CN107159129B - One-step preparation method and application of PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine spongy carbon material - Google Patents

One-step preparation method and application of PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine spongy carbon material Download PDF

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CN107159129B
CN107159129B CN201710364785.4A CN201710364785A CN107159129B CN 107159129 B CN107159129 B CN 107159129B CN 201710364785 A CN201710364785 A CN 201710364785A CN 107159129 B CN107159129 B CN 107159129B
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pdms
melamine sponge
carbon material
melamine
water
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CN107159129A (en
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张瑞龙
戴江栋
谢阿田
常忠帅
田苏君
葛文娜
闫永胜
周志平
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Jiangsu University
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    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • 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
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/28014—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 form
    • B01J20/28042—Shaped bodies; Monolithic structures
    • B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
    • 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
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/34—Organic compounds containing oxygen
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Analytical Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Hydrology & Water Resources (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention provides a one-step preparation method and application of a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material, which comprises the following steps: step 1, cleaning melamine sponge: soaking melamine sponge in hydrochloric acid for cleaning, washing with water to neutrality, and drying; step 2, PDMS loading: soaking the cleaned melamine sponge in a PDMS solution, and drying to obtain PDMS-loaded melamine sponge; step 3, preparing a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material: and (3) placing the PDMS-loaded melamine sponge in a tubular furnace, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material. The preparation method is simple and feasible, has short flow and is suitable for industrial production and use.

Description

One-step preparation method and application of PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine spongy carbon material
Technical Field
The invention relates to a one-step preparation method and application of a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material, belonging to the technical field of preparation of environment functional materials.
Background
Along with the rapid development of economy, the problem of water resource pollution caused by organic matters is also getting worse, and meanwhile, oil leakage is easy to occur in the processes of oil exploitation, transportation and storage to cause marine pollution events. These oil-contaminated water sources cause great damage to the ecological environment, and much attention has been paid to oil-water separation of oily sewage. The main methods for oil-water separation include centrifugation, gravity, adsorption, biological oxidation, and chemical methods. Of which selective adsorption separation is one of the simplest and most convenient ways. However, the traditional adsorbing material has unobvious interface infiltration characteristic, poor oil absorption capacity and poor water resistance, and can absorb a large amount of water while adsorbing oil, thereby reducing the separation efficiency. Under the circumstances, it is required to develop a novel oil-water separation material which is excellent in hydrophobic-oleophilic property and is environmentally friendly.
The melamine sponge is a foam product with low density, high porosity and strong flexibility. The flame-retardant sound-absorbing material has excellent flame retardance, sound absorption and heat insulation, and is widely applied to the fields of buildings, vehicles, aerospace and the like with the requirements of heat insulation, heat preservation, noise control and the like. The melamine sponge-based super-light porous material has the advantages of super-light porous property, reusability, low price and the like, can be used as a selective adsorption material for oil-water separation, achieves super-hydrophobic performance by rough construction and surface low-energy modification on the surface of the material, and is applied to oil-water separation engineering.
The invention fully utilizes resources, takes the low-density porous melamine sponge as a base material, constructs the low-energy substance on the surface of PDMS (polydimethylsiloxane) and forms a rough structure at the same time, the material shows excellent super-hydrophobic property, shows good selective oil adsorption in an oil-water mixture, and is an adsorption material with good prospect for oil-water separation engineering.
Disclosure of Invention
The invention aims to provide a one-step preparation method of a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material, which comprises the following steps of: soaking melamine sponge in hydrochloric acid water solution for cleaning, washing to be neutral, and drying; PDMS (polydimethylsiloxane) loading: soaking the cleaned melamine sponge in a PDMS solution, and drying to obtain PDMS-loaded melamine sponge; preparing a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material: and (3) placing the PDMS-loaded melamine sponge in a tubular furnace, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material. The technical scheme adopted by the invention is as follows:
a one-step preparation method for constructing a super-hydrophobic melamine sponge carbon material by PDMS comprises the following steps:
step 1, cleaning melamine sponge: soaking melamine sponge in hydrochloric acid for cleaning, washing with water to neutrality, and drying;
step 2, PDMS loading: soaking the cleaned melamine sponge in a PDMS solution, and drying to obtain PDMS-loaded melamine sponge;
step 3, preparing a PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material: and (3) placing the PDMS-loaded melamine sponge in a tubular furnace, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material.
In the step 1, the concentration of the hydrochloric acid used is 0.1-5 mol L-1The soaking temperature is 10-70 ℃, and the soaking time is 0.5-5 h.
In the step 1, the water washing is deionized water or distilled water or hot water washing.
In the step 1, the drying is carried out at the temperature of 40-80 ℃ for 3-8 h.
In the step 2, the PDMS solution is an alkane mixed solution of PDMS and a curing agent, and the curing agent is a silicone oil curing agent.
In the step 2, in the used PDMS solution, the mass of PDMS is 0.1-5% of that of the solvent, and the mass of the curing agent is 1-20% of that of PDMS.
In the step 2, the solvent is at least one of pentane, hexane, cyclohexane and octane.
In the step 2, the drying is carried out at the temperature of 40-80 ℃ for 1-3 h.
In step 3, the inert gas used is nitrogen or argon.
In the step 3, the high-temperature carbonization temperature is 400-900 ℃, and the high-temperature carbonization time is 0.05-2 h.
The prepared PDMS-constructed super-hydrophobic melamine spongy carbon material is used for adsorbing oil stains in water, such as soybean oil on the water surface, underwater carbon tetrachloride and the like.
Has the advantages that:
(1) the base material used in the invention is melamine sponge, and the price is low.
(2) The prepared PDMS-constructed super-hydrophobic melamine sponge carbon material has the performances of high porosity, ultralow density, high adsorption capacity, quick adsorption, strong chemical stability, good regeneration and reutilization property and the like.
(3) The PDMS-structured super-hydrophobic melamine spongy carbon material has the advantages of super-hydrophobic performance, high adsorption capacity, easiness in recycling adsorbed organic matters and the like, and can be widely used in the field of oil stain adsorption in water.
(4) The preparation method is simple and feasible, has short flow and is suitable for industrial production and use.
Drawings
FIG. 1 is a scanning electron micrograph of a melamine sponge not loaded with PDMS in example 1 after carbonization;
FIG. 2 is a scanning electron microscope image of PDMS-structured superhydrophobic melamine sponge carbon material prepared in example 1.
Detailed Description
The invention is further described below with reference to the accompanying drawings:
example 1:
firstly, cleaning of melamine sponge: immersing melamine sponge in 0.5mol L at 50 DEG C-1Washing in hydrochloric acid water solution for 3h, washing with deionized water, distilled water or hot water to neutrality, and oven drying; then, PDMS loading: soaking the cleaned melamine sponge in PDMS alkane solution, wherein PDMS accounts for 1% of the mass of the alkane, and a curing agent accounts for 1% of the mass of the PDMS, and drying at 60 ℃ to obtain PDMS-loaded melamine sponge; and finally, placing the PDMS-loaded melamine sponge in a lower tubular furnace at 600 ℃ for keeping the constant temperature for 0.1h, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material. The alkane is at least one of pentane, hexane, cyclohexane and octane.
FIG. 1 is a scanning electron micrograph of the non-PDMS-loaded melamine sponge of example 1 after carbonization, from which it is clear that there is a large amount of swelling at the nodes of the sponge carbon material.
Fig. 2 is a scanning electron microscope image of the superhydrophobic melamine sponge carbon material constructed by PDMS prepared in example 1, and it can be seen that a layer of dense PDMS is on the surface of the sponge carbon, which indicates that the loading is successful.
Example 2:
firstly, cleaning of melamine sponge: immersing melamine sponge in 5mol L of concentration at 10 DEG C-1Washing with hydrochloric acid water solution for 5h, washing with deionized water, distilled water or hot water to neutrality, and oven drying; then, PDMS loading: soaking the cleaned melamine sponge in PDMS alkane solution, wherein PDMS accounts for 5% of the mass of the alkane, and a curing agent accounts for 1% of the mass of the PDMS, and drying at 80 ℃ to obtain PDMS-loaded melamine sponge; and finally, placing the PDMS-loaded melamine sponge in a lower tubular furnace at 400 ℃ for 2h, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material.
Example 3:
firstly, cleaning of melamine sponge: immersing melamine sponge in 0.1mol L at 70 DEG C-1Washing in hydrochloric acid water solution for 0.5h, washing with deionized water, distilled water or hot water to neutrality, and oven drying; then, PDMS loading: soaking the cleaned melamine sponge in PDMS alkane solution, wherein PDMS accounts for 0.1% of the mass of the alkane, and a curing agent accounts for 20% of the mass of the PDMS, and drying at 40 ℃ to obtain PDMS-loaded melamine sponge; and finally, placing the PDMS-loaded melamine sponge in a 900 ℃ lower tubular furnace, keeping the temperature constant for 0.05h, and carbonizing at high temperature under the protection of inert gas to obtain the PDMS-constructed super-hydrophobic melamine sponge carbon material.
2. The invention is further illustrated by the following examples in which:
the performance evaluation of the oil stain adsorption of the water body in the specific embodiment of the invention is carried out according to the following method: a certain amount of oil, such as low-density oil and high-density oil, is added into deionized water, and a certain mass of PDMS is used for constructing a super-hydrophobic melamine spongy carbon material for carrying out an oil stain adsorption experiment. The oil absorption n is calculated as follows:
wherein M iso(g) And M (g) is the initial mass and the total mass of adsorption saturation of the super-hydrophobic melamine sponge carbon material constructed by PDMS.
Experimental example 1: firstly, 50mL of deionized water is added into a beaker, 50mL of low-density oil (such as soybean oil, cyclohexane, octane and the like) is added into the beaker, 0.1g of PDMS constructed super-hydrophobic melamine sponge carbon material is placed into a mixture containing oil and water, the mixture is taken out after being adsorbed and saturated, the mass of the mixture is weighed, and the oil absorption can be obtained through calculation. The results show that: the PDMS-structured super-hydrophobic melamine spongy carbon material has good adsorption performance on light oil on the surface of a water body.
Experimental example 2: firstly, 50mL of deionized water is added into a beaker, 50mL of high-density oil (such as dichloroethane, carbon tetrachloride and the like) is added into the beaker, 0.1g of PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine sponge carbon material is placed into a mixture containing oil and water, external force is required to be applied in the adsorption process to contact the sponge with the high-density oil, the sponge is taken out after adsorption saturation, the mass of the sponge is weighed, and the oil absorption can be obtained through calculation. The results show that: the PDMS-structured super-hydrophobic melamine spongy carbon material has good adsorption performance on light oil on the surface of a water body.

Claims (7)

1. A one-step preparation method for constructing a super-hydrophobic melamine sponge carbon material by PDMS is characterized by comprising the following steps:
step 1, cleaning melamine sponge: soaking melamine sponge in hydrochloric acid for cleaning, washing with water to neutrality, and drying;
step 2, PDMS loading: soaking the cleaned melamine sponge in a PDMS solution, and drying to obtain PDMS-loaded melamine sponge;
step 3, preparing the PDMS structured super-hydrophobic melamine sponge carbon material, namely placing PDMS-loaded melamine sponge in a tubular furnace, and carbonizing the PDMS-loaded melamine sponge carbon material at a high temperature under the protection of inert gas to obtain the PDMS structured super-hydrophobic melamine sponge carbon material, wherein in the step 2, the used PDMS solution is an alkane mixed solution of PDMS and a curing agent, the alkane is at least one of pentane, hexane, cyclohexane and octane, in the used PDMS solution, the mass of PDMS is 0.1 ~ 5% of that of a solvent, and the mass of the curing agent is 1 ~ 20% of that of PDMS, in the step 3, the high-temperature carbonization temperature is 400 ~ 900 ℃, and the high-temperature carbonization time is 0.05 ~ 2 h.
2. The one-step preparation method of PDMS-made superhydrophobic melamine sponge carbon material according to claim 1, wherein the hydrochloric acid concentration used in step 1 is 0.1 ~ 5mol L-1The soaking temperature is 10 ~ 70 ℃, and the soaking time is 0.5 ~ 5 h.
3. The one-step preparation method of PDMS-structured superhydrophobic melamine spongy carbon material according to claim 1, wherein in step 1, the washing with water is deionized water, distilled water or hot water.
4. The one-step preparation method of PDMS-structured superhydrophobic melamine sponge carbon material according to claim 1, wherein in step 1, the drying is performed at 40 ~ 80 ℃ for 3 ~ 8 h.
5. The one-step preparation method of PDMS-structured superhydrophobic melamine sponge carbon material according to claim 1, wherein in the step 2, the drying is performed at 40 ~ 80 ℃ for 1 ~ 3 h.
6. The one-step preparation method of PDMS-structured superhydrophobic melamine sponge carbon material according to claim 1, wherein in step 3, the inert gas used is nitrogen or argon.
7. Use of a PDMS-structured superhydrophobic melamine spongy carbon material prepared by the method of any one of claims 1 ~ 6 for adsorbing oil stains in a water body.
CN201710364785.4A 2017-05-22 2017-05-22 One-step preparation method and application of PDMS (polydimethylsiloxane) constructed super-hydrophobic melamine spongy carbon material Expired - Fee Related CN107159129B (en)

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