CN111101208A - Preparation method of inorganic solvent wet spinning acrylic fibers - Google Patents
Preparation method of inorganic solvent wet spinning acrylic fibers Download PDFInfo
- Publication number
- CN111101208A CN111101208A CN201811246832.6A CN201811246832A CN111101208A CN 111101208 A CN111101208 A CN 111101208A CN 201811246832 A CN201811246832 A CN 201811246832A CN 111101208 A CN111101208 A CN 111101208A
- Authority
- CN
- China
- Prior art keywords
- range
- extrusion
- spinning
- spinneret
- speed
- 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.)
- Pending
Links
- 229920002972 Acrylic fiber Polymers 0.000 title claims abstract description 17
- 238000002166 wet spinning Methods 0.000 title claims abstract description 11
- 239000003049 inorganic solvent Substances 0.000 title claims abstract description 10
- 229910001867 inorganic solvent Inorganic materials 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract description 52
- 238000009987 spinning Methods 0.000 claims abstract description 35
- 238000009998 heat setting Methods 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 24
- 230000001112 coagulating effect Effects 0.000 claims description 17
- VGTPCRGMBIAPIM-UHFFFAOYSA-M sodium thiocyanate Chemical compound [Na+].[S-]C#N VGTPCRGMBIAPIM-UHFFFAOYSA-M 0.000 claims description 17
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 15
- 238000000280 densification Methods 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 9
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 5
- SZHIIIPPJJXYRY-UHFFFAOYSA-M sodium;2-methylprop-2-ene-1-sulfonate Chemical compound [Na+].CC(=C)CS([O-])(=O)=O SZHIIIPPJJXYRY-UHFFFAOYSA-M 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 3
- 238000010622 cold drawing Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010409 ironing Methods 0.000 abstract 1
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 230000015271 coagulation Effects 0.000 description 16
- 238000005345 coagulation Methods 0.000 description 16
- 239000007921 spray Substances 0.000 description 4
- HGINCPLSRVDWNT-UHFFFAOYSA-N acrylaldehyde Natural products C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000003960 organic solvent Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- -1 Acrylonitrile Methacrylic acid methyl ester Vinyl acetate ester Chemical class 0.000 description 1
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012792 core layer Substances 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000002522 swelling effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/253—Formation of filaments, threads, or the like with a non-circular cross section; Spinnerette packs therefor
-
- 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
- D01F6/28—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/38—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds comprising unsaturated nitriles as the major constituent
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The invention relates to a preparation method of inorganic solvent wet spinning acrylic fiber. The method comprises the following steps: dissolving raw materials by an inorganic solvent, carrying out spinning extrusion, carrying out solidification bath forming twice, densifying, carrying out heat setting and the like. The acrylic fiber prepared by the method is applied to the field of fur, has lower ironing temperature, and simultaneously, the manufactured fur has soft hand feeling and good stiffness.
Description
Technical Field
The invention belongs to the field of acrylic fiber preparation, and particularly relates to a preparation method of an inorganic solvent wet spinning process of acrylic fibers with soft hand feeling and fiber stiffness.
Background
The flat acrylic fibers have a relatively large aspect ratio, generally more than 5, so that the fibers have good softness and are the main raw materials for producing fur. In China, patents on the production of flat acrylon are more, for example, patent CN205062255U describes a method for producing the flat acrylon by an organic solvent dry method, and patent CN103882547B describes a method for producing the flat acrylon by an organic solvent dimethylacetamide wet spinning method. While the patent on producing the flat acrylic fiber by the inorganic solvent wet spinning process is less, in the related prior art, the sodium thiocyanate inorganic solvent wet spinning is mainly used, and the flat acrylic fiber product is gradually matured. Particularly, due to the characteristics of the inorganic solvent wet spinning process, the flat acrylic fibers are popular in the market because the hot polishing temperature is lower than that of products produced by spinning with an organic solvent in the subsequent application. However, the flat acrylic fibers with different deniers are used for different types of furs, so that the market demands for fibers are different. The coarse denier product has thicker fiber, so that the flexibility and the drapability of the fiber are mainly improved. And the fine denier flat product has reduced fiber stiffness, and the prepared fur is relatively collapsed, so that the appearance and the hand feeling of the product are influenced.
Disclosure of Invention
The invention aims to provide a preparation method of inorganic solvent wet spinning acrylic fibers. The acrylic fibers prepared by the method have soft hand feeling and good stiffness. Specifically, the method comprises the following steps:
(1) dissolving polyacrylonitrile polymer in sodium thiocyanate aqueous solution by a dissolving machine;
wherein, the polyacrylonitrile polymer comprises acrylonitrile with the content range of 85-95 percent, methyl methacrylate or vinyl acetate with the content range of 15-5 percent, and sodium methallyl sulfonate with the content of less than 1 percent; the viscosity average molecular weight of the polyacrylonitrile polymer is 4.5-6.5 ten thousand, and the concentration range of the sodium thiocyanate aqueous solution is 40-60 percent;
(2) the spinning solution is defoamed and filtered, is metered by a spinning metering pump and then is extruded through a spinneret orifice extrusion hole, the length-width ratio range of the spinneret orifice extrusion hole is 1-10, the extrusion hole is approximately rectangular, the length-width ratio range is 2-15, the hole length of the extrusion hole is more than 0.1mm, and the number of the spinneret holes is 10000-30000;
(3) the spinning solution is extruded by a spinneret plate and then enters a coagulating bath to form nascent fiber, the speed of a guide roller at the outlet of the coagulating bath and the extrusion speed of the spinneret plate are adjusted, the variation range of the ratio of the extrusion speed of the spinning solution to the traction speed of the guide roller is 1.0-2.5, the temperature range of the coagulating bath is controlled to be-3-5 ℃, and the concentration range is 11.0-14.5%;
(4) the fiber obtained in the step (3) enters a secondary coagulating bath for forming, and then cold drawing, water washing and hot drawing are carried out, wherein the total drawing multiplying power is less than or equal to 14;
(5) carrying out hot drying densification treatment on the fiber obtained in the step (4), wherein the wet bulb temperature range is 60-80 ℃, and the dry bulb temperature range is 120-150 ℃;
(6) and (4) carrying out heat setting on the fibers obtained in the step (5), wherein the heat setting temperature range is 100-130 ℃, and obtaining the acrylic fiber product.
Preferably, in the step (1), the concentration of the sodium thiocyanate aqueous solution is in the range of 50-60%.
Preferably, in the step (2), the length-width ratio of the extrusion hole of the spinneret plate orifice is in a more preferable range of 4-14, the length-width ratio of the extrusion hole of the spinneret plate orifice is in a more preferable range of 1-5, and the hole length of the extrusion hole of the spinneret plate is greater than 0.3 mm.
Preferably, in the step (3), the ratio of the extrusion speed of the spinning solution to the drawing speed of the guide roll is varied within a range of 1.5 to 2.5.
In the step (1), in order to ensure a better dissolving effect, the sodium thiocyanate solvent needs to be heated to more than 75 ℃. Methyl methacrylate or vinyl acetate mainly has the effects of reducing the regularity of a high molecular chain, reducing the rigidity of molecules and increasing the hand feeling of fibers. The sodium methallyl sulfonate mainly has the function of increasing dyeing sites, so that the fiber is easier to dye.
In the step (2), the spinning solution with the polymer content of 7 wt% -12 wt% is prepared after dissolution. The spinning solution is defoamed, filtered, adjusted in temperature and pressure, then fed into the inlet of a spinning metering pump, and metered by the metering pump and then extruded from a spinneret orifice. The aspect ratios of the pores are different, and the aspect ratios of the fibers are different under the same spinning conditions. The larger the aspect ratio of the spinneret extrusion orifice, the greater the flatness of the fiber, but too large is detrimental to the spin-forming. The extrusion hole aspect ratio of the spray hole is small, and the larger aspect ratio is not beneficial to the flowing of the slurry, thereby influencing the spinning formation. The length of the hole needs to be kept in a proper size, the hole is too long, and the processing difficulty of the spray hole is high; too small hole length is not favorable for macromolecule stress relaxation, and too large extrusion swelling effect is not favorable for controlling fiber shape. The length-width ratio of the extrusion holes of the spray holes of the spinneret plate is 2-15, preferably 4-14, and the length-width ratio of the extrusion holes of the spray holes is 1-10, preferably 1-5. To reduce stress, the length of the extrusion orifice is greater than 0.1mm, preferably greater than 0.3 mm. The number of holes of the spinneret plate is 10000-30000.
In the step (3), the temperature of the coagulating bath is controlled to be-3-5 ℃, and the concentration is 11.0-14.5%. The concentration is too high, the spinning forming is slow, and the slurry stagnation at the spinneret plate is obvious; the spinning forming is too fast, the fiber skin core layer is obvious, and the powder is increased. The temperature is too high, the forming is fast, and the powder is increased; if the temperature is too low, the forming is slow, and the slurry is easy to stagnate. The ratio of the extrusion speed of the solution from the spinneret plate to the drawing speed of the guide roll is 1.0-2.5, for example, the ratio for producing fibers with higher flatness is 1.1-1.4, and the more preferable ratio in the patent is 1.5-2.5.
Compared with the prior art, the invention has the beneficial effects that the sodium thiocyanate wet spinning process is adopted, and the prepared acrylic fiber has the advantages of soft hand feeling, good stiffness, lower lustring temperature and better market prospect.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Table 1 shows the composition ratios of the polyacrylonitrile polymers selected in each of examples 1 to 8.
TABLE 1
Examples | Acrylonitrile | Methacrylic acid methyl ester | Vinyl acetate ester | Sodium methallyl sulfonate |
Example 1 | 85 | 15 | 0.9 | |
Example 2 | 87 | 13 | 0.8 | |
Example 3 | 89 | 11 | 0.7 | |
Example 4 | 90 | 10 | 0.5 | |
Example 5 | 92 | 8 | 0.6 | |
Example 6 | 93 | 7 | 0.2 | |
Example 7 | 95 | 5 | 0.4 | |
Example 8 | 95 | 3 | 2 | 0.1 |
Example 1
Polyacrylonitrile polymer was dissolved in heated 60% aqueous sodium thiocyanate solution to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 3.0, and the length-width ratio of the extrusion hole is 12. The temperature of the coagulation bath is 4 ℃, and the concentration is 13.0%. The ratio of extrusion speed to guide roll speed was 2.3. The wet-bulb temperature of the hot drying densification treatment is 60 ℃, the dry-bulb temperature is 120 ℃, and the heat setting temperature is 100 ℃. The coagulation bath was well formed, and 5.55dtex oval shaped fibers with an aspect ratio of 2:1 were obtained.
Example 2
Polyacrylonitrile polymer was dissolved in a heated 50% aqueous solution of sodium thiocyanate to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 1.0, and the length-width ratio of the extrusion hole is 4.0. The temperature of the coagulation bath is 4 ℃, and the concentration is 13.0%. The ratio of extrusion speed to guide roll speed was 1.5. The wet-bulb temperature of the hot drying densification treatment is 80 ℃, the dry-bulb temperature is 150 ℃, and the heat setting temperature is 130 ℃. The coagulation bath was well formed, and 3.33dtex oval shaped fibers having an aspect ratio of 1.5:1 were obtained.
Example 3
Polyacrylonitrile polymer was dissolved in a heated 50% aqueous solution of sodium thiocyanate to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 5.0, and the length-width ratio of the extrusion hole is 14.0. The temperature of the coagulation bath is 0 ℃, and the concentration is 14.5%. The ratio of extrusion speed to guide roll speed was 1.5. The wet-bulb temperature of the hot drying densification treatment is 70 ℃, the dry-bulb temperature is 135 ℃, and the heat setting temperature is 120 ℃. The coagulation bath was well formed, and 7.77dtex oval shaped fibers with an aspect ratio of 5:1 were obtained.
Example 4
Polyacrylonitrile polymer was dissolved in a heated 56% aqueous solution of sodium thiocyanate to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 2.0, and the length-width ratio of the extrusion hole is 8.0. The temperature of the coagulation bath is 3 ℃, and the concentration is 14.0%. The ratio of extrusion speed to guide roll speed was 1.7. The wet-bulb temperature of the hot drying densification treatment is 75 ℃, the dry-bulb temperature is 130 ℃, and the heat setting temperature is 120 ℃. The coagulation bath was well formed, and 4.44dtex oval shaped fibers with an aspect ratio of 3:1 were obtained.
Example 5
Polyacrylonitrile polymer was dissolved in heated 40% aqueous sodium thiocyanate solution to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 5.0, and the length-width ratio of the extrusion hole is 15. The temperature of the coagulation bath is-2 ℃ and the concentration is 11.0 percent. The ratio of extrusion speed to guide roll speed was 2.0. The wet-bulb temperature, dry-bulb temperature and heat-setting temperature of the heat-drying densification treatment were the same as in example 1. The coagulation bath was well formed, and 5.55dtex oval shaped fibers with an aspect ratio of 2:1 were obtained.
Example 6
Polyacrylonitrile polymer was dissolved in a heated 50% aqueous solution of sodium thiocyanate to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 8.0, and the length-width ratio of the extrusion hole is 2.0. The temperature of the coagulation bath is 1 ℃, and the concentration is 12.0%. The ratio of extrusion speed to guide roll speed was 1.5. The wet-bulb temperature, dry-bulb temperature and heat-setting temperature of the heat-drying densification treatment were the same as in example 2. The coagulation bath was well formed, and 3.33dtex oval shaped fibers having an aspect ratio of 1.5:1 were obtained.
Example 7
Polyacrylonitrile polymer was dissolved in heated 60% aqueous sodium thiocyanate solution to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 10.0, and the length-width ratio of the extrusion hole is 10.0. The temperature of the coagulation bath is 5 ℃, and the concentration is 11.5%. The ratio of extrusion speed to guide roll speed was 2.5. The wet-bulb temperature, dry-bulb temperature and heat-setting temperature of the heat-drying densification treatment were the same as in example 3. The coagulation bath was well formed, and 7.77dtex oval shaped fibers with an aspect ratio of 5:1 were obtained.
Example 8
Polyacrylonitrile polymer was dissolved in heated 40% aqueous sodium thiocyanate solution to form a homogeneous dope. The spinning solution is defoamed, filtered, injected into a spinneret plate by a spinning metering pump, extruded into a coagulating bath through a special-shaped nozzle of the spinneret plate for forming, wherein the length-width ratio of an extrusion hole of the special-shaped nozzle is 1.0, and the length-width ratio of the extrusion hole is 5.0. The temperature of the coagulation bath is-3 ℃ and the concentration is 12.5 percent. The ratio of extrusion speed to guide roll speed was 1.0. The wet-bulb temperature, dry-bulb temperature and heat-setting temperature of the heat-drying densification treatment were the same as in example 4. The coagulation bath was well formed, and 4.44dtex oval shaped fibers with an aspect ratio of 3:1 were obtained.
Claims (4)
1. The preparation method of the inorganic solvent wet spinning acrylic fiber is characterized by comprising the following steps:
(1) dissolving polyacrylonitrile polymer in sodium thiocyanate aqueous solution by a dissolving machine;
wherein, the polyacrylonitrile polymer comprises acrylonitrile with the content range of 85-95 percent, methyl methacrylate or vinyl acetate with the content range of 15-5 percent, and sodium methallyl sulfonate with the content of less than 1 percent; the viscosity average molecular weight of the polyacrylonitrile polymer is 4.5-6.5 ten thousand, and the concentration range of the sodium thiocyanate aqueous solution is 40-60 percent;
(2) the spinning solution is defoamed and filtered, is metered by a spinning metering pump and then is extruded through a spinneret orifice extrusion hole, the length-width ratio range of the spinneret orifice extrusion hole is 1-10, the extrusion hole is approximately rectangular, the length-width ratio range is 2-15, the hole length of the extrusion hole is more than 0.1mm, and the number of the spinneret holes is 10000-30000;
(3) the spinning solution is extruded by a spinneret plate and then enters a coagulating bath to form nascent fiber, the speed of a guide roller at the outlet of the coagulating bath and the extrusion speed of the spinneret plate are adjusted, the variation range of the ratio of the extrusion speed of the spinning solution to the traction speed of the guide roller is 1.0-2.5, the temperature range of the coagulating bath is controlled to be-3-5 ℃, and the concentration range is 11.0-14.5%;
(4) the fiber obtained in the step (3) enters a secondary coagulating bath for forming, and then cold drawing, water washing and hot drawing are carried out, wherein the total drawing multiplying power is less than or equal to 14;
(5) carrying out hot drying densification treatment on the fiber obtained in the step (4), wherein the wet bulb temperature range is 60-80 ℃, and the dry bulb temperature range is 120-150 ℃;
(6) and (4) carrying out heat setting on the fibers obtained in the step (5), wherein the heat setting temperature range is 100-130 ℃, and obtaining the acrylic fiber product.
2. The method of claim 1, wherein in step (1), the concentration of the aqueous sodium thiocyanate solution is in the range of 50% to 60%.
3. The method of claim 1, wherein in step (2), the spinneret orifice extrusion orifice aspect ratio is preferably in the range of 4 to 14, the spinneret orifice extrusion orifice aspect ratio is preferably in the range of 1 to 5, and the spinneret extrusion orifice has an orifice length greater than 0.3 mm.
4. The method of claim 1, wherein in step (3), the ratio of the extrusion speed of the spinning solution to the pulling speed of the guide roll varies from 1.5 to 2.5.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811246832.6A CN111101208A (en) | 2018-10-25 | 2018-10-25 | Preparation method of inorganic solvent wet spinning acrylic fibers |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811246832.6A CN111101208A (en) | 2018-10-25 | 2018-10-25 | Preparation method of inorganic solvent wet spinning acrylic fibers |
Publications (1)
Publication Number | Publication Date |
---|---|
CN111101208A true CN111101208A (en) | 2020-05-05 |
Family
ID=70418151
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811246832.6A Pending CN111101208A (en) | 2018-10-25 | 2018-10-25 | Preparation method of inorganic solvent wet spinning acrylic fibers |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN111101208A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116334778A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1566421A (en) * | 2003-06-12 | 2005-01-19 | 中国石油化工股份有限公司 | Flameproof polyacrylonitrile fibre and method for preparing same |
CN101240462A (en) * | 2008-03-14 | 2008-08-13 | 东华大学 | Method for preparing acrylics-protein-copper salt composite antistatic fiber |
CN101445967A (en) * | 2008-12-12 | 2009-06-03 | 浙江杭州湾腈纶有限公司 | Preparation method of flat acrylic fiber |
CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
CN103205821A (en) * | 2013-04-27 | 2013-07-17 | 东华大学 | Preparation method of moisture-absorption flat polyacrylonitrile fiber |
CN103668532A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl acetate |
US20140106167A1 (en) * | 2012-10-17 | 2014-04-17 | The University Of Kentucky Research Foundation | Method for hybrid dry-jet gel spinning and fiber produced by that method |
CN104562270A (en) * | 2013-10-11 | 2015-04-29 | 中国石油化工股份有限公司 | Wet spinning method for improving acrylic fiber glossiness |
CN104862828A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | High thermal conductivity carbon fiber and preparation method thereof |
US20160153121A1 (en) * | 2013-07-12 | 2016-06-02 | The University Of Tokyo | Flame resistant polymer, polymer solution, flame resistant fiber, carbon fiber, and methods of producing same |
CN106498515A (en) * | 2016-10-31 | 2017-03-15 | 朱锦 | High speed acrylic spinning technique |
-
2018
- 2018-10-25 CN CN201811246832.6A patent/CN111101208A/en active Pending
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1566421A (en) * | 2003-06-12 | 2005-01-19 | 中国石油化工股份有限公司 | Flameproof polyacrylonitrile fibre and method for preparing same |
CN101240462A (en) * | 2008-03-14 | 2008-08-13 | 东华大学 | Method for preparing acrylics-protein-copper salt composite antistatic fiber |
CN101445967A (en) * | 2008-12-12 | 2009-06-03 | 浙江杭州湾腈纶有限公司 | Preparation method of flat acrylic fiber |
CN101922059A (en) * | 2010-08-17 | 2010-12-22 | 东华大学 | Production process of colored flat acrylic fiber and production line thereof |
CN103668532A (en) * | 2012-09-25 | 2014-03-26 | 中国石油化工股份有限公司 | Method for preparing anti-pilling acrylic fibers from acrylonitrile and vinyl acetate |
US20140106167A1 (en) * | 2012-10-17 | 2014-04-17 | The University Of Kentucky Research Foundation | Method for hybrid dry-jet gel spinning and fiber produced by that method |
CN103205821A (en) * | 2013-04-27 | 2013-07-17 | 东华大学 | Preparation method of moisture-absorption flat polyacrylonitrile fiber |
US20160153121A1 (en) * | 2013-07-12 | 2016-06-02 | The University Of Tokyo | Flame resistant polymer, polymer solution, flame resistant fiber, carbon fiber, and methods of producing same |
CN104562270A (en) * | 2013-10-11 | 2015-04-29 | 中国石油化工股份有限公司 | Wet spinning method for improving acrylic fiber glossiness |
CN104862828A (en) * | 2015-04-09 | 2015-08-26 | 浙江泰索科技有限公司 | High thermal conductivity carbon fiber and preparation method thereof |
CN106498515A (en) * | 2016-10-31 | 2017-03-15 | 朱锦 | High speed acrylic spinning technique |
Non-Patent Citations (1)
Title |
---|
沈新元: "《化学纤维手册》", 30 September 2008, 中国纺织出版社 * |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116334778A (en) * | 2023-05-26 | 2023-06-27 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
CN116334778B (en) * | 2023-05-26 | 2023-07-21 | 吉林富博纤维研究院有限公司 | Preparation method of high-performance PAN-based carbon fiber precursor |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN101492837B (en) | Process for producing bacteria cellulose fibre with high degree of polymerization | |
CN102493016B (en) | Porous superfine polyamide 6 fully-drawn yarn, preparation method thereof, and equipment thereof | |
CN106555240B (en) | Preparation method of high-performance polyethylene fiber and fiber | |
CN1536107A (en) | Preparation method of polyacrylonitrile carbon raw yarn | |
CN101240468A (en) | Polyacrylonitrile-chitin composite fiber and its production process | |
WO2016127833A1 (en) | Acetic nitrile fibre and preparation method therefor | |
CN105463607A (en) | Manufacturing method for 48K polyacrylonitrile-based carbon fiber precursor | |
CN103882547A (en) | Flat acrylic fiber and production method thereof | |
JP2022519806A (en) | Flame-retardant cellulosic fiber and its preparation method | |
CN103184582B (en) | Preparation method of PVA composite high-strength high-modulus cellulose fiber | |
CN103603070A (en) | Preparation method of high-comfort triangular hollow microporous fiber | |
CN104831392A (en) | High-strength low-elongation viscose and preparing method thereof | |
CN101240466B (en) | Solvent method cellulose cotton and bamboo composite fiber and preparation method thereof | |
CN106048741A (en) | Method for preparing cellulose fibers by dry-wet spinning | |
CN102453972B (en) | Preparation method of polyacrylonitrile precursor | |
CN104562270A (en) | Wet spinning method for improving acrylic fiber glossiness | |
CN111101208A (en) | Preparation method of inorganic solvent wet spinning acrylic fibers | |
CN104846453A (en) | Superfine viscose fiber and preparation method thereof | |
CN110835786B (en) | Preparation method of flat acrylic fiber | |
CN110699762B (en) | Preparation method of polyacrylonitrile spinning solution and preparation method of polyacrylonitrile fibers | |
CN110230130B (en) | Preparation method of high-strength medium-modulus carbon fiber precursor | |
CN106435802A (en) | Acrylic fibers with peanut-shaped cross section and production method thereof | |
CN102851756A (en) | Polyacrylonitrile fiber stretching method | |
CN103668532B (en) | Utilize the method that acrylonitrile and vinylacetate prepare anti-pilling acrylic fiber | |
CN102154723B (en) | Method for preparing polyacrylonitrile-based carbon fiber precursors without skin-core structure |
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 | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200505 |
|
RJ01 | Rejection of invention patent application after publication |