CN106115726A - A kind of preparation method of ferrum carbon modified mesoporous molecular sieve - Google Patents
A kind of preparation method of ferrum carbon modified mesoporous molecular sieve Download PDFInfo
- Publication number
- CN106115726A CN106115726A CN201610440274.1A CN201610440274A CN106115726A CN 106115726 A CN106115726 A CN 106115726A CN 201610440274 A CN201610440274 A CN 201610440274A CN 106115726 A CN106115726 A CN 106115726A
- Authority
- CN
- China
- Prior art keywords
- preparation
- molecular sieve
- ferrum carbon
- hydrogel
- alkali
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/026—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses the preparation method of a kind of ferrum carbon modified mesoporous molecular sieve.The present invention specifically comprises the following steps that mesopore molecular sieve, alkali and water are mixed by (1), or silicon source, aluminum source, alkali and water is mixed, and makes hydrogel；(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；(4) product is calcined, i.e. prepare ferrum carbon modified mesoporous molecular sieve.Compared with prior art, mesopore molecular sieve is modified by the present invention by adding ferrum carbon, substantially increases the efficiency of composite degradation organic pollution, and preparation process is simple, and motility is high, and silica alumina ratio adjustable extent is relatively big, has good application prospect.
Description
Technical field
The invention belongs to modified mesoporous molecular sieve technical field, especially relate to the system of a kind of ferrum carbon modified mesoporous molecular sieve
Preparation Method.
Background technology
Along with agricultural and the fast development of industry, create substantial amounts of waste water, natural environment and human body etc. are caused pole
Big harm.Agricultural and industrial wastewater rich in pollutant, such as Organic substance.These organic compound enter water by different approaches
Environment, becomes the nutrient of algal grown, causes algal bloom, produces wawter bloom phenomenon.Animal husbandry, city and agricultural are useless
Water, industrial wastewater all can increase the organic concentration in water environment.The organic wastewater of organic wastewater, particularly high concentration comes
Source is many, discharge capacity is big, unprocessed or process incomplete organic wastewater and can cause greatly harm to environment.The most highly concentrated
The process of the organic wastewater of degree enjoys the concern of people.Mainly there are coking chemical waste water, coal gas in the source of high-concentration organic substance wastewater
Waste water, gourmet powder waste water, fertilizer waste water, percolate and breeding wastewater anaerobic nitrification liquid etc..
Absorption method is one of effective ways of organics removal, especially the Technical comparing of mesopore molecular sieve organics removal
Generally.Although mesopore molecular sieve organics removal effect is preferable, but it is disadvantageous in that removal capacity is less, causes removing height
The dosage of concentration organic is bigger, adds freight.Therefore, mesopore molecular sieve exists bigger in actual applications
Problem.
Summary of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of by iron-carbon micro-electrolysis and mesoporous molecular
The preparation method of the ferrum carbon modified mesoporous molecular sieve that the absorption property of sieve combines.Preparation method of the present invention is simple, the ferrum obtained
Carbon modified mesoporous molecular sieve can be effectively improved it to organic removal capacity.
The present invention provides the preparation method of a kind of ferrum carbon modified mesoporous molecular sieve, specifically comprises the following steps that
(1) mesopore molecular sieve is mixed with alkali in water, or silicon source, aluminum source and alkali are mixed in water, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined, i.e. prepare ferrum carbon modified mesoporous molecular sieve.
In above-mentioned steps (1), mesopore molecular sieve is selected from one or more of MCM-41, MCM-48, KIT-6 or SBA-15；
Described alkali is sodium hydroxide or potassium hydroxide.Described silicon source is selected from Ludox, waterglass or organo-silicon compound；Described
Aluminum source selected from sodium metaaluminate, boehmite or aluminum isopropylate..
In above-mentioned steps (1), the inventory of mesopore molecular sieve is 0.01-0.05g/mL water.
In above-mentioned steps (1), silicon source, aluminum source are converted into SiO2And Al2O3, SiO2And Al2O3Mol ratio be 10:1-50:
1。
In above-mentioned steps (1), when silicon source, aluminum source and alkali mix in water, it is additionally added surfactant；Preferably, surface
Activating agent is C16TMABr, silicon source, aluminum source are converted into SiO2And Al2O3, (SiO2+Al2O3): alkali: C16TMABr:H2The mol ratio of O
For 1:(0.05-0.5): (0.01-0.3): (80-200).
In above-mentioned steps (1), hydrogel reacts preparation in 7 hours～36 hours at a temperature of room temperature～100 DEG C.
In above-mentioned steps (2), ferrum carbon is 1:20～5:1 with the mass ratio of hydrogel.
In above-mentioned steps (3), crystallization is carried out under 80 DEG C～150 DEG C of temperature, self-generated pressures, crystallization time be 3 hours～
10 days.
In above-mentioned steps (4), calcination condition is: in 300-700 DEG C, under atmospheric pressure calcine, and the control time is 2-
12 hours.
Compared with prior art, the beneficial effects of the present invention is:
Preparation process is simple, and motility is high, and silica alumina ratio adjustable extent is bigger.
The modified mesoporous molecular sieve that the present invention prepares has magnetic, can be separated from sewage by magnetic separation technique
Out, modified mesoporous molecular sieve is except carrying out high-enriched organics removal, it is also possible to for technical fields such as catalytic cracking.
Compared with unmodified front mesopore molecular sieve, the organic matter removal capacity of ferrum carbon modified mesoporous molecular sieve substantially increases
Greatly, and along with the increase of ferrum carbon dosage increase.
Accompanying drawing explanation
Fig. 1 is that the material of embodiment 1, embodiment 2, embodiment 3 and embodiment 4 preparation is to 30mL 1 × 10-5mol L-1Sub-
The clearance diagram of methyl blue.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
By 8.2g MCM-41 and 40g NaOH in 200mL water, after stirring 9 hours under the conditions of 100 DEG C, form water-setting
Glue.Ferrum carbon is mixed homogeneously with hydrogel, and ferrum carbon is 1:2 with the mass ratio of hydrogel, carries out under 105 DEG C and self-generated pressure
Crystallization 24 hours, then carry out separating, wash, be dried.Finally, in atmospheric conditions, carry out under the conditions of 550 DEG C calcining 4 hours,
To ferrum carbon modified mesoporous molecular sieve.
Embodiment 2
By 15.5g MCM-48 and 20g NaOH in 100mL water, stir 4 hours under the conditions of 120 DEG C, form water-setting
Glue.Ferrum carbon is mixed homogeneously with hydrogel, and ferrum carbon is 1:4 with the mass ratio of hydrogel, carries out under 110 DEG C and self-generated pressure
Crystallization 10 hours, then carry out separating, wash, be dried.Finally, in atmospheric conditions, carry out under the conditions of 500 DEG C calcining 5 hours,
To ferrum carbon modified mesoporous molecular sieve.
Embodiment 3
A kind of preparation method of ferrum carbon modified mesoporous molecular sieve, employing following steps:
(1) by silicon source, aluminum source C16TMABr, alkali mix in proportion in water, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined under the high temperature conditions, i.e. prepare ferrum carbon modified mesoporous molecular sieve.
In step (1), silicon source is Ludox, and aluminum source is sodium metaaluminate, (SiO in hydrogel2+Al2O3):NaOH:
C16TMABr:H2The mol ratio of O is 1:0.5:0.06:200.Wherein, SiO2:Al2O3Mol ratio be 20:1.
In step (2), ferrum carbon is 1:2 with the mass ratio of hydrogel.
In step (3), the condition of Crystallizing treatment is: carry out crystallization under 120 DEG C and self-generated pressure, and the control time is 10 little
Time.
The condition of the calcination processing described in step (4) is: in 600 DEG C, calcine under a nitrogen atmosphere, controls the time
It it is 3 hours.
Embodiment 4
A kind of preparation method of ferrum carbon modified mesoporous molecular sieve, employing following steps:
(1) by silicon source, aluminum source, C16TMABr, alkali mix in proportion in water, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined under the high temperature conditions, i.e. prepare ferrum carbon modified mesoporous molecular sieve.
In step (1), silicon source is Ludox, and aluminum source is sodium metaaluminate, (SiO in hydrogel2+Al2O3):NaOH:
C16TMABr:H2The mol ratio of O is 1:0.05:0.2:100.Wherein, SiO2:Al2O3Mol ratio be 40:1.
In step (2), ferrum carbon is 1:4 with the mass ratio of hydrogel.
In step (3), the condition of Crystallizing treatment is: carry out crystallization under 100 DEG C and self-generated pressure, and the control time is 5 little
Time.
The condition of the calcination processing described in step (4) is: in 400 DEG C, calcine under a nitrogen atmosphere, controls the time
It it is 10 hours.
Embodiment 5
A kind of preparation method of ferrum carbon modified mesoporous molecular sieve, employing following steps:
(1) silicon source and aluminum source are mixed with aqueous slkali in proportion, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined under the high temperature conditions, i.e. prepare described nanometer silver/titanium dioxide-zeolite hybridization and be situated between
Porous molecular sieve composite.
In step (1), silicon source is Ludox, and aluminum source is sodium metaaluminate, (SiO in hydrogel2+Al2O3):NaOH:
C16TMABr:H2The mol ratio of O is 1:0.15:0.05:200.Wherein, SiO2:Al2O3Mol ratio be 30:1.
In step (2), ferrum carbon is 1:4 with the mass ratio of hydrogel.
In step (3), the condition of Crystallizing treatment is: carry out crystallization under 130 DEG C and self-generated pressure, and the control time is 18 little
Time.
The condition of the calcination processing described in step (4) is: in 500 DEG C, calcine under a nitrogen atmosphere, controls the time
It it is 6 hours.
Embodiment 6
A kind of preparation method of ferrum carbon modified mesoporous molecular sieve, employing following steps:
(1) just silicon source and aluminum source mix with aqueous slkali in proportion, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined under the high temperature conditions, i.e. prepare described nanometer silver/titanium dioxide-zeolite hybridization and be situated between
Porous molecular sieve composite.
In step (1), silicon source is Ludox, and aluminum source is sodium metaaluminate, (SiO in hydrogel2+Al2O3):NaOH:
C16TMABr:H2The mol ratio of O is 1:0.05:0.3:80.Wherein, SiO2:Al2O3Mol ratio be 50:1.
In step (2), ferrum carbon is 1:3 with the mass ratio of hydrogel.
In step (3), the condition of Crystallizing treatment is: carry out crystallization under 120 DEG C and self-generated pressure, and the control time is 8 little
Time.
The condition of the calcination processing described in step (4) is: in 550 DEG C, calcine under a nitrogen atmosphere, controls the time
It it is 12 hours.
Application Example
It is that the material prepared of embodiment 1, embodiment 2, embodiment 3 and embodiment 4 is to 30mL 1 × 10 by Fig. 1-5mol L-1
Methylene blue is removed, and result is as shown in Figure 1.
Claims (10)
1. the preparation method of a ferrum carbon modified mesoporous molecular sieve, it is characterised in that specifically comprise the following steps that
(1) mesopore molecular sieve is mixed with alkali in water, or silicon source, aluminum source and alkali are mixed in water, make hydrogel；
(2) ferrum carbon is joined in hydrogel, mix homogeneously, prepare mixed gel；
(3) mixed gel is carried out Crystallizing treatment, after crystallization terminates, carry out separating, wash and being dried by product；
(4) product is calcined, i.e. prepare ferrum carbon modified mesoporous molecular sieve.
Preparation method the most according to claim 1, it is characterised in that in step (1), mesopore molecular sieve selected from MCM-41,
One or more of MCM-48, KIT-6 or SBA-15；Described alkali is sodium hydroxide or potassium hydroxide；Described silicon source choosing
From Ludox, waterglass or organo-silicon compound；Described aluminum source is selected from sodium metaaluminate, boehmite or aluminum isopropylate..
Preparation method the most according to claim 1, it is characterised in that in step (1), the inventory of mesopore molecular sieve is
0.05-0.1g/mL water.
Preparation method the most according to claim 1, it is characterised in that in step (1), silicon source, aluminum source are converted into SiO2With
Al2O3, SiO2And Al2O3Mol ratio be 10:1-50:1.
Preparation method the most according to claim 1, it is characterised in that in step (1), silicon source, aluminum source and alkali are mixed in water
During conjunction, it is additionally added surfactant.
Preparation method the most according to claim 5, it is characterised in that surfactant is C16TMABr, silicon source, aluminum source are changed
It is counted as SiO2And Al2O3, SiO2+Al2O3, alkali, C16TMABr and H2The mol ratio of O is 1:(0.05-0.5): (0.01-0.3):
(80-200)。
Preparation method the most according to claim 1, it is characterised in that in step (1), hydrogel is room temperature～100 DEG C
At a temperature of react 7 hours～36 hours preparation.
Preparation method the most according to claim 1, it is characterised in that in step (2), ferrum carbon with the mass ratio of hydrogel is
1:20～5:1.
Preparation method the most according to claim 1, it is characterised in that in step (3), crystallization 80 DEG C～150 DEG C of temperature,
Carrying out under self-generated pressure, crystallization time is 3 hours～10 days.
Preparation method the most according to claim 1, it is characterised in that in step (4), the condition of calcining is: in 300-
700 DEG C, under atmospheric pressure calcining, the control time is 2-12 hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610440274.1A CN106115726B (en) | 2016-06-18 | 2016-06-18 | A kind of preparation method of iron carbon modified mesoporous molecular sieve |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610440274.1A CN106115726B (en) | 2016-06-18 | 2016-06-18 | A kind of preparation method of iron carbon modified mesoporous molecular sieve |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106115726A true CN106115726A (en) | 2016-11-16 |
| CN106115726B CN106115726B (en) | 2018-08-17 |
Family
ID=57470054
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610440274.1A Active CN106115726B (en) | 2016-06-18 | 2016-06-18 | A kind of preparation method of iron carbon modified mesoporous molecular sieve |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106115726B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040875A (en) * | 2019-05-06 | 2019-07-23 | 上海应用技术大学 | A kind of minimizing technology of the useless Organic substance in water of coating material production |
| CN113426171A (en) * | 2021-07-05 | 2021-09-24 | 苏州合芯生物技术有限公司 | Filter element material of medical filter element structure and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880045A (en) * | 2009-05-08 | 2010-11-10 | 李宏愿 | Mesoporous molecular sieve and preparation method thereof |
| CN102951759A (en) * | 2012-11-13 | 2013-03-06 | 云南春城实业集团有限公司 | Method for treating highly-difficult-to-treat industrial wastewater through catalytic oxidation and micro-electrolysis |
-
2016
- 2016-06-18 CN CN201610440274.1A patent/CN106115726B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101880045A (en) * | 2009-05-08 | 2010-11-10 | 李宏愿 | Mesoporous molecular sieve and preparation method thereof |
| CN102951759A (en) * | 2012-11-13 | 2013-03-06 | 云南春城实业集团有限公司 | Method for treating highly-difficult-to-treat industrial wastewater through catalytic oxidation and micro-electrolysis |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110040875A (en) * | 2019-05-06 | 2019-07-23 | 上海应用技术大学 | A kind of minimizing technology of the useless Organic substance in water of coating material production |
| CN113426171A (en) * | 2021-07-05 | 2021-09-24 | 苏州合芯生物技术有限公司 | Filter element material of medical filter element structure and application thereof |
| CN113426171B (en) * | 2021-07-05 | 2022-05-10 | 东莞果核生物技术有限公司 | Filter element material of medical filter element structure and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106115726B (en) | 2018-08-17 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106076335B (en) | A kind of preparation method and application of heterogeneous Fenton catalyst | |
| CN107626335B (en) | Bismuth-based/carbon nitride composite catalyst and preparation method and application thereof | |
| CN112657465B (en) | Preparation method of magnetic biochar and method for treating tailing wastewater | |
| CN103464094B (en) | A kind of preparation method of Nanoscale Iron modified zeolite | |
| CN108114744B (en) | Supported iron-molybdenum-based catalyst and preparation and application thereof | |
| CN108129524B (en) | Method for preparing fulvic acid salt by activating low-rank coal through composite photocatalyst | |
| CN108239536A (en) | A kind of soil conditioner and preparation method thereof | |
| CN103506139A (en) | Preparation method and application of hydrothermal synthesized CdSe quantum dot photocatalyst | |
| CN105251462A (en) | Garbage penetrating fluid efficient wastewater treating agent based on modified fly ash and preparation method | |
| CN106076407A (en) | Nanometer Ag/TiO2the preparation method of zeolite hybridization mesoporous molecular sieve composite material | |
| CN106943835B (en) | Method for preparing air purification material and compound fertilizer by using sludge and livestock and poultry manure | |
| CN106179473B (en) | Nano zero valence iron/carbon nanotube/zeolite hybridization mesoporous molecular sieve composite material preparation method | |
| CN106076397B (en) | A kind of preparation method of Zero-valent Iron-carbon nano-tube modification Zeolite composite materials | |
| CN109126714B (en) | TiO 22/SiO2-banana peel biochar composite adsorption material and preparation method thereof | |
| CN104888705A (en) | Preparation method of magnetic ferric oxide/bagasse active carbon | |
| CN109110863A (en) | Utilize the method for fortimicin in chemical activation/micro-wave digestion activation biological carbon materials removal water body | |
| CN108144622A (en) | A kind of Fenton catalysis material and its preparation method and application | |
| CN111634971A (en) | Application of photocatalytic-ferrate synergistic oxidative degradation of antibiotic pollutants | |
| CN106115726B (en) | A kind of preparation method of iron carbon modified mesoporous molecular sieve | |
| CN103495428A (en) | Preparation method of carbon nano-tube based Fenton-like catalyst for advanced oxidation system | |
| CN109046466A (en) | A kind of photochemical catalyst and its preparation method and application that the derivative carbon-based material of ZIF-8 is CdS-loaded | |
| CN107987283B (en) | Method for extracting fulvic acid salt by activating lignite with photocatalyst | |
| CN108585179B (en) | Compound microbial preparation for water pollution treatment and preparation method thereof | |
| CN107715866B (en) | Bismuth tungstate/mussel shell composite photocatalytic material and preparation method thereof | |
| CN107686156B (en) | A kind of Fenton method of efficient degradation organic pollutants |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |