CN113499760A - High-flux super-hydrophobic wood, preparation method and application thereof - Google Patents

High-flux super-hydrophobic wood, preparation method and application thereof Download PDF

Info

Publication number
CN113499760A
CN113499760A CN202110801737.3A CN202110801737A CN113499760A CN 113499760 A CN113499760 A CN 113499760A CN 202110801737 A CN202110801737 A CN 202110801737A CN 113499760 A CN113499760 A CN 113499760A
Authority
CN
China
Prior art keywords
wood
super
hydrophobic
flux
putting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202110801737.3A
Other languages
Chinese (zh)
Inventor
吴文剑
陈卓瀚
苏晓竞
李坤泉
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Dongguan University of Technology
Original Assignee
Dongguan University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Dongguan University of Technology filed Critical Dongguan University of Technology
Priority to CN202110801737.3A priority Critical patent/CN113499760A/en
Publication of CN113499760A publication Critical patent/CN113499760A/en
Priority to PCT/CN2021/135176 priority patent/WO2023284228A1/en
Pending legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28011—Other properties, e.g. density, crush strength
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0202—Separation of non-miscible liquids by ab- or adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
    • B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

The invention relates to the field of super-hydrophobic materials, in particular to a preparation method of high-flux super-hydrophobic wood, which comprises the following steps: firstly, putting wood into a mixed solution of sodium hydroxide and sodium sulfite, heating for 6-12h at 80-100 ℃ to remove partial hemicellulose and lignin, and then putting the wood into a hydrogen peroxide solution, heating for 0.5-2.5h at 80-100 ℃ to further remove the lignin; then, freezing and freeze-drying the wood for 4-10h, soaking the wood in 2-20 wt% of polydimethylsiloxane solution, taking out the wood and curing the wood for 3-6h at the temperature of 60-100 ℃ to obtain the high-flux super-hydrophobic wood; the contact angle of the water drops on the surface of the super-hydrophobic wood prepared by the method can reach 156 degrees, and the super-hydrophobic wood has vertical arrangement and macroporesThe porous structure of the diameter can quickly carry out high-flux oil-water separation under the drive of gravity, and the separation flux can reach 7165 L.m‑2·h‑1(ii) a Compared with the traditional oil-water separation material, the wood has the characteristics of excellent performance, simple preparation, natural and renewable property, low application energy consumption and the like.

Description

High-flux super-hydrophobic wood, preparation method and application thereof
Technical Field
The invention relates to the field of super-hydrophobic materials, in particular to a high-flux super-hydrophobic wood, and a preparation method and application thereof.
Background
The oily wastewater has wide sources and large discharge amount, and causes serious harm to the ecological environment of water. In order to ensure the safety of water resource environment and the sustainable development of society, an efficient and low-cost oil-water separation technology is a current research hotspot. At present, methods such as gravity precipitation, centrifugal separation, air flotation, chemical flocculation and the like are mostly adopted in the oily wastewater treatment process, but the oily wastewater treatment process has the defects of complex and fussy process, large equipment, high investment and operation cost, high energy consumption, low efficiency, easiness in causing secondary pollution and the like.
The super-hydrophobic material is a material which is inspired by phenomena of lotus leaf surface, rose petal, insect wing and the like in nature and is designed, and the static contact angle of water drops is more than 150 degrees. The unique wettability of the material has important research value and application prospect in the field of oil-water separation, and has been paid much attention to by people. However, most of the currently reported super-hydrophobic materials for oil-water separation have the problems of complicated preparation process, additional driving force, low separation efficiency, high cost, high energy consumption, non-renewable materials, easy secondary pollution and the like. Therefore, the development of the high-flux super-hydrophobic wood which is easy to obtain and regenerate, simple in preparation process, high in efficiency, low in energy consumption and driven by gravity is of great significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides the high-flux super-hydrophobic wood with renewable and degradable substrate, high efficiency and low energy consumption.
The invention also provides a preparation method and application of the high-flux super-hydrophobic wood, which are simple in preparation process and application and operation.
The invention adopts the following technical scheme:
a preparation method of high-flux super-hydrophobic wood comprises the following steps:
firstly, putting wood into a mixed solution of sodium hydroxide and sodium sulfite, heating for 6-12h at 80-100 ℃ to remove partial hemicellulose and lignin, and then putting the wood into a hydrogen peroxide solution, heating for 0.5-2.5h at 80-100 ℃ to further remove the lignin;
then, freezing and freeze-drying the wood for 4-10h, soaking the wood in 2-20 wt% of polydimethylsiloxane solution, taking out the wood and curing the wood for 3-6h at the temperature of 60-100 ℃ to obtain the high-flux super-hydrophobic wood.
The technical proposal is further improved in that the ratio of the sodium hydroxide to the sodium sulfite in the mixed solution of the sodium hydroxide and the sodium sulfite is 6:1-1: 1.
The technical proposal is further improved in that the molar concentration of the sodium hydroxide is 10-30 mol/L.
The technical proposal is further improved in that the molar concentration of the hydrogen peroxide is 5-25 mol/L.
The technical proposal is further improved in that the polydimethylsiloxane solution consists of a main body and a curing agent.
The technical proposal is further improved that the preparation method of the polydimethylsiloxane solution comprises the following steps: mixing the main body and the curing agent in a ratio of 10:1, and dissolving in a solvent.
The technical proposal is further improved in that the main body is double bond end-capped polydimethylsiloxane; the curing agent is poly dimethyl siloxane containing polyfunctional silicon-hydrogen bonds; the solvent is one or more of tetrahydrofuran, normal hexane, cyclohexane, toluene and acetone; the mass fraction of the solvent is 2-20 wt%.
The technical proposal is further improved that the wood is natural balsa wood, the density of which is 120-210kg/m3The pore size is 10-150 nm.
High-flux super-hydrophobic wood prepared by the preparation method is provided.
The application of the high-flux super-hydrophobic wood is applied to the field of oil-water separation; during oil-water separation, the high-flux super-hydrophobic wood enters under the driving of gravityA row; the separation flux in the oil-water separation is 7165 L.m-2·h-1。
The invention has the beneficial effects that:
(1) the invention has the characteristics of simple preparation process, low requirements on required experimental instruments and equipment, low cost, natural and renewable wood resources, simple application and operation, excellent performance and the like.
(2) The high-flux super-hydrophobic wood prepared by the method has a vertical arrangement, a large-aperture porous structure and stable super-hydrophobic performance, the contact angle of water drops on the surface can reach 156 degrees, high-flux oil-water separation can be carried out under the driving of gravity, the separation speed is high, the separation efficiency is high, and the separation flux is as high as 7165 L.m-2·h-1。
Drawings
FIG. 1 is an IR spectrum of a high flux superhydrophobic wood prepared in example 1 of the present invention and virgin wood;
FIG. 2 is a scanning electron micrograph and a contact angle chart of virgin wood before preparation of example 1 of the present invention;
fig. 3 is a scanning electron micrograph and a contact angle chart of the high-flux superhydrophobic wood prepared in example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples for better understanding of the present invention, but the embodiments of the present invention are not limited thereto.
Example 1
First, the density was adjusted to 120kg/m3Putting the wood into a mixed solution of 25mol/L sodium hydroxide and 5mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 5:1, then putting the wood into an oil bath pan, heating the wood for 8 hours at 100 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into a 25mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 0.5h at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator for freezing for 10h, and then putting the wood into a freeze drying oven for treating for 6 h; and finally, preparing 10 wt% of polydimethylsiloxane solution by taking tetrahydrofuran as a solvent, placing the solution into the wood, taking out the wood, and curing the wood for 3 hours at 100 ℃ to obtain the high-flux super-hydrophobic wood.
Fig. 1 is an infrared spectrum of the high flux superhydrophobic wood and virgin wood prepared in example 1. Compared with the original wood, the super-hydrophobic wood is 1505cm-1To 1596cm-1The peak intensity of C ═ C stretching vibration (lignin aromatic ring) is reduced, and the peak intensity is 1730cm-1The non-conjugated C ═ O stretching vibration (hemicellulose or lignin) peak disappears, indicating that most of the hemicellulose and delignification is effectively removed from the wood after treatment with sodium hydroxide, sodium sulfite and hydrogen peroxide. In addition, the super-hydrophobic wood is 798cm-1A new stretching vibration peak of Si-C appears, which indicates that the polydimethylsiloxane successfully carries out hydrophobic modification on the wood.
In order to evaluate the superhydrophobicity of wood, contact angle measurement was performed on wood using a contact angle measuring instrument, and the obtained contact angle was 156 °, and the obtained results are shown in table 1.
In order to evaluate the oil-water separation performance of wood, a self-assembled simple oil-water separation device was tested. The device consists of two glass tubes with openings at two ends, super-hydrophobic wood, a clamp and a beaker. Wherein, the super-hydrophobic wood is used as a filter membrane and is fixed between the two glass tubes through a clamp. Mixing 10mL of dichloromethane and 10mL of distilled water to prepare a simple oil-water mixture, wherein the oil is any one of toluene, dichloromethane, n-hexane, trichloromethane, xylene, cyclohexane and petroleum ether. The mixture is poured into a glass tube above a separation device, and due to the super-hydrophobicity and super-lipophilicity of the wood, the organic solvent can rapidly pass through the super-hydrophobic wood and is collected into a small beaker below the glass tube below the super-hydrophobic wood, and water is blocked above the super-hydrophobic wood, so that the separation of the oil-water mixture is successfully realized. The result shows that the prepared super-hydrophobic wood can rapidly separate oil-water mixture under the drive of gravity, and the separation flux reaches 7165 L.m-2·h-1The results are shown in Table 1. As can be seen from fig. 2 and 3, the wood has a porous structure with vertical pore size, and after hemicellulose and lignin are removed, the number of pores is increased and the pore size is increased, so that the superhydrophobic wood has high separation flux in oil-water separation, and oil-water separation is rapidly realized under the action of gravity, wherein in fig. 2 and 3, the image magnification is 100 times, and the picture inserted in the upper right corner is a water contact angle picture.
Example 2
First, the density was set to 140kg/m3Putting the wood into a mixed solution of 20mol/L sodium hydroxide and 5mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 4:1, then putting the wood into an oil bath pan, heating the wood for 7 hours at 100 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into 20mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 1h at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator, freezing the wood for 10h, and then putting the wood into a freeze drying oven for treatment for 5 h; and finally, preparing 5 wt% of polydimethylsiloxane solution by using acetone as a solvent, placing the solution into the wood, and curing the wood for 3 hours at 90 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 154 °, and an experiment was performed using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example is found to be capable of rapidly separating a normal hexane/water mixture under the driving of gravity, and the separation flux reaches 6948L m-2·h-1. The results obtained are shown in Table 1.
Example 3
First, the density was set to 150kg/m3Putting the wood into a mixed solution of 10mol/L sodium hydroxide and 10mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 1:1, then putting the wood into an oil bath pan, heating the wood for 10 hours at 100 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into 15mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 1.5h at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator for freezing for 10h, and then putting the wood into a freeze drying oven for treating for 8 h; and finally, preparing 2 wt% of polydimethylsiloxane solution by taking toluene as a solvent, placing the solution into the wood, and curing the wood for 6 hours at 80 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, an experiment was performed using the oil-water separator of example 1 with a contact angle of 155 °. The super-hydrophobic wood prepared in the experimental example can be used for quickly separating a chloroform/water mixture under the driving of gravityAnd the separation flux can reach 6396 L.m-2·h-1. The results obtained are shown in Table 1.
Example 4
First, the density was adjusted to 160kg/m3Putting the wood into a mixed solution of 30mol/L sodium hydroxide and 10mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 3:1, then putting the wood into an oil bath pan, heating the wood for 11 hours at 100 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into 10mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 2 hours at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator, freezing the wood for 10 hours, and then putting the wood into a freeze drying oven for treatment for 7 hours; and finally, preparing a 20 wt% polydimethylsiloxane solution by using cyclohexane as a solvent, placing the solution into the wood, taking out the wood, and curing the wood for 5 hours at the temperature of 60 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 154 °, and an experiment was performed using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example can be used for quickly separating a xylene/water mixture under the driving of gravity, and the separation flux can reach 6627 L.m-2·h-1. The results obtained are shown in Table 1.
Example 5
First, the density was set to 170kg/m3Putting the wood into a mixed solution of 20mol/L sodium hydroxide and 10mol/L sodium sulfite, namely putting the mixed solution into an oil bath pan with the mass ratio of the sodium hydroxide to the sodium sulfite being 2:1, heating the mixed solution for 12 hours at 100 ℃, taking out the mixed solution and washing the mixed solution for three times by using clear water; then, putting the wood into a 25mol/L hydrogen peroxide solution, then placing the wood in an oil bath pan, heating the wood for 2 hours at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then placing the wood in a refrigerator for freezing for 10 hours, and then placing the wood in a freeze drying oven for treating for 8 hours; and finally, preparing 15 wt% of polydimethylsiloxane solution by taking tetrahydrofuran as a solvent, placing the solution into the wood, and curing the wood for 6 hours at the temperature of 70 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 154 °, and an experiment was performed using the oil-water separator of example 1. It was found that the super-hydrophobic wood prepared in this example can be usedThe cyclohexane/water mixture is quickly separated under the driving of gravity, and the separation flux can reach 6551 L.m-2·h-1. The results obtained are shown in Table 1.
Example 6
First, the density was adjusted to 210kg/m3Putting the wood into a mixed solution of 30mol/L sodium hydroxide and 5mol/L sodium sulfite, namely putting the mixed solution into an oil bath pan with the mass ratio of the sodium hydroxide to the sodium sulfite being 6:1, heating the mixed solution for 8 hours at 100 ℃, taking out the mixed solution and washing the mixed solution for three times by using clear water; then, putting the wood into a 25mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 1.5h at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator for freezing for 10h, and then putting the wood into a freeze drying oven for treating for 6 h; and finally, preparing a 10 wt% polydimethylsiloxane solution by using n-hexane as a solvent, placing the solution into the wood, and curing the wood for 4 hours at 100 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 153 °, and an experiment was performed using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example is found to be capable of rapidly separating a toluene/water mixture under the driving of gravity, and the separation flux reaches 6744 L.m-2·h-1. The results obtained are shown in Table 1.
Comparative example 1
First, the density was adjusted to 120kg/m3Putting the wood into a mixed solution of 25mol/L sodium hydroxide and 5mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 5:1, then putting the wood into an oil bath pan, heating the wood for 8 hours at 80 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into a 25mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 0.5h at the temperature of 80 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator for freezing for 10h, and then putting the wood into a freeze drying oven for treating for 6 h; and finally, preparing 10 wt% of polydimethylsiloxane solution by taking tetrahydrofuran as a solvent, placing the solution into the wood, taking out the wood, and curing the wood for 3 hours at 100 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using the contact angle measuring instrument, the contact angle was 152 °, and the experiment was performed by using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example can be used for quickly separating a dichloromethane/water mixture under the driving of gravity, and the separation flux reaches 5732 L.m-2·h-1. The results obtained are shown in Table 1.
Comparative example 2
First, the density was set to 140kg/m3Putting the wood into a mixed solution of 20mol/L sodium hydroxide and 5mol/L sodium sulfite, namely putting the mixed solution into an oil bath pan with the mass ratio of the sodium hydroxide to the sodium sulfite being 4:1, heating the mixed solution for 7 hours at 60 ℃, taking out the mixed solution and washing the mixed solution for three times by using clear water; then, putting the wood into 20mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 1h at the temperature of 60 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator, freezing the wood for 10h, and then putting the wood into a freeze drying oven for treatment for 5 h; and finally, preparing 5 wt% of polydimethylsiloxane solution by using acetone as a solvent, placing the solution into the wood, and curing the wood for 3 hours at 90 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 150 °, and an experiment was performed using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example is found to be capable of rapidly separating a normal hexane/water mixture under the driving of gravity, and the separation flux reaches 4777 L.m-2·h-1. The results obtained are shown in Table 1.
Comparative example 3
First, the density was set to 150kg/m3Putting the wood into a mixed solution of 5mol/L sodium hydroxide and 15mol/L sodium sulfite, namely putting the mixed solution into an oil bath pan with the mass ratio of the sodium hydroxide to the sodium sulfite being 1:3, heating the mixed solution for 10 hours at 100 ℃, taking out the mixed solution and washing the mixed solution for three times by using clear water; then, putting the wood into 15mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 1.5h at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator for freezing for 10h, and then putting the wood into a freeze drying oven for treating for 8 h; and finally, preparing 2 wt% of polydimethylsiloxane solution by taking toluene as a solvent, placing the solution into the wood, and curing the wood for 6 hours at 80 ℃ to obtain the high-flux super-hydrophobic wood.
Contact angle measurement of super-hydrophobic wood using a contact angle measuring apparatus gives a contact angle of 151 ° as per the examples1 oil-water separator for experiments. The super-hydrophobic wood prepared in the experimental example can be used for quickly separating a chloroform/water mixture under the driving of gravity, and the separation flux can reach 4984 L.m-2·h-1. The results obtained are shown in Table 1.
Comparative example 4
First, the density was adjusted to 160kg/m3Putting the wood into a mixed solution of 30mol/L sodium hydroxide and 3mol/L sodium sulfite, namely the mass ratio of the sodium hydroxide to the sodium sulfite is 10:1, then putting the wood into an oil bath pan, heating the wood for 11 hours at 100 ℃, taking the wood out, and washing the wood for three times by using clear water; then, putting the wood into 10mol/L hydrogen peroxide solution, then putting the wood into an oil bath pan, heating the wood for 2 hours at 100 ℃, taking the wood out, washing the wood for three times by using clear water, then putting the wood into a refrigerator, freezing the wood for 10 hours, and then putting the wood into a freeze drying oven for treatment for 7 hours; and finally, preparing a 20 wt% polydimethylsiloxane solution by using cyclohexane as a solvent, placing the solution into the wood, taking out the wood, and curing the wood for 5 hours at the temperature of 60 ℃ to obtain the high-flux super-hydrophobic wood.
When the contact angle of the super-hydrophobic wood was measured by using a contact angle measuring instrument, the contact angle was 152 °, and an experiment was performed using the oil-water separator of example 1. The super-hydrophobic wood prepared in the experimental example can be used for quickly separating a xylene/water mixture under the driving of gravity, and the separation flux can reach 5332 L.m-2·h-1. The results obtained are shown in Table 1.
Table 1 shows the water contact angle and the oil-water separation flux of the superhydrophobic wood according to the example of the present invention.
Contact Angle/° Flux of separation/m2·h Oil solvent
Example 1 156 7165 Methylene dichloride
Example 2 155 6948 N-hexane
Example 3 154 6396 Chloroform
Example 4 155 6627 Xylene
Example 5 154 6551 Cyclohexane
Example 6 156 6744 Toluene
Comparative example 1 152 5732 Methylene dichloride
Comparison ofExample 2 150 4777 N-hexane
Comparative example 3 151 4984 Chloroform
Comparative example 4 152 5332 Xylene
As can be seen from the contact angle data and the separation flux data of the examples in table 1, the high-flux superhydrophobic wood obtained in examples 1-6 has good superhydrophobic performance and ultrahigh separation flux, and can be rapidly subjected to oil-water separation.
Compared with examples 1, 2, 3 and 4, the contact angles of comparative examples 1, 2, 3 and 4 are slightly reduced, but the contact angles still have better super-hydrophobic performance, and the oil-water separation flux of the comparative examples is greatly reduced, which shows that the wood separation flux can be greatly influenced when the wood treatment conditions are changed. Therefore, the super-hydrophobic wood disclosed by the invention has excellent super-hydrophobic performance and ultrahigh separation flux, and can be used for quickly carrying out oil-water separation under the driving of gravity.
Performance testing
And (3) calculating separation flux: the separation flux J is calculated by the following formula:
Figure BDA0003164961680000091
wherein V is the volume of the separated liquid, A is the effective area of the separation, and Δ t is the time required for separating the liquid.
Contact angle test: the contact angle measurement of the wood was carried out using a contact angle measuring instrument SDC-200S of santong ancient precision instruments ltd, guan city, measuring 5 μ L of water drop, measuring 5 times for each sample, and taking the average value.
The above examples are only a few specific preparation methods and detailed data of the present invention, and those skilled in the art can make modifications or substitutions, which are within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (10)

1. A preparation method of high-flux super-hydrophobic wood is characterized by comprising the following steps:
firstly, putting wood into a mixed solution of sodium hydroxide and sodium sulfite, heating for 6-12h at 80-100 ℃ to remove partial hemicellulose and lignin, and then putting the wood into a hydrogen peroxide solution, heating for 0.5-2.5h at 80-100 ℃ to further remove the lignin;
then, freezing and freeze-drying the wood for 4-10h, soaking the wood in 2-20 wt% of polydimethylsiloxane solution, taking out the wood and curing the wood for 3-6h at the temperature of 60-100 ℃ to obtain the high-flux super-hydrophobic wood.
2. The method for preparing high-throughput superhydrophobic wood according to claim 1, wherein the ratio of sodium hydroxide to sodium sulfite in the mixed solution of sodium hydroxide and sodium sulfite is 6:1-1: 1.
3. The method for preparing high-throughput superhydrophobic wood according to claim 1, wherein the molar concentration of sodium hydroxide is 10-30 mol/L.
4. The method for preparing high-throughput superhydrophobic wood according to claim 1, wherein the molar concentration of hydrogen peroxide is 5-25 mol/L.
5. The method for preparing high throughput superhydrophobic wood according to claim 1, wherein the polydimethylsiloxane solution is composed of a main body and a curing agent.
6. The method for preparing high-throughput superhydrophobic wood according to claim 5, wherein the method for preparing the polydimethylsiloxane solution comprises the following steps: mixing the main body and the curing agent in a ratio of 10:1, and dissolving in a solvent.
7. The method for preparing high throughput superhydrophobic wood according to claim 6, wherein the host is double bond terminated polydimethylsiloxane; the curing agent is poly dimethyl siloxane containing polyfunctional silicon-hydrogen bonds; the solvent is one or more of tetrahydrofuran, normal hexane, cyclohexane, toluene and acetone; the mass fraction of the solvent is 2-20 wt%.
8. The method for preparing high-throughput super-hydrophobic wood according to claim 1, wherein the wood is natural Bassa wood with a density of 120-210kg/m3The pore size is 10-150 nm.
9. High-throughput superhydrophobic wood, wherein the high-throughput superhydrophobic wood is prepared using the preparation method of any one of claims 1-8.
10. The application of the high-flux super-hydrophobic wood is characterized in that the high-flux super-hydrophobic wood is applied to the field of oil-water separation; during oil-water separation, the high-flux super-hydrophobic wood is driven by gravity; the separation flux in the oil-water separation is 7165 L.m-2·h-1。
CN202110801737.3A 2021-07-15 2021-07-15 High-flux super-hydrophobic wood, preparation method and application thereof Pending CN113499760A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN202110801737.3A CN113499760A (en) 2021-07-15 2021-07-15 High-flux super-hydrophobic wood, preparation method and application thereof
PCT/CN2021/135176 WO2023284228A1 (en) 2021-07-15 2021-12-16 High-throughput super-hydrophobic wood, preparation method therefor and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110801737.3A CN113499760A (en) 2021-07-15 2021-07-15 High-flux super-hydrophobic wood, preparation method and application thereof

Publications (1)

Publication Number Publication Date
CN113499760A true CN113499760A (en) 2021-10-15

Family

ID=78012904

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110801737.3A Pending CN113499760A (en) 2021-07-15 2021-07-15 High-flux super-hydrophobic wood, preparation method and application thereof

Country Status (2)

Country Link
CN (1) CN113499760A (en)
WO (1) WO2023284228A1 (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114989482A (en) * 2022-05-23 2022-09-02 南京林业大学 Durable, flexible and super-hydrophobic nano-pore wood film and preparation method and application thereof
CN115006996A (en) * 2022-06-15 2022-09-06 南京林业大学 Janus wood film with asymmetric wettability, preparation method and application thereof
CN115068979A (en) * 2022-06-09 2022-09-20 东莞理工学院 Super-hydrophobic wood with excellent electrothermal and photothermal effects and preparation method and application thereof
CN115350602A (en) * 2022-08-08 2022-11-18 东莞理工学院 Hydrophobic oleophilic film with photo-thermal and electric-thermal effects for oil-water separation and preparation method thereof
WO2023284228A1 (en) * 2021-07-15 2023-01-19 东莞理工学院 High-throughput super-hydrophobic wood, preparation method therefor and application thereof
CN116726889A (en) * 2023-04-26 2023-09-12 中国华电科工集团有限公司 Organic wastewater treatment material, preparation method thereof and organic wastewater treatment device
CN117001796A (en) * 2023-07-03 2023-11-07 东莞理工学院 Super-hydrophobic wood with demulsification capability and preparation method and application thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110237827A (en) * 2019-06-20 2019-09-17 南京林业大学 A kind of preparation method using natural timber building water-oil separation material
CN110497492A (en) * 2019-08-30 2019-11-26 北京林业大学 A kind of preparation method of the super-hydrophobic wooden sponge
CN111330462A (en) * 2020-02-28 2020-06-26 浙江工业大学 Super-hydrophobic demulsification oil-water separation membrane material and preparation method and application thereof
CN112845334A (en) * 2020-12-30 2021-05-28 东莞理工学院 Surface condensation dust removal method

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100503959C (en) * 2007-10-19 2009-06-24 东华大学 Method for bleaching tossa
CN109608683A (en) * 2018-12-14 2019-04-12 中国林业科学研究院木材工业研究所 A kind of wooden sponge oil absorption material and preparation method thereof
CN113499760A (en) * 2021-07-15 2021-10-15 东莞理工学院 High-flux super-hydrophobic wood, preparation method and application thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110237827A (en) * 2019-06-20 2019-09-17 南京林业大学 A kind of preparation method using natural timber building water-oil separation material
CN110497492A (en) * 2019-08-30 2019-11-26 北京林业大学 A kind of preparation method of the super-hydrophobic wooden sponge
CN111330462A (en) * 2020-02-28 2020-06-26 浙江工业大学 Super-hydrophobic demulsification oil-water separation membrane material and preparation method and application thereof
CN112845334A (en) * 2020-12-30 2021-05-28 东莞理工学院 Surface condensation dust removal method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
王开立: ""基于表面微纳结构设计的超疏水木材制备与作用机制"", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2023284228A1 (en) * 2021-07-15 2023-01-19 东莞理工学院 High-throughput super-hydrophobic wood, preparation method therefor and application thereof
CN114989482A (en) * 2022-05-23 2022-09-02 南京林业大学 Durable, flexible and super-hydrophobic nano-pore wood film and preparation method and application thereof
CN114989482B (en) * 2022-05-23 2023-08-04 南京林业大学 Durable, flexible and super-hydrophobic nanometer Kong Mumo, and preparation method and application thereof
CN115068979A (en) * 2022-06-09 2022-09-20 东莞理工学院 Super-hydrophobic wood with excellent electrothermal and photothermal effects and preparation method and application thereof
CN115068979B (en) * 2022-06-09 2023-07-28 东莞理工学院 Super-hydrophobic wood with excellent electrothermal and photo-thermal effects, and preparation method and application thereof
CN115006996A (en) * 2022-06-15 2022-09-06 南京林业大学 Janus wood film with asymmetric wettability, preparation method and application thereof
CN115350602A (en) * 2022-08-08 2022-11-18 东莞理工学院 Hydrophobic oleophilic film with photo-thermal and electric-thermal effects for oil-water separation and preparation method thereof
CN115350602B (en) * 2022-08-08 2023-07-28 东莞理工学院 Hydrophobic and oleophilic film with photo-thermal and electrothermal effects for oil-water separation and preparation method thereof
CN116726889A (en) * 2023-04-26 2023-09-12 中国华电科工集团有限公司 Organic wastewater treatment material, preparation method thereof and organic wastewater treatment device
CN117001796A (en) * 2023-07-03 2023-11-07 东莞理工学院 Super-hydrophobic wood with demulsification capability and preparation method and application thereof
CN117001796B (en) * 2023-07-03 2024-05-28 东莞理工学院 Super-hydrophobic wood with demulsification capability and preparation method and application thereof

Also Published As

Publication number Publication date
WO2023284228A1 (en) 2023-01-19

Similar Documents

Publication Publication Date Title
CN113499760A (en) High-flux super-hydrophobic wood, preparation method and application thereof
Wang et al. An ultralight, elastic, cost-effective, and highly recyclable superabsorbent from microfibrillated cellulose fibers for oil spillage cleanup
CN105542221B (en) A kind of wear-resisting super-hydrophobic super-oleophylic polyurethane sponge, preparation method and its application in grease continuously separates
CN109012237B (en) Super-hydrophobic super-oleophylic nanofiber membrane for oil-water mixture separation and preparation method thereof
CN110368718B (en) Three-dimensional printed super-hydrophilic and underwater super-oleophobic net film and preparation method thereof
CN106693898B (en) Doping-degree-controllable porous reduced graphene oxide oil absorption material and preparation method thereof
CN115068979B (en) Super-hydrophobic wood with excellent electrothermal and photo-thermal effects, and preparation method and application thereof
CN107020071B (en) Super-hydrophobic compound carbon aerogels oil absorption material of one kind and preparation method thereof
CN109289531A (en) A kind of preparation method of the dimethyl silicone polymer for organic solvent nanofiltration/meso-porous nano silicon composite membrane
CN108380062A (en) Have big flux hydrophilic and oleophobic water-oil separationg film and its preparation and application of antibacterial functions
CN109647295B (en) Sodium alginate/N-succinyl chitosan composite aerogel and preparation method and application thereof
Meng et al. Preparation and modification of cellulose sponge and application of oil/water separation
CN113457474B (en) Nanofiber membrane material, preparation method and application thereof
CN111632504A (en) Self-cleaning super-hydrophobic nanofiber membrane and preparation method thereof
Fan et al. Electro-blown spun PS/PAN fibrous membrane for highly efficient oil/water separation
CN115418795B (en) Janus type micro-nano composite fiber membrane with single-sided superhydrophobic and single-sided superhydrophilic properties and preparation method thereof
Yin et al. Cellulose-based aerogel from Eichhornia crassipes as an oil superabsorbent
Shen et al. Antifouling hydrophilic electrostatic spinning PAN membrane based on click chemistry with high efficiency oil-water separation
CN114619748A (en) Carbon nanotube-based unidirectional moisture-conducting photothermal film, preparation method and prepared solar interface evaporation device
CN109610031B (en) Preparation of biomass carbon-doped nanofiber felt and application of biomass carbon-doped nanofiber felt in separation of oil-water mixture
CN115181323A (en) Preparation method and oil absorption application of regenerated protein-based high-strength aerogel
CN113262765A (en) Electrostatic spinning fiber membrane based on polythiocarbonate and preparation method and application thereof
CN109012238B (en) Preparation method of high-strength high-flux oil-water separation membrane and oil-water separation membrane
Dong et al. Preparation of polystyrene and silane-modified nano-silica superhydrophobic and superoleophilic three-dimensional composite fiber membranes for efficient oil absorption and oil-water separation
CN112090116B (en) Preparation method of oil-water separation membrane

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20211015

RJ01 Rejection of invention patent application after publication