- 238000003756 stirring Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 10
- 238000002074 melt spinning Methods 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012216 screening Methods 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 19
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000009987 spinning Methods 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 238000011160 research Methods 0.000 description 7
- 229920000728 polyester Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052731 fluorine Inorganic materials 0.000 description 4
- 239000011737 fluorine Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 238000007790 scraping Methods 0.000 description 4
- 229920001634 Copolyester Polymers 0.000 description 3
- 229920002334 Spandex Polymers 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000004759 spandex Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000013329 compounding 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
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000003678 scratch resistant effect Effects 0.000 description 2
- 238000005507 spraying 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
- 229920004933 Terylene® Polymers 0.000 description 1
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000015572 biosynthetic process 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
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 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
- 238000011049 filling Methods 0.000 description 1
- 125000001153 fluoro group Chemical group F* 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 125000003827 glycol group Chemical group 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000003075 superhydrophobic effect Effects 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 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 manufacturing, in particular to a PBT elastic fiber yarn with high scratch resistance and a preparation method thereof, wherein slag micropowder is introduced into PBT, and the PBT elastic fiber yarn is prepared by high-speed mixing under the conditions of polyvinyl chloride, polyvinyl alcohol and calcium stearate, heating treatment under the nitrogen atmosphere, and melt spinning-stretching-heat treatment, 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 elastic fiber yarn with high scratch resistance and a preparation method thereof.
Background
Polybutylene terephthalate (PBT) is a crystalline linear saturated polyester, has the characteristics of high temperature resistance, moisture resistance, excellent electrical insulation, oil resistance, chemical corrosion resistance and the like, is quickly crystallized and formed, has irreplaceable superiority in industrial application, has become the fifth most common engineering plastic at present, and is widely applied to a plurality of fields of automobile industry, electronic and electrical appliance industry, food and medical instruments, packaging materials, environmental engineering and the like. With the continuous and deep research on the structure and performance of PBT, for example: the engineering plastics with high impact property, heat resistance, flame retardance and the like are widely applied to the aspect of synthetic fibers, and the PBT fibers are prepared, so that the obtained fiber yarns have the advantages of terylene, acrylon, spandex and the like, are soft in hand feeling and are convenient to dye.
However, with the continuous research on the properties of PBT fiber materials, not only the excellent properties of PBT fibers are explored, but also the applicable range of PBT fibers is found to be limited, so that it is necessary to modify PBT to achieve the functional characteristics of differentiated PBT, such as: antistatic, high strength, wear resistance, antifouling, super-hydrophobic and other performances.
For example: the fluorine-containing random copolyester DTY fiber is disclosed in the patent number of 201310447203.0, the fluorine-containing PET-PBT copolyester DTY fiber is disclosed in the patent number of 201310445643.2, the fluorine-containing PBT polyester DTY fiber is disclosed in the patent number of 201310445114.2, and the like, and fluorine atoms are introduced, so that the performances of the fiber in the aspects of super hydrophobicity, oleophobicity, pollution prevention and the like are greatly improved, and the fluorine-containing PET copolyester DTY fiber can be widely applied to the preparation of waterproof clothes, pollution-resistant working clothes and the like.
For another example: the patent number 201610780369.8 discloses that in order to facilitate the degree of the tiny particles such as dyeing and the like entering the interior of the PBT polyester, the dyeing rate is improved, the solution viscosity of the PBT fiber is reduced, the processing temperature is reduced, the degradation rate is reduced, the excellent performance of the PBT fiber is guaranteed, and the glycol chain forging containing a branched chain is introduced into the molecular chain of the modified PBT polyester.
For another example: in order to decolor the surface and ensure high color fastness, the patent number 201810698304.8 discloses super-soft high-elasticity colored silk fiber, and special color master batches (containing PBT) are matched with polyester fiber, so that the coloring rate of the polyester fiber is effectively improved, and the phenomena of decoloration, fading and the like can not occur.
Therefore, in the prior art, the PBT is modified, so that fibers with different properties are obtained, and meanwhile, the important attention of the technical personnel in the field is paid to how to improve the scratch resistance and enhance the wear resistance of the PBT elastic fiber yarn.
Based on the above, the researchers are based on long-term research on PBT fiber materials, introduce the technical idea of changing waste into valuable, and provide a new idea for the production of the PBT elastic fiber yarns.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides the PBT stretch yarn with high scratch resistance and the preparation method thereof.
The method is realized by the following technical scheme:
the invention aims to provide high-scratch-resistance PBT elastic fiber yarns which comprise, 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, the raw materials preferably 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 fine powder. More preferably, 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 micro powder.
Preferably, the slag micro powder is a bottom material obtained by calcining slag at 800-1000 ℃ for at least 30min, then sending the calcined slag into a ball mill for ball milling and sieving the calcined slag with a 1000-mesh sieve. The filling and stacking effects of the slag micro powder can be more excellent.
More preferably, the slag micro powder is a undersize obtained by calcining slag at 900 ℃ for at least 30min, then sending the calcined slag into a ball mill for ball milling and sieving the ball mill with a 1000-mesh sieve.
The slag micro powder is selected from one or more of fluorite tailing micro powder, electrolytic manganese slag micro powder and antimony tailing micro powder.
The invention also aims to provide a preparation method of the PBT elastic fiber yarn with high scratch resistance, which comprises the following steps:
(1) Preparing slag micro powder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for mixing;
(3) Modifying the material obtained in the mixing step in a nitrogen atmosphere;
(4) And (3) carrying out melt spinning, drawing and heat treatment on the material obtained in the modification treatment step to prepare the PBT elastic fiber yarn with high scratch resistance.
In order to mix the materials more uniformly and fill the slag micro powder in gaps among the materials, preferably, in the step (2), the slag micro powder, the polyvinyl chloride, the polyvinyl alcohol and the calcium stearate are sequentially added into the PBT, and are stirred at a stirring speed of at least 1000r/min in the adding process until the calcium stearate is added, and the stirring is continued for at least 30min.
Preferably, the step (3) is to heat the material obtained by 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 technical effects created by the invention are as follows:
the PBT elastic fiber yarn is prepared by introducing slag micro powder, high-speed mixing under the conditions of polyvinyl chloride, polyvinyl alcohol and calcium stearate, heating treatment under the nitrogen atmosphere and 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%.
Detailed Description
The technical solution of the present invention is further defined below with reference to specific embodiments, but the scope of protection is not limited to the description.
In some embodiments, the high scratch resistance PBT elastic fiber 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, 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 micro powder. Or 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 micro powder. Or the raw materials comprise, by mass, 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 micro powder. Or 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, 1 part of slag micropowder and the like, and the slag micropowder with lower cost is introduced through reasonable selection of raw material proportion and raw material components, so that the PBT is modified to prepare the PBT elastic fiber under the action of the polyvinyl alcohol, the calcium stearate and the polyvinyl chloride, the scratch resistance of the fiber is improved, and the breaking strength and the breaking elongation of the elastic fiber are enhanced.
The invention creates in some embodiments that the slag micropowder is obtained by calcining the slag at 800-1000 ℃ for at least 30min, for example: calcining at 800 deg.C for 30min, at 900 deg.C for 30min, and at 1000 deg.C for 30min. And (4) sending the mixture into a ball mill for ball milling, and sieving the mixture through a 1000-mesh sieve to obtain the sieve base material. The slag micro powder is selected from but not limited to fluorite tailing micro powder, electrolytic manganese slag micro powder and/or antimony tailing micro powder, wherein in order to better improve the ductility of elastic fiber formation and improve the tensile elongation at break, the slag micro powder and the antimony tailing micro powder are uniformly mixed according to the mass ratio of 1. Through test trials, after the electrolytic manganese slag micro powder and the antimony tailing micro powder are added according to the mass ratio of 1.
The invention creates a preparation method of PBT stretch yarn with high scratch resistance in certain embodiments, which comprises the following steps:
(1) Preparing slag micro powder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for mixing;
(3) A modification treatment step of mixing the materials obtained in the step under the nitrogen atmosphere;
(4) And (3) carrying out melt spinning, drawing and heat treatment on the material obtained in the modification treatment step to prepare the PBT elastic fiber yarn with high scratch resistance.
Firstly adding slag micropowder, then sequentially adding polyvinyl chloride, polyvinyl alcohol, calcium stearate and the like for uniform mixing, so that the contact time of the slag micropowder and PBT is longer in the mixing process, the environment of the PBT and the slag micropowder is improved by adding the subsequent polyvinyl chloride, polyvinyl alcohol and calcium stearate, and then the PBT elastic fiber yarn prepared by melt spinning-stretching-heat treatment is modified in the nitrogen atmosphere, so that the performances of scratch resistance, strength, tensile elongation, elongation at break and the like are all ensured to be modified.
In certain embodiments, the slag micropowder, the polyvinyl chloride, the polyvinyl alcohol and the calcium stearate are sequentially added into the PBT, and stirring is carried out at a stirring speed of at least 1000r/min during the adding process until the calcium stearate is added completely, and stirring is continued for at least 30min. So that the mixture is more uniform.
In certain embodiments, the step (3) is to heat the material obtained by the step (2) to 100 ℃ for at least 20min under the nitrogen atmosphere and the vacuum degree of 0.1-0.3 MPa.
In order to better verify the technical effects of the technical scheme provided by the invention, 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 fine fluorite slag powder, the fine electrolytic manganese slag powder and the fine antimony slag powder used in the following examples were prepared in the following manner.
Fluorite tailing slag micro powder: calcining fluorite tailing slag at 800 ℃ for 30min, feeding 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 micro powder: calcining the electrolytic manganese slag at 800 ℃ for 30min, 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 tailings micropowder: calcining antimony tailings at 800 ℃ for 30min, feeding the antimony tailings into a ball mill for ball milling, and sieving the antimony tailings with a 1000-mesh sieve.
First, research on single slag micro powder addition test
Example 1
The raw materials comprise, by mass (kg), 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 micro powder.
The preparation method comprises the following steps:
sequentially adding the slag micro powder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into PBT, 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 a mixture.
And heating the mixture to 100 ℃ in a nitrogen atmosphere with the vacuum degree of 0.1-0.3MPa 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) feeding the obtained spinning melt into a spinning box for spinning, spraying out the spinning melt through a spinning plate, stretching through a stretching roller and carrying out heat treatment to obtain the scratch-resistant PBT elastic fiber yarn.
The slag micro powder is fluorite tailing slag micro powder.
Example 2
In addition to example 1, the raw materials in parts by mass (kg) were PBT14 parts, polyvinyl chloride 7 parts, polyvinyl alcohol 0.4 part, calcium stearate 0.3 part, and fine slag powder 0.8 part. The slag micro powder is electrolytic manganese slag micro powder, and the rest is the same as that in the embodiment 1.
Example 3
Based on the embodiment 1, the raw materials comprise, by mass, 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 micro powder. The slag micro powder is antimony tailing micro powder, and the rest is the same as that in the embodiment 1.
Example 4
In addition to example 1, the raw materials in parts by mass were PBT20 parts, polyvinyl chloride 8 parts, polyvinyl alcohol 0.5 parts, calcium stearate 0.5 parts, fine slag powder 1 part, and the others were the same as in example 1.
Example 5
The same procedure as in example 1 was repeated except that calcium stearate of the same quality was used in place of the fine slag powder in example 1.
Example 6
Based on the embodiment 1, siO is adopted for the slag micro powder in the embodiment 1 2 The same procedure as in example 1 was repeated except that the fine silica powder having a content of > 99% was replaced by the same amount by mass.
The sample spandex filaments prepared in the embodiments 1 to 6 are randomly sampled by 5 groups of each group, and 5 groups of measurement data are averaged to obtain measurement results of corresponding indexes, wherein the measurement indexes are as follows: scratch resistance, breaking strength, elongation at break.
Scratch resistance: firstly, measuring the diameter of the PBT elastic fiber yarn, scraping the surface of the PBT elastic fiber yarn after measurement by a five-finger scraping method, controlling the scraping speed to be 100mm/s, and measuring the diameter loss rate (delta L) of the position of the PBT elastic fiber yarn where the PBT elastic fiber yarn is scraped after 10 seconds of scraping.
The breaking strength was determined as required for the stretch yarn obtained from the sample, and the elongation at break was recorded as compared with the elongation at the start of stretching, and the results are reported in table 1 below.
TABLE 1 Single Fine slag 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 of about (%) | 35 | 31 | 34 | 33 | 33 | 26 |
As can be seen from table 1, when the fluorite tailing slag micro powder, the electrolytic manganese slag micro powder and the antimony tailing micro powder are independently added to the PBT elastic fiber raw material, the tensile elongation of the PBT elastic fiber yarn containing the raw materials such as PBT, polyvinyl chloride, polyvinyl alcohol and calcium stearate can be well maintained, and meanwhile, the scratch resistance and tensile strength of the PBT elastic fiber yarn can be improved.
Experiment II, research of composite slag micro powder addition experiment
Example 7
On the basis of the embodiment 1, the slag micro powder is a mixture formed by mixing fluorite tailing slag micro powder and electrolytic manganese slag micro powder according to the mass ratio of 1.
The preparation method comprises the following steps:
sequentially adding the slag micro powder, polyvinyl chloride, polyvinyl alcohol and calcium stearate into PBT, stirring at a stirring speed of 2000r/min in the adding process, and continuously stirring for 30min after the calcium stearate is added to obtain a mixture.
And heating the mixture to 100 ℃ in a nitrogen atmosphere with the vacuum degree of 0.1-0.3MPa 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) feeding the obtained spinning melt into a spinning box for spinning, spraying out the spinning melt through a spinning plate, stretching through a stretching roller and carrying out heat treatment to obtain the scratch-resistant PBT elastic fiber yarn.
The rest of the procedure was the same as in example 1.
Example 8
On the basis of the embodiment 7, the slag micro powder is a mixture formed by mixing fluorite tailing powder and antimony tailing powder according to a mass ratio of 1.
Example 9
On the basis of the embodiment 7, the slag micro powder is a mixture formed by mixing electrolytic manganese slag micro powder and antimony tailing micro powder according to a mass ratio of 1.
Example 10
The electrolytic manganese slag micro powder and the antimony tailing micro powder are mixed according to the mass ratio of 1.
Example 11
The electrolytic manganese slag micro powder and the antimony tailing micro powder are mixed according to the mass ratio of 1.
Example 12
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tailing micro powder are mixed according to the mass ratio of 1.
Example 13
On the basis of the embodiment 9, the electrolytic manganese slag micro powder and the antimony tailing micro powder are mixed according to the mass ratio of 1.
Example 14
On the basis of the embodiment 7, the slag micro powder is a mixture formed by mixing fluorite tailing powder, antimony tailing powder and electrolytic manganese slag micro powder according to the mass ratio of 1.
Example 15
Based on the example 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1.
Example 16
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1.
Example 17
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1.
Example 18
Based on the example 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 1.
Example 19
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.5.
Example 20
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.1.
Example 21
On the basis of the embodiment 14, the fluorite tailing slag micro powder, the antimony tailing micro powder and the electrolytic manganese slag micro powder are mixed according to the mass ratio of 0.1.
The sample spandex 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 composite slag micropowder addition test study
| Scratch resistance (delta L) | Tensile Strength (cn/dex) | Tensile elongation of 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 the slag micropowder is added in a compounding manner, the selected slag micropowder is considered emphatically, and a proper compounding ratio is adopted, so that the scratch resistance of the PBT elastic fiber yarn is improved on the whole, 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 prepared into a product are improved.
Experiment III, research on slag micro-powder treatment process
On the basis of the first test, the raw materials are selected according to the production process and the raw material ratio in the embodiment 1, the adopted slag micro powder is prepared by adopting different processes, and then the process adjustment shows that the scratch resistance of the PBT elastic fiber yarn is influenced, and the scratch resistance is specifically shown in Table 3.
TABLE 3 study of slag micropowder treatment
As can be seen from tables 1 and 3, for the slag micro powder, which is calcined at a temperature higher than 800 ℃, the influence on the scratch resistance is not significant, but for the process of directly drying to constant weight and ball-milling through 1000 mesh sieve, when the processing temperature is far lower than 800 ℃, antimony tailing micro powder is used as the slag micro powder, which has little influence on the scratch resistance, and when electrolytic manganese slag and fluorite tailing slag are used as raw materials of the slag micro powder, which has great influence on the scratch resistance, so that in order to improve the scratch resistance of the PBT elastic fiber after adding the slag micro powder, and simultaneously, when various slag (electrolytic manganese slag, fluorite tailing slag and antimony tailing) are used as raw materials of the slag micro powder, the requirement for improving the scratch resistance of the PBT elastic fiber can be met, the researchers calcine the slag at a temperature higher than 800 ℃ for 30min and then ball-milling through 1000 mesh sieve, so that impurity components are largely burnt and exposed, and the dispersion effect is realized, and the scratch resistance of the PBT elastic fiber is improved.
The invention may be practiced otherwise than as specifically described with reference to the prior art or to any conventional technical means known to those skilled in the art, for example: the processes of melt spinning, drawing, heat treatment and the like mentioned in the creation of the invention refer to the processes introduced in the prior art, such as the process for producing the color silk fiber disclosed by the patent number 201810698304.8.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. The PBT elastic fiber 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.
2. The PBT elastic fiber yarn with high scratch resistance according to claim 1, wherein the raw materials comprise, 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.
3. The PBT stretch yarn with high scratch resistance according to 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. The PBT elastic fiber yarn with high scratch resistance according to claim 1, 2 or 3, wherein the slag micropowder is a mesh bottom material obtained by calcining slag at 800-1000 ℃ for at least 30min, feeding into a ball mill for ball milling and passing through a 1000-mesh sieve.
5. The PBT elastic fiber yarn with high scratch resistance of claim 4, wherein the slag micropowder is a undersize obtained by calcining slag at 900 ℃ for at least 30min, feeding the treated slag into a ball mill for ball milling, and sieving the ball milled slag with a 1000-mesh sieve.
6. The PBT elastic fiber yarn with high scratch resistance according to claim 1, 2, 3 or 5, wherein said fine slag powder is a fine fluorite tailing powder, a fine electrolytic manganese slag powder and/or a fine antimony tailing powder.
7. The preparation method of the PBT elastic fiber yarn with high scratch resistance of any one of claims 1 to 6, which comprises the following steps:
(1) Preparing slag micro powder;
(2) Taking PBT as a base material, adding slag micropowder firstly, and then sequentially adding polyvinyl chloride, polyvinyl alcohol and calcium stearate for mixing;
(3) A modification treatment step of mixing the materials obtained in the step under the nitrogen atmosphere;
(4) And (3) carrying out melt spinning, drawing and heat treatment on the material obtained in the modification treatment step to prepare the PBT elastic fiber yarn with high scratch resistance.
8. The method for preparing the PBT elastic fiber yarn with high scratch resistance according to claim 7, wherein the step (1) is a screen bottom material obtained by calcining the slag at 800-1000 ℃ for at least 30min, feeding the calcined slag into a ball mill for ball milling and screening the calcined slag with a 1000-mesh screen.
9. The method for preparing the PBT elastic fiber yarn with high scratch resistance according to claim 7, wherein the step (2) is to sequentially add the slag micropowder, the polyvinyl chloride, the polyvinyl alcohol and the calcium stearate into the PBT, and the stirring treatment is carried out at a stirring speed of at least 1000r/min during the adding process until the calcium stearate is added, and the stirring is continued for at least 30min.
10. The method for preparing the PBT elastic fiber yarn with high scratch resistance according to claim 7, wherein the step (3) is to heat the material obtained by the step (2) to 100 ℃ for at least 20min under a nitrogen atmosphere and a vacuum degree of 0.1-0.3 MPa.
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|---|---|---|---|---|
| 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 |
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| 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 |
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