CN105063782B - A kind of high-purity viscose rayon and preparation method thereof - Google Patents
A kind of high-purity viscose rayon and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of high-purity viscose rayon and preparation method thereof, content of ashes accounts for 10~200ppm of high-purity viscose rayon butt weight in high-purity viscose rayon；Dry fracture strength >=2.2cN/dtex of high-purity viscose rayon, dry elongation at break >=15%, wet breaking strength >=1.1cN/dtex.When prepared by high-purity viscose rayon of the present invention, after fiberizing after desulfurization, washing, first pass around hydrochloric acid pre-preg, then bleach, oil after washed by alcohol, multiple salt acid dip is washed, then by repeatedly washing, more than 99% impurity, lignin, hemicellulose in fiber are dissolved, and cellulose can be melted safely, Compound Machining is carried out, the application field of viscose rayon has been widened.
Description
Technical field
The present invention relates to viscose rayon technical field, more particularly to a kind of low high-purity viscose rayon of content of ashes.
Background technology
Viscose rayon, is to glue fine full name.Viscous fibre is the cellulose produced using wood pulp or other native celluloses as raw material
Fiber.The physiological requirement that fine moisture percentage meets human body skin is glued, with the spy such as smooth nice and cool, ventilative, antistatic, dyeing is gorgeous
Property.Viscose rayon belongs to regenerated celulose fibre.It is, using native cellulose as raw material, to be made through processes such as alkalization, aging, sulfonation
Soluble cellulose sulphonic acid ester, is re-dissolved in sig water and viscose glue is made, be made through wet spinning.Common viscose fiber ash content (bag
Including impurity, lignin, hemicellulose etc.) content is in 2000~3000ppm.Cellulose fibre be acknowledged as being not suitable for 435F with
On processing temperature under use because lignin remaining in cellulose and hemicellulose can degrade at this temperature, coking,
So as to cause the discoloration of workpiece, peculiar smell can be also produced sometimes.Therefore, this characteristic of common viscose fiber is just in some processing
A definite limitation is received with using field, such as in the application of viscose-based carbon fiber, because the content of ashes of common viscose fiber
It is higher to be accomplished by carrying out specially treated.
At present, in conventional viscose-based carbon fiber preparation process, raw fibre need to be carbonized or graphitization processing, no
Only prepare cost high, and raw fibre non-cellulosic impurity to the performances of carbon fiber manufactured goods, such as high temperature resistant, corrosion-resistant, anti-
Fatigue, creep resistant, conductive have a great impact with heat conduction, adsorption capacity, intensity, modulus etc..And by charing or graphite
Viscose rayon after change processing, the performance indications such as its elongation, intensity can be all greatly affected, and carbon yield is low.
The content of the invention
First technical problem to be solved by this invention be：In view of the deficienciess of the prior art, providing a kind of ash content
The good high-purity viscose rayon of the physical performance indexs such as content is low, elongation at break, intensity, solves and uses common viscose fiber system
Into carbon fiber poor performance, actual carbon yield is low, prepare the high technical problem of cost.
Second technical problem to be solved by this invention be：In view of the deficienciess of the prior art, providing a kind of high-purity
The preparation method of viscose rayon, this method technique is simple, it is easy to industrialized production, high-purity viscose rayon content of ashes of production
The physical performance indexs such as low, elongation at break, intensity are good, solve be made using common viscose fiber carbon fiber poor performance,
Actual carbon yield is low, prepare the high technical problem of cost.
To solve above-mentioned first technical problem, the technical scheme is that：
Content of ashes accounts for the 10 of high-purity viscose rayon butt weight in a kind of high-purity viscose rayon, high-purity viscose rayon
~200ppm；Dry fracture strength >=2.2cN/dtex of high-purity viscose rayon, dry elongation at break >=15%, wet fracture is strong
Degree >=1.1cN/dtex.
To solve above-mentioned second technical problem, the technical scheme is that：
A kind of preparation method of high-purity viscose rayon, comprises the following steps：
(1) using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure.
(2) the soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution.
(3) viscose solution is obtained into spinning viscose by filtering and deaeration.
(4) after the spinning viscose is extruded by spinneret orifice, spun filament is frozen into coagulating bath.
(5) spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg is carried out under normal temperature, it is described pre-
Dipping concentration of hydrochloric acid used is 1~2 g/l, 3~5 minutes pre-preg time.
(6) by the fiber after pre-preg after bleaching, oiling, extruding stem carries out alcohol and washed, with 3~20g/l's at normal temperatures
Ethanol solution is handled 3~10 minutes.
(7) fiber extrusion after alcohol is washed is done, and first of salt acid dip is carried out at normal temperatures first, in 1~5wt% salt
Impregnated 3~5 minutes in acid solution, hydrochloric acid and fiber bath volume ratio are 15~75:1, extruding stem, repeats multiple hydrochloric acid again
Dipping is washed.
(8) fiber extrusion after salt acid dip is done, washed with distilled water, 30~50 DEG C of washing temperature, the time 3~
5 minutes, after extruding stem, repeat washing, extruding repeatedly, last drying obtains the high-purity viscose rayon.
As an improvement technical scheme, during the bleaching use H2O2Solution is as bleaching agent, H in the solution2O2
Concentration be 1~5g/l.
As further improved technical scheme, the bleaching and described oil can be carried out in same step, will be described
H2O2Solution is added in finish, bath temperature be 40~60 DEG C, pH value be progress under the conditions of 8~8.5.
As a kind of perferred technical scheme, the multiple salt acid dip is washed is repeated 2~10 times altogether；The multiple water
Wash and be repeated altogether 2~5 times.
As a kind of perferred technical scheme, the temperature of the coagulating bath is 48~50 DEG C, contains 110 in the coagulating bath
~120g/L H2SO4, 350~400g/L Na2SO4, 5~15g/l ZnSO4。
By adopting the above-described technical solution, the beneficial effects of the invention are as follows：
High-purity viscose rayon of the present invention, after fiberizing after desulfurization, washing, first passes around hydrochloric acid pre-preg, so
After bleaching, oil after washed by alcohol, multiple salt acid dip is washed, then by repeatedly washing, more than 99% impurity in fiber,
Lignin, hemicellulose are dissolved, and content of ashes is less than 200ppm in obtained high-purity fiber；Dry fracture strength >=2.2cN/
Dtex, dry elongation at break >=15%, wet breaking strength >=1.1cN/dtex, the performance of fiber is unaffected, and physical property is good
It is good；High-purity fiber after purification can be used at a high temperature of more than 435F, after lignin and hemicellulose are removed, cellulose
It can safely melt, carry out Compound Machining, widened the application field of viscose rayon；While high-purity viscose rayon of the present invention
Available for the production of carbon fiber, because lignin therein and hemicellulose and some impurity are removed, compared to using common
Viscose rayon cost is low, carbon yield is high, and obtained carbon fiber performance is good after carbonization.
The present invention after desulfurization, washing, first passes around hydrochloric acid pre-preg, then floated in high-purity viscose rayon preparation process
In vain, washed after oiling by alcohol, remove that part is inorganic and organic impurities respectively, then washed by multiple tracks salt acid dip, thoroughly immersion
Impurity, lignin and the hemicellulose in fiber are removed, high-purity viscose rayon that fiber content of ashes is less than 200ppm is obtained.
And washed because the present invention has carried out multiple tracks salt acid dip, the metal oxide and metallic salt in fiber can
It is dissolved and removes, therefore fibre whiteness is improved, and H can be used during bleaching2O2Solution makes in conventional art as bleaching agent
With sodium hypochlorite as bleaching agent, sodium hypochlorite is unstable, and when pH value is less than 8, fiber easily comes to harm, and can corrode modeling
The parts of appliance such as material, and use H2O2Solution is carried out, conditions of bleaching relaxes, no as bleaching agent under the conditions of pH value is 8~8.5
Fiber, and the progress simultaneously that can bleach and oil can be damaged, production stage is eliminated.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
Content of ashes accounts for high-purity viscose rayon butt weight in a kind of high-purity viscose rayon, high-purity viscose rayon
55ppm；The dry fracture strength 2.5cN/dtex of high-purity viscose rayon, dry elongation at break 17.5%, wet breaking strength
1.13cN/dtex。
Embodiment 2
Content of ashes accounts for high-purity viscose rayon butt weight in a kind of high-purity viscose rayon, high-purity viscose rayon
80ppm；The dry fracture strength 2.35cN/dtex of high-purity viscose rayon, dry elongation at break 16.5%, wet breaking strength
1.2cN/dtex。
Embodiment 3
Using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure, will
The soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution, by the viscose solution by filtering and deaeration
Spinning viscose is obtained, after the spinning viscose is extruded by spinneret orifice, spun filament is frozen into coagulating bath.
The spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg, the preimpregnation are carried out under normal temperature
Concentration of hydrochloric acid used in stain is 1.2 g/l, 5 minutes pre-preg time.
By the fiber after pre-preg after bleaching, oiling, extruding stem carries out alcohol and washed at normal temperatures, molten with 5g/l ethanol
Liquid is handled 10 minutes.
Fiber extrusion after alcohol is washed is done, and carries out first of salt acid dip at normal temperatures first, molten in 2.5wt% hydrochloric acid
Impregnated 4 minutes in liquid, hydrochloric acid and fiber bath volume ratio are 25:1, extruding stem, repeats multiple salt acid dip and washes again.
Fiber extrusion after salt acid dip is done, washed with distilled water, 35 DEG C of washing temperature, 5 minutes time, extruding
After dry, washing, extruding are repeated repeatedly, last drying obtains the high-purity viscose rayon.
Embodiment 4
Using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure, will
The soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution, by the viscose solution by filtering and deaeration
Spinning viscose is obtained, after the spinning viscose is extruded by spinneret orifice, spun filament, the coagulating bath are frozen into coagulating bath
Temperature be 49 DEG C, the H containing 110g/L in the coagulating bath2SO4, 365g/L Na2SO4, 8g/l ZnSO4。
The spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg, the preimpregnation are carried out under normal temperature
Concentration of hydrochloric acid used in stain is 2 g/l, 4 minutes pre-preg time.
By the fiber after pre-preg through bleaching, oiling, H is used during the bleaching2O2Solution is as bleaching agent, the solution
Middle H2O2Concentration be 5g/l, then extruding stem carries out alcohol and washed, handled 10 minutes with 5g/l ethanol solution at normal temperatures.
Fiber extrusion after alcohol is washed is done, and carries out first of salt acid dip at normal temperatures first, molten in 2.5wt% hydrochloric acid
Impregnated 4 minutes in liquid, hydrochloric acid and fiber bath volume ratio are 15~35:1, extruding stem, repeats 5 salt acid dips and washes again.
Fiber extrusion after salt acid dip is done, washed with distilled water, 40 DEG C of washing temperature, 4 minutes time, extruding
After dry, washing, extruding 3 times is repeated, last drying obtains the high-purity viscose rayon.
Embodiment 5
Using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure, will
The soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution, by the viscose solution by filtering and deaeration
Spinning viscose is obtained, after the spinning viscose is extruded by spinneret orifice, spun filament, the coagulating bath are frozen into coagulating bath
Temperature be 50 DEG C, the H containing 112g/L in the coagulating bath2SO4, 370g/L Na2SO4, 11g/l ZnSO4。
The spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg, the preimpregnation are carried out under normal temperature
Concentration of hydrochloric acid used in stain is 2 g/l, 3 minutes pre-preg time.
By the fiber after pre-preg through bleaching and oiling, H is used during the bleaching2O2Solution is as bleaching agent, the solution
Middle H2O2Concentration be 2g/l, by the H2O2Solution is added in finish, bath temperature be 55 DEG C, pH value be while entering under the conditions of 8
Row is bleached and oiled, then extruding stem, and alcohol is carried out at normal temperatures and is washed, and is handled 6 minutes with 10g/l ethanol solution.
Fiber extrusion after alcohol is washed is done, and first of salt acid dip is carried out at normal temperatures first, in 3wt% hydrochloric acid solution
Middle dipping 3 minutes, hydrochloric acid and fiber bath volume ratio are 50:1, extruding stem, repeats 8 salt acid dips and washes again.
Fiber extrusion after salt acid dip is done, washed with distilled water, 45 DEG C of washing temperature, 3 minutes time, extruding
After dry, washing, extruding 4 times is repeated, last drying obtains the high-purity viscose rayon.
Embodiment 6
Using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure, will
The soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution, by the viscose solution by filtering and deaeration
Spinning viscose is obtained, after the spinning viscose is extruded by spinneret orifice, spun filament, the coagulating bath are frozen into coagulating bath
Temperature be 49 DEG C, the H containing 118g/L in the coagulating bath2SO4, 360g/L Na2SO4, 12g/l ZnSO4。
The spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg, the preimpregnation are carried out under normal temperature
Concentration of hydrochloric acid used in stain is 1 g/l, 5 minutes pre-preg time.
By the fiber after pre-preg through bleaching and oiling, H is used during the bleaching2O2Solution is as bleaching agent, the solution
Middle H2O2Concentration be 4g/l, by the H2O2Solution is added in finish, bath temperature be 45 DEG C, pH value be under the conditions of 8.5 simultaneously
Bleached and oiled, then extruding stem, alcohol is carried out at normal temperatures and is washed, handled 5 minutes with 10g/l ethanol solution.
Fiber extrusion after alcohol is washed is done, and first of salt acid dip is carried out at normal temperatures first, in 4wt% hydrochloric acid solution
Middle dipping 4 minutes, hydrochloric acid and fiber bath volume ratio are 30:1, extruding stem, repeats 6 salt acid dips and washes again.
Fiber extrusion after salt acid dip is done, washed with distilled water, 40 DEG C of washing temperature, 5 minutes time, extruding
After dry, washing, extruding 3 times is repeated, last drying obtains the high-purity viscose rayon.
Experimental comparison's example 1
Experimental Comparison example 1 does not carry out alcohol and washed, and it is same as Example 6 with step.
Experimental comparison's example 2
Experimental Comparison example 2 alcohol is washed after fiber again after extruding stem, do not carry out multiple salt acid dip and wash, directly with steaming
Distilled water is washed, and it is same as Example 6 with step.
The performance indications for high-purity viscose rayon that above-described embodiment 3-6 and contrast experiment's example 1,2 are prepared are shown in Table 1.
Table 1
Washed it can be seen from data comparison in table 1 without alcohol, organic impurities is not easy to remove on fiber, causes ash content
Content is higher, and is washed without multiple salt acid dip, the farther height prepared higher than the embodiment of the present invention 6 of hydrochloric acid content of ashes
Pure fiber.And their physical performance index difference is little.
Claims (5)
1. a kind of preparation method of high-purity viscose rayon, it is characterised in that comprise the following steps：
(1) using native cellulose pulp as raw material, soluble cellulose xanthate acid is obtained through alkalization, aging, sulfonation procedure；
(2) the soluble cellulose xanthate acid is dissolved in dilute alkaline soln and is prepared into viscose solution；
(3) viscose solution is obtained into spinning viscose by filtering and deaeration；
(4) after the spinning viscose is extruded by spinneret orifice, spun filament is frozen into coagulating bath；
(5) spun filament is carried out after drawing-off, then after desulfurization, washing, hydrochloric acid pre-preg, the pre-preg is carried out under normal temperature
Concentration of hydrochloric acid used is 1~2 g/l, 3~5 minutes pre-preg time；
(6) by the fiber after pre-preg after bleaching, oiling, extruding stem carries out alcohol and washed, with 3~20g/L ethanol at normal temperatures
Solution is handled 3~10 minutes；
(7) fiber extrusion after alcohol is washed is done, and carries out first of salt acid dip at normal temperatures first, molten in 1~5wt% hydrochloric acid
Impregnated 3~5 minutes in liquid, hydrochloric acid and fiber volume bath raio are 15~75:1, extruding stem, repeats multiple salt acid dip again
Wash；
(8) fiber extrusion after salt acid dip is done, washed with distilled water, 30~50 DEG C of washing temperature, 3~5 points of time
After clock, extruding stem, washing, extruding are repeated repeatedly, last drying obtains the high-purity viscose rayon；High-purity viscose glue
Content of ashes accounts for 10~200ppm of high-purity viscose rayon butt weight in fiber；The dry fracture strength of high-purity viscose rayon
>=2.2cN/dtex, dry elongation at break >=15%, wet breaking strength >=1.1cN/dtex.
2. the preparation method of high-purity viscose rayon as claimed in claim 1, it is characterised in that：H is used during the bleaching2O2It is molten
Liquid is as bleaching agent, H in the solution2O2Concentration be 1~5g/L.
3. the preparation method of high-purity viscose rayon as claimed in claim 2, it is characterised in that：The bleaching and described oil can
To be carried out in same step, by the H2O2Solution is added in finish, bath temperature be 40~60 DEG C, pH value be 8~8.5 conditions
It is lower to carry out.
4. the preparation method of high-purity viscose rayon as described in any one of claims 1 to 3, it is characterised in that：The multiple salt
Acid dip is washed to be repeated 2~10 times altogether；The multiple washing is repeated 2~5 times altogether.
5. the preparation method of high-purity viscose rayon as claimed in claim 4, it is characterised in that：The temperature of the coagulating bath is 48
~50 DEG C, the H containing 110~120g/L in the coagulating bath2SO4, 350~400g/L Na2SO4, 5~15g/L ZnSO4。
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| CN107815753A (en) * | 2017-10-23 | 2018-03-20 | 李庆园 | Antistatic imitative hair composite fibre and preparation method thereof |
| CN107881611A (en) * | 2017-10-23 | 2018-04-06 | 李庆园 | Far infrared imitates hair composite fibre and preparation method thereof |
| CN107815752A (en) * | 2017-10-23 | 2018-03-20 | 李庆园 | High-elastic imitative hair composite fibre and preparation method thereof |
| CN109267165B (en) * | 2018-07-26 | 2021-08-27 | 阜宁澳洋科技有限责任公司 | High wet modulus viscose fiber and preparation method thereof |
| CN115182154B (en) * | 2022-07-22 | 2024-01-26 | 江苏米格新材料股份有限公司 | Ultra-high-purity viscose-based graphite felt and preparation method and application thereof |
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Effective date of registration: 20211209 Address after: 224400 Jiangsu Yancheng Funing high tech Industrial Development Zone Aoyang Avenue Saideli (Yancheng) Fiber Co., Ltd Patentee after: Saideli (Yancheng) Fiber Co.,Ltd. Address before: 224400 No. 1, Aoyang Avenue, Aoyang Industrial Park, Funing County, Yancheng City, Jiangsu Province Patentee before: FUNING AOYANG TECHNOLOGY CO.,LTD. |