CN107313123B - A kind of polynosic fibre and preparation method thereof - Google Patents

A kind of polynosic fibre and preparation method thereof Download PDF

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CN107313123B
CN107313123B CN201611035584.1A CN201611035584A CN107313123B CN 107313123 B CN107313123 B CN 107313123B CN 201611035584 A CN201611035584 A CN 201611035584A CN 107313123 B CN107313123 B CN 107313123B
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reinforcing agent
mass concentration
viscose rayon
added
preparation
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CN107313123A (en
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***
徐卫林
李昌垒
李林峰
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Wuhan Textile University
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Wuhan Textile University
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    • 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
    • D01F2/00Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
    • D01F2/06Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
    • D01F2/08Composition of the spinning solution or the bath

Abstract

A kind of polynosic fibre and preparation method thereof, is related to textile fabric processing technique field, which is that the first reinforcing agent is added in viscose glue stoste, is uniformly mixing to obtain mixed solution;Mixed solution is subjected to deaeration, filtering, then passes through spinneret, into the coagulating bath added with the second reinforcing agent, forming obtains viscose rayon;After carrying out drawing-off to viscose rayon, into progress silk bath in the silk bath foam added with third reinforcing agent.The preparation method is to add different reinforcing agents in the different processes of viscose rayon production, be crosslinked between cellulosic molecule, the constantly intensity of enhancing viscose rayon, the wet strong and dry strong higher of polynosic fibre is made, therefore the preparation method and polynosic fibre obtained are suitble to promote and apply.

Description

A kind of polynosic fibre and preparation method thereof
Technical field
The present invention relates to a kind of textile fabric processing technique field, and in particular to a kind of polynosic fibre and its system Preparation Method.
Background technique
Viscose rayon is a kind of textile fabric very widely used at present, is raw by primary raw material of native cellulose The staple fibre of production, the natural cellulosic materials such as cotton, bamboo and wood slurry provide extensive raw material basis for viscose rayon.In addition, viscous Certain performances of glue fiber and natural cotton fiber are very much like, all have preferable hygroscopicity, stainability, antistatic, dress is relaxed It is suitable, have the advantages that chemical fibre is incomparable, product wearability is good.But its disadvantage is also evident from: viscose rayon Intensity difference, especially wet strong lower, usually only dry strong half or so, therefore, the fabric made of viscose rayon is not It can wash by rubbing with the hands strongly, it is short to take the service life.
Over more than 100 years, the production technology of viscose rayon constantly improves, and the viscose rayon of different mechanical properties gradually emerges in large numbers, Such as: high-wet-modulus fibre, high crimped fibre, strong fiber.The Chinese invention patent of application number CN201210183713.7 Application discloses a kind of polynosic fibre and its production method, and specifically include step: by mass percentage: polyvinyl alcohol is molten The ratio of liquid 1~60%, viscose glue stoste 40~99% is blended, and passes through stirring, deaeration, filtering, spinning, drawing-off, crosslinking process stream It is by force 3.4~5.8cN/dtex that journey, which is made dry, and wet be 1.9~4.1cN/dtex by force, and hygrometric state elasticity modulus is 0.65~1.60cN/ The viscose rayon of dtex, the intensity high 30~50% of the slight viscose rayon spun compared with traditional handicraft of gained viscose rayon with On.The technology utilizes the characteristics of unique polyhydroxy mafic of polyvinyl alcohol and high polymerization degree, and it is molten that spinning is made with viscose glue dope blending Liquid, to improve the intensity of viscose rayon.Although the addition of polyvinyl alcohol can improve the wet strong of viscose rayon, in this process Polyvinyl alcohol is not crosslinked, and the hot water resistance of fiber is poor, is still unable to satisfy the subsequent dyeing and printing process of viscose rayon product Demand;Moreover, the dry strong lower of viscose rayon made from polyvinyl alcohol is added, brittleness is larger, easily formation filtration structures, causes The practicability of the technology is very poor.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of polynosic fibre, viscose rayon heat-proof water obtained Property preferable, and dry, wet strength with higher, be suitable for commercial introduction application.
Another object of the present invention is to provide a kind of polynosic fibres, and hot water resistance is preferable, do it is strong, wet by force compared with Height is suitable for commercial introduction application.
The present invention solves its technical problem and adopts the following technical solutions to realize.
The present invention proposes a kind of preparation method of polynosic fibre comprising following steps:
The first reinforcing agent is added in viscose glue stoste, is uniformly mixing to obtain mixed solution;Mixed solution is subjected to deaeration, mistake Then spinneret is passed through in filter, into the coagulating bath added with the second reinforcing agent, forming obtains viscose rayon;To viscose rayon Drawing-off is carried out, into progress silk bath in the silk bath foam added with third reinforcing agent.
Further, in a preferred embodiment of the present invention, the first reinforcing agent is the polyamides that mass concentration is 12%~13% At least one of amine epoxychloropropane aqueous solution, aq. polyethyleneimine that mass concentration is 12%~13%.
Further, in a preferred embodiment of the present invention, the additive amount of the first reinforcing agent is the 1% of the weight of viscose glue stoste ~5%.
Further, in a preferred embodiment of the present invention, the second reinforcing agent is the polyamides that mass concentration is 12%~13% Aq. polyethyleneimine that amine epoxychloropropane aqueous solution, mass concentration are 12%~13%, mass concentration be 12%~ At least one of 13% urea-formaldehyde resin aqueous solution.
Further, in a preferred embodiment of the present invention, the additive amount of the second reinforcing agent is the weight of coagulating bath 0.01%~10%.
Further, in a preferred embodiment of the present invention, third reinforcing agent is the polyamides that mass concentration is 12%~13% At least one of amine epoxychloropropane aqueous solution, casein-formalin that mass concentration is 12%~13%.
Further, in a preferred embodiment of the present invention, the additive amount of third reinforcing agent is the weight of silk bath foam 0.01%~10%.
Further, in a preferred embodiment of the present invention, coagulating bath is by least 60~100g/L sulfuric acid, 200~400g/L Sodium sulphate and 10~80g/L zinc sulfate mix.
A kind of polynosic fibre uses the preparation method of above-mentioned polynosic fibre to be made.
Further, in a preferred embodiment of the present invention, the dry of polynosic fibre is 3.8~6cN/dtex by force, wet It is by force 2.6~4.8cN/dtex.
The beneficial effect of the polynosic fibre of the embodiment of the present invention and preparation method thereof is:
1, the preparation method of the embodiment of the present invention is that the first reinforcing agent is added in viscose glue stoste, is uniformly mixing to obtain mixing Solution;Mixed solution is subjected to deaeration, filtering, then passes through spinneret, into the coagulating bath added with the second reinforcing agent, at Shape obtains viscose rayon;Drawing-off is carried out to viscose rayon, into progress silk bath in the silk bath foam added with third reinforcing agent.Not With different reinforcing agents in process, is added, viscose rayon molecule is acted on, makes to carry out between the cellulose macromolecule of shaped fibers Crosslinking, and then constantly enhance the intensity of the viscose rayon of forming.Just because of be crosslinked between molecule in fiber, then it is obtained Polynosic fibre it is wet strong and dry strong higher, therefore the preparation method and polynosic fibre obtained are suitble to promote Using.
2, the intensity with higher of polynosic fibre obtained by the embodiment of the present invention, 3.8~6cN/ of Gan Qiangwei Dtex, wet be 2.6~4.8cN/dtex by force, and uses conventional traditional handicraft institute's spunbond glue fiber dry strong for 2.1~2.2cN/ Dtex, therefore, fibre strength made from the preparation process using polynosic fibre are higher, and it is with good bullet Property, hygroscopicity, stainability etc., are widely used.
3, the preparation method of the embodiment of the present invention can be directly adjusted in common viscose fiber production technology, without spy Different equipment can produce polynosic fibre in common viscose rayon production equipment;Operating process facilitate it is easily-controllable, easily In realization industrialized production.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, according to normal conditions or manufacturer builds The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase Product.
Polynosic fibre of the embodiment of the present invention and preparation method thereof is specifically described below.
The embodiment of the present invention provides a kind of preparation method of polynosic fibre comprising following steps:
S1, the first reinforcing agent is added in viscose glue stoste, be uniformly mixing to obtain mixed solution.Wherein, the first reinforcing agent is The polyethyleneimine that polyamideepichlorohydrin aqueous solution that mass concentration is 12%~13%, mass concentration are 12%~13% At least one of aqueous solution, above-mentioned solution dissolve in viscose glue stoste, polyamideepichlorohydrin aqueous solution mass concentration Preferably 12.5%, aq. polyethyleneimine mass concentration is preferably 12.5%, and the first reinforcing agent is preferably that mass concentration is 12.5% polyamideepichlorohydrin aqueous solution.The additive amount of first reinforcing agent is the 1%~5% of the weight of viscose glue stoste. Mixed solution specific is the preparation method comprises the following steps: viscose glue stoste and the first reinforcing agent to be put into blender and be stirred, mixing time It is 0.5~2 hour, the revolving speed of blender is 100~2000 revs/min to get mixed solution.
After polyamideepichlorohydrin aqueous solution is added in viscose glue stoste, viscose rayon molecule can be dispersed in It is interior, when viscose rayon obtained is dry after solidification, drawing-off, silk bath for viscose glue stoste, these polyamideepichlorohydrin molecules Be crosslinked with the hydroxyl in cellulose, therefore, product it is dry strong higher, after product is placed in water, daiamid epoxy chlorine third Alkane acts between the molecule of cross filament, keeps its reticular structure, therefore, Related product it is wet strong higher.
After aq. polyethyleneimine is added in viscose glue stoste, containing more in polyethyleneimine polymers strand A cation group, the hydroxyl in the cation group and cellulose form very strong cross-bond, therefore, Related product it is dry strong With it is wet strong higher.
S2, mixed solution is carried out to deaeration, filtering, then passes through spinneret, into the solidification for being added with the second reinforcing agent In bath, forming obtains viscose rayon.Wherein, coagulating bath by least 60~100g/L sulfuric acid, 200~400g/L sodium sulphate and 10~ 80g/L zinc sulfate mixes.Second reinforcing agent be mass concentration be 12%~13% polyamideepichlorohydrin aqueous solution, In the urea-formaldehyde resin aqueous solution that aq. polyethyleneimine that mass concentration is 12%~13%, mass concentration are 12%~13% At least one, dissolve in coagulating bath, and significant reaction will not occur with coagulating bath.Polyamideepichlorohydrin aqueous solution matter Measuring concentration is preferably 12.5%, and aq. polyethyleneimine mass concentration is preferably 12.5%, and urea-formaldehyde resin aqueous solution quality is dense Degree preferably 12.5%, the second reinforcing agent is preferably the aq. polyethyleneimine that mass concentration is 12.5%, the second reinforcing agent Additive amount be coagulating bath weight 0.01%~10%.In the present embodiment, defoaming method are as follows: carry out mixed solution at least Twice filtering, then squeeze into deaeration kettle, it is kept the temperature in 20~25 DEG C, deaeration 2~6 hours.
After aq. polyethyleneimine is added in coagulating bath, containing multiple in polyethyleneimine polymers strand Hydroxyl during cation group, the cation group and viscose rayon surface fiber are plain forms very strong cross-bond, therefore, is made Viscose rayon it is dry strong and wet strong higher.
After polyamideepichlorohydrin aqueous solution is added in coagulating bath, it is deposited on viscose rayon intramolecular or absorption In surface, it can not only enhance the intramolecular structure of viscose rayon, its surface texture can also be enhanced, especially when product is placed in After in water, the polyamideepichlorohydrin molecule cross-link on surface reticulates structure, therefore, Related product it is wet strong higher.
After urea-formaldehyde resin aqueous solution is added in coagulating bath, other reinforcing agents are mainly cooperateed with, improve the wet of product By force.
S3, to viscose rayon carry out drawing-off after, into added with third reinforcing agent silk bath foam in carry out silk bath.Wherein, Third reinforcing agent be mass concentration be 12%~13% polyamideepichlorohydrin aqueous solution, mass concentration be 12%~13% At least one of casein-formalin, polyamideepichlorohydrin aqueous solution mass concentration is preferably 12.5%, junket Element-formalin mass concentration is preferably 12.5%, and third reinforcing agent is preferably that mass concentration is 12.5% daiamid epoxy Chloropropane aqueous solution.The additive amount of third reinforcing agent is the 0.01%~10% of the weight of silk bath foam.
After polyamideepichlorohydrin aqueous solution is added in a bath foam, it is adsorbed in viscose rayon surface, works as product After being placed in water, the polyamideepichlorohydrin molecule cross-link on surface reticulates structure, therefore, product it is wet strong higher.
After casein-formalin is added in a bath foam, casein forms three-dimensional net structure after formaldehyde crosslinking, It is attached to the surface of viscose rayon, improves the dry strong and wet strong of Related product.
S4, it the processes such as is cut off to obtained fiber, washes, dries, polynosic fibre is finally made.
In short, the embodiment of the present invention adds reinforcing agent during preparing viscose rayon, mainly in viscose glue stoste, solidification Different intensity reinforcing agents is added respectively in bath or silk bath foam, in different processes, adds different reinforcing agents, it is therefore an objective to act on It is crosslinked between viscose rayon inner cellulose molecule, and then constantly enhances the intensity of the viscose rayon of forming, so as to The dry and wet intensity of viscose rayon, the mechanism of action is greatly improved are as follows:
The first reinforcing agent is added in viscose glue stoste, since the hydroxyl of cellulose in viscose rayon stoste has negative electrical charge, Can attract each other with the positive charge in the first reinforcing agent, therefore carry out deaeration, after filtering in viscose glue stoste, by spinneret into After entering coagulating bath, cellulosic molecule in viscose glue stoste is able to carry out intramolecular friendship due directly to positive charge attracts each other Connection, this crosslinking are to be crosslinked in reticular structure, therefore fiber obtained has higher intensity.
The second reinforcing agent is added in coagulating bath, is mainly used for depositing in Forming of Viscose Rayon, be permeated in viscose rayon It is interior, or it is adsorbed in the fiber surface after forming, and then reticulate structure with molecule cross-link in fiber, increase the strong of viscose rayon Degree.
Third reinforcing agent is added in silk bath foam, mainly reinforcing agent is adsorbed in viscose rayon surface or further infiltration To fibrous inside, molecule cross-link reticulates structure in third reinforcing agent and fiber, increases the intensity of viscose rayon.
The embodiment of the present invention also provides a kind of polynosic fibre, using the preparation method of above-mentioned polynosic fibre It is made, the dry of the polynosic fibre is 3.8~6cN/dtex by force, and wet be 2.6~4.8cN/dtex by force.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
Embodiment 1 provides a kind of polynosic fibre, prepares in accordance with the following methods:
By 100kg viscose glue stoste and 1kg polyamideepichlorohydrin aqueous solution, (mass concentration 12.5% is by polyamides Amine epoxychloropropane, which is dissolved into water, to be formulated) it is put into blender and is stirred, mixing time is 2 hours, blender Revolving speed is 200 revs/min to get mixed solution.
Mixed solution is squeezed into and carries out deaeration in deaeration kettle, then carries out three filterings, then passes through spinneret, into adding The 100kg coagulating bath of 10kg urea-formaldehyde resin aqueous solution has been added (10kg urea-formaldehyde resin aqueous solution to be added i.e. in 100kg coagulating bath to stir It mixes and uniformly forms, it is that Lauxite is dissolved into water to be formulated that the mass concentration of urea-formaldehyde resin aqueous solution, which is 12.5%) In, forming obtains viscose rayon.
Drawing-off is carried out to viscose rayon, into the 100kg silk bath foam for being added to 10kg polyamideepichlorohydrin aqueous solution In (i.e. in 100kg bath foams be added 10kg polyamideepichlorohydrin aqueous solution stir evenly, daiamid epoxy chlorine third The mass concentration of alkane aqueous solution is 12.5%, is that polyamideepichlorohydrin is dissolved into water to be formulated) carry out silk bath.
Through detecting, the dry of the polynosic fibre is 6cN/dtex by force, and wet be 4.8cN/dtex by force.
Embodiment 2
Embodiment 2 provides a kind of polynosic fibre, prepares in accordance with the following methods:
By 100kg viscose glue stoste and 5kg polyamideepichlorohydrin aqueous solution, (mass concentration 12% is by polyamide Epoxychloropropane is dissolved into water and is formulated) it is put into blender and is stirred, mixing time is 2 hours, and blender turns Speed is for 1000 revs/min to get mixed solution.
Mixed solution is squeezed into and carries out deaeration in deaeration kettle, is then filtered by twice, finally passes through spinneret, into adding Having added 0.01kg polyamideepichlorohydrin aqueous solution, (mass concentration 12% is that polyamideepichlorohydrin is dissolved into water In be formulated) 100kg coagulating bath (coagulating bath is mixed by 6kg sulfuric acid, 30kg sodium sulphate and 1.6kg zinc sulfate) in, Forming obtains viscose rayon.
Drawing-off is carried out to viscose rayon, (mass concentration 12% is into 0.01kg casein-formalin is added to Casein-formaldehyde is dissolved into water and is formulated) 100kg silk bath foam in carry out silk bath.
Through detecting, the dry of the polynosic fibre is 5cN/dtex by force, and wet be 4cN/dtex by force.
Embodiment 3
Embodiment 3 provides a kind of polynosic fibre, prepares in accordance with the following methods:
By 100kg viscose glue stoste and 1kg aq. polyethyleneimine, (mass concentration 13% is that polyethyleneimine is molten Solution, which enters in water, to be formulated) it is put into blender and is stirred, mixing time is 0.5 hour, the revolving speed of blender is 2000 turns/ Divide to get mixed solution.
Mixed solution is subjected to twice filtering, then is squeezed into deaeration kettle, is kept the temperature in 20 DEG C, deaeration 3 hours, then by spray Filament plate, into 5kg aq. polyethyleneimine is added to, (mass concentration 12.5% is that polyethyleneimine is dissolved into water Be formulated) 100kg coagulating bath (coagulating bath is mixed by 5kg sulfuric acid, 20kg sodium sulphate and 1.5kg zinc sulfate) in, at Shape obtains viscose rayon.
Drawing-off is carried out to viscose rayon, (mass concentration 13% is by junket into 5kg casein-formalin is added to Element-formaldehyde is dissolved into water and is formulated) 100kg silk bath foam in carry out silk bath.
Through detecting, the dry of the polynosic fibre is 4cN/dtex by force, and wet be 3cN/dtex by force.
Embodiment 4
Embodiment 4 provides a kind of polynosic fibre, prepares in accordance with the following methods:
By 100kg viscose glue stoste and 5kg polyamideepichlorohydrin aqueous solution, (mass concentration 13% is by polyamide Epoxychloropropane is dissolved into water and is formulated) it is put into blender and is stirred, mixing time is 1 hour, and blender turns Speed is for 800 revs/min to get mixed solution.
Mixed solution is squeezed into and carries out deaeration in deaeration kettle, then carries out twice filtering, by spinneret, into being added to The 100kg coagulating bath of 5kg urea-formaldehyde resin aqueous solution (mass concentration 12% is that Lauxite is dissolved into water to be formulated) In (coagulating bath is mixed by 8kg sulfuric acid, 30kg sodium sulphate and 10kg zinc sulfate), forming obtains viscose rayon.
To viscose rayon carry out drawing-off, into be added to 5kg casein-formalin (mass concentration 12.5%, be by Casein-formaldehyde is dissolved into water and is formulated) 100kg silk bath foam in carry out silk bath, then the works such as cut off, washed, being dried Polynosic fibre is finally made in sequence.
Through detecting, the dry of the polynosic fibre is 5.2cN/dtex by force, and wet be 3.8cN/dtex by force.
In conclusion viscose rayon made from the preparation method of the polynosic fibre of the embodiment of the present invention dry strong and Wet strong higher, i.e. the intensity of viscose rayon is high, is suitble to promote and apply.
Embodiments described above is a part of the embodiment of the present invention, instead of all the embodiments.Reality of the invention The detailed description for applying example is not intended to limit the range of claimed invention, but is merely representative of selected implementation of the invention Example.Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts Every other embodiment, shall fall within the protection scope of the present invention.

Claims (4)

1. a kind of preparation method of polynosic fibre, which is characterized in that itself the following steps are included:
The first reinforcing agent is added in viscose glue stoste, is uniformly mixing to obtain mixed solution;The mixed solution is subjected to deaeration, mistake Then spinneret is passed through in filter, into the coagulating bath added with the second reinforcing agent, forming obtains viscose rayon;To the viscose glue Fiber carry out drawing-off, into added with third reinforcing agent silk bath foam in carry out silk bath,
First reinforcing agent be mass concentration be 12%~13% polyamideepichlorohydrin aqueous solution, mass concentration be At least one of 12%~13% aq. polyethyleneimine, the additive amount of first reinforcing agent are the viscose glue stoste Weight 1%~5%;Second reinforcing agent is that the polyamideepichlorohydrin that mass concentration is 12%~13% is water-soluble The Lauxite that aq. polyethyleneimine that liquid, mass concentration are 12%~13%, mass concentration are 12%~13% is water-soluble At least one of liquid, the additive amount of second reinforcing agent are the 0.01%~10% of the weight of the coagulating bath;Described Three reinforcing agents be mass concentration be 12%~13% polyamideepichlorohydrin aqueous solution, mass concentration be 12%~13% At least one of casein-formalin, the additive amount of the third reinforcing agent are the 0.01% of the weight of the silk bath foam ~10%.
2. the preparation method of polynosic fibre according to claim 1, which is characterized in that the coagulating bath is by least 60~100g/L sulfuric acid, 200~400g/L sodium sulphate and 10~80g/L zinc sulfate mix.
3. a kind of polynosic fibre, which is characterized in that it uses high intensity described in any one of claims 1 to 2 viscous The preparation method of glue fiber is made.
4. polynosic fibre according to claim 3, which is characterized in that the dry of the polynosic fibre be by force 3.8~6cN/dtex, wet be 2.6~4.8cN/dtex by force.
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