CN113818232A - High water absorption fiber and preparation method thereof - Google Patents
High water absorption fiber and preparation method thereof Download PDFInfo
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- CN113818232A CN113818232A CN202110893034.8A CN202110893034A CN113818232A CN 113818232 A CN113818232 A CN 113818232A CN 202110893034 A CN202110893034 A CN 202110893034A CN 113818232 A CN113818232 A CN 113818232A
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- 239000000835 fiber Substances 0.000 title claims abstract description 198
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 60
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 24
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000004132 cross linking Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
- 230000008961 swelling Effects 0.000 claims abstract description 9
- 239000004593 Epoxy Substances 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical group CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 30
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000009210 therapy by ultrasound Methods 0.000 claims description 20
- UWFRVQVNYNPBEF-UHFFFAOYSA-N 1-(2,4-dimethylphenyl)propan-1-one Chemical compound CCC(=O)C1=CC=C(C)C=C1C UWFRVQVNYNPBEF-UHFFFAOYSA-N 0.000 claims description 19
- 239000003513 alkali Substances 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 16
- 229920000742 Cotton Polymers 0.000 claims description 14
- 238000002791 soaking Methods 0.000 claims description 14
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- GAWAYYRQGQZKCR-REOHCLBHSA-N (S)-2-chloropropanoic acid Chemical compound C[C@H](Cl)C(O)=O GAWAYYRQGQZKCR-REOHCLBHSA-N 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 claims description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 240000000111 Saccharum officinarum Species 0.000 claims description 5
- 235000007201 Saccharum officinarum Nutrition 0.000 claims description 5
- 239000002250 absorbent Substances 0.000 claims description 5
- 230000002745 absorbent Effects 0.000 claims description 5
- RVBUZBPJAGZHSQ-UHFFFAOYSA-N 2-chlorobutanoic acid Chemical compound CCC(Cl)C(O)=O RVBUZBPJAGZHSQ-UHFFFAOYSA-N 0.000 claims description 4
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 4
- 229940106681 chloroacetic acid Drugs 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- IVIDDMGBRCPGLJ-UHFFFAOYSA-N 2,3-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(CO)COCC1CO1 IVIDDMGBRCPGLJ-UHFFFAOYSA-N 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 3
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 3
- 240000000560 Citrus x paradisi Species 0.000 claims description 3
- 244000060011 Cocos nucifera Species 0.000 claims description 3
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 3
- 244000082204 Phyllostachys viridis Species 0.000 claims description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 3
- 229920001131 Pulp (paper) Polymers 0.000 claims description 3
- 230000003113 alkalizing effect Effects 0.000 claims description 3
- 239000011425 bamboo Substances 0.000 claims description 3
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 claims description 3
- 150000005846 sugar alcohols Polymers 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 206010042674 Swelling Diseases 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 34
- 239000007788 liquid Substances 0.000 description 16
- 238000000926 separation method Methods 0.000 description 14
- 239000000047 product Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000006266 etherification reaction Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000002504 physiological saline solution Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/11—Compounds containing epoxy groups or precursors thereof
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- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
- D06M13/148—Polyalcohols, e.g. glycerol or glucose
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- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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Abstract
The invention discloses a preparation method of high water absorption fiber, which comprises the following steps: sequentially carrying out alkalization treatment, swelling treatment, hydrophilic treatment and crosslinking curing treatment on the natural fibers to obtain a water-insoluble high-water-absorption fiber finished product; wherein, the cross-linking agent adopted in the cross-linking curing process is one or more of epoxy compound, polyhydroxy alcohol, aziridine and glycerol. Correspondingly, the invention also discloses a high water-absorption fiber which is prepared by adopting the preparation method. By implementing the invention, the water absorption capacity and the water locking capacity of the natural fiber can be greatly improved under the condition of not changing the appearance of the natural fiber.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a high water absorption fiber and a preparation method thereof.
Background
The high water absorption fiber (SAF) is a novel functional fiber developed after high water absorption resin (SAP), and the water absorption rate of the high water absorption fiber is dozens to hundreds of times larger than that of common fibers. The high water absorption fiber not only has the chemical structure characteristics of water absorption, water retention, swelling and the like of the high water absorption resin, but also has the characteristics of high water absorption rate, good processability and the like due to the physical form and size particularity of the fiber, and has wide market application prospect. The method for preparing the high water absorption fiber in the prior art is various, the preparation process is complex, residues or degradation products with certain toxicity can exist in the prepared high water absorption fiber, and the fiber obtained by the traditional preparation method can not necessarily meet the high water absorption requirement.
In view of the above problems, the applicant proposed a patent application (application number: 201811650836.0) of a hyperbranched structure superabsorbent fiber and a preparation method thereof in 2018. The method changes the appearance of the raw material fiber, and has the advantages of complex process and higher preparation cost.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of high water absorption fiber, which has simple process and low cost, and the obtained fiber has strong water absorption performance.
The invention also aims to solve the technical problem of providing the high water absorption fiber.
In order to solve the technical problems, the invention provides a preparation method of high water absorption fiber, which comprises the following steps:
(1) providing a natural fiber;
(2) alkalizing the natural fibers to obtain alkalized fibers;
(3) soaking the alkalized fiber in a solvent to swell the alkalized fiber to obtain swollen fiber;
(4) carrying out grafting reaction on the swelling fiber to obtain hydrophilic fiber;
(5) crosslinking and curing the hydrophilic fiber by using a crosslinking agent to form a finished product of the water-insoluble high-water-absorption fiber;
wherein, the cross-linking agent adopted in the cross-linking curing process is one or more of epoxy compound, polyhydroxy alcohol, aziridine and glycerol.
As an improvement of the technical scheme, the epoxy compound is one or more of ethylene glycol diglycidyl ether, glycerol diglycidyl ether and ethylene glycol diacrylate;
the polyhydric alcohol is one or more selected from ethylene glycol, propylene glycol, butanediol, pentanediol and pentaerythritol;
the natural fiber is selected from one or more of cotton fiber, sugarcane fluff fiber, wood pulp fluff fiber, bamboo fluff fiber, pomelo peel fiber and coconut coir fiber.
As an improvement of the technical scheme, the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol;
the weight ratio of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol is (5-10): 1: (3-5): (3-5).
As an improvement of the technical scheme, the step (5) comprises the following steps:
(5.1) mixing the hydrophilic fiber with a solution containing a cross-linking agent, and standing for 30-60 min to obtain an intermediate;
and (5.2) carrying out heat treatment on the intermediate at 120-150 ℃ to obtain a finished product of the high-water-absorption fiber.
As an improvement of the technical scheme, in the step (5.1), the solution containing the cross-linking agent is obtained by dissolving the cross-linking agent in methanol, and the concentration of the cross-linking agent in the solution is 10-20%;
in the step (5.1), the dosage of the solution containing the cross-linking agent is 5-15% of the mass of the hydrophilic fiber.
As an improvement of the technical scheme, in the step (2), the natural fibers are soaked in alkali liquor for 12-30 hours, and then the alkali liquor is removed to obtain alkalized fibers;
wherein the alkali liquor is NaOH solution and/or KOH solution; the concentration of the alkali liquor is 25-50 wt%;
the dosage of the alkali liquor is 20-40 times of the weight of the natural fiber.
As an improvement of the technical scheme, in the step (2), the natural fibers are soaked in alkali liquor at the temperature of 20-40 ℃ and subjected to ultrasonic treatment for 12-30 hours.
As an improvement of the technical scheme, in the step (3), the solvent is isopropanol and/or n-butanol;
the dosage of the solvent is 10-15 times of the volume of the alkalized fiber.
As an improvement of the technical scheme, in the step (4), the branches are added into the swelling fibers and the solvent obtained in the step (3), and the solvent is removed after ultrasonic treatment is carried out for 2-5 hours at the temperature of 20-40 ℃ to obtain hydrophilic fibers;
wherein the branched compound is one or more of chloroacetic acid, chloropropionic acid and chlorobutyric acid;
the dosage of the branching substance is 1.5-5 times of the weight of the natural fiber.
Correspondingly, the invention also discloses a high water absorption fiber which is prepared by the preparation method.
The implementation of the invention has the following beneficial effects:
(1) the preparation method of the high water absorption fiber takes natural fiber as a raw material, and the natural fiber is subjected to alkalization treatment, swelling treatment and hydrophilic treatment, and then is crosslinked and cured. The fiber has high water absorption performance and water locking performance without changing the appearance of the raw material fiber. Specifically, the water absorption capacity of the high-water-absorption fiber is 50-120 times of the self weight.
(2) According to the preparation method of the high water-absorbing fiber, after hydrophilic treatment, the fiber is subjected to secondary crosslinking and fixation by using a methanol solution of ethylene glycol diglycidyl ether, aziridine, 1,4 butanediol and glycerol to form a three-dimensional crosslinking insoluble system, so that the problem of water solubility of the modified fiber is effectively solved, and the water-insoluble fiber is obtained. In addition, the water absorption performance of the high water absorption fiber is not influenced by curing modification through the crosslinking agents.
Drawings
FIG. 1 is a schematic flow chart of a process for preparing superabsorbent fibers according to the present invention;
FIG. 2 is a graph showing the morphology of natural fibers (cotton fibers) in example 4 of the present invention;
FIG. 3 is a topographical view of superabsorbent fibers in example 4 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings and detailed description.
Referring to fig. 1, the invention provides a method for preparing super absorbent fibers, which comprises the following steps:
s1: providing a natural fiber;
specifically, the natural fiber can be selected from one or more of cotton fiber, sugarcane fluff fiber, wood pulp fluff fiber, bamboo fluff fiber, pomelo peel fiber, and coconut coir fiber, but is not limited thereto.
S2: alkalizing natural fibers to obtain alkalized fibers;
specifically, the natural fibers are soaked in alkali liquor for a preset time, and after solid-liquid separation, the obtained solid is alkalized fibers, so that the obtained liquid is recycled. Through alkalization, hydrogen bonds in the fibers can be weakened, hemicellulose and lignin are dissolved, and modification and crosslinking treatment at the later stage are facilitated.
Specifically, the soaking time of the natural fibers in the alkali liquor is 12-30 hours, and examples are 12 hours, 14 hours, 16 hours, 18 hours, 20 hours, 22 hours, 24 hours, 25 hours or 28 hours, but not limited thereto.
In order to improve the alkalization reaction efficiency, the soaking process can be heated or the ultrasonic treatment can be carried out at normal temperature. Preferably, ultrasonic treatment is carried out at normal temperature (20-40 ℃) so as to enable alkali liquor to fully permeate natural fibers and enable alkalization treatment to be more sufficient. It should be noted that if the treatment temperature during the soaking process is greater than 40 ℃, the strength of the natural fiber is easily damaged, the appearance of the natural fiber is damaged, and the post-processing performance is affected.
Specifically, the alkali solution is a NaOH solution or a KOH solution, but is not limited thereto. The alkali concentration in the alkali solution is 25 to 50wt%, illustratively 25 wt%, 28 wt%, 30 wt%, 32 wt%, 40 wt%, or 45 wt%, but is not limited thereto.
The dosage of the alkali liquor is 20-40 times of the weight of the natural fiber, and is exemplarily 22 times, 23 times, 26 times, 32 times, 35 times or 38 times, but is not limited thereto.
S3: soaking the alkalized fiber in a solvent to swell the alkalized fiber to obtain swollen fiber;
wherein, the solvent can be selected from isopropanol and/or n-butanol, but is not limited to the above.
In order to improve the swelling efficiency, heating or ultrasonic treatment at normal temperature can be carried out in the soaking process. Preferably, the ultrasonic treatment is carried out for 2-5 h at normal temperature (20-40 ℃), and the volatilization of the solvent can be reduced by the normal-temperature treatment.
The amount of the solvent is 10 to 15 times of the volume of the alkalized fiber, and is exemplified by 10 times, 11 times, 12 times, 13 times or 14 times, but is not limited thereto.
S4: carrying out etherification reaction on the swelling fiber to obtain hydrophilic fiber;
specifically, the branches are added into the swelling fiber and the solvent obtained in the step S3, solid-liquid separation is performed after the grafting reaction, the obtained solid is the hydrophilic fiber, and the obtained liquid is determined by the carboxylate radical concentration according to an acid-base titration method and then recycled.
The branched compound may be one or more of chloroacetic acid, chloropropionic acid, and chlorobutyric acid, but is not limited thereto. The amount of the branching substance is 1.5 to 5 times of the weight of the natural fiber, and is illustratively 1.5 times, 2 times, 3 times, 4 times or 4.5 times, but not limited thereto.
The specific conditions of the grafting reaction are as follows: ultrasonic treatment is carried out for 2-5 h at normal temperature (20-40 ℃).
S5: and crosslinking and curing the hydrophilic fiber to form a water-insoluble high-water-absorption fiber finished product.
Specifically, a cross-linking agent is adopted to carry out cross-linking fixation on the hydrophilic fiber to form a three-dimensional cross-linking insoluble system, so that the water-solubility problem caused by a water-soluble modifier formed in the etherification reaction process is solved. Meanwhile, the water locking performance of the high water absorption fiber is also improved.
Wherein the crosslinking agent is one or more of epoxy compound, polyhydroxy alcohol, aziridine, and glycerol. Specifically, the epoxy compound is one or more of ethylene glycol diglycidyl ether, glycerol diglycidyl ether, and ethylene glycol diacrylate, but is not limited thereto; the polyhydric alcohol is selected from one or more of ethylene glycol, propylene glycol, butanediol, pentanediol, and pentaerythritol, but is not limited thereto.
Preferably, the cross-linking agent in the invention is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol, and the cross-linking agent can effectively improve the water absorption performance and the water shrinkage performance of the super absorbent fiber.
Specifically, the weight ratio of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol is (5-10): 1: (3-5): (3-5). Illustratively, the ratio of the four is 5:1:3:3,6:1:3:3,7:1:4:3,7:1:5:4, 9:1:4:4, but is not limited thereto.
Preferably, the cross-linking agent is provided in the form of a solution during the cross-linking curing process, i.e., the cross-linking agent is dissolved in a specific solvent to obtain a cross-linking curing solution, and then the cross-linking curing solution is mixed with the hydrophilic fibers for reaction. Specifically, the solution containing the cross-linking agent is obtained by dissolving the cross-linking agent in methanol, and the concentration of the cross-linking agent in the solution is 10 to 20 wt%, and is exemplarily 11 wt%, 12 wt%, 15 wt% or 18 wt%, but is not limited thereto.
The amount of the solution containing the crosslinking agent is 5 to 15 wt%, illustratively 5 wt%, 8 wt%, 10 wt%, 13 wt% based on the mass of the hydrophilic fiber, but is not limited thereto.
Specifically, in an embodiment of the present invention, S5 may include the following steps:
s51: mixing the hydrophilic fiber with a solution containing a cross-linking agent, and standing for 30-60 min to obtain an intermediate;
specifically, the solution containing the crosslinking agent can be sufficiently permeated by standing. The standing time is 30-60 min, and exemplary time is 32min, 40min, 45min, 52min or 57min, but is not limited thereto.
S52: and carrying out heat treatment on the intermediate at 120-150 ℃ to obtain a high-water-absorption fiber finished product.
Specifically, the temperature of the heat treatment is 120 to 150 ℃, and exemplary temperatures are 125 ℃, 130 ℃, 135 ℃, 140 ℃ or 145 ℃, but not limited thereto. The heat treatment time is 30 to 90min, and exemplary is 35min, 45min, 50min, 70min or 85min, but is not limited thereto.
Correspondingly, the invention also discloses a high water-absorption fiber which is prepared by adopting the method. The high water absorption fiber of the invention has strong water absorption capacity and strong water locking capacity after water absorption.
The present invention will be described below with reference to specific examples.
Example 1
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking sugarcane lint fiber;
(2) 500g of sugarcane villus fiber is soaked in 20kg of KOH solution (22 wt%) at 40 ℃ for 50h, and alkalized fiber is obtained after solid-liquid separation;
(3) soaking the alkalized fiber in isopropanol for 3h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: the volume of isopropanol is 1: 20;
(4) adding 2.5kg of chlorobutyric acid into the system obtained in the step (3), performing ultrasonic treatment for 5 hours at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 13g of ethylene glycol diglycidyl ether and 2g of aziridine, mixing the obtained mixed solution with hydrophilic fiber, and then carrying out heat treatment at 120 ℃ for 120min to obtain a high-water-absorption fiber finished product.
Example 2
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking cotton fibers;
(2) carrying out ultrasonic treatment on 500g of cotton fibers in 15kg of NaOH solution (32 wt%) at 25 ℃ for 22h, and carrying out solid-liquid separation to obtain alkalized fibers;
(3) soaking the alkalized fiber in isopropanol for 2h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: the volume of isopropanol is 1: 12;
(4) adding 1.5kg of chloroacetic acid into the system obtained in the step (3), performing ultrasonic treatment for 3h at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 0.6g aziridine, 2.2g propylene glycol and 2.2g glycerol to obtain a mixed solution, mixing the mixed solution with hydrophilic fiber, standing at room temperature (25 ℃) for 40min, and finally treating at 140 ℃ for 60min to obtain a finished product of the super absorbent fiber.
Example 3
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking cotton fibers;
(2) carrying out ultrasonic treatment on 500g of cotton fibers in 12kg of NaOH solution (45 wt%) at 25 ℃ for 15h, and carrying out solid-liquid separation to obtain alkalized fibers;
(3) soaking the alkalized fiber in isopropanol for 2.5h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: the volume of isopropanol is 1: 13;
(4) adding 2kg of chloropropionic acid into the system obtained in the step (3), performing ultrasonic treatment for 4h at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 50g of solution containing the cross-linking agent with the hydrophilic fiber, standing at room temperature (25 ℃) for 40min, and finally treating at 140 ℃ for 60min to obtain the finished product of the super absorbent fiber.
Wherein the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol, and the weight ratio of the ethylene glycol diglycidyl ether to the aziridine to the 1, 4-butanediol to the glycerol is 4: 1: 6: 5. the above cross-linking agent was dissolved in methanol to obtain a solution (10 wt%).
Example 4
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking cotton fibers;
(2) carrying out ultrasonic treatment on 500g of cotton fibers in 15kg of NaOH solution (35 wt%) at 25 ℃ for 14h, and carrying out solid-liquid separation to obtain alkalized fibers;
(3) soaking the alkalized fiber in isopropanol for 2h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: volume of isopropanol is 1: 14;
(4) adding 1.7kg of chloropropionic acid into the system obtained in the step (3), performing ultrasonic treatment for 3 hours at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 40g of solution containing the cross-linking agent with the hydrophilic fiber, standing at room temperature (25 ℃) for 40min, and finally treating at 130 ℃ for 80min to obtain the finished product of the high-water-absorption fiber.
Wherein the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol, and the weight ratio of the ethylene glycol diglycidyl ether to the aziridine to the 1, 4-butanediol to the glycerol is 7:1:4: 4. the above crosslinking agent was dissolved in methanol to obtain a solution (12.5 wt%).
Example 5
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking cotton fibers;
(2) carrying out ultrasonic treatment on 500g of cotton fibers in 15kg of NaOH solution (35 wt%) at 25 ℃ for 14h, and carrying out solid-liquid separation to obtain alkalized fibers;
(3) soaking the alkalized fiber in isopropanol for 2h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: volume of isopropanol is 1: 14;
(4) adding 1.7kg of chloropropionic acid into the system obtained in the step (3), performing ultrasonic treatment for 3 hours at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 50g of solution containing the cross-linking agent with the hydrophilic fiber, standing at room temperature (25 ℃) for 40min, and finally treating at 130 ℃ for 80min to obtain the finished product of the high-water-absorption fiber.
Wherein the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol, and the weight ratio of the ethylene glycol diglycidyl ether to the aziridine to the 1, 4-butanediol to the glycerol is 8:1:3.5: 3.5. The above cross-linking agent was dissolved in methanol to obtain a solution (10 wt%).
Example 6
This example provides a superabsorbent fiber, which is prepared by the following steps:
(1) taking cotton fibers;
(2) carrying out ultrasonic treatment on 500g of cotton fibers in 15kg of NaOH solution (35 wt%) at 25 ℃ for 14h, and carrying out solid-liquid separation to obtain alkalized fibers;
(3) soaking the alkalized fiber in isopropanol for 2h to fully swell the alkalized fiber to obtain swollen fiber; wherein, the volume of the alkalized fibers: volume of isopropanol is 1: 14;
(4) adding 1.7kg of chloropropionic acid into the system obtained in the step (3), performing ultrasonic treatment for 3 hours at room temperature (25 ℃), and performing solid-liquid separation to obtain a solid, namely the hydrophilic fiber;
(5) mixing 40g of solution containing the cross-linking agent with the hydrophilic fiber, standing at room temperature (25 ℃) for 40min, and finally treating at 130 ℃ for 80min to obtain the finished product of the high-water-absorption fiber.
Wherein the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol, and the weight ratio of the ethylene glycol diglycidyl ether to the aziridine to the 1, 4-butanediol to the glycerol is 6:1:4: 5. The above crosslinking agent was dissolved in methanol to obtain a solution (12.5 wt%).
The results of the tests on the superabsorbent fibers obtained in examples 1 to 6 are shown in the following table.
The method for testing the water absorption multiplying power comprises the following steps: taking a 1.0g sample in a beaker, adding a certain amount of deionized water to soak for 1h, and pouring the sample after water absorption into the beaker1Is kept standing for 1h and weighed as m2The water absorption capacity Q of the sample1＝[(m2-m1)-1]/1。
The method for testing the saline absorption rate in 1min comprises the following steps: weighing 1.0g of sample in a beaker, adding a certain amount of 0.9% physiological saline for soaking for 1min, and then pouring the sample into a beaker with the mass of m3Standing the mixture in a screen mesh for 30min, weighing the mixture, and recording the weight as m4And the saline absorption rate Q of the sample is 1min1＝[(m4-m3)-1]/1。
The reverse osmosis amount measuring method comprises the following steps: placing high water absorption fiber after absorbing water (saline water) for 1h at 25 deg.C and 70% (relative humidity), placing a piece of filter paper on the surface, and recording mass m1Pressing with 250g weight for 6h, and weighing the weight m of the filter paper after 6h2The reverse osmosis amount is m2-m1。
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A method for preparing high water absorption fiber is characterized by comprising the following steps:
(1) providing a natural fiber;
(2) alkalizing the natural fibers to obtain alkalized fibers;
(3) soaking the alkalized fiber in a solvent to swell the alkalized fiber to obtain swollen fiber;
(4) carrying out grafting reaction on the swelling fiber to obtain hydrophilic fiber;
(5) crosslinking and curing the hydrophilic fiber by using a crosslinking agent to form a finished product of the water-insoluble high-water-absorption fiber;
wherein, the cross-linking agent is selected from one or more of epoxy compound, polyhydroxy alcohol, aziridine and glycerol.
2. The method for preparing superabsorbent fiber of claim 1 wherein the epoxy compound is one or more of ethylene glycol diglycidyl ether, glycerol diglycidyl ether, and ethylene glycol diacrylate;
the polyhydric alcohol is one or more selected from ethylene glycol, propylene glycol, butanediol, pentanediol and pentaerythritol;
the natural fiber is selected from one or more of cotton fiber, sugarcane fluff fiber, wood pulp fluff fiber, bamboo fluff fiber, pomelo peel fiber and coconut coir fiber.
3. The method of claim 2, wherein the cross-linking agent is a mixture of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol, and glycerol;
the weight ratio of ethylene glycol diglycidyl ether, aziridine, 1, 4-butanediol and glycerol is (5-10): 1: (3-5): (3-5).
4. The method of preparing superabsorbent fiber of claim 1, wherein step (5) comprises:
(5.1) mixing the hydrophilic fiber with a solution containing a cross-linking agent, and standing for 30-60 min to obtain an intermediate;
and (5.2) carrying out heat treatment on the intermediate at 120-150 ℃ to obtain a finished product of the high-water-absorption fiber.
5. The method for preparing superabsorbent fiber according to claim 4, wherein in step (5.1), the solution containing the crosslinking agent is obtained by dissolving the crosslinking agent in methanol, and the concentration of the crosslinking agent in the solution is 10-20%;
in the step (5.1), the dosage of the solution containing the cross-linking agent is 5-15% of the mass of the hydrophilic fiber.
6. The preparation method of the superabsorbent fiber according to claim 1, wherein in the step (2), the natural fiber is soaked in alkali liquor for 12-30 h, and then the alkali liquor is removed to obtain the alkalized fiber;
wherein the alkali liquor is NaOH solution and/or KOH solution; the concentration of the alkali liquor is 25-50 wt%;
the dosage of the alkali liquor is 20-40 times of the weight of the natural fiber.
7. The method for preparing the super absorbent fiber according to claim 6, wherein in the step (2), the natural fiber is soaked in an alkali solution at 20-40 ℃ and is subjected to ultrasonic treatment for 12-30 h.
8. The method for preparing superabsorbent fiber according to claim 1, wherein in step (3), the solvent is selected from isopropanol and/or n-butanol;
the dosage of the solvent is 10-15 times of the volume of the alkalized fiber.
9. The preparation method of the superabsorbent fiber according to claim 1, wherein in the step (4), the branch compound is added into the swollen fiber and the solvent obtained in the step (3), and the solvent is removed after ultrasonic treatment is carried out for 2-5 h at 20-40 ℃ to obtain the hydrophilic fiber;
wherein the branched compound is one or more of chloroacetic acid, chloropropionic acid and chlorobutyric acid;
the dosage of the branching substance is 1.5-5 times of the weight of the natural fiber.
10. A superabsorbent fiber produced by the production method according to any one of claims 1 to 9.
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| CN202110893034.8A CN113818232B (en) | 2021-08-04 | Super absorbent fiber and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4250306A (en) * | 1978-05-31 | 1981-02-10 | Hoechst Aktiengesellschaft | Process and equipment for preparing swellable cross-linked carboxyalkylcelluloses from natural cellulose or cellulose hydrate and use thereof |
| JPH05123573A (en) * | 1991-10-31 | 1993-05-21 | Oji Paper Co Ltd | Preparation of highly water absorptive cellulose material |
| US5731083A (en) * | 1991-12-09 | 1998-03-24 | Courtaulds Plc | Cellulosic fibres |
| EP1920787A2 (en) * | 2006-10-02 | 2008-05-14 | Weyerhaeuser Company | Crosslinked carboxyalkyl cellulose fibers having permanent and non-permanent crosslinks and methods for its preparation |
| CN111945416A (en) * | 2020-08-31 | 2020-11-17 | 天津工业大学 | Method for surface crosslinking of super absorbent fibers |
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4250306A (en) * | 1978-05-31 | 1981-02-10 | Hoechst Aktiengesellschaft | Process and equipment for preparing swellable cross-linked carboxyalkylcelluloses from natural cellulose or cellulose hydrate and use thereof |
| JPH05123573A (en) * | 1991-10-31 | 1993-05-21 | Oji Paper Co Ltd | Preparation of highly water absorptive cellulose material |
| US5731083A (en) * | 1991-12-09 | 1998-03-24 | Courtaulds Plc | Cellulosic fibres |
| EP1920787A2 (en) * | 2006-10-02 | 2008-05-14 | Weyerhaeuser Company | Crosslinked carboxyalkyl cellulose fibers having permanent and non-permanent crosslinks and methods for its preparation |
| CN111945416A (en) * | 2020-08-31 | 2020-11-17 | 天津工业大学 | Method for surface crosslinking of super absorbent fibers |
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