CN110629300A - Preparation method of continuous filament bundle phenolic fiber - Google Patents
Preparation method of continuous filament bundle phenolic fiber Download PDFInfo
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- CN110629300A CN110629300A CN201910817341.0A CN201910817341A CN110629300A CN 110629300 A CN110629300 A CN 110629300A CN 201910817341 A CN201910817341 A CN 201910817341A CN 110629300 A CN110629300 A CN 110629300A
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- Prior art keywords
- phenolic
- fiber
- solution
- continuous filament
- crosslinking
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Classifications
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- 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
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- 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
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- 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
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- 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
- D01D5/12—Stretch-spinning methods
- D01D5/14—Stretch-spinning methods with flowing liquid or gaseous stretching media, e.g. solution-blowing
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- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/16—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds as constituent
Abstract
The invention relates to a preparation method of continuous filament bundle phenolic fiber, belonging to the technical field of phenolic fiber preparation methods, solving the technical problems of melt spinning process in engineering amplification and large-scale production, and the solution is as follows: by utilizing the characteristic that thermosetting phenolic resin is further crosslinked and cured by heating, the thermosetting phenolic resin is prepared into spinning solution, then the spinning solution, the coagulating bath forming and the drafting are carried out to obtain phenolic resin protofilaments, and the phenolic fibers can be obtained after the heating crosslinking and curing. The invention can prepare the long-tow phenolic fiber which is difficult to prepare by the traditional melt spinning process, and has the advantages of continuous process, easy engineering amplification, energy saving, environmental protection, low requirements on personnel protection and equipment corrosion prevention and the like.
Description
Technical Field
The invention relates to a preparation method of continuous filament bundle fibers, in particular to a novel process for preparing the filament bundle phenolic fibers by spinning a phenolic resin solution.
Background
The phenolic fiber is a special fiber integrating multiple functions of temperature resistance, heat insulation, flame retardance, corrosion resistance, sound insulation and the like. The flame-retardant coating has wide application prospect in the application fields of flame retardance, high-temperature thermal protection, heat preservation and insulation, sound insulation, chemical protection, high-grade indoor flame-retardant decorative materials such as airplanes and submarines and the like, and is monopolized by Kynol company internationally.
At present, the production process of phenolic fiber manufacturers and the test process of scientific research institutions are both focused on the melt spinning process, and due to the limitation of the process method and the structural characteristics of resin, the melt spinning is only suitable for preparing chopped fibers with certain length, and the prepared fibers have lower performance. Although the phenolic fiber prepared by the melt spinning process is improved in multiple ways, the phenolic fiber is still brittle, poor in toughness and low in mechanical property, certain difficulty is brought to the subsequent spinning and weaving process, and the yield is low; the main application of phenolic fibers has been focused on fiber fabrics. Meanwhile, melt spinning of the phenolic fiber can be carried out separately, and continuous production cannot be realized; and the high-temperature and high-concentration hydrochloric acid and formaldehyde solution exist in the curing process, so that serious pollution and corrosion are caused. The process has certain drawbacks and limitations in fiber performance, continuous filament preparation, process continuity, engineering scale-up and environmental protection.
Disclosure of Invention
In order to overcome the defects in the prior art and solve the technical problems of the melt spinning process in engineering amplification and large-scale production, the invention provides a preparation method of continuous filament bundle phenolic fibers.
The design concept of the invention is as follows: the wet spinning process of phenolic fiber is to utilize the characteristic that thermosetting phenolic resin is heated to further react and crosslink, prepare the resin into spinning solution, then obtain phenolic resin protofilament through spinning, coagulating bath forming and drafting, and obtain phenolic fiber after heating, crosslinking and curing.
The invention is realized by the following technical scheme.
A method for preparing continuous filament phenolic tow fibers comprises the following steps:
s1, preparing a spinning solution: preparing a spinning solution from a mixed solution of thermosetting phenolic resin and PVA, wherein the viscosity range of the prepared spinning solution is 5000-20000 mPa.s;
s2, preparing a coagulating bath solution: the coagulating bath solution consists of a complexing crosslinking agent, a dehydrating agent, an acid-base neutralizing agent and water;
the complexing crosslinking agent mainly comprises boric acid or borate such as calcium borate, sodium borate, magnesium borate, potassium borate and the like, and the content is 1-6 wt%;
the dehydrating agent mainly comprises inorganic salts with dehydrating effect such as magnesium sulfate, sodium sulfate, copper sulfate, calcium chloride and the like, and the content is the concentration of the aqueous solution in a near saturated state;
the acid-base neutralizing agent mainly comprises inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid and the like, and the concentration is 1-5 wt%;
s3, drawing and solidifying: drafting the spinning solution prepared in the step S1 in the coagulating bath solution prepared in the step S2, wherein the drafting coagulation process is 3-7 sections, and the total drafting multiple is 3-15 times;
s4, heating, curing and crosslinking of the fiber: and (5) washing and drying the fiber drafted in the step S3, heating, curing and crosslinking at the curing and crosslinking temperature of 100-180 ℃ for 10-200 minutes, oiling and collecting the fiber to obtain the continuous filament beam phenolic fiber.
The invention has the following beneficial effects:
the preparation method of the continuous filament bundle phenolic fiber provided by the invention can be used for directly preparing the continuous filament bundle phenolic fiber, has good continuity between sections, and can realize continuous production of the process; and high-pollution and high-corrosiveness chemical reagents do not exist, and the requirements on personnel protection and equipment corrosion prevention are low. Meanwhile, the spinning section of the invention has no high-temperature melting process, the high-temperature curing and crosslinking time is greatly shortened, and the energy-saving effect is obvious.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
A method for preparing continuous filament phenolic tow fibers comprises the following steps:
s1, preparing a spinning solution: preparing a spinning stock solution from a mixed solution of thermosetting phenolic resin and PVA, wherein the preparation of the spinning stock solution adopts a stock solution for spinning phenolic fibers and a preparation method in a preparation method (201110319102.6), and the viscosity range of the prepared spinning stock solution is 5000 mPa.s;
s2, preparing a coagulating bath solution: the coagulating bath solution is an aqueous solution of 1wt% sodium borate, 37wt% sodium sulfate and 3% sulfuric acid;
s3, drawing and solidifying: drafting the spinning solution prepared in the step S1 in the coagulating bath solution prepared in the step S2, wherein the drafting coagulation process is 7 sections, and the total drafting multiple is 15 times;
s4, heating, curing and crosslinking of the fiber: and (4) washing and drying the fiber drafted in the step S3, heating, curing and crosslinking at the curing and crosslinking temperature of 100 ℃ for 200 minutes, oiling and collecting the fiber to obtain the continuous filament bundle phenolic fiber.
Example 2
A method for preparing continuous filament phenolic tow fibers comprises the following steps:
s1, preparing a spinning solution: preparing a spinning solution from a mixed solution of thermosetting phenolic resin and PVA, wherein the viscosity range of the prepared spinning solution is 20000 mPa.s;
s2, preparing a coagulating bath solution: the coagulating bath solution is an aqueous solution of 4wt% of calcium borate, 74wt% of calcium chloride and 5% of hydrochloric acid;
s3, drawing and solidifying: drafting the spinning solution prepared in the step S1 in the coagulating bath solution prepared in the step S2, wherein the drafting coagulation process is 3 sections, and the total drafting multiple is 3 times;
s4, heating, curing and crosslinking of the fiber: and (4) washing and drying the fiber drafted in the step S3, heating, curing and crosslinking at 200 ℃ for 10 minutes, oiling and collecting the fiber to obtain the continuous filament bundle phenolic fiber.
Example 3
A method for preparing continuous filament phenolic tow fibers comprises the following steps:
s1, preparing a spinning solution: preparing a spinning solution from a mixed solution of thermosetting phenolic resin and PVA, wherein the viscosity range of the prepared spinning solution is 13000 mPa.s;
s2, preparing a coagulating bath solution: the coagulating bath solution is an aqueous solution of 6wt% boric acid, 25wt% magnesium sulfate and 1% phosphoric acid;
s3, drawing and solidifying: drafting the spinning solution prepared in the step S1 in the coagulating bath solution prepared in the step S2, wherein the drafting coagulation process is 5 sections, and the total drafting multiple is 8 times;
s4, heating, curing and crosslinking of the fiber: and (4) washing and drying the fiber drafted in the step S3, heating, curing and crosslinking at the curing and crosslinking temperature of 140 ℃ for 100 minutes, oiling and collecting the fiber to obtain the continuous filament bundle phenolic fiber.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and the technical solutions of the embodiment are equally replaced by one or more technical parameters to form a new technical solution, which is also within the scope of the present invention; it will be apparent to those skilled in the art that various modifications and variations can be made in the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. A method for preparing continuous filament phenolic fiber is characterized by comprising the following steps:
s1, preparing a spinning solution: preparing a spinning solution from a mixed solution of thermosetting phenolic resin and PVA, wherein the viscosity range of the prepared spinning solution is 5000-20000 mPa.s;
s2, preparing a coagulating bath solution: the coagulating bath solution is an aqueous solution consisting of a complexing crosslinking agent, a dehydrating agent and an acid-base neutralizing agent, wherein the content of the complexing crosslinking agent is 1-6wt%, the concentration of the acid-base neutralizing agent is 1-5wt%, and the dehydrated content agent is the concentration of the aqueous solution in a near-saturated state;
s3, drawing and solidifying: drafting the spinning solution prepared in the step S1 in the coagulating bath solution prepared in the step S2, wherein the drafting coagulation process is 3-7 sections, and the total drafting multiple is 3-15 times;
s4, heating, curing and crosslinking of the fiber: and (5) washing and drying the fiber drafted in the step S3, heating, curing and crosslinking at the curing and crosslinking temperature of 100-180 ℃ for 10-200 minutes, oiling and collecting the fiber to obtain the continuous filament beam phenolic fiber.
2. The method of making a continuous filament tow phenolic fiber according to claim 1, wherein: in step S2, the complex crosslinking agent includes boric acid or a borate, and the borate is one or more of calcium borate, sodium borate, magnesium borate and potassium borate.
3. The method of making a continuous filament tow phenolic fiber according to claim 1, wherein: in the step S2, the dehydrating agent is one or more of magnesium sulfate, sodium sulfate, copper sulfate and calcium chloride.
4. The method of making a continuous filament tow phenolic fiber according to claim 1, wherein: in step S2, the acid-base neutralization reagent is one of hydrochloric acid, sulfuric acid, and phosphoric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201910817341.0A CN110629300A (en) | 2019-08-30 | 2019-08-30 | Preparation method of continuous filament bundle phenolic fiber |
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| CN201910817341.0A CN110629300A (en) | 2019-08-30 | 2019-08-30 | Preparation method of continuous filament bundle phenolic fiber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113564749A (en) * | 2021-05-31 | 2021-10-29 | 东华大学 | Preparation method of phenolic resin/modified polyvinyl alcohol composite fiber adhesive |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2211547A1 (en) * | 1972-12-20 | 1974-07-19 | Nippon Kynol Inc | |
| CN101205634A (en) * | 2007-09-29 | 2008-06-25 | 中国科学院山西煤炭化学研究所 | Method for controlling hollowness of hollow pnenolic fiber |
| CN107815742A (en) * | 2017-11-10 | 2018-03-20 | 中国科学院山西煤炭化学研究所 | A kind of clotting method of thermosetting phenolic resin precursor |
| CN109112666A (en) * | 2018-07-27 | 2019-01-01 | 中原工学院 | A method of phenolic fibre is prepared by wet spinning |
| CN109183187A (en) * | 2018-07-27 | 2019-01-11 | 中原工学院 | A method of the high ortho phenolic fiber of boron modification is prepared using wet spinning |
| CN109733013A (en) * | 2019-01-28 | 2019-05-10 | 圣华盾防护科技股份有限公司 | A kind of fire retardant protective clothing fabric and protective garment |
| CN109881290A (en) * | 2019-01-28 | 2019-06-14 | 圣华盾防护科技股份有限公司 | A kind of fire prevention protective garment, fabric and fiber |
-
2019
- 2019-08-30 CN CN201910817341.0A patent/CN110629300A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2211547A1 (en) * | 1972-12-20 | 1974-07-19 | Nippon Kynol Inc | |
| CN101205634A (en) * | 2007-09-29 | 2008-06-25 | 中国科学院山西煤炭化学研究所 | Method for controlling hollowness of hollow pnenolic fiber |
| CN107815742A (en) * | 2017-11-10 | 2018-03-20 | 中国科学院山西煤炭化学研究所 | A kind of clotting method of thermosetting phenolic resin precursor |
| CN109112666A (en) * | 2018-07-27 | 2019-01-01 | 中原工学院 | A method of phenolic fibre is prepared by wet spinning |
| CN109183187A (en) * | 2018-07-27 | 2019-01-11 | 中原工学院 | A method of the high ortho phenolic fiber of boron modification is prepared using wet spinning |
| CN109733013A (en) * | 2019-01-28 | 2019-05-10 | 圣华盾防护科技股份有限公司 | A kind of fire retardant protective clothing fabric and protective garment |
| CN109881290A (en) * | 2019-01-28 | 2019-06-14 | 圣华盾防护科技股份有限公司 | A kind of fire prevention protective garment, fabric and fiber |
Non-Patent Citations (2)
| Title |
|---|
| 《化工百科全书》编辑委员会编: "《化工百科全书 第4卷 发光材料-氟 fa-fu》", 30 September 1993, 化学工业出版社 * |
| 上海市纺织科学研究院: "《科研成果报告汇编 第七集（1980~1985）》", 31 October 1986, 上海市纺织工业局印刷厂 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113564749A (en) * | 2021-05-31 | 2021-10-29 | 东华大学 | Preparation method of phenolic resin/modified polyvinyl alcohol composite fiber adhesive |
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