CN116854989A - Method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon blended fabric and product - Google Patents
Method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon blended fabric and product Download PDFInfo
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- CN116854989A CN116854989A CN202310828393.4A CN202310828393A CN116854989A CN 116854989 A CN116854989 A CN 116854989A CN 202310828393 A CN202310828393 A CN 202310828393A CN 116854989 A CN116854989 A CN 116854989A
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- vinylon
- regenerated cellulose
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- polyester
- dissolving pulp
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- 229920002978 Vinylon Polymers 0.000 title claims abstract description 128
- 239000004744 fabric Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 89
- 229920000875 Dissolving pulp Polymers 0.000 title claims abstract description 81
- 239000004627 regenerated cellulose Substances 0.000 title claims abstract description 78
- 239000002699 waste material Substances 0.000 title claims abstract description 61
- 229920000742 Cotton Polymers 0.000 claims abstract description 84
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 57
- 238000002156 mixing Methods 0.000 claims abstract description 41
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 235000019253 formic acid Nutrition 0.000 claims abstract description 30
- 229920000433 Lyocell Polymers 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 29
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 23
- 229920000297 Rayon Polymers 0.000 claims abstract description 19
- 238000004061 bleaching Methods 0.000 claims abstract description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims description 62
- 238000010411 cooking Methods 0.000 claims description 56
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 48
- OSVXSBDYLRYLIG-UHFFFAOYSA-N dioxidochlorine(.) Chemical compound O=Cl=O OSVXSBDYLRYLIG-UHFFFAOYSA-N 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- -1 polyethylene Polymers 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 24
- 229910021641 deionized water Inorganic materials 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 24
- 239000000835 fiber Substances 0.000 claims description 22
- 239000011259 mixed solution Substances 0.000 claims description 20
- 239000004155 Chlorine dioxide Substances 0.000 claims description 19
- 235000019398 chlorine dioxide Nutrition 0.000 claims description 19
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 17
- QPCDCPDFJACHGM-UHFFFAOYSA-N N,N-bis{2-[bis(carboxymethyl)amino]ethyl}glycine Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(=O)O)CCN(CC(O)=O)CC(O)=O QPCDCPDFJACHGM-UHFFFAOYSA-N 0.000 claims description 17
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims description 17
- 150000004056 anthraquinones Chemical class 0.000 claims description 17
- 229960003330 pentetic acid Drugs 0.000 claims description 17
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 17
- 239000004698 Polyethylene Substances 0.000 claims description 16
- 229920004933 Terylene® Polymers 0.000 claims description 16
- 229920000573 polyethylene Polymers 0.000 claims description 16
- 238000007789 sealing Methods 0.000 claims description 16
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 16
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 15
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 15
- 238000004898 kneading Methods 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 13
- 230000029087 digestion Effects 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 229960001484 edetic acid Drugs 0.000 claims description 7
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 abstract description 39
- 238000010025 steaming Methods 0.000 abstract description 17
- 230000015556 catabolic process Effects 0.000 abstract description 10
- 238000006731 degradation reaction Methods 0.000 abstract description 10
- 229920002678 cellulose Polymers 0.000 description 14
- 239000001913 cellulose Substances 0.000 description 14
- 239000004745 nonwoven fabric Substances 0.000 description 12
- 238000009835 boiling Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 238000004064 recycling Methods 0.000 description 9
- 238000004090 dissolution Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 238000000926 separation method Methods 0.000 description 7
- 238000010306 acid treatment Methods 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000009987 spinning Methods 0.000 description 3
- LFTLOKWAGJYHHR-UHFFFAOYSA-N N-methylmorpholine N-oxide Chemical compound CN1(=O)CCOCC1 LFTLOKWAGJYHHR-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004537 pulping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920004934 Dacron® Polymers 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
- D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
- D06L4/20—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen
- D06L4/22—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen using inorganic agents
- D06L4/24—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs using agents which contain halogen using inorganic agents using chlorites or chlorine dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Paper (AREA)
Abstract
The application relates to a method for preparing regenerated cellulose dissolving pulp by using waste polyester and vinylon blended fabrics and a product thereof, which sequentially comprise the procedures of fabric opening, vinylon dissolving, polyester steaming, metal ion removing and bleaching; the vinylon dissolving and removing process comprises the following steps: adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 68-78 wt% for mixing and stirring; the polymerization degree of the regenerated cellulose dissolving pulp is 400-700; the prepared regenerated cellulose dissolving pulp is used for preparing regenerated cellulose fibers and products. According to the method for preparing the dissolving pulp from the waste polyester-vinylon cotton blended fabric, disclosed by the application, the polyester-vinylon blended fabric is effectively removed, the iron ion content is reduced, the whiteness of pulp is improved, and meanwhile, the cotton fiber component is effectively protected from serious degradation; the prepared regenerated cellulose dissolving pulp can be further used for preparing high-value regenerated cellulose products such as viscose and Lyocell with good mechanical properties.
Description
Technical Field
The application belongs to the technical field of high-value recycling of waste textiles, and relates to a method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabrics and a product thereof.
Background
The existing waste cotton dissolving pulp mostly adopts waste pure cotton with single component or waste polyester cotton textile with relatively simple component. However, most of textiles used in daily life are blended by different yarns with different properties, the components of the fabric and the hybridization material are complex, and the effective separation between the components is more difficult. A considerable part of civil clothes and military clothes fabrics are polyester-vinylon cotton blended materials, and an important raw material is provided for recycling waste textiles. The high-value recycling of the cotton component in the complex fabric is not reported in research. How to realize the effective separation of vinylon and terylene components and the protection of the polymerization degree of cotton fibers (without significant degradation) is the key of the high-value recycling of the cotton components in the waste spinning materials.
The current method for preparing cellulose dissolving pulp aiming at waste polyester cotton fabrics is mature, and mainly adopts hydrolysis method or alcoholysis method to depolymerize polyester into monomers to be dissolved in black liquor, and further filters cotton fiber components for preparing the dissolving pulp. As in patent CN112608513a, a high-temperature alkaline digestion process is adopted to decompose the polyester component in the polyester-cotton fabric into monomers, dissolve the monomers in the black liquor, and recover the rest cotton fibers to prepare high-quality cellulose pulp. However, if the method is aimed at polyester-vinylon blended fabrics, cotton components and vinylon cannot be separated.
Another method for recycling cotton components is to directly utilize NMMO/H 2 And dissolving cotton components by using solvents such as O and the like, filtering to remove insoluble terylene components, and further carrying out Lyocell spinning for recycling. However, the adhesion of the system after dissolution of the cotton component (cellulose) in such a process is high and excessiveThe filtration efficiency is extremely low, and the removal of dissolved impurities, dyes and the like in the waste spinning system is extremely difficult, so that the large-scale industrialized production is difficult. If the method is aimed at polyester-vinylon blended fabrics, vinylon and polyester are not dissolved in NMMO aqueous solution, so the method is not applicable, and similar problems exist.
In summary, the existing methods have certain limitations and cannot meet the requirement of effectively recycling cotton components in polyester-vinylon cotton blended fabrics. The method for directly dissolving cotton fibers has low filtration efficiency, is difficult to remove impurities, dyes and the like in the system, and cannot be used for large-scale production; the digestion hydrolysis method is a relatively promising separation mode, but is only suitable for recycling pure cotton or polyester cotton blended fabrics with simple components, and vinylon components in the polyester and vinylon cotton blended fabrics cannot be effectively removed.
Therefore, in order to effectively expand the range of recycling raw materials of waste textiles, it is necessary to develop a separation pulping method of waste polyester-vinylon cotton blended fabrics, which can effectively separate and remove vinylon and polyester components in cotton components while protecting the cotton components from severe degradation, and prepare high-quality regenerated cellulose dissolving pulp and products thereof by using cotton component products.
Disclosure of Invention
In order to solve the problems in the prior art, the application provides a method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabrics and a product thereof;
in order to achieve the above purpose, the application adopts the following scheme:
a method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric sequentially comprises the procedures of fabric opening, vinylon dissolving, polyester digestion, metal ion removal and bleaching;
the vinylon dissolving and removing process comprises the following steps: adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 68-78 wt% for mixing and stirring;
the polymerization degree of the regenerated cellulose dissolving pulp is 400-700, and the polymerization degree test method adopts FZ/T50010.3-2011.
As a preferable technical scheme:
according to the method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric, in the vinylon dissolving and removing process, the solid-to-liquid ratio of the waste polyester-vinylon blended fabric to the formic acid solution is 1:15-35, and the stirring time is 0.5-2 h.
The method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric comprises the following fabric opening procedures: crushing and opening the waste polyester-vinylon blended fabric into yarns with the length of 2-3 cm, and mechanically crushing and opening the yarns to ensure that vinylon dissolving liquid and cooking liquid fully contact the fabric, thereby shortening the time of vinylon removal and terylene removal treatment processes.
The method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric comprises the following steps of: fully washing and drying the product after vinylon is dissolved, and mixing the product with cooking liquor according to a solid-to-liquid ratio (the ratio of absolute dry mass of a cooking sample to mass of all water in a cooking system) of 1:5-10 for high-temperature cooking; the cooking temperature is 140-165 ℃.
According to the method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric, the cooking liquor is a mixed aqueous solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquor is 0.04-0.08 wt%, and the alkali consumption (the ratio of NaOH mass to oven dry mass of a cooking sample is expressed as mass percent) is 20-55%.
The method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric comprises the following metal ion removing steps: mixing the pulp obtained after the digestion with a metal ion removing liquid to obtain a mixture, intermittently stirring for a period of time at a certain temperature, and then centrifugally washing by using deionized water;
the metal ion removing liquid is prepared by mixing sulfuric acid, sodium Hexametaphosphate (SHMP), ethylenediamine tetraacetic acid (EDTA), diethylenetriamine pentaacetic acid (DTPA) and deionized water;
the certain temperature is 50-70 ℃ and the period of time is 30-60 min;
intermittent stirring means stirring once every 3-10 min for 30-60 s each time.
According to the method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon cotton blended fabric, the mass ratio of pulp obtained after digestion to metal ion removing liquid is 1:5-20;
in the metal ion removing liquid, the mass fraction of sulfuric acid is 1-4%, the mass fraction of diethylenetriamine pentaacetic acid is 0.6-1.0%, the mass fraction of ethylenediamine tetraacetic acid is 0.1-0.4%, and the mass fraction of sodium hexametaphosphate is 0.1-0.4%.
The method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric comprises the following bleaching steps: firstly, mixing pulp after metal ion removal with sulfuric acid solution with concentration of 0.3-1.0wt%, filling the mixture into a polyethylene sealing bag, and then introducing a certain amount of chlorine dioxide (ClO) 2 ) Intermittently kneading the gas at a certain temperature for a period of time, and finally centrifugally washing by using deionized water;
the pulp after metal ion removal is contained in the mixed solution in a polyethylene sealing bag, and the concentration of the pulp after metal ion removal is 5-10wt%;
the concentration of the dissolved chlorine dioxide is 0.4 to 0.8 weight percent;
the certain temperature is 50-70 ℃ and the period of time is 60-120 min;
the intermittent kneading time interval is 5-15 min, and the single kneading time is 15-30 s.
According to the method for preparing the regenerated cellulose dissolving pulp from the waste polyester-vinylon cotton blended fabric, the ISO whiteness of the regenerated cellulose dissolving pulp obtained after the treatment of the steaming, the metal ion removal and the bleaching process is more than or equal to 80%, the alpha fiber content in the regenerated cellulose dissolving pulp is 90-97%, and the iron ion content is less than or equal to 15ppm; the method for testing the content of the alpha-fiber adopts FZ/T50010.4; the ISO whiteness test method adopts FZ/T50010.7-1998; the iron ion content test method adopts FZ/T50010.6-1998.
The application also provides the application of the regenerated cellulose dissolving pulp prepared by the method according to any one of the above steps, which is used for preparing regenerated cellulose fibers and products;
regenerated cellulose fibers and articles include viscose, lyocell, viscose nonwoven, lyocell nonwoven and Lyocell film.
The regenerated cellulose fiber and the product have better mechanical properties, for example, the dry state breaking strength of the prepared regenerated Lyocell fiber is 3.80-4.60 cN/dtex, and the breaking elongation is 7.0-9.0%.
The principle of the application is as follows:
compared with the existing method for preparing waste cotton regenerated pulp (cellulose dissolving pulp) by using waste pure cotton or polyester cotton blended fabrics, the waste polyester and vinylon cotton blended fabrics are complex in components, vinylon and polyester components in the waste polyester and vinylon cotton blended fabrics need to be effectively separated and removed, and the cellulose dissolving pulp with high quality is prepared based on proper metal ion removal and bleaching processes. Therefore, the cellulose can be degraded by the processes of vinylon removal treatment by formic acid, polyester removal treatment by high-temperature alkaline digestion, bleaching and the like, which are more in requirements and process steps involved in the pulp preparation process, and the more severe the condition is, the better the removal effect is, but the more significant the degradation of the cellulose is. However, the formic acid treatment or the high-temperature alkaline digestion treatment has too mild conditions to completely remove vinylon and polyester components in the polyester-vinylon cotton blended fabric, so that the core aim and the requirements are to achieve the effective vinylon and polyester separation and removal effects, and to simultaneously prevent the cotton components from excessively degrading and further remarkably reduce the polymerization degree parameters of pulp. The vinylon component can not be removed by directly utilizing the existing polyester cotton digestion pulping process.
The application is based on a large number of exploring experiments, and the vinylon component in the polyester and vinylon blended fabric can be effectively removed by utilizing the high-concentration formic acid solution, and the polyester component in the blended fabric can be further effectively removed by a high-temperature alkaline cooking process. The application also discovers that the strategy of firstly removing vinylon and then removing vinylon has better effect than the strategy of firstly removing vinylon and then removing vinylon through comparative study, namely, the effect of removing vinylon and terylene in the product obtained by exchanging formic acid solution treatment and high-temperature alkaline cooking treatment procedures is different based on the same technological parameter conditions, wherein the effect of removing vinylon by adopting formic acid firstly and then cooking at high Wen Jianfa is better.
In addition, compared with the two-component polyester-cotton blended fabric with the same polyester-cotton ratio, the polyester in the three-component polyester-cotton blended fabric subjected to the vinylon removal treatment by the formic acid can be separated and removed more easily. The method is characterized in that vinylon in the yarns of the polyester-vinylon three-component fabric can be effectively removed after being treated by the formic acid solution, and the polyester fiber structure in the yarns can be damaged to a certain extent in a high-concentration formic acid environment, so that corrosion cracks appear on the surfaces of the polyester fibers, and hydrolysis is more likely to occur in the subsequent steaming process. Meanwhile, as vinylon is removed, the fabric density of the yarn is smaller, the structure is more loose, the surface of polyester fiber is also more rough, the sufficient contact and infiltration of cooking liquor are more facilitated in the subsequent cooking process, and the efficiency of cooking and removing polyester is further improved. If the high Wen Jianfa is adopted to cook and remove the terylene component in the terylene and vinylon cotton three-component yarn, the vinylon fiber can obviously shrink in a high-temperature cooking environment, so that the yarn structure is tightened, the winding with the other two components becomes tighter, the separation of the terylene component is not facilitated, and the subsequent formic acid treatment to remove the vinylon component can be adversely affected. Therefore, more severe digestion conditions and formic acid treatment conditions are required to completely remove the terylene and vinylon components, which consumes more energy and resources and also remarkably reduces the polymerization degree of cotton fibers.
In a comprehensive view, the higher the formic acid concentration is, the higher the alkali concentration and the boiling temperature are in alkaline boiling are, the removal of vinylon and terylene is facilitated, but too high formic acid concentration and too severe high-temperature alkaline boiling also obviously reduce the polymerization degree of cotton fibers, because the cotton fibers are gradually stripped and degraded in the process of separating and removing vinylon and terylene components. The polymerization degree of cellulose dissolving pulp is one of key factors influencing the spinnability and the mechanical properties of regenerated cellulose products, and the dissolving pulp with too low polymerization degree has poor spinnability and the prepared fiber has poor mechanical properties.
In order to effectively reconcile the contradiction, the application specially designs a formic acid vinylon removing process and a high-temperature alkaline steaming polyester removing process. In the vinylon removal treatment process of formic acid: when the concentration of formic acid is too low (less than 68 percent), the effective vinylon removing effect can not be achieved; with the improvement of the concentration of formic acid, the vinylon removal efficiency in the waste polyester-vinylon blended fabric is higher, but the rate of cotton fiber degradation is also higher, and the degradation degree of cotton fiber is positively correlated with the formic acid treatment time. The application adopts the process ranges of milder formic acid concentration (68-78%), treatment time (0.5-2 h) and the like, and reduces the degradation of cotton fiber as much as possible while ensuring the complete removal of vinylon components. In the further process of steaming and removing terylene: if the alkali concentration is too low, the steaming temperature and the steaming time are too short, the effective terylene removing effect cannot be achieved, and if the conditions are more severe, the terylene removing efficiency is higher, but the polymerization degree of cotton fibers is closely related to the steaming temperature, the steaming time and the alkali consumption, and the polymerization degree of the prepared regenerated cotton dissolving pulp is lower when the temperature is higher, the time is longer and the alkali consumption is higher. Therefore, the application adopts the relatively mild alkali consumption (20-55%), the cooking temperature (140-165 ℃) and the cooking time (1.5-2.5 h) and other technological ranges to completely remove the terylene component, and simultaneously reduces the cooking condition to bring serious degradation to the cotton fiber as far as possible. Meanwhile, a very small amount of anthraquinone is added into the cooking liquid to effectively reduce the reducing terminal of cellulose, so that alkaline degradation and peeling reaction of cotton fibers are slowed down, and excessive degradation and polymerization of cotton components are protected to a certain extent.
In addition, in the subsequent refining processes such as bleaching, the application adopts a mild chlorine dioxide bleaching process, and compared with a hypochlorous acid and hydrogen peroxide bleaching system, the chlorine dioxide bleaching system has less influence on the polymerization degree of cotton pulp. And finally, the vinylon and the terylene are effectively separated and removed, meanwhile, the cotton component is protected from excessive polymerization, and finally, the cellulose dissolving pulp with the polymerization degree of 400-700, the iron ion content of less than or equal to 15ppm and the whiteness of more than or equal to 80% is successfully prepared, and the pulp can be further used for preparing regenerated cellulose products such as viscose, lyocell and the like with good mechanical properties.
Advantageous effects
(1) According to the method for preparing regenerated cellulose dissolving pulp from the waste polyester-vinylon cotton blended fabric, disclosed by the application, the polyester-vinylon blended component is effectively removed, the iron ion content is reduced, the whiteness of pulp is improved, and meanwhile, the cotton fiber component is effectively protected from severe depolymerization.
(2) According to the method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon blended fabric, the waste polyester-vinylon blended fabric is utilized to prepare high-quality cellulose dissolving pulp, and the prepared cellulose dissolving pulp can be further used for preparing high-valued regenerated cellulose products such as viscose and Lyocell with good mechanical properties.
Drawings
Fig. 1 is an infrared spectrum of the products of the polyester and cotton blend fabrics, virgin cotton pulp, example 1 and comparative example 1 of the present application.
Detailed Description
The application is further described below in conjunction with the detailed description. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. Furthermore, it should be understood that various changes and modifications can be made by one skilled in the art after reading the teachings of the present application, and such equivalents are intended to fall within the scope of the application as defined in the appended claims.
The test method adopted in the application is as follows:
ISO whiteness: measured using FZ/T50010.7-1998.
Degree of polymerization: measured using FZ/T50010.3-2011.
Content of alpha fibers: measured using FZ/T50010.4.
Iron ion content: measured using FZ/T50010.6-1998.
In the embodiment, the waste polyester and vinylon blended fabric is waste camouflage clothing fabric.
Example 1
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into 2cm yarns;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 78wt percent according to the solid-to-liquid ratio of 1:15, mixing and stirring for 0.5h;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with cooking liquid according to a solid-to-liquid ratio of 1:5, and cooking at a high temperature of 165 ℃ for 1.5 hours;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.04wt% and the alkali consumption is 20%;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 1%, the mass fraction of diethylenetriamine pentaacetic acid is 0.6%, the mass fraction of ethylenediamine tetraacetic acid is 0.1%, and the mass fraction of sodium hexametaphosphate is 0.1%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:5 to obtain a mixture, stirring at 50 ℃ for 30 seconds every 3 minutes, stirring for 30 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.3wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, kneading once every 5min at 50 ℃, kneading for 15s for 60min, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, the concentration of the pulp after metal ion removal is 5wt% in the mixed solution filled in the polyethylene sealing bag; the concentration of chlorine dioxide after dissolution was 0.4wt%.
The ISO whiteness of the prepared regenerated cellulose dissolving pulp is 82.3 percent, and the polymerization degree is 700; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 90.4 percent, and the content of iron ions is 15ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Comparative example 1
The method for preparing cellulose dissolving pulp by using waste polyester-vinylon blended fabric is basically the same as that in example 1, and only the difference is that the sequence of the step (2) and the step (3) is reversed (namely, the step of steaming to remove polyester is performed in advance, and the step of dissolving to remove vinylon is performed).
Comparing example 1 with comparative example, it was found that the process parameters were not changed by merely exchanging the front and rear sequences of the steps of removing vinylon formate and removing polyester by steaming, so that the polyester fiber could not be completely removed to prepare regenerated cellulose dissolving pulp (as shown in FIG. 1, wherein 3430cm -1 Is characterized by cotton cellulose hydroxyl characteristic absorption peak, 1720cm -1 Is characterized by the characteristic absorption peak of polyester carbonyl and 730cm -1 The vinylon ether bond characteristic absorption peak), because vinylon can appear comparatively obvious shrink in high temperature cooking environment, will lead to yarn structure to tighten up, twine with other two components becomes more inseparable, is unfavorable for the separation of dacron component, also can bring adverse effect to follow-up formic acid treatment and remove vinylon component.
Example 2
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into 2cm yarns;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 74 weight percent according to the solid-to-liquid ratio of 1:20, mixing and stirring for 1h;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with a cooking solution according to a solid-to-liquid ratio of 1:8, and cooking at a high temperature of 150 ℃ for 2 hours;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.05wt% and the alkali consumption is 30%;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 1.5%, the mass fraction of diethylenetriamine pentaacetic acid is 0.7%, the mass fraction of ethylenediamine tetraacetic acid is 0.15%, and the mass fraction of sodium hexametaphosphate is 0.2%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:8 to obtain a mixture, stirring at 55 ℃ for 35 seconds every 4 minutes, stirring for 35 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.4wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, kneading once every 8min at 55 ℃, kneading for 18s for a total of 70min, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, the concentration of the pulp after metal ion removal is 8wt% in the mixed solution filled in the polyethylene sealing bag; the concentration of chlorine dioxide after dissolution was 0.5wt%.
The ISO whiteness of the prepared regenerated cellulose dissolving pulp is 84.2 percent, and the polymerization degree is 611; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 94.8 percent, and the content of iron ions is 14.1ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Example 3
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into yarns with the length of 2.5 cm;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 76 weight percent according to the solid-to-liquid ratio of 1:30, mixing and stirring for 1h;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with cooking liquid according to the solid-to-liquid ratio of 1:7, and cooking at a high temperature of 155 ℃ for 2 hours;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.06wt%, and the alkali consumption is 45%;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 2.5%, the mass fraction of diethylenetriamine pentaacetic acid is 0.8%, the mass fraction of ethylenediamine tetraacetic acid is 0.2%, and the mass fraction of sodium hexametaphosphate is 0.25%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:10 to obtain a mixture, stirring at 65 ℃ for 40 seconds every 5 minutes, stirring for 40 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.5wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, kneading once every 10min at 60 ℃ for 20s, kneading for 80min in total, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, in the mixed solution in the polyethylene sealing bag, the concentration of the pulp after metal ion removal is 7wt%; the concentration of chlorine dioxide after dissolution was 0.6wt%.
The prepared regenerated cellulose dissolving pulp has 86.5% of ISO whiteness and 578 of polymerization degree; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 93.5 percent, and the content of iron ions is 12.6ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Example 4
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into yarns with the length of 2.5 cm;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 70 weight percent according to the solid-to-liquid ratio of 1:25, mixing and stirring for 2 hours;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with cooking liquid according to a solid-to-liquid ratio of 1:6, and cooking at 160 ℃ for 1.5h;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.08wt percent, and the alkali consumption is 40 percent;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 2%, the mass fraction of diethylenetriamine pentaacetic acid is 1%, the mass fraction of ethylenediamine tetraacetic acid is 0.25%, and the mass fraction of sodium hexametaphosphate is 0.3%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:15 to obtain a mixture, stirring at 60 ℃ for 45 seconds every 6 minutes, stirring for 45 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.8wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, kneading once every 12min at 65 ℃ for 25s, kneading for 100min, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, the concentration of the pulp after metal ion removal is 8wt% in the mixed solution filled in the polyethylene sealing bag; the concentration of chlorine dioxide after dissolution was 0.7wt%.
The ISO whiteness of the prepared regenerated cellulose dissolving pulp is 90.0%, and the polymerization degree is 512; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 95.1 percent, and the content of iron ions is 12.3ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Example 5
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into yarns with the length of 3 cm;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 72wt% according to the solid-to-liquid ratio of 1:30, mixing and stirring for 1.5h;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with cooking liquid according to the solid-to-liquid ratio of 1:9, and cooking at 145 ℃ for 2.5 hours;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.07wt percent, and the alkali consumption is 50 percent;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 3%, the mass fraction of diethylenetriamine pentaacetic acid is 0.9%, the mass fraction of ethylenediamine tetraacetic acid is 0.3%, and the mass fraction of sodium hexametaphosphate is 0.35%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:18 to obtain a mixture, stirring at 67 ℃ for 50 seconds every 8 minutes, stirring for 50 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.7wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, rubbing once every 13min at 70 ℃, rubbing for 28s once, rubbing for 110min altogether, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, in the mixed solution in the polyethylene sealing bag, the concentration of the pulp after metal ion removal is 7wt%; the concentration of chlorine dioxide after dissolution was 0.8wt%.
The ISO whiteness of the prepared regenerated cellulose dissolving pulp is 89.2 percent, and the polymerization degree is 455; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 92.1 percent, and the content of iron ions is 10.8ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Example 6
A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric comprises the following specific steps:
(1) A fabric opening procedure;
crushing and opening the waste polyester-vinylon cotton blended fabric into yarns with the length of 3 cm;
(2) A vinylon dissolving and removing step;
adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 68 weight percent according to the solid-to-liquid ratio of 1:35, mixing and stirring for 2 hours;
(3) A polyester steaming and boiling step;
fully washing and drying the product after vinylon is dissolved, mixing the product with a cooking solution according to a solid-to-liquid ratio of 1:10, and cooking at a high temperature of 140 ℃ for 2.5 hours;
wherein, the cooking liquid is a mixed water solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquid is 0.08wt percent, and the alkali consumption is 55 percent;
(4) A metal ion removing step;
(4.1) mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water to prepare a metal ion removing liquid; wherein, in the metal ion removing liquid, the mass fraction of sulfuric acid is 4%, the mass fraction of diethylenetriamine pentaacetic acid is 1%, the mass fraction of ethylenediamine tetraacetic acid is 0.4%, and the mass fraction of sodium hexametaphosphate is 0.4%;
(4.2) mixing the pulp obtained after the cooking in the step (3) with a metal ion removing liquid in a mass ratio of 1:20 to obtain a mixture, stirring at 70 ℃ for 60 seconds every 10 minutes, stirring for 60 minutes, and then centrifugally washing by using deionized water;
(5) Bleaching;
firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 1wt% to obtain mixed solution, filling the mixed solution into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, rubbing once every 15min at 70 ℃ for 30s, rubbing for 120min altogether, and finally, centrifugally washing by using deionized water to obtain regenerated cellulose dissolving pulp;
wherein, the concentration of the pulp after metal ion removal is 10wt% in the mixed solution filled in the polyethylene sealing bag; the concentration of chlorine dioxide after dissolution was 0.8wt%.
The ISO whiteness of the prepared regenerated cellulose dissolving pulp is 91.1 percent, and the polymerization degree is 400; the content of alpha-fiber in the regenerated cellulose dissolving pulp is 96.9 percent, and the content of iron ions is 9.5ppm; the prepared regenerated cellulose dissolving pulp can be used for preparing viscose fibers, lyocell fibers, viscose non-woven fabrics, lyocell non-woven fabrics and Lyocell films.
Claims (10)
1. A method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric is characterized by comprising the following steps: sequentially comprises the procedures of fabric opening, vinylon dissolving, terylene removing by stewing, metal ion removing and bleaching;
the vinylon dissolving and removing process comprises the following steps: adding the opened polyester-vinylon cotton blended fabric into a formic acid solution with the concentration of 68-78 wt% for mixing and stirring;
the polymerization degree of the regenerated cellulose dissolving pulp is 400-700.
2. The method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabric according to claim 1, wherein in the vinylon dissolving and removing process, the solid-to-liquid ratio of the waste polyester-vinylon cotton blended fabric to formic acid solution is 1:15-35, and the stirring time is 0.5-2 h.
3. The method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabric according to claim 1, wherein the fabric opening procedure is as follows: crushing and opening the waste polyester-vinylon cotton blended fabric into yarns with the length of 2-3 cm.
4. The method for preparing regenerated cellulose dissolving pulp from waste polyester-cotton blend fabrics according to claim 1, which is characterized in that the polyester-removing procedure by digestion is as follows: fully washing and drying the product after vinylon is dissolved, and mixing the product with a cooking liquid according to a solid-liquid ratio of 1:5-10 for high-temperature cooking; the cooking temperature is 140-165 ℃.
5. The method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon blended fabric according to claim 4, wherein the cooking liquor is a mixed aqueous solution of NaOH and anthraquinone, the content of anthraquinone in the cooking liquor is 0.04-0.08 wt%, and the alkali consumption is 20-55%.
6. The method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabric according to claim 1, wherein the metal ion removing process is as follows: mixing the pulp obtained after the digestion with a metal ion removing liquid to obtain a mixture, intermittently stirring for a period of time at a certain temperature, and then centrifugally washing by using deionized water;
the metal ion removing liquid is prepared by mixing sulfuric acid, sodium hexametaphosphate, ethylenediamine tetraacetic acid, diethylenetriamine pentaacetic acid and deionized water;
the certain temperature is 50-70 ℃ and the period of time is 30-60 min;
intermittent stirring means stirring once every 3-10 min for 30-60 s each time.
7. The method for preparing regenerated cellulose dissolving pulp from waste polyester-vinylon cotton blended fabric according to claim 6, wherein the mass ratio of pulp obtained after digestion to metal ion removing liquid is 1:5-20;
in the metal ion removing liquid, the mass fraction of sulfuric acid is 1-4%, the mass fraction of diethylenetriamine pentaacetic acid is 0.6-1.0%, the mass fraction of ethylenediamine tetraacetic acid is 0.1-0.4%, and the mass fraction of sodium hexametaphosphate is 0.1-0.4%.
8. The method for preparing regenerated cellulose dissolving pulp by using waste polyester-vinylon blended fabric as claimed in claim 1, wherein the bleaching process is as follows: firstly, mixing pulp after metal ion removal with sulfuric acid solution with the concentration of 0.3-1.0wt%, filling the mixture into a polyethylene sealing bag, then introducing a certain amount of chlorine dioxide gas, intermittently kneading for a period of time at a certain temperature, and finally, centrifugally washing by using deionized water;
the pulp after metal ion removal is contained in the mixed solution in a polyethylene sealing bag, and the concentration of the pulp after metal ion removal is 5-10wt%;
the concentration of the dissolved chlorine dioxide is 0.4 to 0.8 weight percent;
the certain temperature is 50-70 ℃ and the period of time is 60-120 min;
the intermittent kneading time interval is 5-15 min, and the single kneading time is 15-30 s.
9. The method for preparing regenerated cellulose dissolving pulp by using the waste polyester-vinylon cotton blended fabric as claimed in claim 1, wherein the ISO whiteness of the regenerated cellulose dissolving pulp is more than or equal to 80%, the alpha-fiber content in the regenerated cellulose dissolving pulp is 90-97%, and the iron ion content is less than or equal to 15ppm.
10. Use of the regenerated cellulose dissolving pulp produced by the method according to any one of claims 1 to 9, characterized in that: used for preparing regenerated cellulose fiber and products;
regenerated cellulose fibers and articles include viscose, lyocell, viscose nonwoven, lyocell nonwoven and Lyocell film.
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| CN118127847A (en) * | 2024-05-08 | 2024-06-04 | 江苏恒力化纤股份有限公司 | Method for preparing cellulose dissolving pulp from waste polyester-spandex cotton blended fabric and product |
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| CN118127847A (en) * | 2024-05-08 | 2024-06-04 | 江苏恒力化纤股份有限公司 | Method for preparing cellulose dissolving pulp from waste polyester-spandex cotton blended fabric and product |
| CN118127847B (en) * | 2024-05-08 | 2024-09-24 | 江苏恒力化纤股份有限公司 | Method for preparing cellulose dissolving pulp from waste polyester-spandex cotton blended fabric and product |
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