CN113550024A - Preparation method of superfine high-elastic latex yarn - Google Patents

Preparation method of superfine high-elastic latex yarn Download PDF

Info

Publication number
CN113550024A
CN113550024A CN202110702621.4A CN202110702621A CN113550024A CN 113550024 A CN113550024 A CN 113550024A CN 202110702621 A CN202110702621 A CN 202110702621A CN 113550024 A CN113550024 A CN 113550024A
Authority
CN
China
Prior art keywords
latex
yarn
parts
vulcanized
casein
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.)
Granted
Application number
CN202110702621.4A
Other languages
Chinese (zh)
Other versions
CN113550024B (en
Inventor
孔娜
陶金龙
李志锋
丁宏达
罗梓蓉
张吉振
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.)
Agricultural Products Processing Research Institute of CATAS
Original Assignee
Agricultural Products Processing Research Institute of CATAS
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 Agricultural Products Processing Research Institute of CATAS filed Critical Agricultural Products Processing Research Institute of CATAS
Priority to CN202110702621.4A priority Critical patent/CN113550024B/en
Publication of CN113550024A publication Critical patent/CN113550024A/en
Application granted granted Critical
Publication of CN113550024B publication Critical patent/CN113550024B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/02Preparation of spinning solutions
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D1/00Treatment of filament-forming or like material
    • D01D1/10Filtering or de-aerating the spinning solution or melt
    • D01D1/103De-aerating
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01DMECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00Formation of filaments, threads, or the like
    • D01D5/06Wet spinning methods
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties

Landscapes

  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Artificial Filaments (AREA)

Abstract

The invention discloses a superfine high-elastic latex yarn and a preparation method thereof, wherein natural latex is used as a main raw material, firstly, the natural latex is pre-vulcanized, then, the natural latex is concentrated and defoamed to obtain spinning solution with the solid content of 65-70 wt%, the spinning solution is extruded into yarn, the yarn is solidified and formed in a coagulating bath, and then, the finished product of the latex yarn is prepared through vulcanization, cooling and powder sticking treatment. The method of the invention can prepare superfine latex yarn products with excellent tensile property. Meanwhile, the production process is simple, continuous and batch production can be realized, the product quality is stable, and industrial production is easy to realize.

Description

Preparation method of superfine high-elastic latex yarn
Technical Field
The invention relates to the technical field of production of latex yarns, in particular to a preparation method of superfine high-elasticity latex yarns.
Background
The latex yarn is natural rubber yarn, and is a linear latex product with smooth surface and uniform thickness, which is prepared by taking natural latex as a main raw material, adding other industrial raw materials, mixing, homogenizing, extruding, solidifying and molding. The high-quality latex yarn has excellent tensile strength, elongation, retraction, wear resistance, washing resistance and the like. Latex filaments have a wide range of uses, such as elastic fabrics used in everyday life, sports fitness products, medical and health products, and industrial and aerospace elastic cords.
At present, the main production process of latex filaments is basically fixed, namely raw materials such as latex, inert filler, an activating agent, an accelerating agent and the like are mixed to prepare mixed glue solution and are cooled, the mixed glue solution is extruded into filaments, the filaments are formed through acetic acid gelation, and the formed latex filaments are washed, dried, vulcanized and cooled to prepare finished latex filaments. The latex yarn prepared by the traditional process at present has the following defects: 1) the diameter of the latex yarn is thick, which seriously restricts the development of the production of the superfine high-elasticity latex yarn. According to the national standard for latex filaments (HGT2889-2011), the specification of the latex filaments (count) is from 100 to 24, and the corresponding nominal diameter is 0.25mm to 1.06 mm. However, the latex yarn on the market is mainly 20 to 48 yarns, and the production of the superfine latex yarn still has technical difficulties. 2) At present, the tensile rate of the latex yarn product is low, and the requirement of high-performance latex yarn cannot be met.
Disclosure of Invention
The invention aims to provide superfine high-elastic latex yarn and a preparation method thereof, aiming at solving the problems in the prior art, the invention takes natural latex as a main raw material, firstly carries out prevulcanization on the natural latex (the prevulcanization can uniformly mix various dispersions into the latex and rubber particles, so that the subsequent vulcanization process is simple and high in efficiency, and the performance of the product is improved), then concentrates and defoams to obtain spinning solution with the solid content of 65-70 wt%, extrudes the spinning solution into yarn, carries out coagulation forming by a coagulation bath, and then carries out vulcanization, cooling and powder adhesion treatment to prepare the finished product of the latex yarn. The method can obtain the superfine latex yarn with the diameter less than 0.2mm, and the prepared latex yarn has good tensile property and the maximum elongation of 1400 percent.
In order to achieve the purpose, the invention provides the following scheme:
the superfine high-elastic latex yarn comprises the following raw materials in parts by weight: 1000 parts of natural latex, 35-40 parts of prevulcanized dispersoid, 0.7-0.9 part of casein, 1-1.5 parts of KOH, 2-5 parts of reinforcing agent and 2.7-4.6 parts of deionized water;
the raw materials of the pre-vulcanized dispersion comprise the following components in parts by weight: 0.8-1 part of sulfur, 0.4-0.6 part of ZnO, 0.7-1 part of accelerator ZDC, 0.1-0.4 part of accelerator PX, 2640.2-0.7 part of anti-aging agent, 0.2-0.4 part of anti-aging agent WSL, 0.2-0.3 part of KOH and 0.1-0.2 part of casein.
Further, the reinforcing agent is carbon black or white carbon black. The invention does not add inert filler, but adds a small amount of reinforcing agent to improve the physical and mechanical properties and aging resistance of the rubber material.
Furthermore, the raw materials of the superfine high-elastic latex yarn also comprise color paste. The color paste is one of permanent yellow, permanent red and Hualan.
The invention also provides a preparation method of the superfine high-elastic latex yarn, which comprises the following steps:
(1) preparation of the prevulcanised dispersion:
mixing and dispersing sulfur, ZnO, a promoter ZDC, a promoter PX, an anti-aging agent 264, an anti-aging agent WSL, KOH, casein and deionized water to obtain a pre-vulcanized dispersion;
(2) pre-vulcanizing:
adding casein, KOH and a reinforcing agent into natural latex, uniformly mixing, heating, adding the prevulcanized dispersion, continuously heating to 55-70 ℃, and reacting for 2-3h to obtain prevulcanized latex;
(3) concentration:
concentrating and defoaming the prevulcanized latex solution to obtain a spinning solution;
(4) and (3) extrusion molding:
extruding the spinning solution into gel filaments, and solidifying and forming the gel filaments in a coagulating bath to obtain to-be-vulcanized latex filaments;
(5) and (3) vulcanization:
and vulcanizing the latex yarn to be vulcanized to obtain vulcanized latex yarn, cooling and coating powder to obtain the superfine high-elasticity latex yarn.
Further, in the step (2), the casein and the KOH are respectively added in the form of aqueous solutions, wherein the mass ratio of the casein to the water is 0.9:10, and the mass ratio of the KOH to the water is 1.5: 15.
Further, in step (2), the pre-vulcanized dispersion is added by heating to 35 ℃.
Further, in the step (3), the concentration is to concentrate the pre-vulcanized latex solution to a solid content of 65-70 wt%, and the defoaming treatment is to perform vacuum defoaming under a negative pressure condition, wherein the negative pressure is 75-100mm Hg.
Further, in the step (4), the coagulating bath is a mixed coagulating bath of ethanol and water, and the volume ratio of the ethanol to the water is 70-80: 20-30.
Further, in the step (5), the temperature of the vulcanization treatment is 120 ℃ for 5 minutes.
In the traditional process, the solid content of the latex is improved by adding the inert filler, and the extrusion molding capacity of the latex is improved, however, the addition of the inert filler can cause the agglomeration of rubber particles in the latex, the gel is not easy to settle and filter, the bubbles are not easy to escape, and the nozzle is easy to block, so the stability of the latex is poor. The common inert fillers comprise kaolin, talcum powder, calcium carbonate and the like, and the dosage of the inert fillers is 2-8% of the weight of the latex. On the basis of not adding inert filler, the invention directly improves the concentration of the latex to meet the requirement of extrusion molding, further improves the extrusion molding capability of the latex, and is not easy to cause the phenomenon of end cap, so that a thinner extrusion head can be selected in the extrusion process to form a thinner latex wire.
At present, the production of latex filaments mainly adopts an extrusion acid coagulation process technology, and the working principle of the process is that ions with positive charges in an acid solution are neutralized to ions with negative charges in latex by using an ion precipitation method, so that the extruded filament-shaped latex is converted into a gel state from a flowing state. The acid content, pH and temperature in the coagulating acid tank need to be strictly controlled within a specified range, and meanwhile, the running time of the rubber filament in the acid tank is controlled, so that the condition that the rubber fiber is easy to deform due to insufficient gelation or the rubber fiber is too high in hardness due to excessive gelation is prevented, and the final product performance of the rubber fiber is influenced by the gelation pH value, the gelation temperature and the gelation time in the gelation process. At present, the rubber fiber is produced by adopting a formic acid or acetic acid solidification process, and the problems of corrosivity, irritation, safety and the like exist.
Compared with the traditional acid coagulation bath, the coagulation bath has the advantages that the gelation speed of the latex extruded by the extrusion head in the ethanol/water mixed coagulation bath is mild, the formation of a gelled shell is avoided, and the tensile property of the product is favorably improved. The method avoids the use of a large amount of corrosive acid solution, reduces the corrosion to production equipment and reduces the pollution to the working environment.
The detection method of the breaking elongation of the latex yarn comprises the following steps:
(1) fixing a certain length (about 2 cm) of latex wire in a universal stretcher fixture, finely adjusting the distance between the fixtures to enable the latex wire to be straightened but not stressed, and recording the distance between the fixtures as L0;
(2) starting a stretching device of a stretcher, stretching the sample at a constant speed (the speed is 1cm/min) along the axial direction of the rubber filament until the sample is broken, and reading the stretching stroke delta L when the sample is broken;
(3) calculating the elongation at break epsilon as Δ L/L0 × 100%;
(4) each set of samples was tested in parallel for 3 sets and the average elongation at break of the set was calculated.
The invention discloses the following technical effects:
(1) the invention can prepare superfine latex yarn products by improving the stability and the processability of the spinning solution and using ethanol/water mixed coagulating bath for coagulation forming, and the minimum diameter can reach 100 mu m;
(2) the latex yarn obtained by the invention has high tensile property, and the elongation at break is as high as 1400%;
(3) the invention does not adopt inert filler, reduces the agglomeration of rubber particles in latex, and is not easy to cause the phenomenon of choke plug, so that a thinner extrusion head can be selected in the extrusion process to form a thinner latex wire;
(4) the invention adopts the ethanol/water mixed solution as the coagulating bath, is environment-friendly, reduces the loss of production equipment and also improves the working environment of production workers;
(5) the production process flow used by the invention is simple, the power consumption is low, and the production cost is effectively saved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a flow chart of a method for preparing ultra-fine high elastic latex yarn;
FIG. 2 is a cross-sectional scanning electron micrograph of an ultra-fine high-elastic latex yarn prepared in example 3;
FIG. 3 is a scanning electron microscope image of the cross section of the ultra-fine high-elastic latex filament prepared in example 4;
fig. 4 is a graph comparing stress-strain curves of latex filaments prepared in example 3 and comparative example 3.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the invention, the detailed description should not be construed as limiting the invention but as a more detailed description of certain aspects, features and embodiments of the invention.
It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference herein for the purpose of disclosing and describing the methods and/or materials associated with the documents. In case of conflict with any incorporated document, the present specification will control.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The description and examples are intended to be illustrative only.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
The "parts" in the present invention are all parts by mass unless otherwise specified.
Example 1
1. Preparation of the prevulcanised dispersion: adding 1 part by weight of sulfur, 0.6 part by weight of ZnO, 1 part by weight of accelerator ZDC, 0.4 part by weight of accelerator PX, 2640.7 parts by weight of anti-aging agent, 0.4 part by weight of anti-aging agent WSL, 0.3 part by weight of KOH, 0.2 part by weight of casein and 4.6 parts by weight of deionized water into a ball mill, emulsifying and dispersing to prepare a pre-vulcanized dispersion with a solid content of 50 wt%;
2. pre-vulcanizing: adding a casein solution (0.9 part of casein dissolved in 10 parts of water), a KOH solution (1.5 parts of potassium hydroxide dissolved in 15 parts of water) and 2 parts of a reinforcing agent into 1000 parts of natural latex (the solid content of the latex is 60 wt%), uniformly mixing, heating to raise the temperature to 35 ℃, adding 35 parts of a prevulcanized dispersion, continuously raising the temperature to 55 ℃, and carrying out heat preservation reaction for 3 hours;
3. concentration: concentrating the pre-vulcanized latex in a centrifugal concentration mode until the solid content is 65 wt%, forming a negative pressure of 75mm Hg by using a vacuum pump, and performing defoaming treatment to obtain a spinning solution;
4. and (3) extrusion molding: introducing the spinning solution into an extrusion cylinder, selecting an extrusion needle with the inner diameter of 0.16mm, extruding the spinning solution into a coagulating bath (the volume ratio of ethanol to water is 80:20) for coagulation forming, and obtaining the latex yarn to be vulcanized;
5. and (3) vulcanization: drawing the latex filaments to be vulcanized to a vulcanization area by a tractor, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 5 minutes, so as to obtain vulcanized latex filaments;
6. and (3) post-treatment: and cooling and coating the vulcanized latex yarn with powder to obtain the finished latex yarn.
The superfine high-elastic latex yarn with the diameter of 150 mu m can be prepared by the embodiment, and the breaking elongation of the superfine high-elastic latex yarn can reach 1400%.
Example 2
1. Preparation of the prevulcanised dispersion: adding 0.8 part of sulfur, 0.4 part of ZnO, 0.7 part of accelerator ZDC, 0.1 part of accelerator PX, 2640.2 parts of anti-aging agent, 0.2 part of anti-aging agent WSL, 0.2 part of KOH, 0.1 part of casein and 2.7 parts of deionized water into a ball mill by weight part, emulsifying and dispersing to prepare a pre-vulcanized dispersion with the solid content of 50 wt%;
2. pre-vulcanizing: adding casein solution (0.7 part dissolved in 10 parts of water), KOH solution (1 part of potassium hydroxide dissolved in 15 parts of water) and reinforcing agent into 1000 parts of natural latex (the solid content of the latex is 60 wt%), uniformly mixing, heating to raise the temperature, adding 40 parts of prevulcanized dispersoid after the temperature is raised to 35 ℃, continuing to raise the temperature to 70 ℃, and carrying out heat preservation reaction for 2 hours;
3. concentration: concentrating the pre-vulcanized latex in a centrifugal concentration mode until the solid content is 65 wt%, forming a negative pressure of 100mm Hg by using a vacuum pump, and performing defoaming treatment to obtain a spinning solution;
4. and (3) extrusion molding: introducing the spinning solution into an extrusion cylinder, selecting an extrusion needle with the inner diameter of 0.16mm, extruding the spinning solution into a coagulating bath (the volume ratio of ethanol to water is 80:20) for coagulation forming, and obtaining the latex yarn to be vulcanized;
5. and (3) vulcanization: drawing the solidified latex filaments to a vulcanization area by a tractor, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 5 minutes, so as to obtain vulcanized latex filaments;
6. and (3) post-treatment: and cooling and coating the vulcanized latex yarn with powder to obtain the finished latex yarn.
The superfine high-elastic latex yarn with the diameter of 150 mu m can be prepared by the embodiment, and the breaking elongation can reach 1305%.
Example 3
1. Preparation of the prevulcanised dispersion: adding 0.9 part of sulfur, 0.5 part of ZnO, 0.8 part of accelerator ZDC, 0.2 part of accelerator PX, 2640.5 parts of anti-aging agent, 0.3 part of anti-aging agent WSL, 0.25 part of KOH, 0.15 part of casein and 3.6 parts of deionized water into a ball mill by weight part, emulsifying and dispersing to prepare a pre-vulcanized dispersion with 50 wt% of solid content;
2. pre-vulcanizing: adding casein solution (0.8 part dissolved in 10 parts of water), KOH solution (1.3 parts of potassium hydroxide dissolved in 15 parts of water) and 2 parts of reinforcing agent into 1000 parts of natural latex (the solid content of the latex is 60 wt%), uniformly mixing, heating to raise the temperature to 35 ℃, adding 38.4 parts of prevulcanized dispersoid, continuously raising the temperature to 65 ℃, and carrying out heat preservation reaction for 2.5 hours.
3. Concentration: concentrating the prevulcanized latex by adopting a centrifugal concentration mode to reach the solid content of 65 wt%, forming a negative pressure of about 90mm Hg by using a vacuum pump, and performing defoaming treatment to obtain a spinning solution;
4. and (3) extrusion molding: introducing the spinning solution into an extrusion cylinder, selecting an extrusion needle with the inner diameter of 0.11mm, extruding the spinning solution into a coagulating bath (the volume ratio of ethanol to water is 70:30) for coagulation forming, and obtaining the latex yarn to be vulcanized;
5. and (3) vulcanization: drawing the vulcanized latex yarn to a vulcanization area by a tractor, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 5 minutes, so as to obtain the vulcanized latex yarn;
6. and (3) post-treatment: and cooling and coating the vulcanized latex yarn with powder to obtain the finished latex yarn.
The cross-sectional scanning electron microscope of the ultra-fine high elastic latex yarn with a diameter of 100 μm prepared by this example is shown in FIG. 2, and according to the test result of FIG. 4, the breaking elongation of the latex yarn can reach 1400%.
Example 4
1. Preparation of the prevulcanised dispersion: adding 0.9 part of sulfur, 0.5 part of ZnO, 0.8 part of accelerator ZDC, 0.2 part of accelerator PX, 2640.5 parts of anti-aging agent, 0.3 part of anti-aging agent WSL, 0.25 part of KOH, 0.15 part of casein and 3.6 parts of deionized water into a ball mill by weight part, emulsifying and dispersing to prepare a pre-vulcanized dispersion with 50 wt% of solid content;
2. pre-vulcanizing: adding casein solution (0.9 part dissolved in 10 parts of water), KOH solution (1.5 parts of potassium hydroxide dissolved in 15 parts of water) and 2 parts of reinforcing agent into 1000 parts of natural latex (the solid content of the latex is 60 wt%), uniformly mixing, heating to raise the temperature, adding 38.4 parts of prevulcanized dispersoid after the temperature is raised to 35 ℃, continuing to raise the temperature to 55 ℃, and carrying out heat preservation reaction for 2.5 hours;
3. concentration: concentrating the prevulcanized latex by adopting a centrifugal concentration mode to reach the solid content of 70 wt%, forming a negative pressure of about 90mm Hg by using a vacuum pump, and performing defoaming treatment to obtain a spinning solution;
4. and (3) extrusion molding: introducing the spinning solution into an extrusion cylinder, selecting an extrusion needle with the inner diameter of 0.21mm, extruding the spinning solution into a coagulating bath (the volume ratio of ethanol to water is 80:20) for coagulation forming, and obtaining the latex yarn to be vulcanized;
5. and (3) vulcanization: drawing the latex filaments to be vulcanized to a vulcanization area by a tractor, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 5 minutes, so as to obtain vulcanized latex filaments;
6. and (3) post-treatment: and cooling and coating the vulcanized latex yarn with powder to obtain the finished latex yarn.
The ultra-fine high-elastic latex yarn with the diameter of 200 μm can be prepared by the embodiment, the cross-sectional scanning electron microscope picture of the ultra-fine high-elastic latex yarn is shown in figure 3, and the breaking elongation of the latex yarn can reach 1390%.
Example 5
1. Preparation of the prevulcanised dispersion: adding 0.9 part of sulfur, 0.5 part of ZnO, 0.8 part of accelerator ZDC, 0.2 part of accelerator PX, 2640.5 parts of anti-aging agent, 0.3 part of anti-aging agent WSL, 0.25 part of KOH, 0.15 part of casein and 3.6 parts of deionized water into a ball mill by weight part, emulsifying and dispersing to prepare a pre-vulcanized dispersion with 50 wt% of solid content;
2. pre-vulcanizing: adding casein solution (0.9 parts dissolved in 10 parts of 50 ℃ warm water), KOH solution (1.5 parts of potassium hydroxide dissolved in 15 parts of water), 2 parts of reinforcing agent and 2 parts of color paste (permanent yellow) into 1000 parts of natural latex (the solid content of the latex is 60 wt%), uniformly mixing, heating to raise the temperature to 35 ℃, adding 38.4 parts of prevulcanized dispersoid, continuously raising the temperature to 55 ℃, and carrying out heat preservation reaction for 2.5 hours;
3. concentration: concentrating the prevulcanized latex by adopting a centrifugal concentration mode to reach the solid content of 70 wt%, forming a negative pressure of about 90mm Hg by using a vacuum pump, and performing defoaming treatment to obtain a spinning solution;
4. and (3) extrusion molding: introducing the spinning solution into an extrusion cylinder, selecting an extrusion needle with the inner diameter of 0.21mm, extruding the spinning solution into a coagulating bath (the volume ratio of ethanol to water is 70:30) for coagulation forming, and obtaining the latex yarn to be vulcanized;
5. and (3) vulcanization: drawing the latex filaments to be vulcanized to a vulcanization area by a tractor, wherein the vulcanization temperature is 120 ℃, and the vulcanization time is 5 minutes, so as to obtain vulcanized latex filaments;
6. and (3) post-treatment: and cooling and coating the vulcanized latex yarn with powder to obtain the finished latex yarn.
The superfine high-elastic color latex yarn with the diameter of 200 mu m can be prepared by the embodiment, and the breaking elongation can reach 1370%.
Comparative example 1
The difference from example 1 is only that comparative example 1 is not pre-vulcanized and concentrated, that is, the raw material components are added, mixed uniformly, defoamed, and then extruded into filaments directly, and kaolin is also added into the latex in the following amount: 20 parts of kaolin clay is added to 1000 parts of natural rubber latex (60 wt% solids content of the latex).
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously discharge the latex yarn, and the latex yarn with the diameter of 300 microns can be prepared after the extrusion head is adjusted. The comparative example adopts a large amount of inert filler, which can cause the agglomeration of rubber particles in latex, gel is not easy to settle and filter, bubbles are not easy to escape, and a nozzle is easy to block, so that the stability of the latex is poor, only the latex filaments with the diameter of about 300 mu m can be obtained, and the breaking elongation can reach 1009%.
Comparative example 2
The only difference from example 1 is that comparative example 2 is not prevulcanized and concentrated, i.e. the raw material components are added and mixed homogeneously, defoamed and then extruded directly into filaments.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex yarn with the diameter of 500 microns after the extrusion head is adjusted.
The spinning solution prepared by the comparative example does not contain inert filler, so that the latex is more stable, and the agglomeration of rubber particles in the latex is reduced, but a new problem is caused, namely the latex cannot meet the requirement of extrusion molding, so that only the latex yarn with the diameter of about 500 mu m can be prepared, and the requirement of superfine latex yarn cannot be met.
Comparative example 3
The only difference from example 1 is that in the precuring step, the reaction was maintained at a temperature of 50 ℃.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex yarn with the diameter of 290 mu m, and the breaking elongation of the latex yarn can reach 915% after the extrusion head is adjusted.
Comparative example 4
The only difference from example 2 is that in the precuring step, the reaction was maintained at a temperature of 75 ℃.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex filaments with the diameter of 360 mu m after the extrusion head is adjusted, and the breaking elongation of the latex filaments can reach 1070 percent.
Comparative example 5
The only difference from example 2 is that the reaction was maintained for 1.5 hours in the precuring step.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex yarn with the diameter of 260 mu m after the extrusion head is adjusted, and the breaking elongation of the latex yarn can reach 1109%.
Comparative example 6
The only difference from example 1 is that in the precuring step, the reaction was maintained for 3.5 hours.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex yarn with the diameter of 240 microns after the extrusion head is adjusted, and the breaking elongation of the latex yarn can reach 1015%.
Comparative example 7
The only difference from example 1 is that in the precuring step, the precured dispersion was added in an amount of 30 parts.
By the comparison example, the extrusion needle with the inner diameter of 0.16mm can not stably and continuously produce the filament, and the emulsion filament with the diameter of 280 μm can be prepared after the extrusion head is adjusted, and the breaking elongation can reach 1021%.
Comparative example 8
The only difference from example 2 is that in the precuring step, the precured dispersion was added in an amount of 45 parts.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the latex yarn with the diameter of 260 mu m after the extrusion head is adjusted, and the breaking elongation of the latex yarn can reach 1100%.
Comparative example 9
The only difference from example 3 is that comparative example 9 uses an acetic acid coagulation bath with a volume ratio of acetic acid to water of 30: 70.
According to the comparative example, the extrusion needle with the inner diameter of 0.11mm cannot stably and continuously produce the latex yarn with the diameter of 250 microns, and the breaking elongation of the latex yarn is lower and only reaches 903% according to the test result of figure 4.
Comparative example 10
The only difference from example 1 is that comparative example 10 uses a pure ethanol coagulation bath.
According to the comparative example, the extrusion needle with the inner diameter of 0.16mm cannot stably and continuously produce the filament, the latex filament with the diameter of 300 mu m can be prepared after the extrusion head is adjusted, and the breaking elongation can reach 1005%.
Comparative example 11
The only difference from example 3 is that the volume ratio of ethanol to water in the mixed coagulation bath of ethanol and water is 60: 40.
According to the comparative example, the extrusion needle with the inner diameter of 0.11mm cannot stably and continuously produce the latex yarn with the diameter of 340 mu m after the extrusion head is adjusted, and the breaking elongation of the latex yarn can reach 890 percent.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.

Claims (9)

1. The superfine high-elastic latex yarn is characterized by comprising the following raw materials in parts by weight: 1000 parts of natural latex, 35-40 parts of prevulcanized dispersoid, 0.7-0.9 part of casein, 1-1.5 parts of KOH and 2-5 parts of reinforcing agent;
the raw materials of the pre-vulcanized dispersion comprise the following components in parts by weight: 0.8-1 part of sulfur, 0.4-0.6 part of ZnO, 0.7-1 part of accelerator ZDC, 0.1-0.4 part of accelerator PX, 2640.2-0.7 part of anti-aging agent, 0.2-0.4 part of anti-aging agent WSL, 0.2-0.3 part of KOH, 0.1-0.2 part of casein and 2.7-4.6 parts of deionized water.
2. The ultra-fine high-elastic latex yarn as claimed in claim 1, wherein said reinforcing agent is carbon black or white carbon black.
3. The ultra-fine high-elastic latex yarn as claimed in claim 1, wherein the raw material of said ultra-fine high-elastic latex yarn further comprises a color paste.
4. A method for preparing the ultra-fine high elastic latex yarn as claimed in any one of claims 1 to 2, comprising the steps of:
(1) preparation of the prevulcanised dispersion:
mixing and dispersing sulfur, ZnO, a promoter ZDC, a promoter PX, an anti-aging agent 264, an anti-aging agent WSL, KOH, casein and deionized water to obtain a pre-vulcanized dispersion;
(2) pre-vulcanizing:
adding casein, KOH and a reinforcing agent into natural latex, uniformly mixing, heating, adding the prevulcanized dispersion, continuously heating to 55-70 ℃, and reacting for 2-3h to obtain prevulcanized latex;
(3) concentration:
concentrating and defoaming the prevulcanized latex solution to obtain a spinning solution;
(4) and (3) extrusion molding:
extruding the spinning solution into gel filaments, and solidifying and forming the gel filaments in a coagulating bath to obtain to-be-vulcanized latex filaments;
(5) and (3) vulcanization:
and vulcanizing the latex yarn to be vulcanized to obtain vulcanized latex yarn, cooling and coating powder to obtain the superfine high-elasticity latex yarn.
5. The method according to claim 4, wherein in step (2), casein and KOH are added in the form of aqueous solutions, respectively, wherein the mass ratio of casein to water is 0.9:10 and the mass ratio of KOH to water is 1.5: 15.
6. The method according to claim 4, wherein in the step (2), the precured dispersion is added by heating to 35 ℃.
7. The method according to claim 4, wherein in the step (3), the concentration is carried out to concentrate the pre-vulcanized latex solution to a solid content of 65-70 wt%, and the defoaming treatment is carried out under vacuum at a negative pressure of 75-100mm Hg.
8. The production method according to claim 4, wherein in the step (4), the coagulation bath is a mixed coagulation bath of ethanol and water, and the volume ratio of ethanol to water is 70-80: 20-30.
9. The production method according to claim 4, wherein in the step (5), the temperature of the vulcanization treatment is 120 ℃ for 5 minutes.
CN202110702621.4A 2021-06-24 2021-06-24 Preparation method of superfine high-elastic latex yarn Active CN113550024B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110702621.4A CN113550024B (en) 2021-06-24 2021-06-24 Preparation method of superfine high-elastic latex yarn

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110702621.4A CN113550024B (en) 2021-06-24 2021-06-24 Preparation method of superfine high-elastic latex yarn

Publications (2)

Publication Number Publication Date
CN113550024A true CN113550024A (en) 2021-10-26
CN113550024B CN113550024B (en) 2022-03-11

Family

ID=78102341

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110702621.4A Active CN113550024B (en) 2021-06-24 2021-06-24 Preparation method of superfine high-elastic latex yarn

Country Status (1)

Country Link
CN (1) CN113550024B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114134597A (en) * 2021-12-13 2022-03-04 罗莱生活科技股份有限公司 Latex-lyocell composite fiber and preparation method thereof
CN115948819A (en) * 2022-12-26 2023-04-11 广东国兴乳胶丝有限公司 Method for manufacturing high-toughness ultra-fine-diameter latex yarn

Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102181949A (en) * 2011-03-22 2011-09-14 开平市冠威乳胶设备制造有限公司 Production process of rubber latex thread
CN103320884A (en) * 2012-03-22 2013-09-25 福建三信织造有限公司 Latex thread formula
CN103320903A (en) * 2013-06-19 2013-09-25 福建三信织造有限公司 High-temperature-resistant latex yarn
CN103319630A (en) * 2013-06-19 2013-09-25 福建三信织造有限公司 Low-temperature-resistant latex yarn
CN103342831A (en) * 2013-06-19 2013-10-09 福建三信织造有限公司 Recovery method for waste of dry glue
CN104499094A (en) * 2014-12-12 2015-04-08 广东国兴乳胶丝有限公司 Superfine latex thread and production method thereof
CN106243416A (en) * 2016-08-23 2016-12-21 刘勇 A kind of rubber latex thread Recipe
CN108129711A (en) * 2017-11-23 2018-06-08 苏州嘉乐威企业发展有限公司 Antimicrobial form rubber condoms and preparation method thereof
CN108779257A (en) * 2016-03-10 2018-11-09 日本瑞翁株式会社 The latex and its manufacturing method of synthetic rubber
CN109294007A (en) * 2018-09-25 2019-02-01 桂林紫竹乳胶制品有限公司 A kind of hybrid dispersions and preparation method thereof for Heveatex presulfurization
CN110294848A (en) * 2019-07-04 2019-10-01 中国热带农业科学院农产品加工研究所 The method and latex product of fresh Heveatex presulfurization

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102181949A (en) * 2011-03-22 2011-09-14 开平市冠威乳胶设备制造有限公司 Production process of rubber latex thread
CN103320884A (en) * 2012-03-22 2013-09-25 福建三信织造有限公司 Latex thread formula
CN103320903A (en) * 2013-06-19 2013-09-25 福建三信织造有限公司 High-temperature-resistant latex yarn
CN103319630A (en) * 2013-06-19 2013-09-25 福建三信织造有限公司 Low-temperature-resistant latex yarn
CN103342831A (en) * 2013-06-19 2013-10-09 福建三信织造有限公司 Recovery method for waste of dry glue
CN104499094A (en) * 2014-12-12 2015-04-08 广东国兴乳胶丝有限公司 Superfine latex thread and production method thereof
CN108779257A (en) * 2016-03-10 2018-11-09 日本瑞翁株式会社 The latex and its manufacturing method of synthetic rubber
CN106243416A (en) * 2016-08-23 2016-12-21 刘勇 A kind of rubber latex thread Recipe
CN108129711A (en) * 2017-11-23 2018-06-08 苏州嘉乐威企业发展有限公司 Antimicrobial form rubber condoms and preparation method thereof
CN109294007A (en) * 2018-09-25 2019-02-01 桂林紫竹乳胶制品有限公司 A kind of hybrid dispersions and preparation method thereof for Heveatex presulfurization
CN110294848A (en) * 2019-07-04 2019-10-01 中国热带农业科学院农产品加工研究所 The method and latex product of fresh Heveatex presulfurization

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
卢秋余等: "硅藻土在乳胶丝胶乳中的应用研究", 《橡胶科技》 *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114134597A (en) * 2021-12-13 2022-03-04 罗莱生活科技股份有限公司 Latex-lyocell composite fiber and preparation method thereof
CN114134597B (en) * 2021-12-13 2023-10-31 罗莱生活科技股份有限公司 Latex-lyocell composite fiber and preparation method thereof
CN115948819A (en) * 2022-12-26 2023-04-11 广东国兴乳胶丝有限公司 Method for manufacturing high-toughness ultra-fine-diameter latex yarn

Also Published As

Publication number Publication date
CN113550024B (en) 2022-03-11

Similar Documents

Publication Publication Date Title
CN113550024B (en) Preparation method of superfine high-elastic latex yarn
CN106832261B (en) A kind of High-performance graphene/nylon 6 nano-composite and preparation method thereof
CN109722022B (en) Extrusion and blow molding grade glass fiber reinforced nylon material and preparation method thereof
CN101691445A (en) Alcoholysis resistant PA66 composite material used for automobiles and preparation method thereof
CN111423633A (en) Nano hybrid filler reinforced rubber material and preparation process thereof
CN109836734B (en) Modification method of anti-ultraviolet PVC composite material
CN111205587B (en) Antistatic high-strength ABS (acrylonitrile-butadiene-styrene) modified material and preparation method thereof
CN113845704B (en) Natural latex ultrathin condom and preparation method thereof
CN116575184B (en) Preparation method of polytetrafluoroethylene nanofiber membrane
CN109776830A (en) A kind of polyurethane/carboxymethyl chitosan/PAn conducting membrane preparation method
CN108948468A (en) A kind of preparation method of the corrosion-resistant vulcanization rubber compound of the oil resistant of the alumina filled modification of graphene oxide-glass fibre-
CN112500619A (en) Aramid fiber reinforced nitrile rubber composite material and preparation method thereof
CN110734593A (en) Method for preparing emulsion polymerized styrene butadiene rubber from modified graphene
CN114834076B (en) Preparation method and device for directly forming large-diameter latex filaments
CN114539646A (en) High-strength wear-resistant rubber and preparation method thereof
CN115558220A (en) Antistatic SPU sole material and preparation method thereof
CN115044111A (en) Preparation method and application of light-color spinning rubber roll high polymer material
CN112646275B (en) Conductive polyolefin master batch and preparation method thereof
CN114262513A (en) Glass fiber reinforced nylon 6 composite material
CN110734589A (en) Method for preparing emulsion polymerized styrene butadiene rubber from modified graphene
CN111978570A (en) Method for vulcanizing and packaging graphene modified natural latex
CN109265883A (en) A kind of engine fuel rubber tube and preparation method thereof
CN118374068B (en) Preparation method and application of diatomite and zinc oxide composite high-density rubber material
CN114031698B (en) Butadiene rubber raw rubber and preparation method thereof
CN115490936A (en) High-resilience and high-strength organic silicon rubber and preparation method thereof

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