CN115182162B - Preparation method and application method of special sizing agent for nitride fibers - Google Patents

Preparation method and application method of special sizing agent for nitride fibers Download PDF

Info

Publication number
CN115182162B
CN115182162B CN202210863127.0A CN202210863127A CN115182162B CN 115182162 B CN115182162 B CN 115182162B CN 202210863127 A CN202210863127 A CN 202210863127A CN 115182162 B CN115182162 B CN 115182162B
Authority
CN
China
Prior art keywords
sizing agent
parts
agent
weight
sizing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN202210863127.0A
Other languages
Chinese (zh)
Other versions
CN115182162A (en
Inventor
罗飘
方正
包海峰
张磊昂
吕雪莲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuhan Textile University
Original Assignee
Wuhan Textile University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Wuhan Textile University filed Critical Wuhan Textile University
Priority to CN202210863127.0A priority Critical patent/CN115182162B/en
Publication of CN115182162A publication Critical patent/CN115182162A/en
Application granted granted Critical
Publication of CN115182162B publication Critical patent/CN115182162B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/227Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of hydrocarbons, or reaction products thereof, e.g. afterhalogenated or sulfochlorinated
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/224Esters of carboxylic acids; Esters of carbonic acid
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/244Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
    • D06M15/256Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/53Polyethers
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/35Abrasion, pilling or fibrillation resistance
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/40Reduced friction resistance, lubricant properties; Sizing compositions
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/50Modified hand or grip properties; Softening compositions
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

A process for preparing the sizing agent for nitride fibres includes such steps as adding 86-90 wt.% of water to 0.5-2.0 wt.% of primary slurry, stirring to obtain transparent solution, adding 0.5-2.0 wt.% of stabilizer, adding 0.5-2.0 wt.% of emulsifier, adding 2.0-4.0 wt.% of filming assistant, adding 2.0-4.0 wt.% of softening agent, and stirring. The design not only can promote the mechanical property and the surface property of the nitride fiber, but also has simple preparation and stable overall property.

Description

Preparation method and application method of special sizing agent for nitride fibers
Technical Field
The invention relates to a special sizing agent for nitride fibers, belongs to the technical field of sizing agents, and particularly relates to a preparation method and an application method of the special sizing agent for nitride fibers.
Background
The nitride fiber has excellent performances of high temperature resistance, high strength, high modulus, creep resistance, ablation resistance, oxidation resistance, wave transmission, wave absorption and the like, and has application or application potential in the aspects of ultra-high speed accurate guidance radome, thermal protection systems of aerospace aircrafts, aerospace power, aerospace thermal structures, space structures and the like. In addition, the method has application value in the fields of nuclear fission reactor nuclear fuel cladding, nuclear fusion reactor first wall materials and the like.
However, nitride ceramic fibers have problems such as high brittleness and low mechanical strength. In the preparation process, the problems of fiber breakage, broken filaments and the like can occur, so that on one hand, the abrasion of the fiber product in the packaging, transporting and knitting processes can be caused, and on the other hand, the subsequent technological processes such as fiber knitting and the like are not facilitated. In order to solve the problems, the surface of the nitride fiber is coated with sizing agent for sizing, so that the effects of protecting the fiber, reducing the filament quantity of the fiber and improving the knitting performance and mechanical property of the nitride fiber can be achieved. Therefore, development of a sizing agent excellent in performance has become particularly important.
The surface physical and chemical properties of the nitride fiber are special, the requirement on the sizing agent is very high, the formula of the sizing agent belongs to top-grade commercial confidentiality, the formula of the sizing agent of foreign companies is difficult to find, the research of the nitride fiber in China starts later, and the development of the sizing agent suitable for the nitride fiber is less.
The disclosure of this background section is only intended to increase the understanding of the general background of the application and should not be taken as an admission or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
The invention aims to overcome the defect and problem of the prior art that a sizing agent capable of improving the mechanical property and the surface property of nitride fibers is lacking, and provides a preparation method and an application method of a special sizing agent for nitride fibers, which can improve the mechanical property and the surface property of the nitride fibers.
In order to achieve the above object, the technical solution of the present invention is: a method for preparing a sizing agent special for nitride fibers, comprising the following steps:
the first step: firstly, adding 86-90 parts by weight of water into 0.5-2.0 parts by weight of main slurry while stirring, continuing stirring at room temperature until a uniform transparent solution is formed after the addition, and adding 0.5-2.0 parts by weight of stabilizer at room temperature under high-speed shearing until the mixture is uniformly mixed to prepare a mixture system A;
and a second step of: adding 0.5-2.0 parts by weight of an emulsifier to the mixture system A at room temperature under high-speed shearing until the mixture system A is uniformly mixed to prepare a milky mixture system B;
and a third step of: adding 2.0 to 4.0 parts by weight of a film-forming auxiliary to the mixture system B at room temperature under high-speed shearing to obtain a mixture system C;
fourth step: firstly, adding 2.0-4.0 parts by weight of softening agent into the mixture system C under high-speed shearing at room temperature until the softening agent is uniformly mixed, and then standing to obtain the special sizing agent for the nitride fiber, wherein the sizing agent is milky white.
In the first step, the amount of the main slurry is 1.3 parts by weight, the amount of the water is 88 parts by weight, and the amount of the stabilizer is 1.25 parts by weight;
in the second step, the emulsifier is 1.3 parts by weight;
in the third step, 3 parts by weight of the film forming auxiliary agent;
in the fourth step, the softener is 3 parts by weight.
In the first step, the parameters of continuous stirring are 1000-2400 r/min, and the parameters of high-rotation-speed shearing are 5000-30000 r/min;
in the second step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the third step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the fourth step, the high-rotation-speed shearing parameter is 5000-30000 r/min.
The main sizing agent is ethylene acrylic acid copolymer (EAA) special high molecular emulsion, and the model is TL-205.
The water, the stabilizer, the emulsifier, the film forming auxiliary agent and the softener are any combination after the following single selection;
the water is any one of deionized water, pure water, tap water and distilled water;
the stabilizer is any one of paraffin-aluminum base, methylol melamine derivative, chromium stearate complex, pyridine quaternary ammonium salt, organic silicon, fluorocarbon and fluorine-free;
the emulsifier is any one of polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan dioleate, polyoxyethylene sorbitan monostearate, polyoxyethylene glycerol monolaurate, oleate, polyoxyethylene sucrose monooleate, alkylphenol polyoxyethylene ether, polyoxyethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, sodium alkyl sulfate, sodium dodecyl benzene sulfonate, dialkyl sulfosuccinate and fatty alcohol polyoxyethylene ether;
the film forming auxiliary agent is any one of benzyl alcohol BA, ethylene glycol, propylene glycol, hexanediol, texano alcohol ester, ethylene glycol butyl ether EB, propylene glycol methyl ether PM, propylene glycol ethyl ether, propylene glycol butyl ether and the like, hexanediol butyl ether acetate, 3-ethoxypropionic acid ethyl ester EEP and dodecanol ester;
the softening agent is any one of non-surface active mineral oil, higher fatty alcohol ester, surfactant sulfuric acid ester or sulfonate compound, fatty acid polyol ester, fatty acid diethanolamide, anhydride derivative, epoxy derivative, high polymer emulsion comprising polyethylene emulsion and organosilicon, and polyethylene emulsion.
The water is deionized water, the stabilizer is fluorocarbon copolymer, the emulsifier is fatty alcohol polyoxyethylene ether, the film forming auxiliary agent is dodecanol ester, and the softener is polyethylene emulsion.
The room temperature is 23-27 ℃.
The application method of the special sizing agent for the nitride fiber comprises the steps of coating the sizing agent on the surface of the nitride fiber to be treated or soaking the nitride fiber in the sizing agent after the coating is finished or after the soaking is finished to obtain an intermediate, and drying the intermediate to obtain the treated fiber, wherein the sizing rate of the treated fiber is 0.5% -1.5%.
The sizing rate of the treated fiber was 1.0%.
The soaking time was 2 minutes.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention relates to a preparation method and an application method of a special sizing agent for nitride fibers, wherein the preparation of the sizing agent mainly comprises the sequential addition of main sizing agent, water, stabilizing agent, emulsifying agent, film forming auxiliary agent and softening agent, the limitation of addition conditions and the limitation of the dosage of various raw materials until the raw materials are uniformly mixed, and then standing is carried out to obtain the special sizing agent for nitride fibers, wherein the sizing agent is milky white and belongs to water-soluble emulsion sizing agents, and the preparation method has the advantages that: firstly, after the sizing agent is used for sizing nitride fibers, the interface can be effectively improved, a good protection effect is achieved on the fiber interface, loose fiber monofilaments can be effectively gathered into a bundle, the tensile strength, softness, friction resistance and the like of the fibers are improved, the quantity of broken filaments of the fibers is effectively reduced, the bundling property is improved, and the follow-up weaving processing of the fiber bundles is facilitated; secondly, the preparation process is simple, the operation is easy, no special environment is needed, if the heating process is needed, the raw materials are easy to obtain, and the price is low; and the sizing agent prepared by the invention is stable and uniform in milky white, and does not generate phenomena of demulsification, flocculation, coagulation, layering and the like after being placed for a long time at room temperature, such as 25 ℃, and has good storage performance. Therefore, the invention not only can improve the mechanical property and the surface property of the nitride fiber, but also has simple preparation and stable overall property.
2. The raw materials used in the preparation method and the application method of the special sizing agent for the nitride fiber comprise main sizing agent, water, stabilizing agent, emulsifying agent, film forming auxiliary agent and softening agent, which are all nontoxic and harmful raw materials, and meanwhile, the whole preparation process is carried out at normal temperature, so that no harmful waste gas or waste liquid is generated, the environment is not polluted, and the health of operators is not endangered. Therefore, the invention has stronger environmental protection.
3. The main sizing agent is preferably ethylene acrylic acid copolymer (EAA) special polymer emulsion, the model is TL-205, the special polymer emulsion contains vinyl and acrylic acid groups, is light-colored semitransparent emulsion, has a pH value of 8.0-10.0, a solid content of 15-25%, and a melting point of 75-85 ℃, is soluble in water, has better adhesion to fibers, good film forming property, good film stiffness and toughness and high tensile strength, has carboxylic acid groups, can improve the film forming stability through a crosslinking reaction, improves the interfacial property of a final product sizing agent to the fibers, endows the sizing agent with good wettability on the surfaces of the fibers, has better matching use effect with polyethylene emulsion (softening agent), can facilitate uniform film forming of the sizing agent on the surfaces of the fibers, and improves the strength and flexibility of the yarns. Therefore, the invention limits the main sizing agent, not only can improve the mechanical property and the surface property of the final product for the nitride fiber, but also can cooperate with other raw materials, thereby being convenient for obtaining better overall effect.
4. According to the preparation method and the application method of the special sizing agent for the nitride fiber, when the special sizing agent is applied, the sizing rate of the treated fiber is 0.5% -1.5%, preferably 1.0%, so that the special sizing agent can effectively protect the nitride fiber through lower sizing rate, improve the wear resistance and tensile property of the special sizing agent, enable the fiber to have the capability of resisting friction during weaving, avoid the defect that the fiber is more fragile and hard and is easy to bend and damage during weaving caused by over-high sizing rate, and simultaneously, the sizing agent has the advantages of low sizing rate and short film forming time, has the advantage of being short in time, can be used for carrying out good surface modification on the nitride fiber, is short in sizing time, directly causes the drying time, and is beneficial to shortening the operation time of the whole application process. Therefore, the invention has low sizing rate, short film forming time and good sizing modification effect.
5. In the preparation method and the application method of the special sizing agent for the nitride fiber, when the special sizing agent is applied, the sizing rate of the treated fiber is 0.5% -1.5%, preferably 1.0%, and the technical characteristics are that the advantages of the sizing rate per se are brought about, the advantages can be improved on the residual weight rate, the residual weight rate= (the mass of the sized fiber after high-temperature calcination-the original mass of the fiber)/the mass of the sized fiber multiplied by 100%, and the advantages of the residual weight rate can be fully exerted, so that the special sizing agent for the nitride fiber belongs to the high-temperature resistant ceramic fiber, and can be better applied to a thermal protection system of an aerospace vehicle or a thermal protection system of a radar protection cover. Therefore, the residual weight rate of the invention is better.
Drawings
FIG. 1 is a schematic view of the long-term storage stability of a sizing agent made in accordance with the present invention.
Fig. 2 is an SEM image of a sizing agent made in accordance with the present invention after sizing on nitride fibers.
Fig. 3 is a schematic drawing showing a tensile strength test of the sizing agent prepared according to the present invention after sizing the nitride fiber.
FIG. 4 is a schematic diagram of a test of the amount of hairiness of the sizing agent of the present invention after sizing the nitride fiber.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings and detailed description.
Referring to fig. 1 to 4, a method for preparing a sizing agent special for nitride fibers, the method comprising the steps of:
the first step: firstly, adding 86-90 parts by weight of water into 0.5-2.0 parts by weight of main slurry while stirring, continuing stirring at room temperature until a uniform transparent solution is formed after the addition, and adding 0.5-2.0 parts by weight of stabilizer at room temperature under high-speed shearing until the mixture is uniformly mixed to prepare a mixture system A;
and a second step of: adding 0.5-2.0 parts by weight of an emulsifier to the mixture system A at room temperature under high-speed shearing until the mixture system A is uniformly mixed to prepare a milky mixture system B;
and a third step of: adding 2.0 to 4.0 parts by weight of a film-forming auxiliary to the mixture system B at room temperature under high-speed shearing to obtain a mixture system C;
fourth step: firstly, adding 2.0-4.0 parts by weight of softening agent into the mixture system C under high-speed shearing at room temperature until the softening agent is uniformly mixed, and then standing to obtain the special sizing agent for the nitride fiber, wherein the sizing agent is milky white.
In the first step, the amount of the main slurry is 1.3 parts by weight, the amount of the water is 88 parts by weight, and the amount of the stabilizer is 1.25 parts by weight;
in the second step, the emulsifier is 1.3 parts by weight;
in the third step, 3 parts by weight of the film forming auxiliary agent;
in the fourth step, the softener is 3 parts by weight.
In the first step, the parameters of continuous stirring are 1000-2400 r/min, and the parameters of high-rotation-speed shearing are 5000-30000 r/min;
in the second step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the third step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the fourth step, the high-rotation-speed shearing parameter is 5000-30000 r/min.
The main sizing agent is ethylene acrylic acid copolymer (EAA) special high molecular emulsion, and the model is TL-205.
The water, the stabilizer, the emulsifier, the film forming auxiliary agent and the softener are any combination after the following single selection;
the water is any one of deionized water, pure water, tap water and distilled water;
the stabilizer is any one of paraffin-aluminum base, methylol melamine derivative, chromium stearate complex, pyridine quaternary ammonium salt, organic silicon, fluorocarbon and fluorine-free;
the emulsifier is any one of polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan dioleate, polyoxyethylene sorbitan monostearate, polyoxyethylene glycerol monolaurate, oleate, polyoxyethylene sucrose monooleate, alkylphenol polyoxyethylene ether, polyoxyethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, sodium alkyl sulfate, sodium dodecyl benzene sulfonate, dialkyl sulfosuccinate and fatty alcohol polyoxyethylene ether;
the film forming auxiliary agent is any one of benzyl alcohol BA, ethylene glycol, propylene glycol, hexanediol, texano alcohol ester, ethylene glycol butyl ether EB, propylene glycol methyl ether PM, propylene glycol ethyl ether, propylene glycol butyl ether and the like, hexanediol butyl ether acetate, 3-ethoxypropionic acid ethyl ester EEP and dodecanol ester;
the softening agent is any one of non-surface active mineral oil, higher fatty alcohol ester, surfactant sulfuric acid ester or sulfonate compound, fatty acid polyol ester, fatty acid diethanolamide, anhydride derivative, epoxy derivative, high polymer emulsion comprising polyethylene emulsion and organosilicon, and polyethylene emulsion.
The water is deionized water, the stabilizer is fluorocarbon copolymer, the emulsifier is fatty alcohol polyoxyethylene ether, the film forming auxiliary agent is dodecanol ester, and the softener is polyethylene emulsion.
The room temperature is 23-27 ℃.
The application method of the special sizing agent for the nitride fiber comprises the steps of coating the sizing agent on the surface of the nitride fiber to be treated or soaking the nitride fiber in the sizing agent after the coating is finished or after the soaking is finished to obtain an intermediate, and drying the intermediate to obtain the treated fiber, wherein the sizing rate of the treated fiber is 0.5% -1.5%.
The sizing rate of the treated fiber was 1.0%.
The soaking time was 2 minutes.
The principle of the invention is explained as follows:
the film forming aid in the present invention is preferably a dodecanol ester, which has advantages for use in the present invention including: (1) the addition of the film forming aid can reduce the Minimum Film Forming Temperature (MFFT); (2) the film forming auxiliary agent is a high-boiling point organic compound with larger molecular weight, has low migration speed and low volatilization rate, can fully contact and infiltrate the sizing agent with the fiber, ensures that the sizing effect is not only that the sizing agent stays on the surface of the fiber bundle filament, but also enters the fiber monofilament, fully sizes each fiber, ensures that the filaments inside the fiber are not bonded together, and can uniformly form a film between the filaments inside the fiber, thereby achieving better sizing effect. (3) In designing the sizing formulation, it is important to consider the layering phenomenon of the emulsion, the aqueous emulsion is a two-phase system, mainly an aqueous phase and a polymer phase, the concentration of the film forming auxiliary agent mainly depends on the hydrophilic and lipophilic balance of the polymer and the solvent, and the film forming auxiliary agent is closely involved in the film forming process to determine the degree of coalescence of polymer latex particles into a complete continuous film, thereby determining the performance of the fiber after sizing.
The emulsifier in the invention is preferably fatty alcohol polyoxyethylene ether, and forms oil-in-water emulsion with oil-soluble dodecyl alcohol ester (the film forming auxiliary agent is dodecyl alcohol ester), so that the sizing agent forms a uniform and stable system.
The stabilizer in the invention is preferably fluorocarbon copolymer, which endows the emulsion with excellent stability, and the fiber has water and oil repellent performance after sizing.
The softening agent in the invention is preferably a polyethylene emulsion, which imparts good softness and smoothness to the fiber.
The reason why the high-speed shearing parameter is limited to 5000-30000 r/min in the invention is that: too low a rotational speed, the emulsion is not uniformly dispersed, the components of the emulsion cannot be well mixed uniformly, the treatment time is long, and too high a rotational speed, the emulsion is easy to splash out, the machine is damaged, and the energy consumption is increased.
Example 1:
a method for preparing a sizing agent special for nitride fibers, comprising the following steps:
the first step: firstly, adding 91 parts by weight of water into 0.5 part by weight of main slurry (namely film forming agent) dropwise while stirring, continuing stirring at room temperature until a uniform transparent solution is formed after the dropwise addition is finished, and adding 2.0 parts by weight of stabilizing agent under high-speed shearing at room temperature until the mixture is uniformly mixed to prepare a mixture system A;
and a second step of: adding 0.5 weight part of emulsifier into the mixture system A under high-speed shearing at room temperature until the mixture system A is uniformly mixed to prepare a milky mixture system B;
and a third step of: adding 4.0 parts by weight of a film forming auxiliary to the mixture system B at room temperature under high-speed shearing to obtain a mixture system C;
fourth step: firstly, adding 2.0 parts by weight of softening agent into a mixture system C under high-rotation-speed shearing at room temperature until the softening agent is uniformly mixed, and standing to obtain the special sizing agent for the nitride fiber, wherein the sizing agent is milky white and named sizing agent 01.
Meanwhile, according to the same preparation method, sizing agent 02, sizing agent 03, sizing agent 04 and sizing agent 05 are respectively obtained as follows:
sizing agent 02: 0.5 part of film forming agent, 4 parts of film forming auxiliary agent, 0.5 part of emulsifying agent, 2 parts of stabilizing agent, 2.5 parts of softening agent and 90.5 parts of deionized water.
Sizing agent 03: 0.5 part of film forming agent, 4 parts of film forming auxiliary agent, 0.5 part of emulsifying agent, 2 parts of stabilizing agent, 3 parts of softening agent and 90 parts of deionized water.
Sizing agent 04: 0.5 part of film forming agent, 4 parts of film forming auxiliary agent, 0.5 part of emulsifying agent, 2 parts of stabilizing agent, 3.5 parts of softening agent and 89.5 parts of deionized water.
Sizing agent 05: 0.5 part of film forming agent, 4 parts of film forming auxiliary agent, 0.5 part of emulsifying agent, 2 parts of stabilizing agent, 4 parts of softening agent and 89 parts of deionized water.
Referring to FIG. 1, the storage stability of the above 5 sizing agents was studied, and the results showed that the prepared sizing agents were all in a stable and uniform milky white shape, and the phenomena of demulsification, flocculation, coagulation, delamination, etc. were not substantially occurred after long-term storage at room temperature (25 ℃), thus showing that the obtained sizing agents all had good storage stability.
And coating the sizing agent on the surface of the nitride fiber to be treated or soaking the nitride fiber in the sizing agent, obtaining an intermediate after coating or soaking, and drying the intermediate to obtain the treated fiber.
Sizing percentage= (fiber mass after sizing drying-fiber mass before sizing)/fiber mass before sizing x 100%. Sizing rates for the 5 sizing agents are shown in the following table:
sample name Sizing agent 01 Sizing agent 02 Sizing agent 03 Sizing agent 04 Sizing agent 05
Sizing percentage 1.0% 0.8% 1.0% 0.9% 0.9%
Nitride fibers are relatively brittle, and in actual weaving, the fibers are subject to relatively large damage due to repeated friction and bending, and the ability of the fibers to withstand such damage determines the weaving adaptability of the fibers. Therefore, it is important to examine the difference of the wear resistance before and after sizing, and the wear resistance is also an important reference for examining the performance of sizing agents, and the method comprises the following steps:
the nitride fiber is uniformly cut into fiber segments with the length of 100cm, the fiber is respectively immersed into the 5 sizing agent solutions for 10min, the fiber is taken out and dried (dried for 2min at 140 ℃), the wear resistance is referred to FZ/T01058-1999 'reciprocating grinding roller method of yarn wear resistance test method', and the movement time when the fiber is broken is recorded as the wear resistance time, which is specifically as follows:
example 2:
the basic operation is the same as the preparation method of sizing agent 01 in example 1, except that the usage amount of the film forming agent is 0.5 part of the film forming agent, 1.0 part of the film forming agent, 1.5 parts of the film forming agent and 2.0 parts of the film forming agent respectively.
Referring to fig. 2, a SEM image of the 4 sizing agents above after sizing the nitride fibers is compared to the original nitride fibers.
Example 3:
referring to fig. 3, the basic operation is the same as that of the preparation method of sizing agent 01 in example 1, except that the amounts of the film-forming aids are respectively: 2.0 parts of film forming auxiliary agent, 2.5 parts of film forming auxiliary agent, 3.0 parts of film forming auxiliary agent, 3.5 parts of film forming auxiliary agent and 4.0 parts of film forming auxiliary agent.
After the 5 sizing agents are sized on the nitride fiber, tensile strength tests are respectively carried out, and the tensile performance is greatly improved compared with the nitride fiber adopting the sizing agents.
Example 4:
referring to fig. 4, the basic operation is the same as the preparation method of sizing agent 01 in example 1, except that the amounts of the film forming agents are respectively:
0.5 part of film forming agent, 1.0 part of film forming agent, 1.5 parts of film forming agent and 2.0 parts of film forming agent.
After sizing the nitride fibers with the 4 sizing agents, the fiber friction filament amounts were compared to examine the fiber friction resistance, comprising the following steps:
firstly, 100cm long nitride fiber bundles are taken and clamped in polyurethane sponge (the sponge size is 60 multiplied by 50 multiplied by 20 mm), a weight with the mass of 200g is placed on the sponge to apply certain pressure, then the nitride fibers are horizontally moved at the speed of 1m/min until the fibers completely pass through the polyurethane sponge, the mass of the polyurethane sponge before and after the nitride fiber bundles pass through friction is evenly weighed by using an electronic day, the difference value is calculated, each group of samples are measured for 10 times, and the average value is taken as the friction yarn quantity of the nitride fibers, and referring to fig. 4, which is a comparison test picture, the yarn quantity of the nitride fibers after sizing is relatively less.
The above description is merely of preferred embodiments of the present invention, and the scope of the present invention is not limited to the above embodiments, but all equivalent modifications or variations according to the present disclosure will be within the scope of the claims.

Claims (8)

1. A preparation method of a special sizing agent for nitride fibers is characterized by comprising the following steps: the preparation method comprises the following steps:
the first step: firstly, adding 86-90 parts by weight of water into 0.5-2.0 parts by weight of main slurry while stirring, continuing stirring at room temperature until a uniform transparent solution is formed after the addition, and adding 0.5-2.0 parts by weight of stabilizer at room temperature under high-speed shearing until the mixture is uniformly mixed to prepare a mixture system A;
and a second step of: adding 0.5-2.0 parts by weight of an emulsifier to the mixture system A at room temperature under high-speed shearing until the mixture system A is uniformly mixed to prepare a milky mixture system B;
and a third step of: adding 2.0 to 4.0 parts by weight of a film-forming auxiliary to the mixture system B at room temperature under high-speed shearing to obtain a mixture system C;
fourth step: firstly, adding 2.0-4.0 parts by weight of softening agent into a mixture system C under high-rotation-speed shearing at room temperature until the softening agent is uniformly mixed, and standing to obtain the special sizing agent for the nitride fibers, wherein the sizing agent is milky white;
the main sizing agent is ethylene acrylic acid copolymer (EAA) special high molecular emulsion, and the model is TL-205;
the water, the stabilizer, the emulsifier, the film forming auxiliary agent and the softener are any combination after the following single selection;
the water is any one of deionized water, pure water, tap water and distilled water;
the stabilizer is any one of paraffin-aluminum base, methylol melamine derivative, chromium stearate complex, pyridine quaternary ammonium salt, organic silicon, fluorocarbon and fluorine-free;
the emulsifier is any one of polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan dioleate, polyoxyethylene sorbitan monostearate, polyoxyethylene glycerol monolaurate, oleate, polyoxyethylene sucrose monooleate, alkylphenol polyoxyethylene ether, polyoxyethylene fatty amine, polyethylene glycol fatty acid ester, sodium oleate, sodium abietate, sodium alkyl sulfate, sodium dodecyl benzene sulfonate, dialkyl sulfosuccinate and fatty alcohol polyoxyethylene ether;
the film forming auxiliary agent is any one of benzyl alcohol BA, ethylene glycol, propylene glycol, hexanediol, texano alcohol ester, ethylene glycol butyl ether EB, propylene glycol methyl ether PM, propylene glycol diethyl ether, propylene glycol butyl ether, hexanediol butyl ether acetate, 3-ethoxypropionic acid ethyl ester EEP and dodecanol ester;
the softening agent is any one of non-surface active mineral oil, higher fatty alcohol ester, surfactant sulfuric acid ester or sulfonate compound, fatty acid polyol ester, fatty acid diethanolamide, anhydride derivative, epoxy derivative, high polymer emulsion comprising polyethylene emulsion and organosilicon, and polyethylene emulsion.
2. The method for preparing the special sizing agent for nitride fibers according to claim 1, wherein the method comprises the following steps:
in the first step, the amount of the main slurry is 1.3 parts by weight, the amount of the water is 88 parts by weight, and the amount of the stabilizer is 1.25 parts by weight;
in the second step, the emulsifier is 1.3 parts by weight;
in the third step, 3 parts by weight of the film forming auxiliary agent;
in the fourth step, the softener is 3 parts by weight.
3. The method for preparing a sizing agent special for nitride fibers according to claim 1 or 2, characterized in that:
in the first step, the parameters of continuous stirring are 1000-2400 r/min, and the parameters of high-rotation-speed shearing are 5000-30000 r/min;
in the second step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the third step, the high-rotation-speed shearing parameter is 5000-30000 r/min;
in the fourth step, the high-rotation-speed shearing parameter is 5000-30000 r/min.
4. The method for preparing a sizing agent special for nitride fibers according to claim 1 or 2, characterized in that: the water is deionized water, the stabilizer is fluorocarbon copolymer, the emulsifier is fatty alcohol polyoxyethylene ether, the film forming auxiliary agent is dodecanol ester, and the softener is polyethylene emulsion.
5. The method for preparing a sizing agent special for nitride fibers according to claim 1 or 2, characterized in that: the room temperature is 23-27 ℃.
6. The application method of the special sizing agent for the nitride fiber is characterized by comprising the following steps of: after obtaining the special sizing agent for the nitride fiber prepared in the above claim 1, the sizing agent is coated on the surface of the nitride fiber to be treated or the nitride fiber is soaked in the sizing agent, an intermediate is obtained after the coating or the soaking is finished, and the intermediate is dried to obtain the treated fiber, wherein the sizing rate of the treated fiber is 0.5% -1.5%.
7. The method for applying a sizing agent special for nitride fibers according to claim 6, wherein the method comprises the following steps: the sizing rate of the treated fiber was 1.0%.
8. The method for applying a sizing agent special for nitride fibers according to claim 6, wherein the method comprises the following steps: the soaking time was 2 minutes.
CN202210863127.0A 2022-07-21 2022-07-21 Preparation method and application method of special sizing agent for nitride fibers Active CN115182162B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210863127.0A CN115182162B (en) 2022-07-21 2022-07-21 Preparation method and application method of special sizing agent for nitride fibers

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210863127.0A CN115182162B (en) 2022-07-21 2022-07-21 Preparation method and application method of special sizing agent for nitride fibers

Publications (2)

Publication Number Publication Date
CN115182162A CN115182162A (en) 2022-10-14
CN115182162B true CN115182162B (en) 2023-12-22

Family

ID=83519700

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210863127.0A Active CN115182162B (en) 2022-07-21 2022-07-21 Preparation method and application method of special sizing agent for nitride fibers

Country Status (1)

Country Link
CN (1) CN115182162B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101858037A (en) * 2010-06-18 2010-10-13 济南大学 Emulsion type carbon fiber sizing agent and preparation method and application thereof
CN104420204A (en) * 2013-09-10 2015-03-18 济南大学 Carbon fiber water-soluble epoxy resin sizing agent
CN106894238A (en) * 2017-03-24 2017-06-27 武汉龙图新材料科技有限公司 A kind of silicon carbide fibre sizing agent and preparation method thereof
CN106948176A (en) * 2017-03-24 2017-07-14 武汉龙图新材料科技有限公司 A kind of silicon nitride fiber sizing agent and preparation method thereof
CN109853238A (en) * 2019-03-06 2019-06-07 福建立亚新材有限公司 A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application
CN111088699A (en) * 2018-10-23 2020-05-01 中国石油化工股份有限公司 Sizing agent for polypropylene/carbon fiber interface and preparation method and application thereof
CN111518443A (en) * 2020-04-29 2020-08-11 湖北中科博策新材料科技有限公司 High-modulus carbon fiber reinforced water paint and production process thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101858037A (en) * 2010-06-18 2010-10-13 济南大学 Emulsion type carbon fiber sizing agent and preparation method and application thereof
CN104420204A (en) * 2013-09-10 2015-03-18 济南大学 Carbon fiber water-soluble epoxy resin sizing agent
CN106894238A (en) * 2017-03-24 2017-06-27 武汉龙图新材料科技有限公司 A kind of silicon carbide fibre sizing agent and preparation method thereof
CN106948176A (en) * 2017-03-24 2017-07-14 武汉龙图新材料科技有限公司 A kind of silicon nitride fiber sizing agent and preparation method thereof
CN111088699A (en) * 2018-10-23 2020-05-01 中国石油化工股份有限公司 Sizing agent for polypropylene/carbon fiber interface and preparation method and application thereof
CN109853238A (en) * 2019-03-06 2019-06-07 福建立亚新材有限公司 A kind of silicon carbide or silicon nitride fiber sizing agent and its preparation method and application
CN111518443A (en) * 2020-04-29 2020-08-11 湖北中科博策新材料科技有限公司 High-modulus carbon fiber reinforced water paint and production process thereof

Also Published As

Publication number Publication date
CN115182162A (en) 2022-10-14

Similar Documents

Publication Publication Date Title
CN107829306B (en) Coated carbon fiber precursor oiling agent and preparation method thereof
JP4094546B2 (en) Carbon fiber sizing agent, carbon fiber sizing method using the sizing agent, sized carbon fiber, and knitted fabric using the carbon fiber
US20050066448A1 (en) Finishing of textile fibers, tissues, and fabrics
CA2054277C (en) Cardable hydrophobic polyolefin fiber, material and method for preparation thereof
CN101100356A (en) Direct untwisted roving soaking agent
US4751258A (en) Sizing agents for carbon yarns
CN112029032B (en) Preparation method of durable fabric waterproof finishing agent and product thereof
EP0559865B1 (en) Glass size compositions and glass fibers coated therewith
CN101100355A (en) Soaking agent capable of increasing glass fiber acid resistance
JP2008063713A (en) Fiber treating agent and method for producing synthetic fiber using the same
Peled et al. Treatments of polypropylene fibres to optimize their reinforcing efficiency in cement composites
WO1996006971A1 (en) High cohesion fiber finishes
CN115182162B (en) Preparation method and application method of special sizing agent for nitride fibers
Chowdhury Effect of special finishes on the functional properties of cotton fabrics
CN108505342A (en) It is a kind of continuously to spin viscose filament yarn finish and its preparation method and application
JP4305081B2 (en) Oil for carbon fiber production and method for producing carbon fiber
US4654153A (en) Spinning preparations for melt spinning synthetic fibers
US4322302A (en) Agent for the liquid paraffin waxing of yarns
EP1451122B1 (en) Sizing composition for glass yarns, the glass yarns thus obtained and composite materials comprising said yarns
EP0605727A1 (en) Process for high-speed spinning of polyester fiber
JPS6256267B2 (en)
EP1966433B1 (en) Fiber modifying method
JPH0491276A (en) Spinning oil for acrylic fiber
CN111648135A (en) High-efficiency cold paste containing polysiloxane acrylate and preparation method thereof
JP4990195B2 (en) Carbon fiber precursor acrylic fiber bundle and method for producing the same

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant