CN109225343A - A kind of delignification wood chip/Fe3O4Composite material and preparation method and application - Google Patents
A kind of delignification wood chip/Fe3O4Composite material and preparation method and application Download PDFInfo
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- CN109225343A CN109225343A CN201811206795.6A CN201811206795A CN109225343A CN 109225343 A CN109225343 A CN 109225343A CN 201811206795 A CN201811206795 A CN 201811206795A CN 109225343 A CN109225343 A CN 109225343A
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- wood chip
- aqueous solution
- delignification
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
Abstract
The invention belongs to the preparation technical fields of catalyst and composite material, and in particular to a kind of delignification wood chip/Fe3O4Composite material and preparation method and application.This method uses sodium chlorite solution or NaOH and Na first2SO3Mixed aqueous solution removal wood chip in lignin, the wood chip for removing lignin is successively then immersed into FeCl3And FeCl2Mixed aqueous solution, in NaOH aqueous solution, make Fe3O4In-situ preparation in wood chip for nano particle to obtain the final product.The catalyst uses timber for raw material, resourceful, easy to handle, flexibility is good and renewable.In addition, the porous of timber itself has suction-operated, and the nanoaperture generated after delignification is conducive to ferroso-ferric oxide in-situ preparation, therefore absorption and the Fe of timber3O4Nanoparticle can play synergistic effect in non-Fenton's reaction, be used for the heterogeneous class Fenton's reaction of efficient catalytic.The preparation process condition of the catalyst is mild, not high to equipment requirement, low in raw material price, no pollution to the environment, and waste liquid is easy recycling, is conducive to industrialized production.
Description
Technical field
The invention belongs to the preparation technical fields of catalyst and composite material, and in particular to a kind of delignification wood chip/Fe3O4
Composite material and preparation method and application.
Background technique
The waste water from dyestuff pollution that weaving, plastics and paper industry cause is the environmental problem of global concern.Currently, environmental law
The processing for strictly making waste water from dyestuff increasingly of rule has mandatory and height restrictive.Fenton oxidation technology (Fenton reaction)
There is efficient, cheap, low toxicity and selection as a kind of high-level oxidation technology (Advanced Oxidation Process, AOP)
The features such as property is small, therefore the extensive concern of domestic and international scientist is caused, it has been applied to the fields such as dye wastewater treatment.Its
In, AOP is the high activity hydroxyl radical free radical by generation come the technology of decomposing organic pollutant.But current Fenton oxidation technology is still
So there are certain limitation, as the hydroxide sludge accumulation on a catalyst of iron causes catalyst to be difficult to regeneration issues.Cause
This, developing into for heterogeneous Fenton-type catalysts more preferably selects.
Heterogeneous Fenton-type catalysts are usually by the ferropexy of various valence states in catalyst carrier (such as clay, aluminium oxide, silicon
Zeolite and carbon material) on.When heterogeneous Fenton or class Fenton's reaction, reaction is typically occurred on solid-liquid interface, and iron is as mineral
Or adion substantially remains in solid catalysis agent carrier.Therefore, a porosity height, with iron compounds bind make good use of and
Recyclable carrier is most important to the reaction efficiency of heterogeneous Fenton or class Fenton and cost control.
Summary of the invention
The primary purpose of the present invention is that providing a kind of delignification wood chip/Fe3O4The preparation method of composite material.This method
Ferroso-ferric oxide is fixed on delignification wood surface, makes suction-operated and the Fe of wood chip3O4Nanoparticle is in Fenton's reaction
Synergistic effect is formed, the catalytic activity of the composite material is greatly improved.
Another object of the present invention is to provide the delignification obtained by above-mentioned preparation method wood chip/Fe3O4Composite material.
A further object of the present invention is to provide above-mentioned delignification wood chip/Fe3O4The application of composite material.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of delignification wood chip/Fe3O4The preparation method of composite material, comprising the following steps:
(1) NaClO is used2Aqueous solution or NaOH and Na2SO3Mixed aqueous solution by wood chip lignin remove, gone
The wood chip of lignin.
(2) wood chip of delignification is immersed into FeCl3And FeCl2Mixed aqueous solution in, take out, then to immerse NaOH water-soluble
In liquid, make in-situ preparation Fe on the wood chip of delignification3O4Nano particle washs to get the delignification wood chip/Fe is arrived3O4
Composite material.
Step uses NaClO described in (1)2Wood chip is preferably soaked the method for the lignin removal in wood chip by aqueous solution
Enter NaClO2In aqueous solution, NaClO is adjusted2Then wood chip is taken out, is washed, done by the pH value of aqueous solution to acidity, heating reaction
It is dry to get arrive the delignification wood chip.
The NaClO2The concentration of aqueous solution is more preferably 1~2wt%.
The conciliation NaClO2The pH value of aqueous solution is to acid method further preferably with acetic acid buffer solution tune
The pH=4.6 of aqueous solution.
The condition of the heating reaction further preferably reacts 6~12h at 80~90 DEG C.
The mode of the washing further preferably successively uses distilled water, dehydrated alcohol and acetone rinsing.
The mode of the drying is further preferably freeze-dried.
NaOH and Na is used described in step (1)2SO3Mixed aqueous solution by wood chip lignin removal method it is excellent
It is selected as wood chip immersing NaOH and Na2SO3Mixed aqueous solution in, heating reaction, then wood chip is taken out, wash, with anhydrous second
Alcohol impregnates, then is placed in the liquid lime chloride of boiling, does not stir, and takes out, rinses after the yellow on wood chip disappears, it is dry to get
To the wood chip of the delignification.
The NaOH and Na2SO3Mixed aqueous solution in, the concentration of NaOH is more preferably 1.5~2.5mol/L,
Na2SO3Concentration be more preferably 0.1~0.4mol/L.
The condition of the heating reaction further preferably reacts 6~12h at 90~100 DEG C.
The mode of the washing is further preferably flushed three times with hot distilled water.
Described is more preferably 3~4 hours with the duration of soaked in absolute ethyl alcohol.
The liquid lime chloride is more preferably the H of concentration 30wt.%2O2。
The mode of the drying is further preferably freeze-dried.
FeCl described in step (2)3And FeCl2The concentration of mixed aqueous solution be preferably 0.01~0.1wt%, wherein
FeCl3And FeCl2Molar ratio be 2:1.
The wood chip of delignification is immersed into FeCl described in step (2)3And FeCl2Mixed aqueous solution in duration it is excellent
It is selected as 5 minutes to 3 hours.
The concentration of NaOH aqueous solution described in step (2) is preferably 0.1~1mol/L.
The duration immersed in NaOH aqueous solution again described in step (2) is preferably 10 minutes to 1 hour.
The present invention further provides a kind of delignification wood chip/Fe obtained by above-mentioned preparation method3O4Composite material, tool
There are nanometer and micro-void, specific surface area is 0.130~2.06m2/ g, Fe3O4Content be 0.01~0.1wt%.
The present invention further provides above-mentioned delignification wood chip/Fe3O4The application of composite material, by the delignification wood chip/
Fe3O4Composite material is for being catalyzed heterogeneous class Fenton's reaction.
Compared with prior art, the present invention having the following advantages and benefits:
The present invention uses timber and prepares for raw material the carrier of catalyst, has the raw material of catalyst resourceful, easy
Processing, the advantages that flexibility is good, renewable.In addition, timber sheet has suction-operated as natural porous material, and go wooden
Wood chip after element more generates nanoaperture, is conducive to the in-situ preparation of ferroso-ferric oxide, therefore absorption and the Fe of timber3O4Nanometer
Particle can play synergistic effect in non-Fenton's reaction.The preparation process condition of the catalyst is mild, not high to equipment requirement, former
Expect cheap, no pollution to the environment, waste liquid is easy recycling, is conducive to industrialized production.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, and embodiments of the present invention are not limited thereto.
For not specifically specified technological parameter, routine techniques progress can refer to.
Embodiment 1
The present embodiment provides a kind of delignification wood chip/Fe3O4Composite material and preparation method.
The preparation method is as follows: wood chip is put into 200mL NaOH containing 1.5mol/L and 0.1mol/LNa2SO3Mixing it is water-soluble
In liquid, stirs 12 hours at 90 DEG C, then washed with hot distilled water, it is rear to use soaked in absolute ethyl alcohol 3 hours, then be with concentration
The H of 30wt%2O2In the case where boiling is not stirred, reaction is until the removal of wood chip yellow.Wood chip is taken out, after being washed with deionized
Freeze-drying, obtains the wood chip of the white delignification containing nanometer and micro-void.The wood chip of delignification is immersed into concentration
For the FeCl of 0.01wt%3And FeCl2Mixed aqueous solution in (FeCl3And FeCl2Molar ratio be 2:1) 3 hours, then again
It immerses in the NaOH aqueous solution that concentration is 0.1mol/L 1 hour, in-situ preparation Fe3O4Nano particle is washed to get delignification is arrived
Wood chip/Fe3O4Composite material.
Gained composite material surface adheres to the magnetic Fe of black bands3O4, BET specific surface area is about 1.35m2/g。
Embodiment 2
The present embodiment provides a kind of delignification wood chip/Fe3O4Composite material and preparation method.
The preparation method is as follows: wood chip is put into 200mL NaOH containing 2.5mol/L and 0.4mol/L Na2SO3Mixing it is water-soluble
In liquid, stirs 6 hours at 100 DEG C, then washed with hot distilled water, it is rear to use soaked in absolute ethyl alcohol 4 hours, then be with concentration
The H of 30wt%2O2In the case where boiling is not stirred, reaction is until the removal of wood chip yellow.Wood chip is taken out, after being washed with deionized
Freeze-drying, obtains the wood chip of the white delignification containing nanometer and micro-void.The wood chip of delignification is immersed into concentration
For the FeCl of 0.1wt%3And FeCl2Mixed aqueous solution in (FeCl3And FeCl2Molar ratio be 2:1) 2 hours, then soak again
Enter in the NaOH aqueous solution that concentration is 1mol/L 10 minutes, in-situ preparation Fe3O4Nano particle, washing is to get wooden to delignification
Piece/Fe3O4Composite material.
Gained composite material surface adheres to the magnetic Fe of black bands3O4, BET specific surface area is about 2.06m2/g。
Embodiment 3
The present embodiment provides a kind of delignification wood chip/Fe3O4Composite material and preparation method.
The preparation method is as follows: wood chip is put into the sodium chlorite aqueous solution of 1wt%, pH=4.6 is adjusted with acetic acid, 80
It stirs 6 hours at DEG C, is then successively washed with distilled water, dehydrated alcohol, acetone, be freeze-dried, delignification can be obtained
Wood chip.The wood chip of delignification is immersed into the FeCl that concentration is 0.01wt%3And FeCl2Mixed aqueous solution in (FeCl3With
FeCl2Molar ratio be 2:1) 5 minutes, then immerse again in aqueous solution containing 1wt%NaOH 10 minutes, in-situ preparation Fe3O4Nanometer
Particle is washed to get delignification wood chip/Fe is arrived3O4Composite material.
Gained composite material surface adheres to the magnetic Fe of black bands3O4, BET specific surface area is about 0.13m2/g。
Embodiment 4
The present embodiment provides a kind of delignification wood chip/Fe3O4Composite material and preparation method.
The preparation method is as follows: wood chip is put into the sodium chlorite aqueous solution of 2wt%, pH=4.6 is adjusted with acetic acid, 90
It stirs 12 hours at DEG C, is then successively washed with distilled water, dehydrated alcohol, acetone, be freeze-dried, delignification can be obtained
Wood chip.The wood chip of delignification is immersed into the FeCl that concentration is 0.1wt%3And FeCl2Mixed aqueous solution in (FeCl3With
FeCl2Molar ratio be 2:1) 3 hours, then immerse again in aqueous solution containing 1wt%NaOH 1 hour, in-situ preparation Fe3O4Nanometer
Particle is washed to get delignification wood chip/Fe is arrived3O4Composite material.
Gained composite material surface adheres to the magnetic Fe of black bands3O4, BET specific surface area is about 1.95m2/g。
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of delignification wood chip/Fe3O4The preparation method of composite material, which comprises the following steps:
(1) NaClO is used2Aqueous solution or NaOH and Na2SO3Mixed aqueous solution by wood chip lignin remove, obtain wooden
The wood chip of element；
(2) wood chip of delignification is immersed into FeCl3And FeCl2Mixed aqueous solution in, take out, then immerse in NaOH aqueous solution,
Make in-situ preparation Fe on the wood chip of delignification3O4Nano particle washs to get the delignification wood chip/Fe is arrived3O4It is compound
Material.
2. delignification wood chip/Fe according to claim 13O4The preparation method of composite material, it is characterised in that: step (1)
Described in use NaClO2The method of lignin removal in wood chip is that wood chip is immersed NaClO by aqueous solution2In aqueous solution, adjust
Save NaClO2Then wood chip is taken out, is washed by the pH value of aqueous solution to acidity, heating reaction, dry to remove wood to get to described
The wood chip of quality.
3. delignification wood chip/Fe according to claim 23O4The preparation method of composite material, it is characterised in that:
The NaClO2The concentration of aqueous solution is 1~2wt%；
The conciliation NaClO2The pH value of aqueous solution to acid method is the pH=that aqueous solution is adjusted with acetic acid buffer solution
4.6；
The condition of the heating reaction is that 6~12h is reacted at 80~90 DEG C；
The mode of the washing is successively to use distilled water, dehydrated alcohol and acetone rinsing；
The mode of the drying is freeze-drying.
4. delignification wood chip/Fe according to claim 13O4The preparation method of composite material, it is characterised in that: step (1)
Described in use NaOH and Na2SO3Mixed aqueous solution by wood chip lignin removal method be by wood chip immerse NaOH with
Na2SO3Mixed aqueous solution in, then wood chip is taken out, is washed, with soaked in absolute ethyl alcohol, then is placed in boiling by heating reaction
It in liquid lime chloride, does not stir, takes out, rinse after the yellow on wood chip disappears, it is dry to get the wood for arriving the delignification
Piece.
5. delignification wood chip/Fe according to claim 43O4The preparation method of composite material, it is characterised in that:
The NaOH and Na2SO3Mixed aqueous solution in, the concentration of NaOH is 1.5~2.5mol/L, Na2SO3Concentration be
0.1~0.4mol/L；
The condition of the heating reaction is that 6~12h is reacted at 90~100 DEG C；
The mode of the washing is to be flushed three times with hot distilled water；
It is described with soaked in absolute ethyl alcohol when it is 3~4 hours a length of；
The liquid lime chloride is the H of concentration 30wt%2O2；
The mode of the drying is freeze-drying.
6. delignification wood chip/Fe according to claim 13O4The preparation method of composite material, it is characterised in that: step (2)
Described in FeCl3And FeCl2The concentration of mixed aqueous solution be 0.01~0.1wt%, wherein FeCl3And FeCl2Molar ratio
For 2:1.
7. delignification wood chip/Fe according to claim 13O4The preparation method of composite material, it is characterised in that: step (2)
Described in the wood chip of delignification is immersed into FeCl3And FeCl2Mixed aqueous solution in when it is 5 minutes to 3 hours a length of.
8. delignification wood chip/Fe according to claim 13O4The preparation method of composite material, it is characterised in that:
The concentration of NaOH aqueous solution described in step (2) is 0.1~1mol/L；
Immersed again described in step (2) in NaOH aqueous solution when it is 10 minutes to 1 hour a length of.
9. a kind of delignification wood chip/Fe3O4Composite material, it is characterised in that: by any one of claim 1~8 preparation method
It obtains, with nanometer and micro-void, specific surface area is 0.130~2.06m2/ g, Fe3O4Content be 0.01~
0.1wt%.
10. delignification wood chip/Fe as claimed in claim 93O4The application of composite material, it is characterised in that: by the delignification wood
Piece/Fe3O4Composite material is for being catalyzed heterogeneous class Fenton's reaction.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109986665A (en) * | 2019-04-04 | 2019-07-09 | 南京林业大学 | A kind of high conductivity high-flexibility nickel plating wood chip and preparation method thereof |
| CN110931266A (en) * | 2019-11-12 | 2020-03-27 | 陕西科技大学 | 3D flowering rod-shaped nickel sulfide/wood electrode material and preparation method and application thereof |
| CN111463028A (en) * | 2020-04-09 | 2020-07-28 | 陕西科技大学 | rGO-L iOH micro-spring/wood composite electrode material, and preparation method and application thereof |
| CN112657494A (en) * | 2020-12-08 | 2021-04-16 | 汕头大学 | Iron oxide yellow/carbonized wood composite membrane Fenton catalyst, preparation method and application thereof |
| CN113060719A (en) * | 2021-03-17 | 2021-07-02 | 山东省科学院新材料研究所 | Wood-based carbon foam and preparation method thereof, cathode electrocatalyst, cathode and metal-air battery |
| CN113334515A (en) * | 2021-06-11 | 2021-09-03 | 浙江农林大学 | Processing method for adjusting chromatic aberration of wood veneer |
| CN113558264A (en) * | 2021-07-06 | 2021-10-29 | 中国农业科学院油料作物研究所 | Preparation method of nutrient-loaded wood-based reel, product and application thereof |
| CN114851332A (en) * | 2022-05-31 | 2022-08-05 | 东北林业大学 | Preparation method of wood robot with magnetic anisotropy |
| CN115283213A (en) * | 2022-08-19 | 2022-11-04 | 浙江农林大学 | Inductor and electromagnetic shielding synergistic wood, and preparation method and application thereof |
| CN115367857A (en) * | 2022-07-28 | 2022-11-22 | 南京大学 | Method for promoting degradation of organic pollutants by heterogeneous Fenton-like technology through sulfite |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109986665A (en) * | 2019-04-04 | 2019-07-09 | 南京林业大学 | A kind of high conductivity high-flexibility nickel plating wood chip and preparation method thereof |
| CN110931266A (en) * | 2019-11-12 | 2020-03-27 | 陕西科技大学 | 3D flowering rod-shaped nickel sulfide/wood electrode material and preparation method and application thereof |
| CN110931266B (en) * | 2019-11-12 | 2021-04-20 | 陕西科技大学 | 3D flowering rod-shaped nickel sulfide/wood electrode material and preparation method and application thereof |
| CN111463028A (en) * | 2020-04-09 | 2020-07-28 | 陕西科技大学 | rGO-L iOH micro-spring/wood composite electrode material, and preparation method and application thereof |
| CN111463028B (en) * | 2020-04-09 | 2021-06-29 | 陕西科技大学 | rGO-LiOH micro-spring/wood composite electrode material and preparation method and application thereof |
| CN112657494A (en) * | 2020-12-08 | 2021-04-16 | 汕头大学 | Iron oxide yellow/carbonized wood composite membrane Fenton catalyst, preparation method and application thereof |
| CN113060719A (en) * | 2021-03-17 | 2021-07-02 | 山东省科学院新材料研究所 | Wood-based carbon foam and preparation method thereof, cathode electrocatalyst, cathode and metal-air battery |
| CN113334515A (en) * | 2021-06-11 | 2021-09-03 | 浙江农林大学 | Processing method for adjusting chromatic aberration of wood veneer |
| CN113558264A (en) * | 2021-07-06 | 2021-10-29 | 中国农业科学院油料作物研究所 | Preparation method of nutrient-loaded wood-based reel, product and application thereof |
| CN113558264B (en) * | 2021-07-06 | 2022-07-19 | 中国农业科学院油料作物研究所 | Preparation method of nutrient-loaded wood-based reel, product and application thereof |
| CN114851332A (en) * | 2022-05-31 | 2022-08-05 | 东北林业大学 | Preparation method of wood robot with magnetic anisotropy |
| CN114851332B (en) * | 2022-05-31 | 2023-02-17 | 东北林业大学 | Preparation method of wood robot with magnetic anisotropy |
| CN115367857A (en) * | 2022-07-28 | 2022-11-22 | 南京大学 | Method for promoting degradation of organic pollutants by heterogeneous Fenton-like technology through sulfite |
| CN115283213A (en) * | 2022-08-19 | 2022-11-04 | 浙江农林大学 | Inductor and electromagnetic shielding synergistic wood, and preparation method and application thereof |
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