CN112574467B - Castor oil/cellulose composite aerogel and preparation method and application thereof - Google Patents
Castor oil/cellulose composite aerogel and preparation method and application thereof Download PDFInfo
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Abstract
A castor oil/cellulose composite aerogel and a preparation method and application thereof are disclosed, wherein cellulose nano-fiber aqueous dispersion is prepared, the pH value is adjusted to 8-9, subsequently tannic acid and silanized castor oil are added, and the castor oil/cellulose composite aerogel is prepared after freeze drying. The aerogel raw materials prepared by the method are all derived from biomass, have the characteristics of high hydrophobicity and super lipophilicity, can be used in the field of oil-water separation, and cannot cause pollution to the environment.
Description
Technical Field
The invention belongs to the field of high-value utilization of biomass, particularly relates to a biomass composite aerogel, and particularly relates to a castor oil/cellulose composite aerogel and a preparation method and application thereof.
Background
Oil pollution brings great harm to the water environment, so that the human health and the ecological environment are influenced, and research and development of technologies and materials capable of effectively removing the oil pollutants are urgently needed. The currently common oil removal methods include combustion, microbial degradation, adsorption and the like, wherein the adsorption method draws wide attention of researchers due to the characteristics of low cost, high efficiency, easiness in recovery and treatment and the like. The traditional oil absorption material has the defects of low oil absorption capacity, partial material non-biodegradability, easy secondary pollution to the environment and the like, so that the development of the high-efficiency oil absorption material with light weight, large oil absorption capacity and biodegradability becomes a research hotspot in recent years. The cellulose aerogel is green, environment-friendly and low-cost, and has the characteristics of high specific surface area and high porosity of aerogel materials and the advantages of rich sources, reproducibility and biodegradability of cellulose. Due to abundant hydroxyl groups in cellulose molecules, the cellulose has hydrophilicity, is easy to absorb moisture in air to cause pore structure collapse, and limits the application of the cellulose in the field of oil-water separation. Hydrophobic modification becomes an effective method for preparing the high-efficiency cellulose aerogel oil absorption material. However, most of the currently used modifiers are synthetic materials, and do not meet the requirements of green chemistry and sustainable development, so that the development of the full-biomass aerogel oil absorption material becomes a research focus.
Disclosure of Invention
The technical problem to be solved is as follows: aiming at the problems of the existing cellulose aerogel materials, the invention provides a castor oil/cellulose composite aerogel taking tannic acid as a mediating layer and castor oil as a hydrophobic modifier, and a preparation method and application thereof.
The technical scheme is as follows: a preparation method of castor oil/cellulose composite aerogel comprises the following steps of (1) mixing the following components in a molar ratio of (2.8-3.8): 1 mixing isocyanatopropyltriethoxysilane and castor oil, heating to 80 ℃, and reacting for 20-60 mim in a nitrogen atmosphere to obtain the silanized castor oil. (2) Dispersing cellulose nanofibers in ultrapure water, adding NaOH to adjust the pH value to 8-9, and uniformly stirring to obtain a cellulose nanofiber aqueous dispersion with the mass concentration of 0.1-1.5 wt%; (3) adding tannic acid into the cellulose nanofiber water dispersion, stirring for 30min, wherein the dosage of the tannic acid is 4-6 wt% of the dry weight of the cellulose nanofiber, then adding a silanized castor oil ethanol solution, the dosage ratio of the silanized castor oil to the cellulose nanofiber is (0.2-2.2): 1, and continuously stirring for 6-12 h to obtain a mixed solution; (4) and pouring the mixed solution into a mold, and freeze-drying to obtain the castor oil/cellulose composite aerogel.
The molar ratio of the isocyanatopropyltriethoxysilane to the castor oil is 3.3: 1.
the reaction time for the preparation of the silanized castor oil is 30 min.
The mass concentration of the cellulose nano-fiber aqueous dispersion is 0.5-1.0 wt%.
The amount of the tannic acid is 5 wt% of the dry weight of the cellulose nano-fiber.
The ratio of the amount of the silanized castor oil to the amount of the cellulose nanofibers is 0.4-1.8: 1.
The castor oil/cellulose composite aerogel prepared by the method.
The castor oil/cellulose composite aerogel is applied to preparation of oil-water separation products.
Has the advantages that: the preparation method of the castor oil/cellulose composite aerogel is provided, and the aerogel prepared by the method has high hydrophobic property and high oil-water selectivity and can be used for oil-water separation; the cellulose nanofiber used in the method is derived from natural material cellulose, is rich in reserves, renewable and biodegradable, and uses biomass castor oil and tannic acid as modifiers, so that secondary pollution to the environment is avoided, the method is a preparation method of the aerogel oil absorption material, is green, environment-friendly and low in cost, and is beneficial to large-area use in actual life.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
The preparation method of the silanized castor oil comprises the following steps: adding 33mmol of isocyanate propyl triethoxy siloxane and 10mmol of castor oil into a reaction vessel, uniformly mixing, introducing nitrogen, heating to 80 ℃, and continuously stirring for reaction for 30min to obtain the silanized castor oil.
Example 1
A preparation method of castor oil/cellulose composite aerogel comprises the following steps of dispersing 1g of cellulose nanofiber in 100mL of ultrapure water, adding NaOH to adjust the pH of the solution to 8.5, and magnetically stirring for 3h to form uniform cellulose nanofiber aqueous dispersion; (2) adding 50mg of tannic acid into cellulose nanofiber aqueous dispersion, stirring for 30min, dissolving 0.4g of silanized castor oil in 5mL of absolute ethanol to form an ethanol solution, adding the ethanol solution into the cellulose nanofiber aqueous dispersion, and continuously stirring for 6h to obtain a mixed solution; pouring the mixed solution into a mold, and freeze-drying for 72 hours at-72 ℃ under the condition of 1pa to obtain the castor oil/cellulose composite aerogel. The aerogel has super oleophylic performance, the oil contact angle is 0 degree, and the water contact angle is 56 degrees.
Example 2
A preparation method of castor oil/cellulose composite aerogel comprises the following steps of dispersing 1g of cellulose nanofiber in 200mL of ultrapure water, adding NaOH to adjust the pH of the solution to 8.5, and magnetically stirring for 3h to form uniform cellulose nanofiber aqueous dispersion; (2) adding 50mg of tannic acid into cellulose nanofiber aqueous dispersion, stirring for 30min, dissolving 0.8g of silanized castor oil in 5mL of absolute ethanol to form an ethanol solution, adding the ethanol solution into the cellulose nanofiber aqueous dispersion, and continuously stirring for 6h to obtain a mixed solution; pouring the mixed solution into a mold, and freeze-drying for 72 hours at-72 ℃ under the condition of 1pa to obtain the castor oil/cellulose composite aerogel. The aerogel has super oleophylic performance, the oil contact angle is 0 degree, and the water contact angle is 107 degrees.
Example 3
A preparation method of castor oil/cellulose composite aerogel comprises the following steps of dispersing 1g of cellulose nanofiber in 200mL of ultrapure water, adding NaOH to adjust the pH of the solution to 8.5, and magnetically stirring for 3h to form uniform cellulose nanofiber aqueous dispersion; (2) adding 50mg of tannic acid into cellulose nanofiber aqueous dispersion, stirring for 30min, dissolving 1.2g of silanized castor oil in 5mL of absolute ethanol to form an ethanol solution, adding the ethanol solution into the cellulose nanofiber aqueous dispersion, and continuously stirring for 6h to obtain a mixed solution; pouring the mixed solution into a mold, and freeze-drying for 72 hours at-72 ℃ under the condition of 1pa to obtain the castor oil/cellulose composite aerogel. The aerogel has super oleophylic performance, the oil contact angle is 0 degree, and the water contact angle is 125 degrees.
Example 4
A preparation method of castor oil/cellulose composite aerogel comprises the following steps of dispersing 1g of cellulose nanofiber in 200mL of ultrapure water, adding NaOH to adjust the pH of the solution to 8.5, and magnetically stirring for 3h to form uniform cellulose nanofiber aqueous dispersion; (2) adding 50mg of tannic acid into cellulose nanofiber aqueous dispersion, stirring for 30min, dissolving 1.8g of silanized castor oil in 5mL of absolute ethanol to form an ethanol solution, adding the ethanol solution into the cellulose nanofiber aqueous dispersion, and continuously stirring for 6h to obtain a mixed solution; pouring the mixed solution into a mold, and freeze-drying for 72 hours at-72 ℃ under the condition of 1pa to obtain the castor oil/cellulose composite aerogel. The aerogel has super oleophylic performance, the oil contact angle is 0 degree, and the water contact angle is 142 degrees.
Comparing examples 1-4, it is found that the composite aerogel prepared in example 4 has the highest water contact angle and the best oil-water selectivity, and the oil absorption performance is tested. Specifically, diesel oil, silicone oil, cyclohexane, toluene and dichloromethane are taken and placed in a beaker, the prepared composite aerogel is placed in oil and an organic solvent, the composite aerogel is fully adsorbed until the composite aerogel is saturated, the composite aerogel is taken out and weighed, and the adsorption capacity is calculated. The composite aerogel is found to be capable of rapidly adsorbing oils and organic solvents, and the maximum adsorption capacity of the composite aerogel on methylene dichloride reaches 98 g/g.
Claims (7)
1. The preparation method of the castor oil/cellulose composite aerogel is characterized by comprising the following steps of (1) mixing the following raw materials in a molar ratio of (2.8-3.8): 1 mixing isocyanatopropyltriethoxysilane and castor oil, heating to 80 ℃, and reacting for 20-60 mim in a nitrogen atmosphere to obtain silanized castor oil; (2) dispersing cellulose nanofibers in ultrapure water, adding NaOH to adjust the pH value to 8-9, and uniformly stirring to obtain a cellulose nanofiber aqueous dispersion with the mass concentration of 0.1-1.5 wt%;
(3) adding tannic acid into the cellulose nanofiber water dispersion, stirring for 30min, wherein the dosage of the tannic acid is 4-6 wt% of the dry weight of the cellulose nanofiber, then adding a silanized castor oil ethanol solution, the dosage ratio of the silanized castor oil to the cellulose nanofiber is 0.8-1.8: 1, and continuously stirring for 6-12 h to obtain a mixed solution; (4) and pouring the mixed solution into a mold, and freeze-drying to obtain the castor oil/cellulose composite aerogel.
2. The method for preparing the castor oil/cellulose composite aerogel according to claim 1, wherein the molar ratio of the isocyanatopropyltriethoxysilane to the castor oil is 3.3: 1.
3. The preparation method of the castor oil/cellulose composite aerogel according to claim 1, wherein the reaction time for preparing the silanized castor oil is 30 min.
4. The preparation method of the castor oil/cellulose composite aerogel according to claim 1, wherein the mass concentration of the cellulose nanofiber aqueous dispersion is 0.5-1.0 wt%.
5. The method for preparing the castor oil/cellulose composite aerogel according to claim 1, wherein the amount of tannic acid is 5 wt% of the dry weight of the cellulose nanofibers.
6. A castor oil/cellulose composite aerogel obtained by the production method according to any one of claims 1 to 5.
7. Use of the castor oil/cellulose composite aerogel according to claim 6 for the preparation of oil-water separation products.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513177A (en) * | 2017-09-30 | 2017-12-26 | 中国林业科学研究院林产化学工业研究所 | A kind of vegetable fat modified bacteria cellulose aeroge oil absorption material and preparation method thereof |
| CN110183722A (en) * | 2019-06-12 | 2019-08-30 | 南京林业大学 | Super-amphiphobic nano-cellulose aerogel and its preparation method and application based on orientation freezing |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107513177A (en) * | 2017-09-30 | 2017-12-26 | 中国林业科学研究院林产化学工业研究所 | A kind of vegetable fat modified bacteria cellulose aeroge oil absorption material and preparation method thereof |
| CN110183722A (en) * | 2019-06-12 | 2019-08-30 | 南京林业大学 | Super-amphiphobic nano-cellulose aerogel and its preparation method and application based on orientation freezing |
Non-Patent Citations (2)
| Title |
|---|
| Bio-inspired hydrophobic modification of cellulose nanocrystals with castor oil;Shang, QQ et al;《Carbohydrate Polymers》;20180701;第191卷;第168-175页 * |
| 交联型超双疏细菌纤维素复合气凝胶;陈苏琴等;《纤维素科学与技术》;20200328;第28卷(第1期);第1-7页 * |
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