CN115920862B - Super-hydrophobic lignocellulose compound for oil-water separation and preparation method thereof - Google Patents
Super-hydrophobic lignocellulose compound for oil-water separation and preparation method thereof Download PDFInfo
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- 238000000926 separation method Methods 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract description 18
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 18
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract description 17
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- 239000002131 composite material Substances 0.000 claims description 30
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 18
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 18
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 3
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 abstract description 13
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 abstract description 10
- 230000008569 process Effects 0.000 abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract description 7
- 229940057995 liquid paraffin Drugs 0.000 abstract description 6
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- 235000019476 oil-water mixture Nutrition 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 15
- 239000000463 material Substances 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 8
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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Classifications
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
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Abstract
The invention relates to a super-hydrophobic lignocellulose compound for oil-water separation and a preparation method thereof, comprising the following steps: (1) Carrying out hot pickling treatment and drying on lignocellulose to obtain pretreated lignocellulose; (2) Dispersing pretreated lignocellulose in hot water, then adding nano ceramic particles, and stirring to perform grafting reaction so that the nano ceramic particles are grafted on the surface of the pretreated lignocellulose; and then cooling to room temperature, adding PDMS solution containing curing agent and binder, stirring to perform surface modification reaction, casting into a mould after the reaction is finished, and performing thermosetting integrated molding to obtain the super-hydrophobic lignocellulose compound for oil-water separation. The method has the advantages of simple process flow, integrated molding, stable structure, low cost, degradability, easy recovery and environmental protection; the oil-water separation efficiency of the oil-water mixture of toluene, normal hexane, liquid paraffin, methylene dichloride, chloroform and the like reaches more than 96 percent.
Description
Technical Field
The invention relates to the technical field of super-hydrophobic materials, in particular to a super-hydrophobic lignocellulose compound for oil-water separation and a preparation method thereof.
Background
With the frequent occurrence of petroleum leakage events and the discharge of land oily wastewater, the global water circulation system is under tremendous pressure, and simply collecting the oily wastewater cannot treat pollution problems, and can also cause the waste of available oil-water resources. In the early stage of treatment of oily wastewater, traditional methods such as combustion, scooping and the like are used for realizing the oil-water separation result, but the traditional methods have higher cost and complicated means, can not thoroughly solve the oil-water separation problem of the oily wastewater, and even can damage the atmospheric environment and land resources. Therefore, development of an efficient and rapid-response oil-water separation material and an oil-water separation method with low cost and simple preparation have become urgent problems to be solved.
Based on natural superhydrophobic phenomena such as lotus leaves, butterfly wings and the like, the superhydrophobic material researched by researchers has excellent hydrophobicity and lipophilicity, and can separate oil and water in oily wastewater. Many sponge, coating, film, stainless steel/copper mesh and cotton fabric materials have been developed for use in the field of oil-water separation. However, the preparation process of the materials has the problems of complex preparation method and difficult recovery and degradation of the prepared materials.
Lignocellulose has been found to be an organic material with a rich reserve and is available from a variety of sources, including various wood in forests, crop residues, and various grasses. The lignocellulose mainly comprises cellulose, hemicellulose and lignin, has a unique three-dimensional structure, has relatively strong rigidity and strength, and has the characteristics of environmental protection, reproducibility, degradability and the like. There is relatively little research currently done to prepare superhydrophobic materials from lignocellulose and for oil-water separation applications. Patent application number 201610091406.4 discloses a preparation method of super-hydrophobic cellulose/chitosan composite aerogel oil-water separation material, which requires long-time freeze drying at-50 ℃, and has complex and harsh preparation conditions and unknown durability.
Disclosure of Invention
Aiming at the problems that the preparation method is complex, the prepared material is not easy to recover and degrade and is not durable in the preparation process of sponge, coating, film, stainless steel net/copper net and cotton fabric materials used in the oil-water separation field at present, the super-hydrophobic lignocellulose compound used for oil-water separation and the preparation method thereof are provided. The superhydrophobic lignocellulose composite obtained by the method has the advantages of simple process flow, integrated molding, stable structure, low cost, degradability, easy recovery and environmental protection; the oil-water separation efficiency of the oil-water mixture of toluene, normal hexane, liquid paraffin, methylene dichloride, chloroform and the like reaches more than 96 percent.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
The preparation method of the super-hydrophobic lignocellulose compound for oil-water separation comprises the following steps:
(1) Carrying out hot pickling treatment and drying on lignocellulose to obtain pretreated lignocellulose;
In the process of heating and pickling, partial hemicellulose and lignin on the surface of lignocellulose undergo hydrolysis reaction, and in the hydrolysis reaction process, the surface of lignocellulose expands after being pre-wetted and heated, so that a larger attachment surface can be provided for the grafting of nano silicon carbide particles in the next step; the monosaccharide and the oligosaccharide generated by partial hydrolysis have specific structural viscosity, and can provide certain adhesive force for grafting of lignocellulose and nano silicon carbide, so that the overall combination stability of the lignocellulose and the nano silicon carbide graft is improved;
(2) Dispersing the pretreated lignocellulose in hot water, then adding nano ceramic particles, and stirring to perform grafting reaction so that the nano ceramic particles are grafted on the surface of the pretreated lignocellulose; and then cooling to room temperature, adding PDMS solution containing a curing agent and a binder, stirring to perform surface modification reaction, casting into a mould after the reaction is finished, and performing thermosetting integrated molding to obtain the super-hydrophobic lignocellulose compound for oil-water separation.
Further, the hot pickling treatment comprises the following steps: stirring the lignocellulose for 0.5-1.5h at 70-85 ℃ by using 0.5-3mol/L hydrochloric acid solution, then regulating the pH value of the system to be neutral, continuously stirring for 0.5-1.5h, and then washing to wash out impurities in the lignocellulose and degrade lignin.
Further, the lignocellulose has a diameter of 20-30 μm and a length of 100-200 μm; the nano ceramic particles are silicon carbide, and the particle size is 20-50nm; the binder is ethyl orthosilicate.
Further, the grafting reaction is carried out at a temperature of 90-105 ℃ for 0.5-1.5 hours; the stirring speed is 2000-3000rpm.
Further, the PDMS solution containing the curing agent is prepared from PDMS prepolymer and D65 curing agent according to a mass ratio of 10:1.
Further, the mass ratio of the pretreated lignocellulose to the nano ceramic particles to the water is 10 (0.5-1.5) (500-800); the volume ratio of the PDMS solution containing the curing agent, the binder and the water is 10 (1.5-2.5) (250-400). Preferably, the mass ratio of the pretreated lignocellulose, the nano ceramic particles and the water is 10:1:600; the volume ratio of the PDMS solution containing the curing agent, the binder and the water is 5:1:600.
In another aspect, the invention provides a superhydrophobic lignocellulosic composite for oil-water separation obtained by the above preparation method.
The beneficial technical effects are as follows:
the invention adopts a simple one-pot method to prepare the lignocellulose-based superhydrophobic compound. The pretreated lignocellulose, silicon carbide and polydimethylsiloxane are combined, and the lignocellulose absorbs water and heats up to expand and dry and lose water to shrink, so that the material is integrally formed. The prepared super-hydrophobic lignocellulose material not only has excellent hydrophobic and oleophylic properties, but also has good mechanical stability and ultraviolet aging resistance. The preparation method has the advantages of simple process, easy realization and low cost, and solves the problem of complex laboratory process. The lignocellulose-based superhydrophobic compound is environment-friendly, renewable and degradable, has excellent flexibility and air permeability, and can be applied to the fields of treatment of oily wastewater, oil absorption, separation and the like.
The preparation process of the super-hydrophobic lignocellulose compound is simple, integrally formed, stable in structure, low in cost, degradable, easy to recycle and environment-friendly. The prepared super-hydrophobic lignocellulose compound has good stability and ultraviolet aging resistance. The prepared super-hydrophobic lignocellulose compound has super-fast oil absorption rate and high oil-water separation efficiency, and the oil-water separation efficiency of the mixture of toluene, normal hexane, liquid paraffin, dichloromethane and chloroform oil-water reaches over 96 percent.
Drawings
FIG. 1 is a graph showing the effect of superhydrophobic-superhydrophilic properties of the superhydrophobic lignocellulosic composite of example 1.
FIG. 2 shows the surface morphology of the superhydrophobic lignocellulosic composites of example 1 at different magnifications, wherein (a) is 200 μm on a scale, (b) is 5 μm on a scale, and (c) is 2 μm on a scale.
FIG. 3 is a graph showing the effect (g-i) of the super-hydrophobic lignocellulose complex of example 1 on the absorption and separation of n-hexane (a-c), liquid paraffin (d-f) and methylene chloride.
Fig. 4 is the change in contact angle of the aging resistance test of the superhydrophobic lignocellulose composite of example 1.
Fig. 5 shows the oil-water separation efficiency and oil flux of the superhydrophobic lignocellulose of example 1 for different oils.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The numerical values set forth in these examples do not limit the scope of the present invention unless specifically stated otherwise. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative, and not a limitation. Thus, other examples of the exemplary embodiments may have different values.
The experimental methods in the following examples, for which specific conditions are not noted, are generally determined according to national standards; if the national standard is not corresponding, the method is carried out according to the general international standard or the standard requirements set by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
The preparation method of the super-hydrophobic lignocellulose compound for oil-water separation comprises the following steps:
(1) Pretreatment of lignocellulose:
adding lignocellulose serving as a raw material into a 1mol/L dilute hydrochloric acid solution at 80 ℃ and magnetically stirring for 1h for pickling; then continuing to add 1mol/L sodium hydroxide solution at the temperature to ensure that the pH value of the system is=7, and continuing to magnetically stir for 1h; then washing with deionized water to remove impurities in lignocellulose and degrade lignin;
In the process of heating and pickling, partial hemicellulose and lignin on the surface of lignocellulose undergo hydrolysis reaction, and in the hydrolysis reaction process, the surface of lignocellulose expands after being pre-wetted and heated, so that a larger attachment surface can be provided for the grafting of nano silicon carbide particles in the next step; the monosaccharide and the oligosaccharide generated by partial hydrolysis have specific structural viscosity, and can provide certain adhesive force for grafting of lignocellulose and nano silicon carbide, so that the overall combination stability of the lignocellulose and the nano silicon carbide graft is improved;
(2) Obtaining a superhydrophobic lignocellulose complex:
Mixing 5g of the pretreated lignocellulose (with the diameter of 20-30 mu m and the length of 100-200 mu m) in the step (1) with 300mL of deionized water under the heating condition of water bath 100 ℃ to prewet the lignocellulose, adding 0.5g of nano SiC particles (with the particle size of 20-50 nm) and magnetically stirring for 1h (rotating speed of 2000 rpm) to carry out grafting reaction so as to enable the nano SiC particles to be grafted on the surface of the hydrolyzed lignocellulose;
Then, the system temperature is reduced to room temperature, 10mL of PDMS solution (PDMS prepolymer: D65 curing agent mass ratio is 10:1) and 2mL of ethyl silicate are added, and the mixture is continuously stirred for 1h for surface modification to obtain a mixed system;
And then pouring the mixed system into a mould, and carrying out vacuum drying at 80 ℃ and heat curing for 3 hours to obtain the super-hydrophobic wood fiber composite for oil-water separation.
The surface of the superhydrophobic lignocellulose composite of the embodiment has superhydrophobic-superhydrophilic effect, and the superhydrophobic-superhydrophilic effect is shown in fig. 1.
The surface morphology of the superhydrophobic wood fiber composite of the embodiment is shown in fig. 2, and as can be seen from fig. 2, the composite has a good gully and pore structure, and provides necessary conditions for superhydrophobic and oil absorption.
Example 2
The preparation method of the super-hydrophobic lignocellulose compound for oil-water separation comprises the following steps:
(1) The pretreatment of lignocellulose was obtained in the same way as in example 1, step 1;
(2) Obtaining a superhydrophobic lignocellulose complex:
Mixing 5g of the pretreated lignocellulose (with the size of 25 mu m) in the step (1) with 250mL of deionized water under the heating condition of water bath 100 ℃ to prewet the lignocellulose, adding 0.6g of nano SiC particles (with the particle size of 20-50 nm) and magnetically stirring for 1h (with the rotating speed of 2000 rpm) to carry out grafting reaction so as to enable the nano SiC particles to be grafted on the surface of the hydrolyzed lignocellulose;
Then, the system temperature is reduced to room temperature, 10mL of PDMS solution (PDMS prepolymer: D65 curing agent mass ratio is 10:1) and 2mL of ethyl silicate are added, and the mixture is continuously stirred for 1h for surface modification to obtain a mixed system;
And then pouring the mixed system into a mould, and carrying out vacuum drying at 80 ℃ and heat curing for 3 hours to obtain the super-hydrophobic wood fiber composite for oil-water separation.
The surface of the superhydrophobic lignocellulose composite of the embodiment has a superhydrophobic-superhydrophilic effect.
The surface morphology of the superhydrophobic lignocellulosic composites of this example is similar to example 1, with good ravines and pore structures as well.
Example 3
The preparation method of the super-hydrophobic lignocellulose compound for oil-water separation comprises the following steps:
(1) The pretreatment of lignocellulose was obtained in the same way as in example 1, step 1;
(2) Obtaining a superhydrophobic lignocellulose complex:
Mixing 5g of the pretreated lignocellulose (with the size of 25 mu m) in the step (1) with 400mL of deionized water under the heating condition of water bath 100 ℃ to prewet the lignocellulose, adding 0.7g of nano SiC particles (with the particle size of 20-50 nm) and magnetically stirring for 1h (with the rotating speed of 3000 rpm) to carry out grafting reaction so as to enable the nano SiC particles to be grafted on the surface of the hydrolyzed lignocellulose;
Then, the system temperature is reduced to room temperature, 10mL of PDMS solution (PDMS prepolymer: D65 curing agent mass ratio is 10:1) and 2mL of ethyl silicate are added, and the mixture is continuously stirred for 1h for surface modification to obtain a mixed system;
And then pouring the mixed system into a mould, and carrying out vacuum drying at 80 ℃ and heat curing for 3 hours to obtain the super-hydrophobic wood fiber composite for oil-water separation.
The surface of the superhydrophobic lignocellulose composite of the embodiment has a superhydrophobic-superhydrophilic effect.
The surface morphology of the superhydrophobic lignocellulosic composites of this example is similar to example 1, with good ravines and pore structures as well.
Comparative example 1
The preparation of the lignocellulosic composites of this comparative example was: the pretreated lignocellulose, nano SiC particles, PDMS solution and ethyl silicate are mixed and stirred for 2 hours at room temperature, the obtained mixed system is poured into a mould, vacuum drying is carried out at 80 ℃ for heat curing for 3 hours, and the super-hydrophobic wood fiber composite for oil-water separation is obtained, and the raw material consumption is kept consistent with that of the embodiment 1.
Test example 1
The surface contact angle and the rolling angle were measured for the above examples and comparative examples, and then the surface contact angle and the rolling angle were measured after ultraviolet irradiation was performed for 144 hours, respectively. The results are shown in Table 1.
Table 1 contact angle and roll angle data before and after aging resistance of examples and comparative examples
As can be seen from table 1, in comparative example 1, the pretreated cellulose was not grafted with the nano silicon carbide particles, and the prepared composite had a certain hydrophobicity in the initial state, but did not reach the superhydrophobic effect; in the embodiment 1, the nano silicon carbide particles are grafted to the surface of the hydrolyzed lignocellulose, and then a compound is prepared, and the change of the water contact angle and the rolling angle of the super-hydrophobic lignocellulose compound in the embodiment 1 along with the ultraviolet aging time is shown in fig. 4, so that the super-hydrophobic wood fiber compound has better super-hydrophobicity in an initial state, and the super-hydrophobic effect is basically unchanged even after ultraviolet irradiation for 144 hours, so that the super-hydrophobic wood fiber compound has better stability.
Test example 2
The composites of the above examples and comparative examples were placed in a funnel, toluene (TOL), n-hexane (CYH), liquid Paraffin (LP), methylene chloride (DMC) and Chloroform (CF) were respectively mixed with water to form an oil-water mixture (volume ratio of oil to water is 1:1), the oil-water mixtures containing different oils were poured into the funnel filled with the composites, respectively, and gravity was used to separate, water was isolated from seeping, the seeped oil was collected, the oil absorbed by the composites was collected by suction filtration, and then the oil-water separation efficiency was calculated. Oil flux was also tested. The specific results are shown in Table 2 and FIG. 5.
Table 2 the complexes of the examples and comparative examples are for different species
As is clear from Table 2, the separation efficiency of the compound prepared by simple blending in comparative example 1 for various oils was about 50%, and the oil flux was less than 5500L/m 2. H. Bar; as can be seen from FIG. 5, the superhydrophobic lignocellulosic composite of the invention has a separation efficiency of 95% or more for different oils, and an oil flux of at least 6500L/m 2 h bar or more.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (7)
1. The preparation method of the super-hydrophobic lignocellulose composite for oil-water separation is characterized by comprising the following steps of:
(1) Carrying out hot pickling treatment and drying on lignocellulose to obtain pretreated lignocellulose;
(2) Dispersing the pretreated lignocellulose in hot water, then adding nano ceramic particles, and stirring to perform grafting reaction so that the nano ceramic particles are grafted on the surface of the pretreated lignocellulose; then cooling to room temperature, adding PDMS solution containing curing agent and binder, stirring to perform surface modification reaction, casting into a mould after the reaction is finished, and performing thermosetting integrated molding to obtain the super-hydrophobic lignocellulose compound for oil-water separation;
the nano ceramic particles are silicon carbide, and the particle size is 20-50nm;
the binder is ethyl orthosilicate.
2. The method for preparing the super-hydrophobic lignocellulose composite for oil-water separation according to claim 1, wherein the hot pickling treatment comprises the following steps: stirring the lignocellulose for 0.5-1.5h at 70-85 ℃ by using 0.5-3mol/L hydrochloric acid solution, then regulating the pH value of the system to be neutral, continuously stirring for 0.5-1.5h, and then washing with water.
3. The method for preparing a superhydrophobic lignocellulose composite for oil-water separation according to claim 1, wherein the lignocellulose has a diameter of 20-30 μm and a length of 100-200 μm.
4. The method for preparing a superhydrophobic lignocellulose composite for oil-water separation according to claim 1, wherein the grafting reaction temperature is 90-105 ℃ and the reaction time is 0.5-1.5h; the stirring speed is 2000-3000rpm.
5. The preparation method of the super-hydrophobic lignocellulose composite for oil-water separation, according to claim 1, wherein the PDMS solution containing the curing agent is prepared from PDMS prepolymer and D65 curing agent according to a mass ratio of 10:1.
6. The preparation method of the super-hydrophobic lignocellulose composite for oil-water separation, according to claim 1, wherein the mass ratio of the pretreated lignocellulose to the nano ceramic particles to the water is 10 (0.5-1.5) (500-800); the volume ratio of the PDMS solution containing the curing agent, the binder and the water is 5 (0.5-1.5) (500-800).
7. The superhydrophobic lignocellulose composite for oil-water separation obtained according to the preparation method of any one of claims 1-6.
Priority Applications (1)
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| CN109385173A (en) * | 2017-08-10 | 2019-02-26 | 中国科学院苏州纳米技术与纳米仿生研究所 | Oleophobic coating material, oil-water separating function material, preparation method and the usage |
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