CN111379041B - Flat regenerated cellulose fiber and preparation method thereof - Google Patents
Flat regenerated cellulose fiber and preparation method thereof Download PDFInfo
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- CN111379041B CN111379041B CN201811637458.2A CN201811637458A CN111379041B CN 111379041 B CN111379041 B CN 111379041B CN 201811637458 A CN201811637458 A CN 201811637458A CN 111379041 B CN111379041 B CN 111379041B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F2/00—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof
- D01F2/06—Monocomponent artificial filaments or the like of cellulose or cellulose derivatives; Manufacture thereof from viscose
- D01F2/08—Composition of the spinning solution or the bath
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Abstract
The invention belongs to the field of regenerated cellulose fibers, and particularly discloses a flat regenerated cellulose fiber and a preparation method thereof. The prepared regenerated cellulose fiber has obvious flat shape and high flatness, so that the surface area of the fiber is increased, and the hydrophilic hydroxyl on the surface of the fiber is also obviously increased, thereby greatly improving the moisture absorption and moisture conductivity of the fiber.
Description
Technical Field
The invention belongs to the field of cellulose fibers, and particularly relates to a flat regenerated cellulose fiber and a preparation method thereof.
Background
With the improvement of the modern living standard, more and more consumers not only consider the quality and the wearability of the textile when purchasing or wearing the textile, but also begin to put forward the consumption requirements on environmental protection, health and functionality, and the development of the 'green' functional textile product becomes a necessary development trend. The viscose staple fibers belong to regenerated cellulose fibers, and textiles manufactured by the viscose staple fibers are comfortable to wear, absorb moisture and dry quickly, can be naturally degraded, are green and environment-friendly, so that the development of functional viscose staple fiber products is urgent.
The flat viscose staple fibers have large specific surface area, and when the flat viscose staple fibers are woven into a fabric, the side surface area of the filaments in unit volume is large, the contact area between the filaments is large, the friction coefficient is large, and the friction force between the filaments is large. Therefore, the shape retention of fabrics and clothes made of the flat viscose staple fibers is better than that of fabrics and clothes made of common regenerated cellulose fibers. Meanwhile, the specific surface area is increased, and the hydrophilic hydroxyl on the surface of the fiber is also obviously increased, so that the dilutability and the moisture conductivity of the fiber are greatly improved. The flat fibers and the round fibers with the equal cross sections are easy to form a large number of gaps in the yarns, and the yarns and the fabrics have soft hand feeling, moisture permeability, air permeability, bulkiness, good heat retention property and light and comfortable wearing; has better strength and elasticity, warmth retention and antistatic property.
At present, two production modes of flat regenerated cellulose fiber are provided, the first mode is that the flat regenerated cellulose fiber is obtained by spinning with a specific spinneret orifice shape, for example, Chinese application 201610142296.X proposed by Hengtian Syngnathus New materials Co., Ltd. As is known, a spinneret for producing the flat fiber generally uses precious metals such as gold platinum alloy, tantalum, niobium and the like, and the processing precision is required to be extremely high, and the price of a spray head is very expensive, so the development of the flat fiber is limited.
The other is flat fiber produced by adding carbonate and bicarbonate, for example, Chinese application 2012101561907 proposes a flaky flat regenerated cellulose fiber and a preparation method thereof, wherein carbonate is added into glue solution before spinning after the yellowing is finished. However, the cross section of the flat regenerated cellulose fiber prepared by the method has a large number of pores, so that the fiber strength is reduced, and meanwhile, the flat regenerated cellulose fiber prepared by adding a large number of carbonates before spinning is alkaline, so that the flat regenerated cellulose fiber does not meet the requirements of ecological spinning.
The present invention has been made in view of this situation.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the ecological environment-friendly flat regenerated cellulose fiber which is low in production cost, high in fiber strength and excellent in absorptivity and moisture permeability.
In order to solve the technical problems, the invention provides a preparation method of flat regenerated cellulose fibers, which is characterized in that plant pulp is used as a raw material, a lignosulfonate solution containing reducing sugar is added in any procedure before dissolving to spinning, the pH value of the lignosulfonate solution is controlled to be acidic, and then spinning and post-treatment are carried out to obtain the flat regenerated cellulose fibers.
The lignosulfonate in the invention is a byproduct in the plant pulping process, and is formed by sulfonation reaction of free sulfurous acid and log lignin in wood flour to generate lignosulfonate, and then the lignosulfonate is formed by alkali neutralization, so that the pH value of a lignosulfonate solution is neutral or weakly alkaline. And the lignosulfonate has a complex composition and contains reducing sugars in the lignosulfonate, which are present in the form of lignin-glycan complexes, including: xylose, arabinose, mannose, common sugar, galactose and the like, which are collectively called five-carbon sugar and six-carbon sugar, and these sugars have reducibility. According to the invention, after the lignosulfonate containing reducing sugar is dissolved, the pH value of the lignosulfonate solution is controlled to be acidic, the lignin-polysaccharide complex is hydrolyzed under the acidic condition to generate pentasaccharide and hexasaccharide monosaccharides with reducing property, and then the pentasaccharide and hexasaccharide monosaccharides are added into any working procedure before being dissolved to be spun, and the flat regenerated cellulose fiber is obtained through processes of spinning refining and the like.
In the present invention, the method for producing the flat regenerated cellulose fiber includes the steps of dipping, aging, yellowing, dissolving, filtering, defoaming, spinning, washing with water, and desulfurizing, and the lignosulfonate solution is added in any step from the step of dissolving to the step of spinning, preferably during the dissolving process or in the spinning dope.
Preferably, a lignosulfonate solution is added in the process of dissolving the plant pulp subjected to yellowing treatment, then, a spinning solution is obtained through filtration, and the obtained spinning solution is subjected to spinning, refining and other processes to obtain flat regenerated cellulose fibers;
or adding lignosulfonate solution into the filtered spinning solution of the plant pulp subjected to the yellowing treatment, and then carrying out processes such as spinning refining to obtain the flat regenerated cellulose fibers.
The flat regenerated cellulose fiber takes plant pulp as a raw material, wherein the plant pulp comprises but is not limited to one or the mixture of more than two of wood pulp, cotton pulp, bamboo pulp or hemp pulp. In the process of manufacturing the flat regenerated cellulose fiber by the plant pulp, except adding the lignosulfonate solution, other process procedures and process parameters can adopt the method disclosed by the prior art. The dipping comprises dipping the plant pulp in an alkali solution with the temperature of 45-55 ℃; the aging is carried out in an aging drum, and the temperature is controlled to be 15-60 ℃. In the yellowing process, the addition amount of the carbon disulfide is 25-45 wt% of the content of the methyl fiber, and the yellowing temperature is 20 +/-2 ℃. The spinning method of the invention is a spinning method of plain regenerated cellulose fiber disclosed in the prior art, and the common spinning method is to prepare the regenerated cellulose fiber after the spinning solution is precipitated in an acid coagulating bath and then the processes of drafting, cutting, washing, desulfurizing, oiling, drying and the like are carried out. The acidic coagulation bath consists of 110-150 g/L sulfuric acid, 250-350 g/L sodium sulfate and 12.5-13.5 g/L zinc sulfate, and the temperature of the coagulation bath is 40-55 ℃.
The performance of the plant pulp of the invention meets the prevention industry standards FZ/T51001-2009 of the people's republic of China, FZ/T
51002-2006. The plant pulp of the present invention can be prepared by the vegetarian pulping process disclosed in the prior art. Generally, in the preparation process of the plant pulp, plants are used as raw materials, and the plant pulp is prepared through the processes of cooking, bleaching, acid treatment and the like.
Further, controlling the pH value of the lignosulfonate solution to be 2-6.5;
preferably, the pH value of the lignosulfonate solution is controlled to be 2.5-4.
The pH value is controlled within the range, so that the corrosion to spinning equipment is avoided on the premise of ensuring the high hydrolysis of the lignin-polysaccharide complex, and meanwhile, the solubility of the lignosulfonate is the maximum within the pH value range.
Further, the preparation method of the lignosulfonate solution comprises the following steps: adding an acidic reagent into a lignosulfonate solution, controlling the pH value of the solution to be 2-6.5, reacting for 3-6h at the temperature of 60-100 ℃, and maximizing the hydrolysis degree of reducing sugar at the temperature and in the time. Preferably, the pH value of the solution is controlled to be 2.5-4, and the reaction is carried out for 4-5h at the temperature of 70-90 ℃. The acid reagent is sulfuric acid solution or hydrochloric acid solution.
Further, the content of reducing sugar in the lignosulfonate is more than 5 wt% of the content of viscose methyl cellulose; preferably, the content of the reducing sugar in the lignosulfonate is more than or equal to 18 wt% of the content of the viscose methylcellulose.
According to the invention, when the content of reducing sugar in the lignosulfonate is controlled to be more than 5 wt%, the yield of the prepared flat regenerated cellulose fiber is more than 80%, and when the content of reducing sugar is controlled to be more than or equal to 18 wt%, the flat regenerated cellulose fiber with the yield of 100% can be obtained.
Furthermore, the addition amount of the lignosulfonate is 0.5-10.0 wt% of the content of the viscose methyl fibers;
preferably, the lignosulfonate is added in an amount of 1.5-2.5% of the viscose rayon content.
Further, the concentration of the lignosulfonate solution is 5-20% in terms of lignin;
preferably, the concentration of the added lignosulfonate solution is 7-10% in terms of lignin.
Further, the lignosulfonate is a byproduct in a sulfite pulping process.
Further, adding waste liquid generated in the sulfite pulping process in the step before dissolving to spinning, and adjusting the pH value of the waste liquid to be 2-6.5.
Further, the lignosulfonate comprises one or more of sodium lignosulfonate, potassium lignosulfonate, calcium lignosulfonate, magnesium lignosulfonate and ammonium lignosulfonate;
One or a mixture of two of sodium lignosulfonate and calcium lignosulfonate is preferred.
The invention also provides a flat regenerated cellulose fiber, which has a flat section, the flatness is more than or equal to 6, and the fiber section is smooth and compact.
Furthermore, the dry breaking strength of the flat regenerated cellulose fiber is more than or equal to 2.1cN/dtex, and the wet breaking strength is more than or equal to 1.3cN/dtex
In the invention, after the lignosulfonate solution is added into any procedure before the spinning, the reducing sugar existing in the lignosulfonate in the form of lignin-polysaccharide complex is hydrolyzed into the reducing sugar monomer under the acidic condition, and in the spinning process, the reducing sugar in the spinning solution is on the one hand hydrolyzed into the reducing sugar monomer together with CS in the spinning solution2After esterification reaction, reducing sugar and CS are separated out in a coagulating bath2On the other hand, the reducing sugar precipitated in the coagulation bath undergoes oxidation-reduction reaction again with the sulfuric acid in the coagulation bath to produce SO2Gas, with CS2、SO2The gas continuously overflows, the unset filaments are broken, and then the fluffy nascent filaments are drawn by the spinning nozzle and the filament guiding piece to be stretched into a flaky flat shape, and folds with different depths are formed on the surface of the flat fiber longitudinally.
The invention can prepare flat fiber by adding a small amount of lignosulfonate (0.5-10.0 wt% of viscose methylcellulose content) because the reducing sugar in the lignosulfonate and the solvent CS in the spinning solution on one hand2Precipitation of CS in a coagulation bath after esterification2The reducing sugar precipitated simultaneously with the gas also undergoes an oxidation-reduction reaction with sulfuric acid in the coagulation bath to produce SO2On the other hand, the reducing sugar precipitated along with the primary fiber has a structure similar to that of the primary fiber, and according to the principle that the similar and soluble sugars permeate into the primary fiber, most of generated gas acts on the primary fiber, so that the gas generated by adding a small amount of lignosulfonate can break the unset filaments, and then the filaments are drawn by a spinneret and a guide wire to prepare the flat fiber. Meanwhile, the situation that the density of the fiber is reduced and the strength of the fiber is reduced due to the fact that a large amount of gas is generated instantly to cause more air holes in the fiber can not occur when a small amount of lignosulfonate is added. Meanwhile, a small amount of lignosulfonate is added, so that the spinning solution is not easy to gel, and a spinneret orifice is not easy to block.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. The prepared fiber has obvious flat shape and high flatness, so that the surface area of the fiber is increased, and the hydrophilic hydroxyl on the surface of the fiber is also obviously increased, thereby greatly improving the moisture absorption and moisture conductivity of the fiber; the surface of the fiber is longitudinally provided with longitudinal folds with different depths so as to further improve the moisture absorption; the prepared flat regenerated cellulose fiber has the performances of pilling resistance, static resistance and good elasticity, and is full and fluffy in hand feeling;
2. the method for preparing the flat regenerated cellulose fiber does not need to install a high-price spinning nozzle, so that the production cost is obviously reduced, and meanwhile, the prepared flat regenerated cellulose fiber and non-flat cellulose fiber can share spinning equipment, so that the production benefit is obviously improved;
3. the preparation method of the invention can be worth of flat fiber by adding a small amount of lignosulfonate, and the spinning solution can not generate the risk of gelation and can not cause the blockage of the spinneret orifice.
4. The lignosulfonate used in the method expands the application field of the lignosulfonate, and improves the utilization additional value of the plant pulping waste liquid.
The following describes embodiments of the present invention in further detail with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention, are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention without limiting the invention to the right. It is obvious that the drawings in the following description are only some embodiments, and that for a person skilled in the art, other drawings can be derived from them without inventive effort. In the drawings:
FIGS. 1 and 2 are electron micrographs of flat regenerated cellulose fibers prepared by the preparation process of example 1 under different magnification of a microscope;
FIG. 3 is an electron micrograph of regenerated cellulose fibers obtained by the production method of comparative example 1;
fig. 4 is an electron microscope image of regenerated cellulose fibers obtained by the production method of comparative example 2.
It should be noted that the drawings and the description are not intended to limit the scope of the inventive concept in any way, but to illustrate it by a person skilled in the art with reference to specific embodiments.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and the following embodiments are used for illustrating the present invention and are not intended to limit the scope of the present invention.
In the description of the present invention, it should be noted that the terms "inside", "outside", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, which are only for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and operate, and thus, should not be construed as limiting the present invention.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," "contacting," and "communicating" are to be construed broadly, e.g., as meaning fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1
In this example, the bamboo pulp is used as the raw material, and the process includes the following steps: the bamboo pulp is subjected to the yellowing treatment, wherein a sodium lignosulfonate solution with the concentration of 10% and the pH value of 6.4 is added in the dissolving process of the bamboo pulp, the content of reducing sugar in the sodium lignosulfonate is 19.8 wt% of the content of viscose methyl fibers, and the addition amount of the sodium lignosulfonate is 2.5 wt% of the content of the viscose methyl fibers. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the thickness of 1.33dtex multiplied by 38mm, wherein the flatness is 9.7, the dry strength of the fiber is 2.2cN/dtex, and the wet strength of the fiber is 1.3 cN/dtex.
Example 2
In the present embodiment, the wood pulp is used as the raw material, and the method comprises the following steps: the method comprises the following steps of dipping, ageing, yellowing, dissolving, filtering, defoaming, spinning, washing, desulfurizing and the like, wherein an ammonium lignosulfonate solution with the concentration of 15% and the pH value of 4.4 is added in the process of dissolving the wood pulp subjected to the yellowing treatment, the content of reducing sugar in the ammonium lignosulfonate is 10 wt% of the content of viscose methyl fibers, and the adding amount of the ammonium lignosulfonate is 4 wt% of the content of the viscose methyl fibers. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the flatness of 1.38dtex multiplied by 38mm, wherein the flatness is 7.9, the dry strength of the fiber is 2.4cN/dtex, and the wet strength of the fiber is 1.4 cN/dtex.
Example 3
In this embodiment, hemp pulp is used as a raw material, and the method includes the following processes of dipping, aging, yellowing, dissolving, filtering, defoaming, spinning, washing, desulfurizing and the like, wherein a magnesium lignosulfonate solution with a concentration of 10% and a PH value of 3 is added to filtered, matured, defoamed and filtered spinning glue by using a syringe pump, the content of reducing sugar in the magnesium lignosulfonate is 8.66 wt% of the content of viscose methylcellulose, and the addition amount of the magnesium lignosulfonate is 3 wt% of the content of the methylcellulose in the slurry mucus. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber filament, wherein the flatness is 9.2, the dry strength of the fiber is 2.6cN/dtex, and the wet strength of the fiber is 1.5 cN/dtex.
Example 4
In the embodiment, the cotton pulp is used as the raw material, and the method comprises the following steps: the bamboo pulp is subjected to dissolving, wherein sodium lignosulfonate and calcium lignosulfonate (the mass ratio of the sodium lignosulfonate to the calcium lignosulfonate is 1:1) solutions with the total concentration of 10% and the pH value of 5.1 are added in the dissolving process of the bamboo pulp subjected to yellowing treatment, the content of reducing sugar in the mixed solution of the sodium lignosulfonate and the calcium lignosulfonate is 5.56 wt% of the content of viscose methylcellulose, and the adding amount of the sodium lignosulfonate and the calcium lignosulfonate is 6 wt% of the content of the viscose methylcellulose. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the thickness of 1.67 multiplied by 38mm, wherein the flatness is 8.6, the dry strength of the fiber is 2.3cN/dtex, and the wet strength of the fiber is 1.3 cN/dtex.
Example 5
In this example, 20% wood pulp and 80% cotton pulp are used as raw materials, and the process comprises the following steps: the production process comprises the steps of dipping, ageing, yellowing, dissolving, filtering, defoaming, spinning, washing, desulfurizing and the like, wherein calcium lignosulfonate with the total concentration of 5% and the pH of 3.9 is added into the filtered, matured, defoamed and filtered spinning glue by using an injection pump, the content of reducing sugar in the calcium lignosulfonate is 15 wt% of the content of viscose fibers, and the addition amount of the calcium lignosulfonate is 4.5 wt% of the content of the viscose fibers. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the thickness of 1.51 multiplied by 38mm, wherein the flatness is 8.8, the dry strength of the fiber is 2.12cN/dtex, and the wet strength of the fiber is 1.33 cN/dtex.
Example 6
In this example, 34% wood pulp and 64% hemp pulp are used as raw materials, and the process comprises the following steps: the bamboo pulp is dissolved, sodium lignosulfonate and calcium lignosulfonate (the mass ratio of the sodium lignosulfonate to the calcium lignosulfonate is 5:1) solution with the total concentration of 12% and the pH value of 3.5 is added in the dissolving process of the bamboo pulp subjected to yellowing treatment, the content of reducing sugar in the mixed solution of the sodium lignosulfonate and the calcium lignosulfonate is 12.2 wt% of the content of viscose methyl fibers, and the adding amount of the sodium lignosulfonate and the calcium lignosulfonate is 2.5 wt% of the content of the viscose methyl fibers. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the diameter of 2.22 multiplied by 38mm, wherein the flatness is 7.6, the dry strength of the fiber is 2.22cN/dtex, and the wet strength of the fiber is 1.39 cN/dtex.
Example 7
In this example, the bamboo pulp is used as the raw material, and the process includes the following steps: the bamboo pulp is treated by the steps of dipping, ageing, yellowing, dissolving, filtering, defoaming, spinning, washing, desulfurizing and the like, wherein a sodium lignosulfonate solution with the concentration of 7% and the pH value of 2.1 is added in the process of dissolving the bamboo pulp subjected to the yellowing treatment, the content of reducing sugar in the sodium lignosulfonate is 18 wt% of the content of viscose methyl fibers, and the addition amount of the sodium lignosulfonate is 1.5 wt% of the content of the viscose methyl fibers. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the flatness of 1.33dtex multiplied by 38mm, wherein the flatness is 7.9, the dry strength of the fiber is 2.1cN/dtex, and the wet strength of the fiber is 1.3 cN/dtex.
Example 8
In this example, 20% wood pulp and 80% bamboo pulp are used as raw materials, and the process includes the following steps: the method comprises the following steps of dipping, ageing, yellowing, dissolving, filtering, defoaming, spinning, washing, desulfurizing and the like, wherein waste liquor obtained by pulping and cooking wood by adopting a sulfite method is added in the process of dissolving the bamboo pulp subjected to yellowing treatment, the content of reducing sugar in the waste liquor is 22 wt% of the content of viscose methyl fibers, the PH value of the waste liquor is adjusted to be 3.9, the addition amount of the waste liquor is calculated by the amount of evaporation solid matters, and the addition amount of the evaporation solid matters is 8 wt% of the content of the methyl fibers in the pulp mucus. And then plasticizing, drawing, cutting, washing, desulfurizing, oiling and drying to obtain the flat regenerated cellulose fiber with the diameter of 2.35 multiplied by 38mm, wherein the flatness is 10.8, the dry strength of the fiber is 2.61cN/dtex, and the wet strength of the fiber is 1.5 cN/dtex.
Comparative example 1
This comparative example produced a flat regenerated cellulose fiber by the production method of application No. 2012101561907.
Comparative example 2
This comparative example differs from example 1 in that the pH of the sodium lignosulfonate solution was not adjusted to be acidic prior to addition of the sodium lignosulfonate solution.
Experimental example 1
This experimental example compares the appearance, properties and spinneret changing period of the regenerated cellulose fibers obtained in example 1 and comparative examples 1 to 3, and is shown in Table 1.
Table 1:
from the experimental results, it can be seen that the regenerated cellulose fibers obtained in example 1 (as shown in FIGS. 1 and 2) and comparative example 1 (as shown in FIG. 3) have a very small difference in flatness, but the dry strength and wet strength of the fibers obtained in example 1 are significantly higher than those obtained in comparative example 1, and the fibers obtained in example 1 are acidic, whereas the fibers obtained in comparative example 1 are alkaline, and the exchange cycle of the spinneret holes in comparative example 1 is significantly shorter than that in example 1. This is because in comparative example 1, a large amount of carbonate (accounting for 30 to 50 wt% of the content of the viscose rayon fibers) is added to the spinning solution, and the carbonate reacts with acid in the coagulation bath to generate a large amount of carbon dioxide gas in a short time, which causes the decrease in the compactness of the fibers, so that the fibers contain many pores inside (see fig. 3), resulting in the decrease in the strength of the fibers; meanwhile, a large amount of carbonate can cause the gel risk of the spinning solution, and the spinneret orifices are easy to block in the spinning process, so that the replacement period of the spinneret orifices is greatly shortened. In addition, a large amount of Na is added with the carbonate+Or K+Or NH4+When the fibers are wrapped in the fibers when being solidified and separated out, the fibers are alkaline and do not meet the requirements of ecological textiles (the PH value is 5.5-7), and meanwhile, Na +Or K+Or NH4+Etc. may also reduce the fiber strength to some extent.
The invention can prepare flat fiber by adding a small amount of lignosulfonate (0.5-10.0 wt% of viscose methylcellulose content) because the reducing sugar in the lignosulfonate and the solvent CS in the spinning solution on one hand2Precipitation of CS in a coagulation bath after esterification2The reducing sugar precipitated simultaneously with the gas also undergoes an oxidation-reduction reaction with sulfuric acid in the coagulation bath to produce SO2On the other hand, the reducing sugar separated out with the primary fiber and the primary fiberThe fiber structure is similar, according to the principle that the similarity is dissolved mutually, the reducing sugar permeates into the primary fiber, most of generated gas acts on the primary fiber, so that the unset strand silk is broken, and then the flat fiber is prepared by drawing through a spinning jet and a yarn guide piece. Meanwhile, the situation that the compactness of the fiber is reduced and the strength of the fiber is low due to the fact that a large amount of gas is generated instantly to cause more air holes in the fiber can not occur when a small amount of lignosulfonate is added. Meanwhile, a small amount of lignosulfonate is added, so that the spinning solution is not easy to gel, and a spinneret orifice is not easy to block.
The regenerated cellulose fiber obtained in comparative example 2 (as shown in FIG. 4) had a flatness of approximately 1, indicating that the lignin-polysaccharide complex in the lignosulfonate could not be hydrolyzed to reducing sugar monomers and could not be reacted with CS in the spinning dope without adjusting the pH of the lignosulfonate solution to acidic before adding the lignosulfonate solution to the spinning dope2Reaction takes place and CS is precipitated in the coagulation bath2The gas may be partially hydrolyzed to generate CS in the acidic coagulation bath2However, the amount of gas generated is not sufficient to flatten the fibers, and thus flat fibers cannot be obtained.
Experimental example 2
In this experimental example, the yield of the flat regenerated cellulose fiber obtained by adding the lignosulfonate containing the reducing sugars in different proportions according to the preparation method of example 1 is shown in table 2.
Table 2:
according to the experimental results, when the content of the reducing sugar in the lignosulfonate is more than 5 wt% of the content of the viscose methyl cellulose, the content of the flat fibers in the obtained cellulose fibers is more than 80%. And as the content of reducing sugar increases, the yield of flat fibers also increases, and when the content of reducing sugar is more than 18% of the content of viscose rayon, the yield of flat fibers reaches 100%. When lignosulfonate is used The reducing sugar content in the fiber is less than 5 wt%, and the yield of flat fiber is low, because the reducing sugar content of lignin is less than 5 wt% of the viscose methyl fiber, and the CS gas generated in the spinning process2Gas and SO2Too little gas to obtain a high yield of flat regenerated cellulose fibers.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (16)
1. A preparation method of flat regenerated cellulose fibers is characterized in that plant pulp is used as a raw material, a lignosulfonate solution containing reducing sugar is added in any process from dissolution to spinning, the pH value of the lignosulfonate solution is controlled to be acidic, and then spinning and post-treatment are carried out to obtain the flat regenerated cellulose fibers.
2. The method for preparing flat regenerated cellulose fibers according to claim 1, characterized in that the pH value of the lignosulfonate solution is controlled to be 2-6.5.
3. The method for preparing flat regenerated cellulose fibers according to claim 1, characterized in that the pH value of the lignosulfonate solution is controlled within a range of 2.5-4.
4. The method for preparing flat regenerated cellulose fibers according to claim 1, characterized in that the content of reducing sugars in the lignosulfonate is > 5wt% of the content of viscose rayon fibers.
5. The method for preparing flat regenerated cellulose fibers according to claim 1, characterized in that the content of reducing sugars in the lignosulfonate is not less than 18wt% of the content of viscose methyl cellulose.
6. The method for preparing flat regenerated cellulose fibers according to any of claims 1-5, characterized in that the lignosulfonate is added in an amount of 0.5-10.0wt% of the viscose methyl cellulose content.
7. The method for producing flat regenerated cellulose fibers according to any one of claims 1-5, characterized in that the lignosulfonate is added in an amount of 1.5-2.5% of the viscose methyl cellulose content.
8. The method for producing flat regenerated cellulose fibers according to any one of claims 1 to 5, characterized in that the concentration of the lignosulfonate solution is 5 to 20% by weight of lignin.
9. The method for producing flat regenerated cellulose fibers according to any one of claims 1 to 5, characterized in that the added lignosulfonate solution has a concentration of 7 to 10% by weight of lignin.
10. Method for the preparation of flattened regenerated cellulose fibres according to any of claims 1-5, characterised in that the lignosulphonate is a by-product of the sulphite pulping process.
11. The method for preparing flat regenerated cellulose fibers according to any one of claims 1-5, characterized in that the lignosulfonate comprises one or more of sodium lignosulfonate, potassium lignosulfonate, calcium lignosulfonate, magnesium lignosulfonate and ammonium lignosulfonate.
12. The method for producing flat regenerated cellulose fibers according to any one of claims 1 to 5, characterized in that the lignosulfonate is one or a mixture of two of sodium lignosulfonate and calcium lignosulfonate.
13. The method for preparing flat regenerated cellulose fibers according to any one of claims 1-5, characterized in that the regenerated cellulose fibers are made of one or more of wood pulp, cotton pulp, bamboo pulp or hemp pulp.
14. The method for producing flattened regenerated cellulose fibers according to any one of claims 1 to 5, characterized in that the raw material of the regenerated cellulose fibers is one or a mixture of two or more of wood pulp and bamboo pulp.
15. Flat regenerated cellulose fibers produced by the production method according to any one of claims 1 to 14, wherein the regenerated cellulose fibers have a flat cross section, a flatness of 6 or more, and a smooth and dense fiber cross section.
16. Flat regenerated cellulose fibres according to claim 15, characterised in that the flat regenerated cellulose fibres have a dry breaking strength of more than or equal to 2.1cN/dtex and a wet breaking strength of more than or equal to 1.3 cN/dtex.
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| CN102002762A (en) * | 2010-11-02 | 2011-04-06 | 山东海龙股份有限公司 | Method for preparing high-strength special-shape cellulose fiber |
| CN102677208B (en) * | 2012-05-17 | 2013-12-18 | 阜宁澳洋科技有限责任公司 | Flaky flat viscose fiber and preparation method thereof |
| CN103215679B (en) * | 2013-04-08 | 2015-02-11 | 宜宾海丝特纤维有限责任公司 | Production technology of viscose flat monofilament |
| CN103526320B (en) * | 2013-10-28 | 2016-01-20 | 唐山三友集团兴达化纤有限公司 | The spinning head used in the production method of flat viscose fiber and production process |
| CN106149081B (en) * | 2015-04-02 | 2019-05-17 | 河北吉藁化纤有限责任公司 | A kind of regenerated celulose fibre preparation method and its fiber |
| CN106521672A (en) * | 2016-08-29 | 2017-03-22 | 山东银鹰化纤有限公司 | Preparation method of ultra-short flat fiber |
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