CN115613347A - Peak grinding process and application thereof - Google Patents
Peak grinding process and application thereof Download PDFInfo
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- CN115613347A CN115613347A CN202211140746.3A CN202211140746A CN115613347A CN 115613347 A CN115613347 A CN 115613347A CN 202211140746 A CN202211140746 A CN 202211140746A CN 115613347 A CN115613347 A CN 115613347A
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Images
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- 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
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Mechanical Engineering (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention belongs to the technical field of material processing, and provides a peak grinding process and application thereof, wherein the material to be processed is annealed, then the material is immersed into alkali liquor in a suspension manner for heating treatment, the material is shaped and annealed firstly, so that the solvent resistance or alkali liquor permeability of the material is improved, the alkali liquor is only gradually hydrolyzed and eroded from the surface of the material, the material after the peak grinding process forms a straight pointed cone-shaped structure, the tensile strength is not lower than 355.86MPa, the elongation at break is not lower than 38.15%, and the material can be well used as a bristle material.
Description
Technical Field
The invention relates to the technical field of material processing, in particular to a peak grinding process and application thereof.
Background
The bristle materials used in toothbrushes sold in the market at present are mainly polypropylene (PP) bristles, polybutylene terephthalate (PBT) bristles, nylon (PA) bristles, polyethylene terephthalate (PET) composite sharpening filaments, and the like. In addition, the brush hair of the current domestic and foreign cosmetic brushes generally adopts artificial fiber hair material PBT fiber. PBT fibers are fibers made by melt spinning high purity terephthalic acid (TPA) or dimethyl terephthalate (DMT) with a 1, 4-butanediol polycondensed linear polymer. Before the fibers are used as the bristle materials, the fibers generally undergo a peak grinding process, the tail ends of the fibers can be changed into a pointed cone shape after the fibers undergo the peak grinding process, the peak grinding process is mainly to hydrolyze the fibers gradually from outside to inside through alkali liquor, and the tail ends of the fibers soaked in the alkali liquor are hydrolyzed more easily, so that the pointed cone shape is formed.
The material for preparing the bristles has good physical properties, good fatigue resistance and heat resistance, low friction coefficient, and hot water and oil resistance. However, all the materials are basically non-biodegradable and are inevitable consumables in daily life, a large amount of waste is generated every day, white pollution is caused, and huge environmental protection pressure is inevitably brought to the natural environment. Also, the above materials are relatively poorly biocompatible (except for nylon materials) and may cause discomfort to the gums or skin during use. Therefore, it is highly desirable to replace the above materials with materials that have good biocompatibility and are biodegradable. At present, the main biodegradable materials include Polyhydroxyalkanoate (PHA), polylactic acid (PLA), polycaprolactone (PCL), polybutylene adipate terephthalate (PBAT), and the like. In particular, PHA has good biodegradability, and can be degraded by household compost and seawater. PHA is a natural high molecular biological material, a cell lactone synthesized by microorganisms. Because of good biocompatibility and biodegradability, the material is one of ideal biomedical materials at present, and can be used as an in-vivo implanted stent, an operation membrane and an in-vivo filler. The PLA fiber is prepared by fermenting starch raw materials such as corn, wheat, cassava, potato, beet and the like to prepare lactic acid, polymerizing to obtain polylactic acid, and finally spinning and forming. PBAT belongs to thermoplastic biodegradable plastic, is a copolymer of butanediol adipate and butanediol terephthalate, has the characteristics of peroxybenzoic acid (PBA) and PBT, and has better ductility, elongation at break and heat resistance and impact performance; in addition, it has excellent biodegradability. The PHA, PLA and PBAT are biodegradable and environment-friendly polyester compounds, and the PHA, PLA and PBAT fibers all meet the requirements of environmental protection and resource recycling, so that the application prospect is wide. Meanwhile, because the PBT fibers have good biocompatibility and excellent skin-friendly performance, the PBT fibers are very suitable for being used as bristles of cosmetic brushes and toothbrush bristles, and just can solve the defects of the PBT fibers.
However, PHA and PLA materials are inferior to PBT materials in temperature resistance and solvent (or alkali) penetration resistance, and are easily penetrated into the material directly by the solvent (or alkali), so that the hydrolysis and peak-grinding process from the surface of the material to the inside cannot be realized, and finally the filament cannot be formed into a tapered filament tip with a certain strength. The material may also be softened due to rapid infiltration and swelling of the solvent or alkali liquor to the material, and hydrolysis reaction occurs inside the material, which finally leads to bonding and conglomeration between filaments and can not form straight tapered fiber filaments. The PBAT cellosilk is too soft to meet the requirements of the brush hair material of the cosmetic brush.
In addition, the PBT has good mechanical property at present, and a coil stock is directly placed on a supporting net rack in the peak grinding process. However, PHA, PLA, PBAT, or a mixture thereof has mechanical properties inferior to PBT, and after a sharp filament is formed by grinding a peak, the sharp filament at a portion in contact with a support frame is easily bent, thereby affecting the overall effect of the filament.
In view of the above, no mature peak grinding process for PHA, PLA and PBAT or mixed material fibers thereof exists in the prior art.
Therefore, under the situation that the environmental protection requirements of low carbon plastic inhibition are more and more urgent, a peak grinding process method suitable for biodegradable material fibers such as PHA, PLA and PBAT or mixed materials thereof is urgently needed to be provided, so that the processed fiber yarns are degradable, have good skin-friendly performance, can not cause gum or skin allergy, have straight pointed cone-shaped structures, and can not generate adhesion agglomeration among the yarns in the peak grinding process.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art described above. At least one end of the material after the peak grinding is changed into a straight taper shape from a cylinder shape, and the material has good mechanical property, the tensile strength is not lower than 355.86MPa, and the elongation at break is not lower than 38.15%.
A first aspect of the invention provides a peak milling process.
Specifically, the peak grinding process comprises the following steps:
(1) Annealing the material to be treated, and standing to obtain the annealed material;
(2) Soaking the material annealed in the step (1) in alkali liquor;
in the step (1), the material to be treated is immersed in alkali liquor in a suspension manner;
in the step (2), the temperature of the alkali liquor is 35-80 ℃; the mass fraction of the alkali liquor is 8-40wt%.
The method comprises the steps of annealing the material to be processed, wherein the annealing before peak grinding is mainly to improve the crystallinity of fiber filaments and is beneficial to the subsequent peak grinding process, then soaking the annealed material in alkali liquor, and because the crystallinity of the annealed material is improved, the solvent resistance or alkali liquor permeation resistance of the material is correspondingly improved, so that the alkali liquor can be gradually hydrolyzed and eroded from the surface of the material, and the problems that the material is softened due to the rapid permeation and swelling of the solvent or alkali liquor to the material, and the material is directly subjected to hydrolysis reaction inside the material, and finally the filaments are bonded and agglomerated, and a straight and high-toughness pointed cone-shaped structure cannot be formed are avoided. In addition, the material to be treated is soaked in the alkali liquor in a hanging manner, so that the problem that the whole effect of the material after peak grinding is influenced because part of sharp wires in contact with the supporting net rack are bent and the straight structure cannot be ensured because the material to be treated is directly placed on the supporting net rack is avoided.
Preferably, the material to be treated is an ungrafted fiber filament, and both ends of the ungrafted fiber filament are cylindrical. The purchased or prepared fiber filaments are subjected to the drawing process in the preparation process, and are subjected to the annealing step in the drawing process.
Preferably, the average diameter of the non-peaked filaments is between 0.01 and 1mm.
More preferably, the average diameter of the unpeaked filaments is from 0.01 to 0.1mm.
Preferably, in the step (1), the annealing treatment includes the following steps:
pretreating the material to be treated for 2-12h at 40-80 deg.C, taking out, and annealing at 25-30 deg.C and relative humidity of 30-50% for more than 4 h.
The annealing process of the invention is that the temperature of the fiber is firstly raised, and then the temperature is lowered to re-crystallize the fiber, thereby improving the crystallinity.
Preferably, the pre-treatment is carried out in an oven.
Preferably, the time of the pretreatment is 6 to 8 hours.
More preferably, the time of the pretreatment is 7h.
Preferably, the temperature of the pretreatment is 50 to 70 ℃.
More preferably, the temperature of the pretreatment is 60 ℃.
Preferably, the material to be treated is a degradable material.
Preferably, the degradable material is one or more of Polyhydroxyalkanoate (PHA), polylactic acid (PLA) and polybutylene adipate terephthalate (PBAT).
Preferably, the fiber filaments treated by the annealing procedure can be used for peak grinding within half a month.
Preferably, in the step (2), the temperature of the alkali liquor is 60-70 ℃; the mass fraction of the alkali liquor is 10-25wt%.
Preferably, the alkali liquor is one or more of sodium hydroxide solution, potassium hydroxide solution and sodium carbonate solution.
More preferably, the lye is a sodium hydroxide solution and/or a potassium hydroxide solution.
Preferably, the alkali liquor is a sodium hydroxide solution, and the mass fraction of the sodium hydroxide solution is 10-30wt%.
More preferably, the alkali liquor is a sodium hydroxide solution, and the mass fraction of the sodium hydroxide solution is 10-25wt%.
Further preferably, the alkali liquor is a sodium hydroxide solution, and the mass fraction of the sodium hydroxide solution is 20wt%.
Preferably, the alkali liquor is a potassium hydroxide solution, and the mass fraction of the potassium hydroxide solution is 10-40wt%.
More preferably, the alkali liquor is a potassium hydroxide solution, and the mass fraction of the potassium hydroxide solution is 15-30wt%.
Further preferably, the alkali liquor is a potassium hydroxide solution, and the concentration of the potassium hydroxide solution is 25wt%.
Preferably, one of the ends of the material to be treated is immersed in the lye in a suspended manner.
Preferably, the depth of immersion of the material to be treated is between 0.5 and 2.5cm.
More preferably, the depth of immersion of the material to be treated is between 1 and 1.5cm.
Preferably, the temperature of the lye is between 45 and 75 ℃.
More preferably, the temperature of the lye is between 50 and 70 ℃.
Preferably, after the alkali liquor is heated to the target temperature, sampling every 10min to observe the peak grinding condition of the fiber filaments.
Preferably, after the step (2) is finished, soaking the fiber filaments in water for washing.
In a second aspect of the invention, a fiber filament is provided that is produced by a peak milling process.
The fiber yarn is prepared by the peak grinding process, at least one end of the fiber yarn is in a taper shape, and the tensile strength of the fiber yarn is not lower than 355.86MPa.
Preferably, the tensile strength of the fiber filament is 355.86-455.05MPa.
Preferably, the fiber filament has an elongation at break of not less than 38.15%.
More preferably, the elongation at break of the fiber filaments is 38.15-42.05%.
Compared with the prior art, the invention has the following beneficial effects:
(1) Annealing the material to be processed, immersing the material in alkali liquor in a suspension manner, and heating, wherein the peak grinding process is carried out under the conditions of proper temperature and alkali liquor with proper concentration, before peak grinding, the material needs to be pretreated by a shaping and annealing procedure so as to further improve the crystallinity and mechanical property of the material, improve the solvent resistance or alkali liquor permeability of the material, avoid the material from softening, even the filaments are bonded into a cluster, and the material after the peak grinding process forms a straight pointed cone structure, has obvious pointed cone shape, good mechanical property, tensile strength not lower than 355.86MPa and elongation at break not lower than 38.15 percent and can be well used as a bristle material;
(2) The invention adopts biodegradable materials such as PHA, PLA and PBAT or mixed materials thereof to prepare the cellosilk, not only has good biocompatibility, but also can improve the skin-friendly property of the cellosilk, avoid skin or gum allergy, and can be degraded to avoid environmental pollution.
Drawings
FIG. 1 is a schematic view of a fiber yarn polishing device according to example 6 of the present invention;
FIG. 2 is a photograph of an un-peaked fiber of example 6 of the present invention;
FIG. 3 is a photograph of the fiber filaments after the peak grinding treatment of example 6 according to the present invention;
FIG. 4 is a photograph of the fiber filaments after the peak-milling treatment of example 7 of the present invention;
FIG. 5 is a photograph of the fiber filaments after the peak milling treatment of example 8 of the present invention;
FIG. 6 is a photograph of the fiber filaments after the peak-grind treatment of example 9 of the present invention;
FIG. 7 is a photograph of the fiber filaments after the peak shaving treatment according to example 10 of the present invention;
FIG. 8 is a photograph of the fiber filaments after the peak milling treatment of example 11 in accordance with the present invention;
FIG. 9 is a photograph of the fiber filaments after the peak grinding treatment according to example 12 of the present invention;
FIG. 10 is a photograph of the fiber filaments after the peak milling treatment of example 13 of the present invention;
FIG. 11 is a photograph of the fiber filaments after the peak milling treatment according to example 14 of the present invention;
FIG. 12 is a photograph of the fiber filaments after the peak milling treatment of example 15 in accordance with the present invention;
FIG. 13 is a photograph of the filaments of example 16 of the present invention after the peak milling treatment;
FIG. 14 is a photograph of a fiber filament after peak milling treatment according to example 17 of the present invention;
FIG. 15 is a photograph of the filaments of example 18 of the present invention after the peak milling treatment;
FIG. 16 is a photograph of the filaments of example 19 of the present invention after the peak milling treatment;
FIG. 17 is a photograph of the fiber filaments after the peak milling treatment of example 20 of the present invention;
FIG. 18 is a photograph of a fiber filament after peak milling treatment according to example 21 of the present invention;
FIG. 19 is a photograph of the filaments of example 22 of the present invention after the peak milling treatment;
FIG. 20 is a photograph of the fiber filaments after the peak milling treatment of example 23 of the present invention;
FIG. 21 is a photograph of the fiber filaments after the peak-milling treatment of comparative example 1;
FIG. 22 is a schematic view of a peak-grinding treatment apparatus of comparative example 21;
FIG. 23 is a photograph of comparative example 21 fiber filaments after peak milling treatment;
FIG. 24 is a photograph of comparative example 22 after a peak-grind treatment;
FIG. 25 is a photograph of filaments after peak milling treatment of comparative example 23.
Detailed Description
In order to make the technical solutions of the present invention more clearly apparent to those skilled in the art, the following examples are given for illustration. It should be noted that the following examples are not intended to limit the scope of the claimed invention.
The starting materials, reagents or apparatuses used in the following examples are, unless otherwise specified, either commercially available from conventional sources or can be obtained by known methods.
The PHAs used in the following examples and comparative examples were poly-3-hydroxybutyrate-co-4-hydroxybutyrate (P34 HB for short, industrial grade) pellet from Zhuhaimai Producer science and technology Co., ltd; PLA and PBAT were purchased from Jinfa science and technology, inc.
Example 1
Setting and annealing the fiber yarns, namely placing a 5cm long PHA fiber yarn coil material in a 60 ℃ oven for 7 hours; then taking out, storing and annealing for more than 6.5h under the conditions that the humidity is 40% and the temperature is 30 ℃ for later use.
Example 2
Reshaping and annealing the fiber, namely placing the 5cm long PHA and PLA blended fiber coil material in a 60 ℃ oven, and placing for 6.5h; then taking out, storing and annealing for more than 4h under the conditions that the humidity is 40% and the temperature is 30 ℃ for later use.
Example 3
Setting and annealing the fiber yarns, namely placing a PHA, PLA and PBAT blended fiber yarn coil material with the length of 5cm in a 60 ℃ oven, and placing for 6.5 hours; then taking out, storing and annealing for more than 4h under the conditions that the humidity is 40% and the temperature is 30 ℃ for later use.
Example 4
Setting and annealing the fiber yarns, placing a 5cm long PLA fiber yarn coil material in a 60 ℃ oven, and placing for 7 hours; then taking out, storing and annealing for more than 6.5h under the conditions that the humidity is 40% and the temperature is 30 ℃ for later use.
Example 5
Setting and annealing the fiber, namely placing a 5 cm-long PLA and PBAT blended fiber coil in a 60 ℃ oven for 7 hours; then taking out, storing and annealing for more than 6.5h under the conditions that the humidity is 40% and the temperature is 30 ℃ for later use.
Example 6
10% (wt%) of sodium hydroxide solution was prepared, the temperature of the solution was raised to 60 ℃, then one end of the PHA filament winding of example 1 was suspended and immersed in an alkali solution at a depth of 1.0cm, and the peak-shaving effect was observed by sampling every 10 minutes for about 90 minutes. After the peak grinding is finished, one end of the fiber filaments soaked in the alkali liquor obviously forms a sharp cone shape. The peak grinding effect is shown in fig. 3, and one end of the fiber filament has a pointed cone structure. FIG. 2 shows the form before peak grinding, and the two ends of the fiber filament have no taper structure. The condition that the fiber filaments are suspended and soaked in the alkali liquor for peak grinding is shown in figure 1, wherein 1 is a temperature-controllable heater, 2 is a beaker, 3 is the alkali liquor, 4 is a fiber filament coil stock, 5 is a thermometer, and 6 is a rope, the alkali liquor 3 is filled in the beaker 2, then the fiber filament coil stock 4 is fixed by the rope 6 and is placed in the alkali liquor 3, and the temperature is raised and heated by the temperature-controllable heater in the process.
Example 7
20% (wt%) of sodium hydroxide solution was prepared, the temperature of the solution was raised to 60 ℃, then, one end of the PHA filament winding of example 1 was suspended and immersed in an alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-grinding effect. The soaking time was about 60 minutes and the filaments formed a sharp cone shape. The peak grinding effect is shown in fig. 4.
Example 8
20% by weight of sodium hydroxide solution was prepared, the temperature of the solution was raised to 70 ℃ and then one end of the PHA filament coil of example 1 was immersed in a 1.0cm deep suspension in an alkali solution, and a sample was taken every 10 minutes to observe the peak-milling effect. The soaking time was about 30 minutes and the filaments apparently formed a sharp cone shape. The peak grinding effect is shown in fig. 5.
Example 9
12 wt% potassium hydroxide solution was prepared, the solution temperature was raised to 60 deg.C, then one end of the PHA filament coil of example 1 was suspended and soaked in alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-milling effect. The soaking time was about 90 minutes and the filaments formed a sharp cone shape. The peak-grinding effect is shown in fig. 6.
Example 10
25wt% potassium hydroxide solution was prepared, the solution temperature was raised to 60 deg.C, then one end of the PHA filament coil of example 1 was suspended and soaked in alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-milling effect. The soaking time was about 60 minutes and the filaments formed a sharp cone shape. The peak grinding effect is shown in fig. 7.
Example 11
25wt% of potassium hydroxide solution was prepared, the temperature of the solution was raised to 70 ℃ and then one end of the PHA filament winding of example 1 was suspended and immersed in an alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-grinding effect. The soaking time was about 30 minutes and the filaments formed a sharp cone shape. The peak-grinding effect is shown in fig. 8.
Example 12
10% (wt%) of sodium hydroxide solution was prepared, the temperature of the solution was raised to 60 ℃, then one end of the PHA and PLA blended tow of example 2 was suspended and immersed in alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-rub effect. The soaking time was about 85 minutes and the filaments formed a sharp cone. The peak-grinding effect is shown in fig. 9.
Example 13
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 50 minutes and the filaments formed a sharp cone. The peak-grinding effect is shown in fig. 10.
Example 14
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 70 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 25 minutes and the filaments formed a sharp cone. The peak-grinding effect is shown in fig. 11.
Example 15
12 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 85 minutes and the filaments apparently formed a sharp taper. The peak-grinding effect is shown in fig. 12.
Example 16
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 50 minutes and the filaments formed a sharp cone. The peak grinding effect is shown in fig. 13.
Example 17
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 70 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 10 minutes to observe the peak grinding effect. The soaking time was about 30 minutes and the filaments formed a sharp cone shape. The peak grinding effect is shown in fig. 14.
Example 18
10 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 10 minutes to observe the peak grinding effect. The soaking time was about 80 minutes and the filaments formed a sharp cone shape. The peak-grinding effect is shown in fig. 15.
Example 19
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor with the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 50 minutes and the filaments formed a sharp cone. The peak-grinding effect is shown in fig. 16.
Example 20
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 70 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 10 minutes to observe the peak grinding effect. The soaking time was about 25 minutes and the filaments apparently formed a sharp cone shape. The peak grinding effect is shown in fig. 17.
Example 21
12 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor with the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 85 minutes and the filaments apparently formed a sharp taper. The peak-grinding effect is shown in fig. 18.
Example 22
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor with the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time was about 50 minutes and the filaments apparently formed a sharp cone shape. The peak-grinding effect is shown in fig. 19.
Example 23
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 70 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 10 minutes to observe the peak grinding effect. The soaking time was about 25 minutes and the filaments formed a sharp cone. The peak grinding effect is shown in fig. 20.
The main parameters of the peak milling method of examples 6-23 are shown in table 1 below.
TABLE 1 Main operating parameters of the Peak grinding method of the examples
| Examples | Kind of alkali liquor | Alkali liquor concentration wt% | Temperature of solution (. Degree.C.) | Soaking time | Fiber yarn | |
| 6 | Sodium hydroxide | 10 | 60 | 90 | Example 1 | |
| 7 | Sodium hydroxide | 20 | 60 | 60 | Example 1 | |
| 8 | Sodium hydroxide | 20 | 70 | 30 | Example 1 | |
| 9 | Potassium hydroxide | 12 | 60 | 90 | Example 1 | |
| 10 | Potassium hydroxide | 25 | 60 | 60 | Example 1 | |
| 11 | Potassium hydroxide | 25 | 70 | 30 | Example 1 | |
| 12 | Sodium hydroxide (NaOH) | 10 | 60 | 85 | Example 2 | |
| 13 | Sodium hydroxide (NaOH) | 20 | 60 | 50 | Example 2 | |
| 14 | Sodium hydroxide (NaOH) | 20 | 70 | 25 | Example 2 | |
| 15 | Potassium hydroxide | 12 | 60 | 85 | Example 2 | |
| 16 | Potassium hydroxide | 25 | 60 | 50 | Example 2 | |
| 17 | Potassium hydroxide | 25 | 70 | 30 | Example 2 | |
| 18 | Sodium hydroxide (NaOH) | 10 | 60 | 80 | Example 3 | |
| 19 | Sodium hydroxide (NaOH) | 20 | 60 | 50 | Example 3 | |
| 20 | Sodium hydroxide | 20 | 70 | 25 | Example 3 | |
| 21 | Potassium hydroxide | 12 | 60 | 85 | Example 3 | |
| 22 | Potassium hydroxide | 25 | 60 | 50 | Example 3 | |
| 23 | Potassium hydroxide | 25 | 70 | 25 | Example 3 |
Comparative example 1
Preparing 20wt% of sodium hydroxide solution, heating the solution to 60 ℃, then suspending and soaking one end of the PHA filament winding material in 1.0cm of depth in alkali liquor, and sampling every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together. As shown in fig. 21.
Comparative example 2
Preparing 20 percent (wt%) of sodium hydroxide solution, heating the solution to 60 ℃, then suspending and soaking one end of the PHA and PLA blended cellosilk roll material in alkali liquor at the depth of 1.0cm, sampling every 5 minutes and observing the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 3
Preparing 20 percent (wt%) of sodium hydroxide solution, heating the solution to 60 ℃, then suspending and soaking one end of the blended fiber filament coil material of PHA, PLA and PABT in alkali liquor at the depth of 1.0cm, and sampling every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 4
Preparing 20 percent (wt%) of sodium hydroxide solution, heating the solution to 60 ℃, then hanging and soaking one end of the PLA fiber filament roll material in alkali liquor at the depth of 1.0cm, and sampling every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 5
Preparing 20 percent (wt%) of sodium hydroxide solution, heating the solution to 60 ℃, then suspending and soaking one end of the PLA and PABT blended cellosilk roll material in alkali liquor at the depth of 1.0cm, sampling every 5 minutes and observing the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 6
20% (wt%) sodium hydroxide solution was prepared, the temperature of the solution was raised to 85 ℃, then one end of the PHA filament winding of example 1 was suspended and immersed in an alkali solution at a depth of 1.0cm, and a sample was taken every 5 minutes to observe the peak-grinding effect. The soaking time is about 10 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 7
Preparing 45 percent (wt%) of sodium hydroxide solution, raising the temperature of the solution to 60 ℃, then hanging and soaking one end of the PLA fiber filament roll material of the example 4 in alkali liquor at the depth of 1.0cm, sampling every 5 minutes and observing the peak grinding effect. The soaking time is about 10 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 8
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then, one end of the PLA fiber filament coil stock of the example 4 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 9
45 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 10
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 11
45 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 12
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor with the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 13
45 wt% potassium hydroxide solution was prepared, the solution temperature was raised to 60 deg.C, then one end of the PHA filament coil of example 1 was suspended and soaked in alkali solution at a depth of 1.0cm, and a sample was taken every 5 minutes to observe the peak-milling effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 14
25wt% potassium hydroxide solution was prepared, the solution temperature was raised to 85 deg.C, then one end of the PHA filament coil of example 1 was suspended and soaked in alkali solution at a depth of 1.0cm, and a sample was taken every 10 minutes to observe the peak-milling effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 15
45 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PLA fiber filament coil stock of the example 4 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 16
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then one end of the PLA fiber filament winding material of the embodiment 4 is hung and soaked in alkali liquor with the depth of 1.0cm, and the peak grinding effect is observed by sampling every 5 minutes. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 17
45 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 18
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then, one end of the PHA and PLA blended fiber filament coil material of the example 2 is hung and soaked in alkali liquor at the depth of 1.0cm, and a sample is taken every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 19
45 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor with the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
Comparative example 20
25 percent (wt%) of potassium hydroxide solution is prepared, the temperature of the solution is raised to 85 ℃, then one end of the PHA, PLA and PBAT blended cellosilk roll material of the example 3 is hung and soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 5 minutes to observe the peak grinding effect. The soaking time is about 15 minutes, the fiber filaments are agglomerated, the soda foam position is whitish, and the filaments are bonded together.
COMPARATIVE EXAMPLE 21 (non-suspended mode)
20wt% sodium hydroxide solution was prepared, the solution temperature was raised to 60 deg.C, then the PHA filament coil of example 1 was placed on a support grid, one end of the filament coil was immersed in alkali solution at a depth of 1.0cm, the peak-milling effect was observed every 10 minutes, and the immersion time was about 65 minutes. After the peak grinding is finished, the tail end of the fiber yarn coil stock soaked in the alkali liquor forms a sharp cone shape, but the sharp yarn part is bent at the position directly contacted with the supporting net rack. The schematic diagram of the peak grinding process is shown in FIG. 22, in which FIG. 22 shows a temperature-controllable heater 1, a support net rack 2, a beaker 3, an alkali solution 4, a fiber reel 5, and a thermometer 6. Firstly, filling alkali liquor 4 in a beaker 3, placing a fiber yarn roll 5 on a support net rack 2, soaking one end of the roll material in the alkali liquor with the depth of 1.0cm, then heating by using a temperature-controllable heater 1, and monitoring by using a thermometer. The fiber filaments after peak grinding are shown in fig. 23.
COMPARATIVE EXAMPLE 22 (non-suspended mode)
20 percent (wt%) of sodium hydroxide solution is prepared, the temperature of the solution is raised to 60 ℃, then, the PHA and PLA blended cellosilk roll material of the example 2 is placed on a supporting net frame, one end of the roll material is soaked in alkali liquor at the depth of 1.0cm, and sampling is carried out every 10 minutes to observe the peak grinding effect. The soaking time is about 60 minutes, the fiber filaments obviously form a sharp cone shape, but the sharp filament part is bent at the position directly contacted with the support net frame. As shown in fig. 24.
COMPARATIVE EXAMPLE 23 (non-suspended mode)
Preparing 20 percent (wt%) of sodium hydroxide solution, heating the solution to 60 ℃, then placing the PHA, PLA and PABT blended cellosilk roll material of the example 3 on a supporting net frame, immersing one end of the roll material in alkali liquor at the depth of 1.0cm, sampling every 10 minutes and observing the peak grinding effect. The soaking time was about 55 minutes, and the filaments formed a sharp cone shape, but where they were in direct contact with the support frame, the sharp filament portion was bent. As shown in fig. 25.
The operating parameters of the peak milling process for comparative examples 1-23 are shown in the table below.
TABLE 2 Peak milling Process operating parameters for respective proportions
Product effectiveness testing
1. Mechanical properties and crystallinity of filaments before and after annealing
(1) Determination of tensile strength and elongation at break of GB/T1040-2006 tensile Properties of plastics;
(2) Differential Scanning Calorimetry (DSC).
The mechanical properties and crystallinity of the filaments of examples 1 to 5 were measured before and after the annealing treatment, and the results are shown in table 3 below.
TABLE 3 mechanical Properties and crystallinity of the filaments before and after annealing
The test results in table 3 show that the tensile strength, the elongation at break and the crystallinity of the annealed fiber are improved, and the annealed fiber can be better applied to the subsequent peak grinding process, and when the annealed fiber is soaked in alkali liquor, the material can be prevented from softening due to the fact that the material is quickly permeated and swelled by a solvent or alkali liquor, and the material is subjected to hydrolysis reaction inside, so that the fiber and the fiber are finally bonded and agglomerated, and straight tapered fiber cannot be formed. The fiber yarn after peak grinding has good strength and toughness, no bonding and agglomeration occur between the yarn and the yarn, and straight cone-shaped fiber yarn can be obtained.
2. Grinding peak treatment results
FIGS. 2-20 are fiber filaments after peak grinding in examples 6-23 of the present invention. As can be seen from the figure, one end of the fiber filament has a tapered structure, and the whole fiber filament is straight.
Fig. 21 is a fiber yarn after the peak grinding treatment of comparative example 1, fig. 21 (a) is a photograph of the bottom after the peak grinding, and whitish appears, and fig. 21 (b) is a fiber yarn after the peak grinding, and the yarn is bonded and agglomerated.
FIGS. 23 to 25 show the fiber filaments after the peak-ground treatment in comparative examples 21 to 23, in which the fiber filaments were formed into a pointed cone shape, but the pointed filaments were bent at the portions directly contacting the support net frame, and thus straight pointed cone-shaped filaments could not be obtained.
3. Mechanical properties of milled filaments
TABLE 4 mechanical Properties of the milled filaments
As can be seen from the above table, the fiber filaments after the peak grinding treatment of the present invention can still maintain high tensile strength and elongation at break. Whereas the filaments of comparative examples 1-20 were bonded together, it was difficult to measure their mechanical properties.
Claims (10)
1. The peak grinding process is characterized by comprising the following steps of:
(1) Annealing the material to be treated, and standing to obtain the annealed material;
(2) Soaking the material annealed in the step (1) in alkali liquor;
in the step (1), the material to be treated is immersed into alkali liquor in a suspension mode;
in the step (2), the temperature of the alkali liquor is 35-80 ℃; the mass fraction of the alkali liquor is 8-40wt%.
2. The peak grinding process according to claim 1, wherein in the step (1), the annealing treatment comprises the following steps:
pretreating the material to be treated for 2-12h at 40-80 deg.C, taking out, and annealing at 25-30 deg.C and relative humidity of 30-50% for more than 4 h.
3. The peak grinding process according to claim 1, wherein the material to be treated is a degradable material.
4. The peak grinding process according to claim 3, wherein the degradable material is one or more of polyhydroxyalkanoate, polylactic acid, and polybutylene adipate/terephthalate.
5. The peak grinding process according to claim 1, wherein in the step (2), the temperature of the alkali liquor is 60-70 ℃; the mass fraction of the alkali liquor is 10-25wt%.
6. The peak grinding process according to claim 1, wherein the alkali solution is one or more of a sodium hydroxide solution, a potassium hydroxide solution and a sodium carbonate solution.
7. The peak grinding process according to claim 6, wherein the alkali liquor is a sodium hydroxide solution, and the mass fraction of the sodium hydroxide solution is 10-30wt%.
8. The peak grinding process according to claim 6, wherein the alkali liquor is a potassium hydroxide solution, and the mass fraction of the potassium hydroxide solution is 10-40wt%.
9. Use of the peak milling process according to any one of claims 1 to 8 for the preparation of a fibre filament.
10. A filament, comprising the peak grinding process according to any one of claims 1 to 8, wherein at least one end of the filament is tapered, and the tensile strength of the filament is not lower than 355.86MPa.
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