CN107902648A - A kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water - Google Patents
A kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water Download PDFInfo
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- CN107902648A CN107902648A CN201711137149.4A CN201711137149A CN107902648A CN 107902648 A CN107902648 A CN 107902648A CN 201711137149 A CN201711137149 A CN 201711137149A CN 107902648 A CN107902648 A CN 107902648A
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- waste water
- inorganic waste
- industrial inorganic
- graphitization
- cation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention relates to a kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water, include the following steps：S1. pretreatment industrial inorganic waste water filtered and concentrated, resin cation is put into pretreated industrial inorganic waste water and is sufficiently mixed, and carries out ion-exchange reactions；S2. the mixture after reaction is filtered, obtained solid carries out high-temperature calcination under inert gas shielding, obtains crude product；S3. the washing of gained crude product, filtering, drying in S2 are taken, obtains graphite particle.This method realizes industrial inorganic waste water high-efficiency recycling to a certain extent, and produces the graphite of the high attached output value.
Description
Technical field
The invention belongs to industrial inorganic wastewater treatment and recycling field, and in particular to one kind utilization handles industrial inorganic and gives up
The method that the cation resin catalyzing of water prepares graphitization particle.
Background technology
Graphite is a kind of excellent carbon material, has good heat endurance, thermal conductance, lubricity and chemical stabilization
Property, it is widely used in fields such as metallurgical, machinery, electric, chemical industry.Since demand is big, native graphite has been unable to meet the mankind
Use demand, this causes Delanium to receive much concern.Now, graphite is industrially manufactured mainly in the bar of 2500 DEG C or so anoxybiotics
The carbon raw material such as calcined petroleum coke, pitch coke, anthracite under part, excessive temperature have aggravated the cost of production graphite.Therefore, such as
It is always the important directions for producing graphite research that what, which reduces reaction temperature and then reduces production cost,.Resin since carbon content is high,
The advantages such as impurity is few during pyrolysis, graphitization temperature is low and be introduced into graphitization field.Research shows, by graphited process
The simple substance and its compound of the elements such as middle addition Ni, Fe, Cr, Cu, Mn can effectively reduce required temperature to 600 as catalyst
℃。
Industrial expansion generates a large amount of inorganic wastewaters, in inorganic wastewater containing excessive metal ion such as nickel, iron,
Chromium, copper, manganese etc., directly discharge can cause serious pollution to soil, water source, air, directly affect health, this also causes
There is stringent standard for metal ion content in industrial discharge waste water.Processing industrial inorganic waste water mainly has Physical at present
And chemical method, these method processing costs are excessive and fail effectively to realize the recycling of waste water.Therefore, how effectively to handle
Industrial inorganic waste water reduces secondary pollution, realizes waste water high-efficiency recycling, lifting process economy becomes urgently to be resolved hurrily ask
Topic.
The content of the invention
The present invention provides a kind of side that graphitization particle is prepared using the cation resin catalyzing for handling industrial inorganic waste water
Method, it is intended to realize industrial inorganic waste water high-efficiency recycling to a certain extent, and produce the graphite of the high attached output value.
The present invention realizes that the technical solution of above-mentioned target is as follows：It is a kind of to utilize the resin cation for handling industrial inorganic waste water
The method that catalysis prepares graphitization particle, includes the following steps：
S1. pretreatment industrial inorganic waste water filtered and concentrated, pretreated work is put into by resin cation
It is sufficiently mixed in industry inorganic wastewater, carries out ion-exchange reactions；
S2. the mixture after reaction is filtered, obtained solid carries out high-temperature calcination under inert gas shielding, obtains
To crude product；
S3. the washing of gained crude product, filtering, drying in S2 are taken, obtains graphite particle.
Based on the above technical solutions, the present invention can also have following further improvement.
Preferably, filtering described in the S1 is to without the particle for being more than 100 μm by industrial inorganic waste water filtering.Institute in S1
It is that to be concentrated into metal ion total concentration be 300-1000mg/L by the heating of industrial inorganic waste water to state concentration.It is above-mentioned to give up to industrial inorganic
The pretreatment that water carries out is only preliminary treatment, easy to operate.
Specifically, the rate of charge that resin cation described in S1 puts into pretreated industrial inorganic waste water is 5-20g:
1L。
Preferably, industrial inorganic waste water described in S1 is mainly one in nickel-plating waste water, electroplating wastewater, mineral processing waste water
Kind or a variety of combinations.Specifically, industrial inorganic waste water described in S1 contains in nickel, iron, manganese, chromium and the corresponding cation of copper
It is at least one.
Preferably, ion-exchange reactions described in S1 is to carry out at ambient temperature, is shaken using magnetic agitation or utilization
Bed is vibrated, and is stirred or is vibrated 6-48h.
Specifically, high-temperature calcination described in S2 is that 1-3h is calcined under the conditions of 600-1600 DEG C, heating rate for 5-20 DEG C/
min。
Preferably, inert gas described in S2 is N2, one or more in Ar, He, flow 0.2-2L/min.
Specifically, washing described in S3 is to carry out pickling using hydrochloric acid, the concentration of hydrochloric acid is 0.5-1mol/L.The acid
Washing lotion is 5-30mL with crude product proportioning:1g, persistently stirs 1-3h.
It should be noted that dry described in S3 refer to placing more than 24h under the conditions of 105 DEG C.People in the art
Member in light of the circumstances can further select above-mentioned reaction condition.
Compared with prior art, beneficial effects of the present invention are：The temperature needed for graphitization in the prior art is high, consumption
Can be serious the problem of, the present invention is effectively combined industrial inorganic waste water high-efficiency recycling with the graphite of the high attached output value of production, ingenious
Ground make use of the metal cation in industrial inorganic waste water to carry out graphitization as catalyst, catalytic resin.The present invention realizes
The reasonable recycling of resource, reduces energy consumption and provides new approaches for production graphite.
Brief description of the drawings
Fig. 1 is that the cation resin catalyzing that a kind of utilization provided by the invention handles industrial inorganic waste water prepares graphitization
The technological process of the method for grain.
Embodiment
Below in conjunction with drawings and the specific embodiments, the present invention is described in further detail, and example is served only for explaining
The present invention, is not intended to limit the scope of the present invention.
Embodiment 1
A kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water, it is included such as
Lower step：
S1. the pretreatment for taking a certain amount of nickel-plating waste water to be filtered and concentrated, makes in nickel-plating waste water without for being more than 100 μm
Grain, heating concentration nickel-plating waste water to wherein nickel ion concentration is 1000mg/L, and resin cation is thrown according to rate of charge for 5g/L
Enter in nickel-plating waste water, products obtained therefrom is placed on rotary shaker vibrates 6h at room temperature；
S2. S1 products obtained therefroms being filtered, solid, which is placed in high temperature process furnances, leads to Ar protections (flow set 0.2L/min),
600 DEG C are heated to 5 DEG C/min, high-temperature calcination 1h is carried out at 600 DEG C；
S3. solid crude product after being calcined in S2 is taken, using washing lotion and crude product as 5mL:The proportioning of 1g adds hydrochloric acid (1mol/
L), 3h is sufficiently stirred, is separated by filtration, dry 24h, obtains high purity graphite particle in 105 DEG C of baking ovens.
The graphite that above-mentioned steps obtain X-ray diffraction (XRD) phenetic analysis degree of graphitization will be passed through.Detection structure table
Bright, the degree of graphitization of the graphite after being handled in the implementation case has reached more than 50%, untreated industrial inorganic under equal conditions
Do not occur graphite transition after the resin cation calcining of waste water, the cation in industrial inorganic waste water is to cation exchange resin
Graphitization have obvious catalytic action.
Embodiment 2
A kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water, it is included such as
Lower step：
S1. the pretreatment for taking a certain amount of nickel-plating waste water to be filtered and concentrated, makes in nickel-plating waste water without for being more than 100 μm
Grain, heating concentration nickel-plating waste water to wherein nickel ion concentration is 500mg/L, and resin cation is thrown according to rate of charge for 10g/L
Enter in nickel-plating waste water, products obtained therefrom is placed on rotary shaker vibrates 12h at room temperature；
S2. S1 products obtained therefroms are filtered, solid, which is placed in high temperature process furnances, leads to N2Protect (flow set 0.5L/min),
1500 DEG C are heated to 10 DEG C/min, high-temperature calcination 3h is carried out at 1500 DEG C；
S3. solid crude product after being calcined in S2 is taken, using washing lotion and crude product as 10mL:The proportioning of 1g adds hydrochloric acid (1mol/
L), 3h is sufficiently stirred, is separated by filtration, dry 24h, obtains high purity graphite particle in 105 DEG C of baking ovens.
The graphite that above-mentioned steps obtain X-ray diffraction (XRD) phenetic analysis degree of graphitization will be passed through.Detection structure table
Bright, the degree of graphitization of the graphite after being handled in the implementation case has reached more than 75%, untreated industrial inorganic under equal conditions
Degree of graphitization is only 15% after the resin cation calcining of waste water, and degree of graphitization is obviously improved.
Embodiment 3
A kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water, it is included such as
Lower step：
S1. the pretreatment for taking a certain amount of nickel-plating waste water to be filtered and concentrated, makes in nickel-plating waste water without for being more than 100 μm
Grain, heating concentration nickel-plating waste water to wherein nickel ion concentration is 300mg/L, and resin cation is thrown according to rate of charge for 20g/L
Enter in nickel-plating waste water, products obtained therefrom is placed on rotary shaker vibrates 48h at room temperature；
S2. S1 products obtained therefroms are filtered, solid, which is placed in high temperature process furnances, leads to He and N2Mixed gas protected (flow is set
It is set to 2L/min), 1600 DEG C are heated to 20 DEG C/min, high-temperature calcination 2h is carried out at 1600 DEG C；
S3. solid crude product after being calcined in S2 is taken, using washing lotion and crude product as 30mL:The proportioning of 1g adds hydrochloric acid
(0.5mol/L), is sufficiently stirred 1h, is separated by filtration, and dry 24h, obtains high purity graphite particle in 105 DEG C of baking ovens.
The graphite that above-mentioned steps obtain X-ray diffraction (XRD) phenetic analysis degree of graphitization will be passed through.Detection structure table
Bright, the degree of graphitization of the graphite after being handled in the implementation case has reached more than 85%, untreated industrial inorganic under equal conditions
Degree of graphitization is only 15% after the resin cation calcining of waste water, and degree of graphitization is obviously improved.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modification, equivalent replacement, improvement and so on, should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method for preparing graphitization particle using the cation resin catalyzing for handling industrial inorganic waste water, its feature exist
In including the following steps：
S1. pretreatment industrial inorganic waste water filtered and concentrated, pretreated industrial nothing is put into by resin cation
It is sufficiently mixed in machine waste water, carries out ion-exchange reactions；
S2. the mixture after reaction is filtered, obtained solid carries out high-temperature calcination under inert gas shielding, obtains thick
Product；
S3. the washing of gained crude product, filtering, drying in S2 are taken, obtains graphitization particle.
2. the cation resin catalyzing that a kind of utilization according to claim 1 handles industrial inorganic waste water prepares graphitization
The method of grain, it is characterised in that filtering described in S1 is to without the particle for being more than 100 μm by industrial inorganic waste water filtering.
3. the cation resin catalyzing that a kind of utilization according to claim 1 handles industrial inorganic waste water prepares graphitization
The method of grain, it is characterised in that concentration described in S1 is that the heating of industrial inorganic waste water is concentrated into metal ion total concentration to be
300-1000mg/L。
4. the cation resin catalyzing that a kind of utilization according to claim 1 handles industrial inorganic waste water prepares graphitization
The method of grain, it is characterised in that the rate of charge that resin cation described in S1 puts into pretreated industrial inorganic waste water is 5-
20g:1L。
5. the cation resin catalyzing that a kind of utilization according to claim 1 handles industrial inorganic waste water prepares graphitization
The method of grain, it is characterised in that industrial inorganic waste water described in S1 contains in nickel, iron, manganese, chromium and the corresponding cation of copper extremely
Few one kind.
6. prepared according to claim 1-5 any one of them is a kind of using the cation resin catalyzing for handling industrial inorganic waste water
The method of graphitization particle, it is characterised in that ion-exchange reactions described in S1 stirs or vibrate 6- at ambient temperature
48h。
7. prepared according to claim 1-5 any one of them is a kind of using the cation resin catalyzing for handling industrial inorganic waste water
The method of graphitization particle, it is characterised in that high-temperature calcination described in S2 is that 1-3h is calcined under the conditions of 600-1600 DEG C, heating
Speed is 5-20 DEG C/min.
8. prepared according to claim 1-5 any one of them is a kind of using the cation resin catalyzing for handling industrial inorganic waste water
The method of graphitization particle, it is characterised in that inert gas described in S2 is N2, one or more in Ar, He.
9. prepared according to claim 1-5 any one of them is a kind of using the cation resin catalyzing for handling industrial inorganic waste water
The method of graphitization particle, it is characterised in that washing described in S3 is to carry out pickling using hydrochloric acid, and the concentration of hydrochloric acid is 0.5-
1mol/L。
10. the cation resin catalyzing that a kind of utilization according to claim 9 handles industrial inorganic waste water prepares graphitization
The method of particle, it is characterised in that the pickling washing lotion is 5-30mL with crude product proportioning:1g, persistently stirs 1-3h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218349A (en) * | 2011-04-02 | 2011-10-19 | 中山大学 | Method for one-step localized synthesizing nanometer carbide-graphitized carbon composite material and method for loading nanometer catalyst thereof |
| CN102992306A (en) * | 2012-11-14 | 2013-03-27 | 中山大学 | Graphitized carbon with high specific surface area and hierarchical pores and preparation method thereof |
| CN106276895A (en) * | 2016-08-05 | 2017-01-04 | 南通绿业中试技术研究院有限公司 | A kind of preparation method of amberlite aliphatic radical material with carbon element |
| CN106495147A (en) * | 2016-11-08 | 2017-03-15 | 株洲时代新材料科技股份有限公司 | A kind of method that catalyzed graphitization prepares high heat conduction graphite |
-
2017
- 2017-11-16 CN CN201711137149.4A patent/CN107902648A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102218349A (en) * | 2011-04-02 | 2011-10-19 | 中山大学 | Method for one-step localized synthesizing nanometer carbide-graphitized carbon composite material and method for loading nanometer catalyst thereof |
| CN102992306A (en) * | 2012-11-14 | 2013-03-27 | 中山大学 | Graphitized carbon with high specific surface area and hierarchical pores and preparation method thereof |
| CN106276895A (en) * | 2016-08-05 | 2017-01-04 | 南通绿业中试技术研究院有限公司 | A kind of preparation method of amberlite aliphatic radical material with carbon element |
| CN106495147A (en) * | 2016-11-08 | 2017-03-15 | 株洲时代新材料科技股份有限公司 | A kind of method that catalyzed graphitization prepares high heat conduction graphite |
Non-Patent Citations (1)
| Title |
|---|
| 陶鹏鹏: "树脂制备石墨化多孔碳和碳/钼复合物及其电化学性能研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Application publication date: 20180413 |