CN106564897A - Method for preparing porous active carbon by using waste PCB - Google Patents
Method for preparing porous active carbon by using waste PCB Download PDFInfo
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- CN106564897A CN106564897A CN201510644985.6A CN201510644985A CN106564897A CN 106564897 A CN106564897 A CN 106564897A CN 201510644985 A CN201510644985 A CN 201510644985A CN 106564897 A CN106564897 A CN 106564897A
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Abstract
The present invention belongs to the technical field of porous active carbon, and more particularly relates to a method for preparing porous active carbon by using a waste printed circuit board (PCB). The method comprises: (1) using waste PCB as a raw material, pre-treating with an inorganic acid, carrying out a reaction on the metal part of the waste PCB, filtering, and separating from the non-metal part; (2) crushing the non-metal part of the waste PCB, screening, drying, and carrying out carbonization treatment at a certain temperature; (3) carrying out mixing impregnation on the prepared carbonization product and an activator, and carrying out activation treatment at a certain temperature; and (4) carrying out acid washing and water washing on the activated product, and drying so as to obtain the porous active carbon. According to the present invention, with the method, the resource in the waste PCB is completely utilized.
Description
Technical field
The invention belongs to the preparing technical field of porous activated carbon, in particular it relates to one kind is more with novel material preparation
The method of mesoporous activated carbon, more particularly to a kind of method for preparing porous activated carbon using discarded PCB.
Background technology
Economic development and scientific and technological progress cause electronic information technology industry fast development, demand of the people to electronic product
Constantly expand.And as electronic product update speed is accelerated, produce a large amount of discarded PCB (Printed Circuit
Board, printed substrate), these garbages contain substantial amounts of noxious substance, including substantial amounts of heavy metal,
Resinae composite and other poisonous and harmful elements, such as brominated flame retardant etc., these are into branch's induction deformity, base
Because of mutation, canceration etc., serious harm is produced to environment and human health.Therefore, PCB recyclings are discarded
Research has become the hot issue of Current electronic garbage disposal.
At present, stress the recovery of metal in wiring board the method for reclaiming for discarded PCB available resources more, it is less to relate to
And account for the resource of the Non-metallic components of total amount more than 50% and innoxious.Nonmetallic separation owner in discarded PCB
If epoxy resin or phenolic resin, in addition with some glass fibre and the metal of remnants.PCB nonmetallic ingredients
Except minority be used as filler in addition to, it is more be as garbage loading embeading or be sent to refuse destructor burning, such process
Mode not only makes the valuable constituents such as resin and glass fibre cannot get effectively utilizes and be lost in, fire retardant therein,
The harmful substances such as residual metal also easily pollute environment by all means.
Resource analysis for discarding nonmetallic ingredient in PCB are broadly divided into two kinds：Physical method is reclaimed and chemistry
Method recycling.
During physical method reclaims discarded PCB, nonmetallic ingredient mainly takes Mechanical Crushing at present, makes metal solution in PCB
From then metal material and nonmetallic materials being separated by the sorting such as electrostatic, magnetic force, gravity mode.With
Non-metal powder does filler and prepares construction material etc., as the filler of composite, for preparing composite.
Y.Zheng in 2009 etc. exists《Journal of Hazardous Materials》On deliver《The reuse of
nonmetals recycled from waste printed circuit boards as reinforcing fillers in the
polypropylene composites》Report and discarded PCB metal materials and Fei Jin are separated using crushing, floatation
After category material, discarded PCB nonmetallic materials are made the enhancing implant in PP composite material.But this method is not
Foot part be wiring board composition and property difference and impurity presence can cause reconstituted product performance decline or
Degrade and use.
The chemical recovery of discarded PCB nonmetallic materials has using form：Pyrolysis absorption method and solvent-recovery process.
Sun Lushi etc. exists《Central China University of Science and Technology's journal》On deliver《The pyrolysis of brominated epoxy resin printed circuit plate is produced
The analysis of thing》In report useless PCB be directly pyrolyzed after pretreatment, nonmetallic materials therein are in noble gases
Uniform temperature is heated under protection pyrolysis occurs, generate gas, liquid (oil), solid (Jiao), reclaimed pyrolysis and produce
Thing is used as industrial chemicals or fuel.But the solid (Jiao) that this method is produced can application it is narrow, value is low.
CN101407596B discloses a kind of recovery epoxy resin and glass fibers from the non-metal powder of discarded PCB
Network polymer matrix in discarded PCB, using organic and inorganic solvent, is decomposed or is hydrolyzed by the method for dimension
Into low molecular linear organic compound, each component in composite is made to be easily isolated and reclaim.Relative to pyrolysis
Method, solvent-recovery process will gently much, it is not necessary to too high temperature.But solvent-recovery process is still in starting research rank
Section, object of study mostly are the thermosetting epoxy resin composite material of laboratory synthesis, also have many skills in research process
An art difficult problem needs to overcome.
Yang Ertao etc. exists《Environmental project journal》On deliver《Granular active carbon is prepared with abandoned printed circuit board》
With《Novel charcoal material》On deliver《Porous charcoal is prepared with abandoned printed circuit board nonmetallic ingredient separator》
In coal tar is with the addition of before carbonization, steam activation to make Carbon Materials molding that roasting goes out, increased PCB non-
The operation and cost of metal component charcoal processing material.
To overcome the shortcomings of above technology, the present invention proposes a kind of side that porous activated carbon is prepared using discarded PCB
Method, the present invention rationally make use of resource, improve the economic worth of discarded PCB.
The content of the invention
The purpose of the present invention is, to solve the above problems, there is provided a kind of to prepare porous activated carbon using discarded PCB
Preparation method.
The method that the discarded PCB of the utilization of the present invention prepares porous activated carbon, comprises the following steps：
(1) with discarded PCB as raw material, by the discarded PCB elder generations inorganic low-kappa numbers of Jing, after filtration, obtain discarded PCB
Non-metallic part, then by the non-metallic part of discarded PCB successively Jing wash, dry, pulverize, sieve, obtain
Powder body；
(2) the powder body carbonization that will be obtained in step (1), makes carbide；
(3) priming reaction is carried out after mixed homogeneously obtained carbide in step (2) with activator, after reaction
Products therefrom Jing pickling, washing are dried, obtain final product porous activated carbon.
The method according to the invention, preferably, the mineral acid described in step (1) is sulphuric acid, hydrochloric acid and nitre
One or several in acid
The method according to the invention, preferably, inorganic acid concentration described in step (1) is 0.5～10mol/L,
Discarded PCB is 1 with mineral acid mass ratio:1～1:10.
The method according to the invention, preferably, described in step (1) will be discarded PCB Jing mineral acids pre-
It is 20～90 DEG C to process reaction temperature used, and the response time is 30～300min.
The method according to the invention, preferably, the non-metallic part of the discarded PCB described in step (1)
After crushing, granularity is 100～1000 mesh.
The method according to the invention, preferably, carbonization temperature scope described in step (2) is 600～1000 DEG C,
30～300min of carbonization time.
The method according to the invention, preferably, the powder body described in step (2) carries out carbonization under shielding gas；
The shielding gas is preferably nitrogen or argon.
The method according to the invention, preferably, carbide described in step (3) presses 1 with activator:1～1:5
Mass ratio mixes.
The method according to the invention, preferably, activator described in step (3) be NaOH, KOH and
Ca(OH)2In one or more, or the activator be NaOH, KOH, Na2CO3And K2CO3In
One or more.
The method according to the invention, preferably, the temperature of step (3) priming reaction is 600～1000 DEG C,
30～300min of soak time.
The method according to the invention, preferably, step (3) pickling, washing, dry concrete operations
Can be the routine operation of this area, for example, it may be product after the activation that step (3) is obtained, sequentially passes through
After 1～10mol/L hydrochloric acid and deionized water cleaning, dry or dry naturally.
Embodiments in accordance with the present invention, specifically, the method that PCB prepares porous activated carbon is discarded in the utilization of the present invention,
Comprise the following steps：
Discarded PCB is immersed in mineral acid, inorganic acid concentration is 0.5～10mol/L, discards PCB and mineral acid
Mass ratio is 1:1～1:10, reaction temperature is 20～90 DEG C, and the response time is 30～300min, after the completion of reaction
Filter；PCB nonmetallic ingredients to obtaining are washed, and be dry, pulverize, are sieved, and granularity is 100～1000
Mesh；The powder body for obtaining is warming up to into 600～1000 DEG C under protective atmosphere, is cooled down after 30～300min of carbonization, is obtained
To carbide；Carbide is pressed into 1 with activator:1～1:5 mass are warming up under protective atmosphere than mix homogeneously
600～1000 DEG C, cool down after 30～300min of activation, obtain activator；Activator is removed in sample with pickling
Most of ash and the impurity such as heavy metal, then be washed with deionized to neutrality, dry naturally or dry, i.e.,
Porous activated carbon prepared by handy discarded PCB.
Activated carbon prepared by the discarded PCB of the utilization of the present invention, the BET specific surface area of activated carbon is 1300～3000
m2/ g, pore volume are 0.77～1.08cm3/g。
Compared with traditional steam activation, the present invention by the carbide of discarded PCB nonmetallic ingredients using NaOH,
KOH and Ca (OH)2One or more activators in carry out the specific surface area of activated carbon and hole obtained by activation processing
Appearance is improved.Other adjuvants such as coal tar are not added with discarded PCB nonmetallic ingredients carbonization and activation process,
Reduce to discard the operation and cost that PCB prepares porous activated carbon, the purposes width of gained porous activated carbon, and produce
Product value is burnt higher than solid.
One of important feature of the present invention is to prepare porous activated carbon for raw material using discarded PCB.The present invention was both reasonable
Resource, and environmental protection are make use of, the economic worth of discarded PCB is improve.Simple production process of the present invention, saves
When, it is laborsaving, it is easy to accomplish large-scale production.The present invention is by discarding porous activated carbon specific surface area prepared by PCB
3030m is may be up to respectively with pore volume2/ g and 1.08cm3/g。
Description of the drawings
Fig. 1 is the process chart of the method that the discarded PCB of utilization of the present invention prepares porous activated carbon.
Nitrogen adsorption-desorption isotherm the figure of porous activated carbons of the Fig. 2 to prepare in the embodiment of the present invention 2.
Specific embodiment
Disclosed in this specification any feature, unless specifically stated otherwise, can be equivalent by other or there is similar purpose
Alternative features replaced.Unless specifically stated otherwise, during each feature is a series of equivalent or similar characteristics
One example.It is described to understand the present invention just for the sake of help, should not be considered as the concrete restriction to the present invention.
Embodiment 1
Discarded PCB is immersed in sulphuric acid, sulfuric acid concentration is 0.5mol/L, it is 1 to discard PCB with sulphuric acid mass ratio:3,
Reaction temperature is 20 DEG C, reacts 0.5h, is filtered after the completion of reaction.PCB nonmetallic ingredients to obtaining enter water-filling
Wash, dry, pulverize, sieve, granularity is 100 mesh.By the powder body for obtaining in N2600 DEG C are warming up under protection,
Cool down after carbonization 30min, obtain carbide.Carbide is pressed into 1 with KOH:1 mass than mix homogeneously, in N2
600 DEG C are warming up under protection, are cooled down after activation 30min, is obtained activator.Activator is sequentially passed through into 1～10
After mol/L hydrochloric acid and deionized water cleaning, dry or dry naturally, specific surface area is obtained for 1453m2/ g, total hole
Hold 0.77cm3The porous activated carbon of/g.
Embodiment 2
Discarded PCB is immersed in hydrochloric acid of the concentration for 3mol/L, it is 1 to discard PCB with hydrochloric acid mass ratio:1, instead
Temperature is answered for 60 DEG C, 2h is reacted.PCB nonmetallic ingredients to obtaining are crushed, and are sieved, and granularity is 300 mesh.
Charing process temperature is 800 DEG C, cools down, obtain carbide after carbonization 1h.By carbonizing production and Ca (OH)2By 1:
4 mass than mix homogeneously, in N2600 DEG C are warming up under protection, 120min is activated, other steps are with embodiment 1.
The porous activated carbon specific surface area obtained in the present embodiment is 2503m2/ g, total pore volume 0.92cm3/g.The present embodiment
The nitrogen adsorption of the porous activated carbon of middle preparation-desorption isotherm figure such as Fig. 2.
Embodiment 3
Discarded PCB is immersed in the nitration mixture that concentration is 3mol/L sulphuric acid and nitric acid, discard PCB and nitration mixture reaction
Temperature is 60 DEG C, reacts 3h, is filtered after the completion of reaction.PCB nonmetallic ingredients to obtaining are crushed, and are sieved,
Granularity is 300 mesh.Charing process temperature is 800 DEG C, cools down, obtain carbide after carbonization 1h.By carbonizing production
1 is pressed with NaOH:5 mass than mix homogeneously, in N2800 DEG C are warming up under protection, 120min is activated, other
Step is with embodiment 1.The porous activated carbon specific surface area obtained in the present embodiment is 3030m2/ g, total pore volume 1.08
cm3The porous activated carbon of/g.
Embodiment 4
Discarded PCB is immersed in the nitration mixture that concentration is 10mol/L sulphuric acid and hydrochloric acid, PCB and nitration mixture quality is discarded
Than for 1:10, discard PCB and nitration mixture reaction temperature be 90 DEG C, react 5h, after the completion of reaction filter.To
The PCB nonmetallic ingredients for arriving are crushed, and are sieved, and granularity is 1000 mesh.Charing process temperature is 1000 DEG C, carbonization
Cool down after 30min, obtain carbide.By carbonizing production and Na2CO3By 1:1 mass than mix homogeneously, in Ar
1000 DEG C are warming up under protection, 300min is activated, other steps are with embodiment 1.The porous obtained in the present embodiment
Activated carbon specific surface area is 1724m2/ g, total pore volume 0.82cm3The porous activated carbon of/g.
Embodiment 5
In being 10mol/L nitric acid by discarded PCB immersion concentration, it is 1 to discard PCB with nitric acid mass ratio:5, discard
PCB and nitric acid reaction temperature be 60 DEG C, react 2h, after the completion of reaction filter.PCB to obtaining is nonmetallic
Component is crushed, and is sieved, and granularity is 500 mesh.Under Ar protections, charing process temperature is 600 DEG C, carbonization 300min
After cool down, obtain carbide.By carbonizing production and K2CO3By 1:4 mass activate 60min than mix homogeneously, its
His step is with embodiment 1.The porous activated carbon specific surface area obtained in the present embodiment is 1314m2/ g, total pore volume 0.87
cm3The porous activated carbon of/g.
Embodiment 6
Discarded PCB is immersed in the nitration mixture that concentration is 0.5mol/L nitric acid and hydrochloric acid, PCB and nitration mixture quality is discarded
Than for 1:3, discard PCB and nitration mixture reaction temperature be 60 DEG C, react 1h, after the completion of reaction filter.To
The PCB nonmetallic ingredients for arriving are crushed, and are sieved, and granularity is 500 mesh.Under Ar protections, charing process temperature is
1000 DEG C, cool down after carbonization 30min, obtain carbide.Carbonizing production is pressed into 1 with NaOH:4 mass ratioes mix
Uniform activation 60min, other steps are with embodiment 1.The porous activated carbon specific surface area obtained in the present embodiment is
2024m2/ g, total pore volume 0.91cm3The porous activated carbon of/g.
Certainly, the present invention can also have various embodiments, in the case of without departing substantially from spirit of the invention and its essence,
Those of ordinary skill in the art can disclosure of the invention make various corresponding changes and deformation, but these phases
The change and deformation answered should all belong to the scope of the claims of the present invention.
Claims (10)
1. a kind of method for preparing porous activated carbon using discarded PCB, comprises the following steps：
(1) with discarded PCB as raw material, by the discarded PCB elder generations inorganic low-kappa numbers of Jing, after filtration, obtain discarded PCB
Non-metallic part, then by the non-metallic part of discarded PCB successively Jing wash, dry, pulverize, sieve, obtain
Powder body；
(2) the powder body carbonization that will be obtained in step (1), makes carbide；
(3) priming reaction is carried out after mixed homogeneously obtained carbide in step (2) with activator, after reaction
Products therefrom Jing pickling, washing are dried, obtain final product porous activated carbon.
2. method according to claim 1, it is characterised in that the mineral acid described in step (1) is sulfur
One or several in acid, hydrochloric acid and nitric acid.
3. method according to claim 1 and 2, it is characterised in that mineral acid is dense described in step (1)
Spend for 0.5～10mol/L, it is 1 to discard PCB with mineral acid mass ratio:1～1:10.
4. method according to claim 1, it is characterised in that described in step (1) by discarded PCB
Reaction temperature used by the inorganic low-kappa numbers of Jing is 20～90 DEG C, and the response time is 30～300min.
5. method according to claim 1, it is characterised in that carbonization temperature scope described in step (2)
For 600～1000 DEG C, 30～300min of carbonization time.
6. method according to claim 1, it is characterised in that the powder body described in step (2) is in protection
Carbonization is carried out under gas；Carbide described in step (3) carries out priming reaction under shielding gas with activator.
7. method according to claim 6, it is characterised in that the shielding gas is nitrogen or argon.
8. method according to claim 1, it is characterised in that carbide described in step (3) and activation
Agent presses 1:1～1:5 mass ratioes mix.
9. the method according to claim 1 or 8, it is characterised in that activator is described in step (3)
NaOH, KOH and Ca (OH)2In one or more, or the activator be NaOH, KOH, Na2CO3
And K2CO3In one or more.
10. method according to claim 1, it is characterised in that the temperature of priming reaction described in step (3)
Spend for 600～1000 DEG C, 30～300min of soak time.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108190887A (en) * | 2017-12-28 | 2018-06-22 | 广州福之源环保科技有限公司 | A kind of method of epoxy resin on recycling waste circuit boards |
| CN109742399A (en) * | 2018-12-18 | 2019-05-10 | 宁波容百新能源科技股份有限公司 | A kind of anode material of lithium-ion battery and preparation method thereof |
| CN110451929A (en) * | 2019-08-27 | 2019-11-15 | 盐城工学院 | The cement base porous filter material and preparation method thereof of waste circuit board non-metal powder preparation |
| CN110660991A (en) * | 2019-09-04 | 2020-01-07 | 江苏理工学院 | Method for preparing F, N co-doped carbon material based on waste circuit board and application |
| CN114249319A (en) * | 2021-12-15 | 2022-03-29 | 安徽农业大学 | Preparation method of waste circuit board active carbon for Congo red adsorption |
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| CN110451929A (en) * | 2019-08-27 | 2019-11-15 | 盐城工学院 | The cement base porous filter material and preparation method thereof of waste circuit board non-metal powder preparation |
| CN110660991A (en) * | 2019-09-04 | 2020-01-07 | 江苏理工学院 | Method for preparing F, N co-doped carbon material based on waste circuit board and application |
| CN114249319A (en) * | 2021-12-15 | 2022-03-29 | 安徽农业大学 | Preparation method of waste circuit board active carbon for Congo red adsorption |
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Application publication date: 20170419 |