CN106540696A - A kind of method prepared by rice husk base metal supported catalyst mesoporous silicon oxide - Google Patents
A kind of method prepared by rice husk base metal supported catalyst mesoporous silicon oxide Download PDFInfo
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- CN106540696A CN106540696A CN201611006071.8A CN201611006071A CN106540696A CN 106540696 A CN106540696 A CN 106540696A CN 201611006071 A CN201611006071 A CN 201611006071A CN 106540696 A CN106540696 A CN 106540696A
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- rice husk
- silicon oxide
- mesoporous silicon
- supported catalyst
- extract
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
Abstract
The present invention relates to a kind of method prepared by rice husk base metal supported catalyst mesoporous silicon oxide.Mainly explore the loaded mesoporous silica of iron optimum preparating condition and in waste water from dyestuff degradation property research.With rice husk as silicon source, with ferric nitrate as source of iron, the mesoporous silicon oxide of load iron, the mesoporous silicon oxide good dispersion size uniformity of supported catalyst, with larger specific surface area and pore volume are prepared using the synergy of lignin in rice husk and polyethylene glycol.Activated carbon from biomass material of the present invention has flourishing pore passage structure and very high specific surface area, and the invention activated carbon from biomass preparation method simple possible, environmental pollution are little, and raw material sources extensively, easily realize industrialized production.
Description
Technical field
This patent relate to a kind of method prepared by rice husk base metal supported catalyst mesoporous silicon oxide, and in particular to
Rice husk is silicon source, with ferric nitrate as source of iron, prepares carried metal using the synergy of lignin in rice husk and polyethylene glycol
Catalyst mesoporous silicon oxide.
Background technology
The science and technology for developing rapidly has promoted the made rapid progress of industry and development, the large quantity of exhaust gas of its discharge, waste liquid, useless
Slag causes huge harm to human health and ecological environment.Especially dye industry, produces during its production and use
Raw waste water accounts for 2% of national wastewater emission amount or so, it has also become main pollution entering the water.The dyestuff yield of China occupies generation
Boundary prostatitis, often produces 1t dyestuffs and will produce about 700m3Waste water, additionally, a large amount of waste water that can also produce during its use.
Contain contents of many kinds of heavy metal ion in waste water from dyestuff, and its constituent is most of for high-molecular complex, stable chemical nature hardly possible
With natural degradation, belong to one of waste water of refractory reason.More seriously, waste water from dyestuff contains a large amount of toxic components, can make life
Thing is carcinogenic and gene mutation, is directly discharged in environment, natural environment can be caused greatly if these waste water are unprocessed
Harm.Additionally, China freshwater resources occupancy volume per person is only the 1/4 of world average level less, freshwater resources famine.Cause
This must seek effective method to process waste water from dyestuff.Fenton oxidation method is most typical a kind of catalysis in advanced oxidation processes
Oxidation technology, compared with other advanced oxidation processes, Fenton catalytic oxidations degradation rate is fast, strong antijamming capability, applicable model
Enclose wide, and final product is O2And H2O, environmentally safe, therefore Fenton catalytic oxidations are considered as most should at present
With the wastewater processing technology of prospect.The essence of Fenton reactions is Fe2+And H2O2Reaction generates hydroxyl radical free radical OH, OH tools
There are higher oxidizing electrode current potential, electronegativity and electron affinity energy, therefore with extremely strong oxidisability.Can be difficult by general oxidizing process
With degrade, baroque organic matter degradation as CO2、H2The simple inorganic matter such as O and inorganic ions.The mechanism of Fenton reactions
Belong to radical reaction.Heterogeneous Fenton oxidation technology degradation efficiency is high, H2O2Consumption is low, pH value is applied widely and
Catalyst reusable edible.Heterogeneous Fenton oxidation technology is to replace homogeneous Fenton oxidation skill with the solid catalyst of iron content
Fe in art reactant liquor2+A kind of catalytic oxidation technologies.Heterogeneous Fenton catalyst can be divided into according to the carrier of catalyst
Two big class of organic carrier type and inorganic carrier type.Mesoporous material as a kind of new nano material, with larger specific surface
Product and pore volume, regular neat and adjustable pore passage structure.Based on these advantages of mesoporous material, mesoporous material gives up in process dyestuff
Have been a great concern in terms of the organic matter of water removal difficult for biological degradation.Rice husk be rice production process Main By product it
One, the annual production of China's rice husk reaches about 40,000,000 tons.As the nutriment of rice husk is few, content of ashes is high, hardness is big, at present
Its producing level is relatively low.Most rice husk is taken as agricultural waste to discard, and causes serious pollution and waste.In rice husk about
Containing 20% silica, pollution problem of the rice husk to environment is not only solved using rice husk production mesoporous silicon oxide, moreover it is possible to
Bring considerable economic benefit.Meso-porous nano silica has larger specific surface area and pore volume, can faster, evenly
It is distributed in solution, can complements each other enhancing degradation capability with Fenton catalyst.This patent is devoted to rice husk as silicon source
The preparation of mesoporous silicon oxide and study on the modification, it is intended to prepare the efficient of heterogeneous Fenton catalytic degradation methylene blue dye
Catalyst.
The content of the invention
To realize that technical scheme provided by the present invention is：
(1) pretreatment of rice husk and sodium metasilicate extract
The rice husk of certain mass is weighed, is immersed in 5% acid solution, solid-to-liquid ratio is 1: 10, be placed in water-bath, 80 DEG C
Lower constant temperature 6h, is cooled to room temperature, and separation of solid and liquid, solid deionized water are washed till neutrality, in 100 DEG C of baking 12h of air dry oven, claims
Take the rice husk after the low-kappa number of a certain amount of drying to be immersed in 5% aqueous slkali, flow back at 100 DEG C 6h, separation of solid and liquid institute
It is containing alkali lignin and sodium metasilicate extract to obtain filtrate；
(2) preparation of silica supported metal catalyst
The extract that 50ml contains sodium metasilicate and alkali lignin is measured, extract, distilled water, ethanol press certain volume ratio
It is put in 250ml there-necked flask flasks, 80 DEG C of water-baths simultaneously stir acid-conditioning solution pH to 9 with 5%, add polyethylene glycol, poly- second
The Mr of glycol is 2000～20000, and the quality of polyethylene glycol is the 30% of the quality of silica in extract, constant temperature 0.5h,
Continue to adjust pH to 7, be subsequently adding molysite, the amount of molysite is 0～20% of silica quality in extract, is slowly added dropwise simultaneously
It is quick to stir, continue reaction 0.5h, adjust pH and be respectively 3～6, continue reaction 3h, solid is washed by separation of solid and liquid, deionized water
To neutrality, in air dry oven, 100 DEG C of baking 12h, are then put into the product of drying in mortar and smash, be put into Muffle furnace
In 600 DEG C calcining 2h, that is, obtain silica supported metal catalyst.
To be best understood from the present invention, the present invention is done with reference to embodiment and further described in detail, but it is of the invention
Claimed scope is not limited to the scope that embodiment is represented.
Embodiment 1：
(1) pretreatment of rice husk and sodium metasilicate extract
The rice husk of certain mass is weighed, is immersed in 5% acid solution, solid-to-liquid ratio is 1: 10, be placed in water-bath, 80 DEG C
Lower constant temperature 6h, is cooled to room temperature, and separation of solid and liquid, solid deionized water are washed till neutrality, in 100 DEG C of baking 12h of air dry oven, claims
Take the rice husk after the low-kappa number of a certain amount of drying to be immersed in 5% aqueous slkali, flow back at 100 DEG C 6h, separation of solid and liquid institute
It is containing alkali lignin and sodium metasilicate extract to obtain filtrate；
(2) preparation of silica supported metal catalyst
The extract that 50ml contains sodium metasilicate and alkali lignin is measured, extract, distilled water, ethanol press certain volume ratio
It is put in 250ml there-necked flask flasks, 80 DEG C of water-baths simultaneously stir acid-conditioning solution pH to 9 with 5%, add polyethylene glycol, poly- second
The Mr of glycol is 2000, the quality of polyethylene glycol be the quality of silica in extract for 10%, constant temperature 0.5h, continue to adjust
Section pH is subsequently adding ferric nitrate to 7, and the amount of ferric nitrate is 10% of silica quality in extract, is slowly added dropwise and quick
Stirring, continues reaction 0.5h, adjusts pH and is respectively 5, continues reaction 3h, and solid is washed till neutrality by separation of solid and liquid, deionized water,
In air dry oven, 100 DEG C of baking 12h, are then put into the product of drying in mortar and smash, be put into 600 DEG C in Muffle furnace
Calcining 2h, that is, obtain metal supported catalyst mesoporous silicon oxide.
Embodiment 2：The Mr for changing polyethylene glycol is 4000, and other steps obtain metal supported catalyst Jie with embodiment 1
Hole silica.
Embodiment 3：Change molysite amount be silica in extract quality 20%, other steps with embodiment 1,
Obtain metal supported catalyst mesoporous silicon oxide.
Embodiment 4：The pH for changing final reaction is 6, and other steps obtain metal supported catalyst mesoporous with embodiment 1
Silica.
Claims (2)
1. a kind of method that prepared by rice husk base metal supported catalyst mesoporous silicon oxide, comprises the following steps that：
(1) pretreatment of rice husk and sodium metasilicate extract
The rice husk of certain mass is weighed, is immersed in 5% acid solution, solid-to-liquid ratio is 1: 10, be placed in water-bath, it is permanent at 80 DEG C
Warm 6h, is cooled to room temperature, and separation of solid and liquid, solid deionized water are washed till neutrality, in 100 DEG C of baking 12h of air dry oven, weighs one
Rice husk after the low-kappa number of quantitative drying is immersed in 5% aqueous slkali, and flow back at 100 DEG C 6h, is filtered obtained by separation of solid and liquid
Liquid is containing alkali lignin and sodium metasilicate extract；
(2) preparation of metal supported catalyst mesoporous silicon oxide
The extract that 50ml contains sodium metasilicate and alkali lignin is measured, extract, distilled water, ethanol are put into by certain volume ratio
In 250ml there-necked flask flasks, 80 DEG C of water-baths simultaneously stir acid-conditioning solution pH to 9 with 5%, add polyethylene glycol, polyethylene glycol
Mr be 2000～20000, the quality of polyethylene glycol be the quality of silica in extract for 30%, constant temperature 0.5h, after
The continuous pH that adjusts is subsequently adding molysite to 7, and the amount of molysite is 0～20% of silica quality in extract, is slowly added dropwise and fast
Speed stirring, continues reaction 0.5h, adjusts pH and is respectively 3～6, continues reaction 3h, and solid is washed till by separation of solid and liquid, deionized water
Neutrality, in air dry oven, 100 DEG C of baking 12h, are then put into the product of drying in mortar and smash, be put in Muffle furnace
600 DEG C of calcining 2h, that is, obtain metal supported catalyst mesoporous silicon oxide.
2. a kind of method that prepared by a kind of rice husk base metal supported catalyst mesoporous silicon oxide as claimed in claim 1, its
It is characterised by：Molysite can be ferric nitrate, ferric acetate, ferric sulfate, iron chloride.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117487515A (en) * | 2023-12-27 | 2024-02-02 | 甬江实验室 | Composite polishing abrasive particles with catalytic activity and preparation method thereof |
| CN117487515B (en) * | 2023-12-27 | 2024-05-03 | 甬江实验室 | Composite polishing abrasive particles with catalytic activity and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804988A (en) * | 2010-05-05 | 2010-08-18 | 吉林大学 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
| CN102145280A (en) * | 2011-02-15 | 2011-08-10 | 常州大学 | Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material |
| CN102701297A (en) * | 2012-05-29 | 2012-10-03 | 华南师范大学 | Mesoporous silicon dioxide microsphere-loaded zero-valent iron nanoparticle (SiO2@ FeOOH@ Fe) and preparation method and application thereof |
| CN104907021A (en) * | 2015-06-01 | 2015-09-16 | 天津工业大学 | Preparation method of porous silicon dioxide pellets loaded with metal catalyst under synergistic effect |
| CN105435764A (en) * | 2015-11-19 | 2016-03-30 | 上海应用技术学院 | Compound mesoporous photocatalyst and preparation method thereof |
-
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- 2016-11-14 CN CN201611006071.8A patent/CN106540696A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101804988A (en) * | 2010-05-05 | 2010-08-18 | 吉林大学 | Novel method for preparing silicon dioxide and active carbon from rice hull ash |
| CN102145280A (en) * | 2011-02-15 | 2011-08-10 | 常州大学 | Method for preparing rice hull active carbon/silicon dioxide/titanium dioxide composite material |
| CN102701297A (en) * | 2012-05-29 | 2012-10-03 | 华南师范大学 | Mesoporous silicon dioxide microsphere-loaded zero-valent iron nanoparticle (SiO2@ FeOOH@ Fe) and preparation method and application thereof |
| CN104907021A (en) * | 2015-06-01 | 2015-09-16 | 天津工业大学 | Preparation method of porous silicon dioxide pellets loaded with metal catalyst under synergistic effect |
| CN105435764A (en) * | 2015-11-19 | 2016-03-30 | 上海应用技术学院 | Compound mesoporous photocatalyst and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117487515A (en) * | 2023-12-27 | 2024-02-02 | 甬江实验室 | Composite polishing abrasive particles with catalytic activity and preparation method thereof |
| CN117487515B (en) * | 2023-12-27 | 2024-05-03 | 甬江实验室 | Composite polishing abrasive particles with catalytic activity and preparation method thereof |
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