CN111304767A - Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber - Google Patents
Preparation method for producing regenerated cellulose fiber by using waste textile regenerated pulp and regenerated cellulose fiber Download PDFInfo
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B16/00—Regeneration of cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B9/00—Cellulose xanthate; Viscose
- C08B9/04—Continuous processes
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/10—Filtering or de-aerating the spinning solution or melt
- D01D1/106—Filtering
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Abstract
The invention belongs to the field of recycling of waste textiles, and particularly relates to a preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp and regenerated cellulose fibers. The preparation method comprises the following steps: (1) pre-crushing, alkaline leaching, squeezing and crushing the waste textile regenerated pulp to obtain alkali cellulose; (2) aging, yellowing and dissolving the alkali cellulose in the step (1) to obtain a regenerated spinning glue solution; (3) spinning the regenerated spinning glue solution obtained in the step (2), or mixing the regenerated spinning glue solution with a common spinning glue solution and then spinning to obtain the regenerated cellulose fiber. The preparation method can fully recycle the waste textiles to prepare the regenerated cellulose fibers, and the obtained regenerated fibers have good performance, the dry breaking strength is more than or equal to 2.05cN/dtex, the dry strength variation coefficient is less than or equal to 14.0 percent, the wet breaking strength is more than or equal to 1.05cN/dtex, and the whiteness is 60-80 percent.
Description
Technical Field
The invention belongs to the field of recycling of waste textiles, relates to a preparation method of regenerated cellulose fibers and regenerated cellulose fibers, and particularly relates to a preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp and regenerated cellulose fibers.
Background
As a world large consumer of clothes, the total yield of finished clothes in China in 2018 is about 456 hundred million according to statistics, and the yield is increased by 7.32 percent in a same period compared with 2017. With the increasing demand for garments, the demand for textile raw materials has also risen synchronously. As is known, cotton is an important raw material for producing clothes, and the increase of the cotton demand reduces the cultivated land area, thereby causing the current situation of 'cotton and grain land competition'. However, the dressing idea of people changes day by day, which leads to the rapid shortening of the clothing renewal period, and greatly accelerates the generation of waste clothing.
According to 2019, the number of waste textiles produced in China can reach 2000 million tons every year, at present, only a very small part of waste textiles are recycled, a small part of waste textiles are incinerated and buried, the vast majority of waste textiles are discarded at will, and the recycling rate of the waste textiles in China is less than 20%. In addition, the waste textiles can generate a large amount of carbon dioxide and toxic substances in the incineration process, thereby causing a serious environmental pollution problem.
At present, few reports are made on the preparation of cellulose fibers by waste textile regenerated pulp, and no systematic and complete research data exists. Meanwhile, because the waste textile regenerated pulp has complex components and longer fibers, besides various colored groups, the contained natural cotton fibers have the characteristics of large molecular weight, high crystallinity, difficult reutilization and the like, and the problem of how to prepare qualified spinning glue solution by utilizing the cellulose components in the waste textile regenerated pulp for spinning is needed to be solved.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp and the regenerated cellulose fibers. The preparation method can fully recycle the waste textiles to prepare the regenerated cellulose fibers, and the obtained regenerated fibers have excellent performance, the dry breaking strength of the regenerated fibers is more than or equal to 2.05cN/dtex, the dry strength variation coefficient of the regenerated fibers is less than or equal to 14.0 percent, the wet breaking strength of the regenerated fibers is more than or equal to 1.05cN/dtex, and the whiteness of the regenerated fibers is 60-80 percent.
In order to solve the technical problems, the invention adopts the technical scheme that:
the first purpose of the invention is to provide a preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp, which comprises the following steps:
(1) pre-crushing, alkaline leaching, squeezing and crushing the waste textile regenerated pulp to obtain alkali cellulose;
(2) aging, yellowing and dissolving the alkali cellulose in the step (1) to obtain a regenerated spinning glue solution;
(3) spinning the regenerated spinning glue solution obtained in the step (2), or mixing the regenerated spinning glue solution with a common spinning glue solution and then spinning to obtain the regenerated cellulose fiber.
The invention provides a preparation method for producing cellulose fibers by using waste textile regenerated pulp, which effectively solves the problem of recycling of waste textiles, increases available resources in the textile industry and realizes value increment of the waste textiles. Meanwhile, the mechanical property of the regenerated cellulose fiber obtained by the preparation method can meet the production requirement, and the diversity of the product is further enriched.
In the waste textile regenerated pulp, the cellulose content is more than or equal to 80 percent, the viscosity is 15-20mpa.s, the iron content is less than or equal to 13ppm, and the whiteness is 30-70 percent.
In the further scheme, in the step (1), after the textile regenerated pulp is subjected to pre-crushing treatment, the average length of the fiber is 0.5-5.0 mm;
preferably, the average length of the fibers is 1.0 to 3.0 mm.
In the scheme, because the fiber length in the waste textile regenerated pulp is mostly larger than 7mm, the regenerated pulp needs to be pre-crushed firstly, specifically, the textile regenerated pulp is crushed by a crusher in a dry state, long fibers in the textile regenerated pulp are cut off, the average length of the fibers is 1.0-3.0mm after the textile regenerated pulp is pre-crushed in the scheme, the fiber length after the pre-crushing is shorter, the contact surface and the channel for immersing alkali liquor can be increased, and the alkali leaching effect can be improved.
In the invention, the alkaline leaching process specifically comprises the following steps: the cellulose is strongly expanded after being treated by the alkali solution, the diameter of the fiber is increased, the length of the fiber is contracted, the hemicellulose and partial impurities are dissolved out, the molecular weight of the cellulose is reduced, the reaction performance is improved, and the new compound alkali cellulose is generated.
In a further scheme, in the step (1), the alkaline leaching conditions include: the concentration of the alkali liquor is 190-260g/L, the temperature is 20-60 ℃, the alkali leaching time is 20-100min, and the bath ratio is 1:10-1: 40;
preferably, the concentration of the alkali liquor is 210-250g/L, the temperature is 30-50 ℃, the alkali leaching time is 20-70min, and the bath ratio is 1:15-1: 30;
preferably, the alkali solution is selected from NaOH, KOH, or Mg (OH)2And more preferably NaOH.
Compared with the general alkaline leaching process, the alkaline leaching process adopted by the invention improves the concentration and temperature of the alkali liquor, prolongs the alkaline leaching time, can effectively remove non-fiber impurities in the regenerated pulp of the textile, can accelerate the degradation speed of the cellulose in the regenerated pulp of the textile, and reduces the macromolecular polymerization degree of the regenerated cellulose, thereby improving the quality of the prepared glue solution.
In a further scheme, a bleaching agent is added in the alkaline leaching process in the step (1), and the concentration of the bleaching agent is 0.5-5g/L, preferably 1-3 g/L;
preferably, the bleaching agent comprises at least one of sodium hypochlorite, calcium hypochlorite, hydrogen peroxide or sodium thiosulfate, and hydrogen peroxide is preferred.
In the scheme of the application, the bleaching agent is added in the alkaline leaching process, so that on one hand, the colored groups carried in the regenerated pulp can be effectively removed, the interference of the bleaching agent on the alkaline leaching effect is reduced, and meanwhile, the phenomenon of uneven color of the finished product is avoided, and the fiber quality is ensured. On the other hand, the bleaching agent is added in the alkaline leaching process, the bleaching agent and the alkaline leaching agent play a synergistic role, the purpose of further reducing the polymerization degree of the fibers can be achieved, the quality of the prepared glue solution is improved, and the spinning performance is improved.
In a further scheme, the squeezing process in the step (1) is to press off the redundant alkali liquor in the pulp, the alkali cellulose is compressed and deformed, and the alkali liquor is discharged through capillary pores of the fibers.
In a further scheme, the crushing process in the step (1) is to crush the squeezed alkali cellulose, so that the specific surface area of the fibers is further increased, and the reaction capability of the fibers in the next step is improved.
Further, a catalyst is added in the crushing process in the step (1), and the adding amount of the catalyst is 150-300 g/ton of cellulose, preferably 180-260 g/ton of cellulose;
preferably, the catalyst comprises at least one of cobalt chloride, manganese dioxide, iron oxide, more preferably cobalt chloride.
The catalyst is added in the crushing process, so that the alkali cellulose can be rapidly degraded under the aerobic condition in the subsequent ageing process, the dosage of the catalyst is further increased, the cellulose degradation speed can be further increased if the addition of the cobalt chloride is increased, the content of the methyl cellulose is increased, the aim of fully utilizing the waste textile regenerated pulp is fulfilled, the concentration of the prepared spinning glue solution is increased, and the spinning requirement is met.
In a further scheme, the definite volume weight of the alkali cellulose after crushing in the step (1) is less than or equal to 130 g/L.
In a further scheme, the aging process in the step (2) refers to the oxidative degradation of cellulose in an alkaline medium, so that the polymerization degree of the cellulose meets the process requirement. In the scheme, the aging temperature is 25-70 ℃, the time is 10-60min, preferably 40-60 ℃, and 20-50 min.
The degradation of the alkali cellulose is rapid in the initial stage, and the degradation speed is continuously reduced along with the time, so that the aging time is not required to be overlong. With the rise of the aging temperature, the polymerization degree of cellulose and the viscosity of the glue solution are gradually reduced, the content of hemicellulose is increased, the selection of the aging temperature is crucial to the quality of the glue solution, and two quality indexes of the polymerization degree and the content of hemicellulose need to be comprehensively considered.
In the further scheme, in the yellowing process in the step (2), a yellow acid group is introduced to cellulose macromolecules, the distance between the cellulose macromolecules is increased, hydrogen bonds between the macromolecules are weakened, and the generated cellulose xanthate is more easily dissolved in alkali liquor.
In the further scheme, in the dissolving process in the step (2), the cellulose xanthate is dispersed in a dilute alkali solution, the xanthate groups are transferred, the cellulose crystal lattice is thoroughly destroyed, and the solvent diffuses and convectively diffuses towards polymer molecules to finally form a uniform solution.
In a further scheme, in the step (3), the filtration is multistage and multistage filtration, wherein:
the first stage of filtration adopts a screen filter which can filter out insoluble blended fiber and large insoluble impurities. The first stage filtration pressure is 0.1-0.4Mpa, the first stage filtration precision is 10-100mm, the second stage filtration pressure is 0.1-0.4Mpa, the second stage filtration precision is 10-70mm, preferably the first stage filtration pressure is 0.1-0.2Mpa, the first stage filtration precision is 20-80mm, the second stage filtration pressure is 0.1-0.2Mpa, and the second stage filtration precision is 20-50 mm.
And a plate-and-frame filter is adopted for secondary filtration, and the plate-and-frame filter is mainly used for filtering fibrous gel which is highly swelled but not dissolved, and part of dust, rust, sand grains and the like. The first-stage filtration pressure is 0.2-0.4MPa, the first-stage filtration precision is 0.1-5mm, the second-stage filtration pressure is 0.2-0.4MPa, the second-stage filtration precision is 0.1-2mm, the third-stage filtration pressure is 0.3-0.4MPa, the third-stage filtration precision is 0.1-0.5mm, preferably the first-stage filtration pressure is 0.2-0.3MPa, the first-stage filtration precision is 0.1-2mm, the second-stage filtration pressure is 0.3-0.4MPa, the second-stage filtration precision is 0.1-1mm, the third-stage filtration pressure is 0.3-0.4MPa, and the third-stage filtration precision is 0.1-0.3 mm.
And the KK filter is adopted in the third-stage filtration, and can filter out incompletely dissolved cellulose macromolecules, cellulose cell walls, chelators of hemicellulose and Fe, Ca and Cu and metal crystals with higher polymerization degree and lower gamma value. The first stage filtration pressure is 0.4-0.8MPa, the filtration precision is 50-200 μm, the second stage filtration pressure is 0.4-0.8MPa, the second stage filtration precision is 5-50 μm, preferably the first stage filtration pressure is 0.4-0.6MPa, the first stage filtration precision is 50-100 μm, the second stage filtration pressure is 0.4-0.6MPa, and the second stage filtration precision is 5-30 μm.
In the step (2), the content of the regenerated spinning glue solution methylcellulose is 5-13%, preferably 6-10%.
In the step (3), the regenerated spinning glue solution and the common spinning glue solution are mixed and then are filtered, defoamed and spun, and the volume mixing ratio of the regenerated spinning glue solution to the common spinning glue solution is 20:80-100: 0;
the regenerated glue solution can be used for spinning independently, and can also be mixed with the common glue solution according to a certain proportion for spinning, so that the quality of the spinning glue solution can be ensured, the spinning stability is ensured, the product performance reaches the standard, the regenerated glue solution can be reasonably utilized, the application field of the regenerated pulp of the textile is widened, and the aim of recycling the textile is fulfilled.
Preferably, the volume mixing ratio of the regenerated spinning glue solution to the common spinning glue solution is 40:60-90: 10;
preferably, the content of the methylcellulose in the common spinning glue solution is 5-13%, the viscosity is 35-50S, and the content of alkali is 4.5-6.5%, more preferably, the content of the methylcellulose in the common spinning glue solution is 7-12%, the viscosity is 39-45S, and the content of alkali is 4.8-6.0%.
In the further scheme, in the defoaming process in the step (3), the glue solution is placed under a negative pressure condition, so that bubbles and dissolved air in the glue solution are discharged, and bubble filaments, defects and broken ends of spinning are avoided.
In a further scheme, the spinning process in the step (3) is wet spinning.
The second purpose of the invention is to provide the regenerated cellulose fiber prepared by the preparation method, wherein the dry breaking strength of the regenerated cellulose fiber is more than or equal to 2.05cN/dtex, the dry strength variation coefficient is less than or equal to 14.0%, the wet breaking strength is more than or equal to 1.05cN/dtex, and the whiteness is 60-80%.
In the invention, the dry strength variation coefficient (dry strength CV value), namely the yarn evenness variation coefficient, is one of yarn evenness test indexes, and the smaller the dry strength variation coefficient, the better the evenness.
After adopting the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp, which is characterized in that the waste textile regenerated pulp is subjected to pre-crushing treatment, the average fiber length after the pre-crushing treatment is 0.5-5.0mm, preferably 1-3mm, and the fibers are short, so that the contact surface and the channels of alkali liquor immersed fibers can be increased, the alkali immersion effect is improved, and the concentration and the quality of glue solution are improved.
2. Because the polymerization degree of cellulose in the waste textile regenerated pulp is higher, in the preparation method, the bleaching agent is added in the alkaline leaching process, and the alkaline leaching and bleaching are combined and have synergistic effect, so that the purpose of reducing the polymerization degree of the fiber glue solution can be better achieved, colored groups can be removed, the whiteness of a fiber finished product is improved, and the purpose of improving the quality of the glue solution is achieved.
3. In the preparation method, the catalyst is added in the crushing process, so that the polymerization degree of the alkali cellulose can be quickly reduced in an aerobic state, the quality of the glue solution is improved, the reaction time is shortened, and the production efficiency is improved.
4. According to the preparation method, the regenerated fiber glue solution is filtered in a multi-stage and multi-section filtering mode, the filtering precision is high, the obtained regenerated fiber glue solution is more favorable for spinning, the yarn evenness is better, and the obtained regenerated cellulose fiber has better physical and chemical properties.
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, and the following embodiments are used for illustrating the present invention and are not used for limiting the scope of the present invention.
Example 1
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of the crushed fiber is 2.0mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 235g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 2 g/L. The pulp after the dipping treatment is pressed and crushed, the catalyst cobalt chloride is added during the crushing, the addition amount is 240 g/ton of cellulose, and the definite volume weight of the obtained alkali cellulose is 126 g/L. And then aging the alkali cellulose at 45 ℃ for 40min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.7%.
The dissolved regenerated spinning glue solution is filtered in multiple stages and sections, wherein a filter screen type filter is adopted for the first stage filtration, the first stage filtration pressure is 0.1Mpa, the filtration precision is 40mm, the second stage filtration pressure is 0.2Mpa, and the filtration precision is 20 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.2Mpa, the filtration precision is 2mm, the second stage filtration pressure is 0.3Mpa, the filtration precision is 1mm, the third stage filtration pressure is 0.3Mpa, and the filtration precision is 0.2 mm; the third stage filtration adopts a KK filter, the first stage filtration pressure is 0.4MPa, the filtration precision is 60 mu m, the second stage filtration pressure is 0.6MPa, and the filtration precision is 20 mu m.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 40:60, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.29cN/dtex, the dry strength variation coefficient is 10.6%, the wet breaking strength is 1.17cN/dtex, and the whiteness is 70.5%.
Example 2
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of the crushed fiber is 2.3mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 240g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 2 g/L. And squeezing and crushing the pulp subjected to the dipping treatment, adding a catalyst cobalt chloride when crushing, wherein the addition amount is 215 g/ton of cellulose, and the obtained alkali cellulose has the definite volume weight of 124 g/L. And then aging the alkali cellulose at 50 ℃ for 40min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.7%.
The dissolved regenerated spinning glue solution is filtered by a plurality of stages and sections, wherein the first stage of filtration adopts a filter screen type filter, the first stage of filtration has the filtration pressure of 0.1Mpa and the filtration precision of 50mm, and the second stage of filtration has the filtration pressure of 0.1Mpa and the filtration precision of 30 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.2Mpa, the filtration precision is 2mm, the second stage filtration pressure is 0.3Mpa, the filtration precision is 1mm, the third stage filtration pressure is 0.4Mpa, and the filtration precision is 0.2 mm; the third stage filtration adopts a KK filter, the first stage filtration pressure is 0.6MPa, the filtration precision is 50 μm, the second stage filtration pressure is 0.8MPa, and the filtration precision is 15 μm.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 50: 50, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.21cN/dtex, the dry strength variation coefficient is 10.9%, the wet breaking strength is 1.14cN/dtex, and the whiteness is 70.2%.
Example 3
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of the crushed fiber is 2.7mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 240g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 1 g/L. The pulp after the dipping treatment is pressed and crushed, the catalyst cobalt chloride is added during the crushing, the addition amount is 180 g/ton of cellulose, and the definite volume weight of the obtained alkali cellulose is 120 g/L. And then aging the alkali cellulose at 55 ℃ for 30min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.5%.
The dissolved regenerated spinning glue solution is filtered in multiple stages and sections, wherein a filter screen type filter is adopted for the first stage filtration, the first stage filtration pressure is 0.1Mpa, the filtration precision is 100mm, the second stage filtration pressure is 0.2Mpa, and the filtration precision is 70 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.2Mpa, the filtration precision is 0.1mm, the second stage filtration pressure is 0.3Mpa, the filtration precision is 0.1mm, the third stage filtration pressure is 0.4Mpa, and the filtration precision is 0.1 mm; the third stage filtration adopts a KK filter, the first stage filtration pressure is 0.4MPa, the filtration precision is 200 mu m, the second stage filtration pressure is 0.6MPa, and the filtration precision is 50 mu m.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 70: 30, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.17cN/dtex, the dry strength variation coefficient is 12.6%, the wet breaking strength is 1.10cN/dtex, and the whiteness is 69.2%.
Example 4
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of the crushed fiber is 0.5mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 240g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 0.5 g/L. The pulp after the dipping treatment is pressed and crushed, and a catalyst cobalt chloride is added during the crushing, the addition amount is 300 g/ton of cellulose, and the definite volume weight of the obtained alkali cellulose is 119 g/L. And then aging the alkali cellulose at 50 ℃ for 10min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.2%.
The dissolved regenerated spinning glue solution is filtered in multiple stages and sections, wherein a filter screen type filter is adopted for the first stage filtration, the first stage filtration pressure is 0.1Mpa, the filtration precision is 60mm, the second stage filtration pressure is 0.1Mpa, and the filtration precision is 20 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.2Mpa, the filtration precision is 4mm, the second stage filtration pressure is 0.2Mpa, the filtration precision is 1mm, the third stage filtration pressure is 0.3Mpa, and the filtration precision is 0.5 mm; the third stage filtration adopts a KK filter, the first stage filtration pressure is 0.4MPa, the filtration precision is 60 mu m, the second stage filtration pressure is 0.4MPa, and the filtration precision is 30 mu m.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 70: 30, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.11cN/dtex, the dry strength variation coefficient is 12.1%, the wet breaking strength is 1.07cN/dtex, and the whiteness is 68.3%.
Example 5
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of crushed fibers is 5.0mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 240g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 1.5 g/L. The pulp after the dipping treatment is pressed and crushed, and a catalyst cobalt chloride is added during the crushing, the addition amount is 245 g/ton of cellulose, and the definite volume weight of the obtained alkali cellulose is 115 g/L. And then aging the alkali cellulose at 70 ℃ for 50min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.1%.
The dissolved regenerated spinning glue solution is filtered in multiple stages and sections, wherein a filter screen type filter is adopted in the first stage of filtration, the first stage of filtration has the filtration pressure of 0.2Mpa and the filtration precision of 10mm, and the second stage of filtration has the filtration pressure of 0.3Mpa and the filtration precision of 10 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.3Mpa, the filtration precision is 3mm, the second stage filtration pressure is 0.4Mpa, the filtration precision is 0.5mm, the third stage filtration pressure is 0.4Mpa, and the filtration precision is 0.1 mm; the third stage filtration adopts a KK filter, the first stage filtration pressure is 0.6MPa, the filtration precision is 50 μm, the second stage filtration pressure is 0.8MPa, and the filtration precision is 20 μm.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 100:0, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.08cN/dtex, the dry strength variation coefficient is 12.7%, the wet breaking strength is 1.07cN/dtex, and the whiteness is 69.5%.
Example 6
The content of the used waste textile regenerated pulp cellulose is 82.9 percent, the viscosity is 16mpa.s, the iron content is 11ppm, and the whiteness is 45.7 percent.
Firstly, pre-crushing waste textile regenerated pulp, wherein the average length of the crushed fiber is 2.8mm, and then soaking the pulp in a sodium hydroxide solution, wherein the concentration of the sodium hydroxide solution is 240g/L, the temperature is 45 ℃, the soaking time is 50min, the bath ratio is 1:20, and the concentration of a bleaching agent hydrogen peroxide is 5 g/L. The pulp after the dipping treatment is pressed and crushed, the catalyst cobalt chloride is added during the crushing, the adding amount is 215 g/ton cellulose, and the definite volume weight of the obtained alkali cellulose is 115 g/L. And then aging the alkali cellulose at 25 ℃ for 60min to obtain a regenerated spinning glue solution, wherein the content of the glue solution methyl cellulose is 8.4%.
The dissolved regenerated spinning glue solution is filtered in multiple stages and sections, wherein a filter screen type filter is adopted in the first stage of filtration, the first stage of filtration has the filtration pressure of 0.4Mpa and the filtration precision of 20mm, and the second stage of filtration has the filtration pressure of 0.4Mpa and the filtration precision of 10 mm; the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.4Mpa, the filtration precision is 5mm, the second stage filtration pressure is 0.4Mpa, the filtration precision is 2mm, the third stage filtration pressure is 0.4Mpa, and the filtration precision is 0.5 mm; and a KK filter is adopted for three-stage filtration, the first-stage filtration pressure is 0.8MPa, the filtration precision is 20 microns, the second-stage filtration pressure is 0.8MPa, and the filtration precision is 5 microns.
Mixing the filtered regenerated spinning glue solution with the common spinning glue solution, wherein the volume mixing ratio is 20:80, wherein the content of the methylcellulose in the common spinning glue solution is 9.4 percent, the viscosity is 42S, the alkali content is 5.3 percent, and the mixed glue solution is defoamed and spun to obtain the regenerated cellulose fibers of the textile.
The dry breaking strength of the obtained waste textile regenerated pulp cellulose fiber is 2.17cN/dtex, the dry strength variation coefficient is 11.6%, the wet breaking strength is 1.10cN/dtex, and the whiteness is 72.8%.
Comparative example 1
The comparative example is the same as example 1 in raw materials and process, except that: in comparative example 1, the waste textile recycled pulp was not pre-crushed.
Comparative example 1 no regenerated spin dope could be prepared.
As can be seen from the comparison between example 1 and comparative example 1, the pre-pulverization treatment in the preparation method is one of the key factors influencing the success of preparing the regenerated spinning glue. When the preparation method is not provided with the pre-crushing step, as the length of the fiber in the waste textile regenerated pulp is larger, alkali liquor can not completely enter the inside of the longer fiber when the alkali leaching treatment is directly carried out, so that the alkali leaching effect is greatly influenced, the alkali leaching effect is not good, the quality of the alkali cellulose obtained after squeezing and crushing is poor, the subsequent yellowing reaction can not be smoothly carried out, the amount of the undissolved fiber is large (the amount of the wool glue is larger), and the spinning glue solution can not be prepared. Therefore, in conclusion, the contact surface and the channel of the alkali liquor immersed in the fiber can be increased by the pre-crushing treatment, so that the alkali immersion effect is improved, and the problems that the waste textile regenerated pulp is difficult to degrade and polymerize and the like are effectively solved.
Comparative example 2
The comparative example is the same as example 1 in raw materials and process, except that: comparative example 2 bleaching was carried out without addition of hydrogen peroxide in the alkaline leaching process.
The dry breaking strength of the waste textile regenerated pulp cellulose fiber obtained in the comparative example 2 is 1.47cN/dtex, the dry strength variation coefficient is 21.7%, the wet breaking strength is 0.76cN/dtex, and the whiteness is 52.3%.
As can be seen from the comparison between example 1 and comparative example 2, the addition of the bleaching agent in the alkaline leaching process in the preparation method can not only improve the whiteness of the prepared fiber, but also improve the properties of the prepared regenerated cellulose fiber, such as dry breaking strength, dry strength variation coefficient, wet breaking strength and the like.
Comparative example 3
The comparative example is the same as example 1 in raw materials and process, except that: comparative example 3 no catalyst was added during the crushing.
Comparative example 3 no regenerated spin dope could be prepared.
As can be seen from the comparison between example 1 and comparative example 3, the addition of the catalyst during the pulverization in the preparation method is also one of the key factors for determining whether the regenerated dope can be successfully prepared. When no catalyst is added in the crushing process, the reduction effect of the polymerization degree in the crushing process is poor, the polymerization degree is still high, the subsequent yellowing reaction is insufficient, the amount of undissolved fiber is large (the amount of crude rubber is large), and the spinning glue solution cannot be generated. Therefore, in summary, the catalyst is added in the crushing process, so that the polymerization degree of the alkali cellulose can be rapidly reduced in an aerobic state, the polymerization reduction efficiency is improved, and the glue solution quality is ensured.
Comparative example 4
The comparative example is the same as example 1 in raw materials and process, except that: in the comparative example 4, three-stage filtration is adopted in the filtration process, but multi-stage refinement is not carried out, wherein a filter screen type filter is adopted in the first-stage filtration, the filtration pressure is 0.2Mpa, and the filtration precision is 30 mm; the secondary filtration adopts a plate-and-frame filter, the filtration pressure is 0.4Mpa, and the filtration precision is 0.3 mm; and a KK filter is adopted for three-stage filtration, the filtration pressure is 0.6MPa, and the filtration precision is 30 mu m.
The waste textile regenerated pulp cellulose fiber obtained by the method of the comparative example 4 has the dry breaking strength of 1.83cN/dtex, the dry strength variation coefficient of 24.7 percent, the wet breaking strength of 0.82cN/dtex and the whiteness of 67.1 percent.
As can be seen from the comparison between the embodiment 1 and the comparative example 4, the preparation method adopts a multi-stage and multi-section filtering mode, so that the dry strength variation coefficient can be obviously reduced, the line uniformity is improved, and the performance of the regenerated cellulose fiber is improved.
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 (10)
1. A preparation method for producing regenerated cellulose fibers by using waste textile regenerated pulp is characterized by comprising the following steps:
(1) pre-crushing, alkaline leaching, squeezing and crushing the waste textile regenerated pulp to obtain alkali cellulose;
(2) aging, yellowing and dissolving the alkali cellulose in the step (1) to obtain a regenerated spinning glue solution;
(3) spinning the regenerated spinning glue solution obtained in the step (2), or mixing the regenerated spinning glue solution with a common spinning glue solution and then spinning to obtain the regenerated cellulose fiber.
2. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp as claimed in claim 1, wherein the waste textile regenerated pulp in step (1) has cellulose content not less than 80%, viscosity of 15-20mpa.s, iron content not more than 13ppm, and whiteness of 30-70%.
3. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp as claimed in claim 1 or 2, characterized in that, in the step (1), the average length of the fiber is 0.5-5.0mm after the waste textile regenerated pulp is pre-crushed;
preferably, the average length of the fibers is 1.0 to 3.0 mm.
4. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp according to any one of claims 1 to 3, characterized in that a bleaching agent is added in the alkaline leaching process in the step (1), and the concentration of the bleaching agent is 0.5 to 5g/L, preferably 1 to 3 g/L;
preferably, the bleaching agent is selected from at least one of sodium hypochlorite, calcium hypochlorite, hydrogen peroxide or sodium thiosulfate, and hydrogen peroxide is more preferred.
5. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp as claimed in any one of claims 1 to 4, characterized in that a catalyst is added during the pulverization in step (1), wherein the addition amount of the catalyst is 150-300 g/ton of cellulose, preferably 180-260 g/ton of cellulose;
preferably, the catalyst is selected from at least one of cobalt chloride, manganese dioxide and ferric oxide, and cobalt chloride is more preferable;
preferably, the definite volume weight of the alkali cellulose after the crushing in the step (1) is less than or equal to 130 g/L.
6. The method for preparing cellulose fiber by using regenerated pulp of textile as claimed in any one of claims 1 to 5, wherein the aging process in step (2) is carried out at an aging temperature of 25 to 70 ℃ for 10 to 60 min;
preferably 40-60 deg.C for 20-50 min.
7. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp according to any one of claims 1 to 6, characterized in that in the step (3), the filtration adopts multistage multi-stage filtration, wherein:
the first stage filtration adopts a filter screen type filter, the first stage filtration pressure is 0.1-0.4Mpa, the first stage filtration precision is 10-100mm, the second stage filtration pressure is 0.1-0.4Mpa, and the second stage filtration precision is 10-70 mm; preferably, the first-stage filtration pressure is 0.1-0.2Mpa, the first-stage filtration precision is 20-80mm, the second-stage filtration pressure is 0.1-0.2Mpa, and the second-stage filtration precision is 20-50 mm;
the second stage filtration adopts a plate-and-frame filter, the first stage filtration pressure is 0.2-0.4Mpa, the first stage filtration precision is 0.1-5mm, the second stage filtration pressure is 0.2-0.4Mpa, the second stage filtration precision is 0.1-2mm, the third stage filtration pressure is 0.3-0.4Mpa, and the third stage filtration precision is 0.1-0.5 mm; preferably, the first-stage filtration pressure is 0.2-0.3MPa, the first-stage filtration precision is 0.1-2mm, the second-stage filtration pressure is 0.3-0.4MPa, the second-stage filtration precision is 0.1-1mm, the third-stage filtration pressure is 0.3-0.4MPa, and the third-stage filtration precision is 0.1-0.3 mm;
the third stage filtration adopts KK filter, the first stage filtration pressure is 0.4-0.8MPa, the filtration precision is 50-200 μm, the second stage filtration pressure is 0.4-0.8MPa, and the second stage filtration precision is 5-50 μm; preferably, the first-stage filtration pressure is 0.4-0.6MPa, the first-stage filtration precision is 50-100 μm, the second-stage filtration pressure is 0.4-0.6MPa, and the second-stage filtration precision is 5-30 μm.
8. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp according to any one of claims 1 to 7, characterized in that in the step (2), the content of the regenerated spinning glue solution methyl cellulose is 5 to 13 percent, preferably 6 to 10 percent.
9. The method for preparing regenerated cellulose fiber by using waste textile regenerated pulp according to any one of claims 1 to 8, characterized in that, in the step (3), the regenerated spinning glue solution and the common spinning glue solution are mixed and then filtered, defoamed and spun, and the volume mixing ratio of the regenerated spinning glue solution and the common spinning glue solution is 20:80-100: 0;
preferably, the volume mixing ratio of the regenerated spinning glue solution to the common spinning glue solution is 40:60-90: 10;
preferably, the content of the methylcellulose in the common spinning glue solution is 5-13%, the viscosity is 35-50S, and the content of alkali is 4.5-6.5%, more preferably, the content of the methylcellulose in the common spinning glue solution is 7-12%, the viscosity is 39-45S, and the content of alkali is 4.8-6.0%.
10. Regenerated cellulose fibers prepared by the preparation method of any one of claims 1 to 9, characterized in that the regenerated cellulose fibers have a dry breaking strength of not less than 2.05cN/dtex, a dry strength variation coefficient of not more than 14.0%, a wet breaking strength of not less than 1.05cN/dtex, and a whiteness of 60 to 80%.
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