CN108905966A - A kind of preparation method and application of graphene oxide-zeolite moulding material - Google Patents
A kind of preparation method and application of graphene oxide-zeolite moulding material Download PDFInfo
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- CN108905966A CN108905966A CN201810746532.8A CN201810746532A CN108905966A CN 108905966 A CN108905966 A CN 108905966A CN 201810746532 A CN201810746532 A CN 201810746532A CN 108905966 A CN108905966 A CN 108905966A
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- graphene oxide
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- moulding material
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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
- B01J20/02—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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
-
- 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
- B01J20/3007—Moulding, shaping or extruding
-
- 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
- B01J20/3042—Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
-
- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- 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
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention provides a kind of graphene oxide-zeolite moulding material preparation method and its applications in sewage treatment, belong to technical field of sewage, it is characterised in that it includes preparing graphene oxide-zeolite mixed-powder, preparing the operating procedures such as graphene oxide-zeolite-CMC mixture, molding；It is that binder is effectively compound with zeolite by graphene oxide by CMC, can be formed well again while moulding material obtained neither influences its original absorption property, and recyclable in sewage treatment.
Description
Technical field
The present invention relates to water-treatment technology fields, and in particular to a kind of preparation side of graphene oxide-zeolite moulding material
Method and application.
Background technique
Currently, widely used adsorbent mainly inhale by active charcoal, zeolite molecular sieve, graphene and natural biological
Attached dose etc..The advantage that they have large specific surface area, physicochemical properties stable, Adsorption heavy metal effect are ideal.Due to
Traditional adsorbent material itself is mostly powder, is unfavorable for the recycling of heavy metal contaminants and recycling for adsorbent, therefore need pair
It does forming processes, however common forming processes can influence its absorption property to a certain extent.Therefore, how to make traditional absorption
Material has recyclable feature concurrently again while possessing the excellent absorption property to heavy metal, at urgently to be resolved
Technical problem.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide one kind neither to influence its original suction
It can be formed well again while attached performance, recyclable graphene oxide-zeolite moulding material preparation method
And application.
The technical solution that the present invention solves above-mentioned technical problem is as follows：A kind of system of graphene oxide-zeolite moulding material
Preparation Method, which is characterized in that include the following steps：
1）Prepare graphene oxide-zeolite mixed-powder：Ultrapure water is added dropwise into graphene oxide powder and zeolite powder, until
Powder complete wetting, is put into ball mill after mixing evenly, keeps its ball milling abundant；Be put into after ball milling in thermostatic drying chamber 40 DEG C-
It is dried at 60 DEG C, ground 50 mesh obtains graphene oxide-zeolite mixed-powder；
Wherein, the mass ratio of graphene oxide powder and zeolite powder is 1：0.5-4, rotational speed of ball-mill are 200r/min-400r/
Min, Ball-milling Time 3h-6h；
Two kinds of powders of ball milling mix it more uniform：Sieving keeps powder quality more fine and smooth uniform；
2）Prepare graphene oxide-zeolite-CMC mixture：By graphene oxide powder-zeolite powder, CMC powder and ultrapure water
It is in mass ratio 2-5：1：The ratio of 7-11 mixes, and stirs evenly；
3）The molding of graphene oxide-zeolitic material：By step 2）Gained mixture according to required trimming and dry to get
Granular graphene oxide-zeolite moulding material, wherein shear action keeps shaped granule more uniform, and is easy to transport and store.
It uses in the present invention by step 2）Gained mixture is made into bulk and is rolled into the form of tablet, and then tablet dries in the air
It can take off to surface skining and completely；Tablet flour stranding machine is squeezed into strips, and is cut into segment, after being dried at 40 DEG C -60 DEG C
Up to granular graphene oxide-zeolite moulding material, the flour stranding machine is using the production of Yongkang kaffir lily Trade Co., Ltd.
FKM-160 type flour stranding machine.
Graphene oxide obtained above-carbon black moulding material, the adsorbent material being used as with recycling in water process.
The beneficial effects of the invention are as follows：
1. preferred CMC has good for graphene oxide-zeolite moulding material that binder cooperates graphene oxide and zeolite to prepare
Good mouldability, and good water resistance can be reached, intensity is high, and can be placed in water 1 month will not even scatter for more time,
It brings great convenience for the recycling of material；Relatively unformed material simultaneously, still keeps good adsorption effect,
Its adsorptivity is not weakened after forming；It can be recycled after washing, and adsorption rate keeps relatively stable, is conducive to water process
Recycling afterwards, does not easily cause secondary pollution；
2. graphene oxide and the zeolite compatibility in molding system are good, adsorption material is formed compared to using one-component to prepare
Material, using the synergistic effect between the two and CMC, can keep good forming ability and reach better adsorption effect；
3. the method for the present invention process conditions are controllable, low raw-material cost, it is with short production cycle, have industrialized feasibility；And it makes
The standby stage without the reaction and treatment process polluted the environment, has significant economic benefit and environmental benefit after industrialization.
Specific embodiment
Embodiment 1
The graphene oxide of the present embodiment-zeolite moulding material preparation method, includes the following steps：
1）Prepare graphene oxide-zeolite mixed-powder：It is dripped into 10g graphene oxide powder and 20g zeolite powder mixture
Add ultrapure water, until powder complete wetting, is put into ball mill after mixing evenly, keeps its ball milling abundant；Ball milling under 400r/min
3h is then placed in thermostatic drying chamber and dries at 50 DEG C, and ground 50 mesh obtains graphene oxide-zeolite mixed-powder；
2）Prepare graphene oxide-zeolite-CMC mixture：By graphene oxide powder-zeolite powder, CMC powder and ultrapure water
It is in mass ratio 4.4：1：10.3 ratio mixing, and stir evenly；
3）The molding of graphene oxide-zeolitic material：By step 2）Gained mixture is made into bulk and is rolled into tablet, then will
Tablet dries in the air to surface skining and can completely take off；Tablet flour stranding machine is squeezed into strips, and is cut into segment, after being dried at 50 DEG C
Up to granular graphene oxide-zeolite moulding material
Embodiment 2
The graphene oxide of the present embodiment-zeolite moulding material preparation method, includes the following steps：
1）Prepare graphene oxide-zeolite mixed-powder：It is dripped into 20g graphene oxide powder and 10g zeolite powder mixture
Add ultrapure water, until powder complete wetting, is put into ball mill after mixing evenly, keeps its ball milling abundant；Ball milling under 200r/min
6h is then placed in thermostatic drying chamber and dries at 40 DEG C, and ground 50 mesh obtains graphene oxide-zeolite mixed-powder；
2）Prepare graphene oxide-zeolite-CMC mixture：By graphene oxide powder-zeolite powder, CMC powder and ultrapure water
It is in mass ratio 2：1：11 ratio mixing, and stir evenly；
3）The molding of graphene oxide-zeolitic material：By step 2）Gained mixture is made into bulk and is rolled into tablet, then will
Tablet dries in the air to surface skining and can completely take off；Tablet flour stranding machine is squeezed into strips, and is cut into segment, after being dried at 40 DEG C
Up to granular graphene oxide-zeolite moulding material, the flour stranding machine is using the production of Yongkang kaffir lily Trade Co., Ltd.
FKM-160 type flour stranding machine.
Embodiment 3
The graphene oxide of the present embodiment-zeolite moulding material preparation method, includes the following steps：
1）Prepare graphene oxide-zeolite mixed-powder：It is added dropwise into 6g graphene oxide powder and 24g zeolite powder mixture
Ultrapure water, until powder complete wetting, is put into ball mill after mixing evenly, keeps its ball milling abundant；Ball milling 5h under 300r/min,
It is then placed in thermostatic drying chamber and is dried at 60 DEG C, ground 50 mesh obtains graphene oxide-zeolite mixed-powder；
2）Prepare graphene oxide-zeolite-CMC mixture：By graphene oxide powder-zeolite powder, CMC powder and ultrapure water
It is in mass ratio 5：1：7 ratio mixing, and stir evenly；
3）The molding of graphene oxide-zeolitic material：By step 2）Gained mixture is made into bulk and is rolled into tablet, then will
Tablet dries in the air to surface skining and can completely take off；Tablet flour stranding machine is squeezed into strips, and is cut into segment, after being dried at 60 DEG C
Up to granular graphene oxide-zeolite moulding material.
Comparative example 1
With embodiment 1, the difference is that CMC is replaced with chitosan.
Comparative example 2
With embodiment 1, the difference is that CMC is replaced with bentonite.
Comparative example 3
With embodiment 1, the difference is that CMC is replaced with diatomite.
Comparative example 4
With embodiment 1, the difference is that CMC is replaced with polymer alumina.
Comparative example 5
10g graphene oxide powder and 20g zeolite powder mixture are directlyed adopt as adsorbent, does not do processing and forming.
Comparative example 6
With embodiment 1, the difference is that graphene oxide powder is not added, using 30g zeolite powder as raw material.
Comparative example 7
With embodiment 1, the difference is that zeolite powder is not added, using 30g graphene oxide powder as raw material.
Observe the discovery of material made from above-described embodiment and comparative example 1-4, embodiment 1, embodiment 2, embodiment 3, comparison
Material appearance consolidation, good moldability made from example 1, and material appearance made from comparative example 2, comparative example 3, comparative example 4 is loosely not
Molding；Then it takes etc. that the embodiments 1 of quality, embodiment 2, embodiment 3, material is respectively put into water made from comparative example 1, observes
It enters the phenomenon discovery after water, and the material of embodiment 1-3 is still able to maintain intact mouldability after putting into water, and in water
Middle immersion is still able to maintain shape after one month well not loose, and material made from comparative example 1 dissipates immediately after putting into water
It opens, is not easy to be recycled, specific test result is referring to table 1.
The molding of 1 embodiment and comparative example of table and water-fast measure of merit result
| Molding effect | It puts into water | Water impregnates 12h | Water impregnates 48h | Water impregnates 5 days | Water impregnates 15 days | Water impregnates 1 month | |
| Embodiment 1 | Good moldability | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter |
| Embodiment 2 | Good moldability | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter |
| Embodiment 3 | Good moldability | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter | It does not scatter |
| Comparative example 1 | Good moldability | It scatters | - | - | - | - | |
| Comparative example 2 | It does not form loosely | - | - | - | - | - | |
| Comparative example 3 | It does not form loosely | - | - | - | - | - | |
| Comparative example 4 | It does not form loosely | - | - | - | - |
From the data in table 1, it can be seen that the present invention cooperates graphene oxide and zeolite to prepare by binder of CMC compared with comparative example 1-4
Graphene oxide-zeolite moulding material have good mouldability, and good water resistance can be reached, 1 can be placed in water
A month even longer time will not scatter, and bring great convenience for the recycling of material.
Material appearance consolidation, good moldability made from comparative example 6 are observed, and material appearance made from comparative example 7 is loosely not
Molding；The above-described embodiment of quality and comparative example 5,6 such as then take to carry out the survey of the adsorption effect to copper ion and ammonia nitrogen respectively
Examination, test result are shown in Table 2.
Test to copper absorption rate is to be respectively placed in adsorbent material above-mentioned with copper-bath for system to be adsorbed
One time of Static Adsorption is carried out in system to be adsorbed, measures absorption front and back copper-bath respectively using atomic absorption spectrography (AAS)
Then the concentration of middle copper ion calculates the adsorption rate of copper ion；
Test to ammonia nitrogen absorption rate is to be respectively placed in adsorbent material above-mentioned to be adsorbed with ammonium chloride solution for system to be adsorbed
One time of Static Adsorption is carried out in system, measures ammonium root in the ammonium chloride solution of absorption front and back respectively using nessler reagent development process
Then the concentration of ion calculates ammonia nitrogen absorption rate.
The molding and absorption property test result of 2 embodiment and comparative example of table
| Molding effect | Copper absorption rate/% | Ammonia nitrogen absorption rate/% | |
| Embodiment 1 | Good moldability | 89.93 | 85.10 |
| Embodiment 2 | Good moldability | 89.89 | 84.93 |
| Embodiment 3 | Good moldability | 89.72 | 85.08 |
| Comparative example 5 | - | 90.02 | 86.50 |
| Comparative example 6 | Good moldability | 63.30 | 65.30 |
| Comparative example 7 | It does not form loosely | - | - |
From the data in table 2, it can be seen that the absorption raw material of comparative example 5 is same as Example 1, but do not form, i.e., in water with powdery shape
Formula exists, and graphene oxide made from the embodiment of the present invention-zeolite moulding material to the adsorption rate of copper ion and ammonia nitrogen with it is right
Quite, i.e., graphene oxide made from the method for the present invention-zeolite moulding material is obtaining good mouldability and water resistance to ratio 5
Meanwhile adsorption effect still keeps good；6 single use zeolite of comparative example makees moulding material and compares, although good forming ability,
It is that adsorptivity is relatively poor, graphene oxide made from the embodiment of the present invention-zeolite moulding material is compared with comparative example 6, to copper
The adsorption rate of ion and ammonia nitrogen is significantly increased, this is because the compatibility of graphene oxide, zeolite is good, therefore can be significantly
Absorption system is improved to the adsorption effect of copper ion in water and ammonia nitrogen.
By the material of the above-mentioned embodiment for carrying out a suction-operated by washing, reused according still further to the above method
It is adsorbed again, then repeats as above to operate, detect its adsorption rate respectively, test result is shown in Table 3.
The adsorption rate test result of 3 embodiment of table
As shown in Table 3, graphene oxide-zeolite moulding material of a suction-operated was carried out after washing, was used further to pair
When the absorption of copper ion and ammonia nitrogen, the adsorption rate of copper ion and ammonia nitrogen is still kept well, not decreased significantly, and equal energy
It is maintained at 84% or more, this is because graphene oxide made from the method for the present invention-zeolite moulding material has good porous knot
Structure, and be used as after adsorbent is washed again and adsorbed again, it is able to maintain more stable adsorption rate, can satisfy adsorbent material
It is recycled and requires.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, modifies, replacement and variant.
Claims (6)
1. a kind of graphene oxide-zeolite moulding material preparation method, which is characterized in that include the following steps：
1）Prepare graphene oxide-zeolite mixed-powder：Ultrapure water is added dropwise into graphene oxide powder and zeolite powder, until
Powder complete wetting, is put into ball mill after mixing evenly, keeps its ball milling abundant；It is put into thermostatic drying chamber and is dried after ball milling
Dry, ground 50 mesh obtains graphene oxide-zeolite mixed-powder；
2）Prepare graphene oxide-zeolite-CMC mixture：By graphene oxide powder-zeolite powder, CMC powder and ultrapure water
It is in mass ratio 2-5：1：The ratio of 7-11 mixes, and stirs evenly；
3）The molding of graphene oxide-zeolitic material：By step 2）Gained mixture according to required trimming and dry to get
Granular graphene oxide-zeolite moulding material.
2. graphene oxide according to claim 1-zeolite moulding material preparation method, which is characterized in that the step
Rapid 1）In the mass ratio of graphene oxide powder used and zeolite powder be 1：0.5-4.
3. graphene oxide according to claim 1-zeolite moulding material preparation method, which is characterized in that the step
Rapid 1）In rotational speed of ball-mill be 200-400r/min, Ball-milling Time 3-6h.
4. graphene oxide according to claim 1-zeolite moulding material preparation method, which is characterized in that the step
Rapid 1）In drying temperature be 40 DEG C -60 DEG C.
5. graphene oxide according to claim 1-zeolite moulding material preparation method, which is characterized in that the step
Rapid 3）In drying temperature be 40 DEG C -60 DEG C.
6. graphene oxide made from claim any one of 1-5-carbon black moulding material is used as in water process with recycling
Adsorbent material.
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| CN115055162A (en) * | 2022-06-21 | 2022-09-16 | 广东恒峰蓝环境工程有限公司 | Preparation method of zeolite molecular sieve adsorption material |
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