CN114249924A - Acid and alkali resistant KHA modified wood pulp cotton material and preparation method and application thereof - Google Patents
Acid and alkali resistant KHA modified wood pulp cotton material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses acid and alkali resistant KHA modified wood pulp cotton, which comprises the following steps: (1) respectively taking Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC), carboxymethyl cellulose (CMC) and the like as main raw materials, respectively placing the main raw materials in sodium hydroxide solution, stirring and swelling, and dissolving for 18h at the temperature of minus 5 ℃. (2) Respectively adding chitosan solution dissolved by 2-5% glacial acetic acid, and stirring in a stirrer at the rotating speed of 260-300 r/min for 30 min. (3) And respectively adding 10mL of KHA solution (w is 10%), 0.2-0.5 g of polyethylene glycol 6000(PEG6000: pore-forming agent), 0.2-0.4 g of glycerol and 1-1.5 g of silane cross-linking agent into the system, continuously stirring for 30min (4), and respectively washing, centrifugally purifying and freeze-drying the product for 24h to obtain KHA/MC, KHA/HPMC and KHA/CMC sponge matrix materials.
Description
Technical Field
The invention belongs to the technical field of novel environment-friendly cellulose sponge, and particularly relates to a high-water-absorption wood pulp cotton material capable of enhancing the mechanical strength of cellulose and resisting acid and alkali.
Background
The novel environment-friendly sponge in the market at present has more demands, such as starch medical sponge, polyurethane and cellulose composite sponge, chitosan composite sponge, PVA and composite sponge thereof and the like. Cellulose contains a large amount of hydroxyl in molecules, hydrogen bonds are easily formed with water, and the sponge material with good water-based property and excellent degradability can be prepared by taking the cellulose as a raw material. At present, cellulose sponge matrix has the characteristics of low cost, fluffiness, degradability, heat resistance, excellent water absorption and the like. Since cellulose has a melting point higher than its decomposition temperature and cannot be melt-processed, the dissolution regeneration method is an important way to prepare cellulose sponge. Cellulose sponges prepared by the dissolution regeneration method have poor mechanical strength, and reinforcing fibers are usually added to increase the mechanical strength.
Humic acid is an organic macromolecule, contains a plurality of active groups, and has a plurality of characteristics such as complexation, cation exchange and surface activity; the humic acid is used for modifying the cellulose, so that the mechanical property and the acid and alkali resistance of the cellulose can be improved, and the application of the humic acid to the wood cotton is of great significance.
Disclosure of Invention
Aiming at the problems in the prior art, the applicant of the invention provides an acid and alkali resistant KHA modified kapok cotton material, and a preparation method and application thereof. The material can resist the environment with pH value of 5-6, and the water absorption rate is more than 250 g/g.
The technical scheme of the invention is as follows:
the preparation method of the modified wood pulp cotton material with the acid and alkali resistance of KHA comprises the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving in a low-temperature environment to obtain a transparent cellulose solution;
(2) adding a chitosan solution dissolved by glacial acetic acid into the transparent solution obtained in the step (1), and stirring in a rotary stirrer to uniformly mix the system;
(3) adding KHA solution, polyethylene glycol, glycerol and a silane coupling agent into the solution obtained in the step (2), and continuing stirring to start reaction;
(4) and (4) washing, centrifugally purifying and freeze-drying the product obtained in the step (3) to obtain 3 kinds of light porous wood cotton substrates.
In the step (1), the alkaline solution is 2-3% sodium hydroxide solution; the low-temperature environment is-5 ℃;
in the step (2), the mass fraction of the glacial acetic acid is 2-5%; the mass ratio of the glacial acetic acid to the chitosan is 1: 25; the amount of the mixed solution is 2-3 ml;
in the step (3), the mass fraction of the solution KHA is 10%; the molecular weight of polyethylene glycol is 6000; the mass of the glycerol is 0.2-0.4 g; the silane coupling agent has a mass of 1 to 1.5 g.
In the step (4), the washing is carried out by using deionized water until the pH value of the solution is neutral; washing with water, and centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero.
The application of the modified wood pulp cotton material is used for water absorption sponges, particularly for water absorption in acid-base environments.
The beneficial technical effects of the invention are as follows:
the humic acid is mainly prepared from low-rank coal, has low production cost, and has the effects of improving soil, enhancing fertilizer efficiency, saving water, resisting drought, promoting crop growth and the like in agriculture. The functional groups such as carboxyl, hydroxyl and the like distributed in the structure have the effects of stimulating the growth and development of plants, complexing metal ions, increasing the stress resistance of crops and improving the nutritional status of the plants.
In addition, cellulose molecules contain a large amount of hydroxyl groups, so that hydrogen bonds can be easily formed with water, and the sponge material with good water-based property and excellent degradability can be prepared by taking the cellulose as a raw material. Therefore, the mechanical property, acid and alkali resistance and water absorption rate of the modified cellulose can be improved by selecting humic acid,
drawings
FIG. 1 is an infrared spectrum of a modified wood pulp cotton material prepared in example 1 of the present invention.
FIG. 2 is an SEM image of a modified wood pulp cotton material prepared in example 2 of the present invention.
FIG. 3 is a diagram showing the acid and alkali resistance and the water absorption effect of the modified wood pulp cotton material prepared in the embodiments 1 to 4 of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings and examples.
Example 1
The preparation method of the acid and alkali resistant KHA modified wood pulp cotton material comprises the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving for 18h at-5 ℃ to obtain a transparent cellulose solution with the mass fraction of 10%;
(2) adding 2ml of glacial acetic acid into the cellulose solution, wherein the mass fraction of the glacial acetic acid is 2%, and the mass ratio of the glacial acetic acid to the chitosan is 1: 25 of a mixed solution; the stirring speed is 260r/min, and the stirring time is 30 min.
(3) Respectively adding 10mL of KHA solution (w is 10%), 0.2g of polyethylene glycol 6000(PEG6000: pore-forming agent), 0.2g of glycerol and 1g of silane cross-linking agent into the system, and continuously stirring for 30min to start reaction;
(4) washing with deionized water to neutrality, centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero. Respectively obtaining the acid and alkali resistant KHA modified wood pulp cotton material
The infrared spectroscopic analysis of the material synthesized in this example is performed, and the result is shown in fig. 1, and it can be seen from the figure that, since humic acid is a macromolecule containing a large number of benzene ring skeletons, the peak position is moved to a low wave number by a conjugation effect generated after the action, which finally shows that strong interaction occurs between molecules of the composite material.
Example 2
The preparation method of the acid and alkali resistant KHA modified wood pulp cotton material comprises the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving for 18h at-5 ℃ to obtain a transparent cellulose solution with the mass fraction of 10%;
(2) adding 3ml of glacial acetic acid into the cellulose solution, wherein the mass fraction of the glacial acetic acid is 2%, and the mass ratio of the glacial acetic acid to the chitosan is 1: 25 of a mixed solution; the stirring speed is 260r/min, and the stirring time is 30 min.
(3) Respectively adding 10mL of KHA solution (w is 10%), 0.2g of polyethylene glycol 6000(PEG6000: pore-forming agent), 0.2g of glycerol and 1g of silane cross-linking agent into the system, and continuously stirring for 30min to start reaction;
(4) washing with deionized water to neutrality, centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero. Respectively obtaining the acid and alkali resistant KHA modified wood pulp cotton material
The shape analysis of the modified wood wool prepared in this example is shown in fig. 2, and it can be seen from the figure that 3 kinds of wood wool form interpenetrating crosslinked networks, all of which have rugged rough surfaces, and the dense and dense mesh structure effectively increases the specific surface area of the sponge matrix, and enables water molecules to rapidly diffuse into the internal network of the sponge matrix, thereby giving the sponge matrix good water absorption and retention properties.
Example 3
The preparation method of the acid and alkali resistant KHA modified wood pulp cotton material comprises the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving for 18h at-5 ℃ to obtain a transparent cellulose solution with the mass fraction of 10%;
(2) adding 2ml of glacial acetic acid into the cellulose solution, wherein the mass fraction of the glacial acetic acid is 4%, and the mass ratio of the glacial acetic acid to the chitosan is 1: 25 of a mixed solution; the stirring speed is 300r/min, and the stirring time is 30 min.
(3) Respectively adding 10mL of KHA solution (w is 10%), 0.2g of polyethylene glycol 6000(PEG6000: pore-forming agent), 0.2g of glycerol and 1g of silane cross-linking agent into the system, and continuously stirring for 30min to start reaction;
(4) washing with deionized water to neutrality, centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero. Respectively obtaining the acid and alkali resistant KHA modified wood pulp cotton material.
Example 4
The preparation method of the acid and alkali resistant KHA modified wood pulp cotton material comprises the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving for 18h at-5 ℃ to obtain a transparent cellulose solution with the mass fraction of 10%;
(2) adding 2ml of glacial acetic acid into the cellulose solution, wherein the mass fraction of the glacial acetic acid is 2%, and the mass ratio of the glacial acetic acid to the chitosan is 1: 25 of a mixed solution; the stirring speed is 300r/min, and the stirring time is 30 min.
(3) Respectively adding 10mL of KHA solution (w is 10%), 0.4g of polyethylene glycol 6000(PEG6000: pore-forming agent), 0.2g of glycerol and 1g of silane cross-linking agent into the system, and continuously stirring for 30min to start reaction;
(4) washing with deionized water to neutrality, centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero. Respectively obtaining the acid and alkali resistant KHA modified wood pulp cotton material.
Test example
(1) Water absorption Performance test
Weighing a proper amount of prepared material as m0, soaking for 0, 30, 60, 90, 120 and 150min respectively, filtering out residual moisture by using a screen, weighing wet weight as m1, and calculating the water absorption (g/g) of the test material under different time conditions according to the following formula:
and (3) testing the water absorption capacity (g/g) of (m 1-m 0)/m0(1) weighing a sponge material with water absorption capacity reaching a saturated state, marking the sponge material as m1, placing the sponge material in an oven at the temperature of 40 ℃, weighing the sponge material at intervals of 3h, marking the sponge material as mi, and calculating according to the following formula:
the modified ligno-cotton of examples 1 to 4 was used for the water absorption test, respectively, in which the water retention (%) (m 1-m 0)/(mi-m 0) × 100% (2).
(2) Acid and alkali resistance test
And (3) acid and alkali resistance test, namely preparing 6 groups of solutions with different pH values, testing the water absorption multiplying power after 3 hours, and calculating according to the formula (1).
The acid and alkali resistance test was performed on the modified ligno-cotton of examples 1 to 4.
Claims (7)
1. The preparation method of the KHA modified wood pulp cotton material is characterized by comprising the following steps:
(1) respectively putting Methyl Cellulose (MC), hydroxypropyl methyl cellulose (HPMC) and carboxymethyl cellulose (CMC) into an alkaline solution, stirring, and dissolving in a low-temperature environment to obtain a transparent cellulose solution;
(2) adding a chitosan solution dissolved by glacial acetic acid into the transparent solution obtained in the step (1), and stirring in a rotary stirrer to uniformly mix the system;
(3) adding KHA solution, polyethylene glycol, glycerol and a silane coupling agent into the solution obtained in the step (2), and continuing stirring to start reaction;
(4) and (4) washing, centrifugally purifying and freeze-drying the product obtained in the step (3) to obtain 3 kinds of light porous wood cotton substrates.
2. The modified wood pulp cotton material of claim 1 wherein: in the step (1), the alkaline solution is 2-3% sodium hydroxide solution; the low temperature environment is-5 ℃.
3. The modified wood pulp cotton material of claim 1 wherein: in the step (2), the mass fraction of the glacial acetic acid is 2-5%; the mass ratio of the glacial acetic acid to the chitosan is 1: 25; the amount of the mixed solution is 2-3 ml; the stirring speed is 260-300 r/min, and the stirring time is 30 min.
4. The modified wood pulp cotton material of claim 1 wherein: in the step (3), the mass fraction of the solution KHA is 10%; the molecular weight of polyethylene glycol is 6000; the mass of the glycerol is 0.2-0.4 g; the silane coupling agent has a mass of 1 to 1.5 g.
5. The modified wood pulp cotton material of claim 1 wherein: in the step (4), the product is a crosslinked hydrogel; washing with water, and centrifuging at 6000r/min for 8 min; and respectively pouring the centrifuged products into polystyrene surface dishes, freezing for 12 hours at the temperature of between 18 ℃ below zero and 20 ℃ below zero, and carrying out vacuum freeze drying for 24 hours at the temperature of between 40 ℃ below zero.
6. Use of a modified wood pulp cotton material according to any one of claims 1 to 5 in which: is used for water-absorbing sponge.
7. Use according to claim 6, characterized in that: acid and alkali resistance and high water absorption.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105344330A (en) * | 2015-12-07 | 2016-02-24 | 华东理工大学 | Preparation method and application of chitosan-inorganic metal ionic composite microsphere adsorbent |
| CN109806847A (en) * | 2019-03-27 | 2019-05-28 | 陕西科技大学 | A kind of humic acid type porous adsorbing material and its preparation method and application |
| CN112029135A (en) * | 2020-09-07 | 2020-12-04 | 江苏恒富新材料科技有限公司 | Preparation method of wood fiber sponge |
| CN112275260A (en) * | 2020-07-13 | 2021-01-29 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with polyethylene glycol as pore-foaming agent and preparation method thereof |
-
2021
- 2021-12-27 CN CN202111614528.4A patent/CN114249924A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105344330A (en) * | 2015-12-07 | 2016-02-24 | 华东理工大学 | Preparation method and application of chitosan-inorganic metal ionic composite microsphere adsorbent |
| CN109806847A (en) * | 2019-03-27 | 2019-05-28 | 陕西科技大学 | A kind of humic acid type porous adsorbing material and its preparation method and application |
| CN112275260A (en) * | 2020-07-13 | 2021-01-29 | 广西科技大学 | Chitosan/fibroin-based dual-structure porous adsorption filter material with polyethylene glycol as pore-foaming agent and preparation method thereof |
| CN112029135A (en) * | 2020-09-07 | 2020-12-04 | 江苏恒富新材料科技有限公司 | Preparation method of wood fiber sponge |
Non-Patent Citations (2)
| Title |
|---|
| 宋洁 等: ""KHA改性不同纤维素型多孔吸水海绵基质的制备及性能研究"", 《应用化工》 * |
| 李鑫等: "HA-PAA-CMC高吸水性树脂的制备及性能", 《工程塑料应用》 * |
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Application publication date: 20220329 |