CN105148896B - A kind of activated carbon recycling method in useless mercury catalyst - Google Patents
A kind of activated carbon recycling method in useless mercury catalyst Download PDFInfo
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- CN105148896B CN105148896B CN201510481291.5A CN201510481291A CN105148896B CN 105148896 B CN105148896 B CN 105148896B CN 201510481291 A CN201510481291 A CN 201510481291A CN 105148896 B CN105148896 B CN 105148896B
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- activated carbon
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Abstract
The present invention relates to activated carbon utilization technology field in useless mercury catalyst, activated carbon recycling method in especially a kind of useless mercury catalyst, after useless mercury catalyst is first mixed with water, ultrasonic processor is used to handle again, adjust pH value, it is filtered under ultrasound environments again, so cause the PVC compositions in activated carbon space obtain it is ultrasonically treated come off, and be shed in solution；Pass it through again after washing, screening process, so that exposed PVC compositions and other impurities in activated carbon surface is departed from, it is calcination processing at 850 900 DEG C to be placed on temperature again, and then cause the gap of activated carbon to obtain comprehensively exposed, and then enhance the activity of activated carbon, the preparation of mercury catalyst is used it for again, and reduction mercury catalyst prepares cost, also reduces the probability of useless mercury catalyst exhaust emission environment.
Description
Technical field
The present invention relates to activated carbon utilization technology field in useless mercury catalyst, activated carbon in especially a kind of useless mercury catalyst
Recycling method.
Background technology
Due to China's oil shortage of resources, rich coal resources, the PVC of carbide production accounts for main share, accounts for PVC total
The 70% of amount.Mercuric chloride catalyst (being commonly called as mercury catalyst) produces acetylene and hydrogen chloride gas synthesis vinyl chloride thereof in PVC as carbide
(VCM) catalyst, is to make carrier, mercury chloride as active material using activated carbon, mercury chloride is carried on into activated carbon surface.Mercury is touched
After a certain period of use time, its activity decrease need to be changed matchmaker, the useless mercury catalyst changed, and general chloride containing mercury 2%~
5% or so, the severe contamination of environment can still be caused in the environment by being discharged, therefore, after useless mercury catalyst is handled
Carrying out discharge again becomes She Gong manufacturing enterprises focus of attention；In the prior art, there is researcher by useless mercury catalyst
After reason, activated carbon in useless mercury catalyst is also reclaimed while reclaiming mercury, and activated carbon is back to useless mercury catalyst produced and processed
Cheng Zhong, and then the manufacturing cost to the mercury catalyst that gives up is reduced, the discharge capacity of discarded object is reduced, and then saved cost and reduced ring
Pollute in border.
But because one of activated carbon its deactivation cause in the mercury catalyst that gives up is exactly the surface of activated carbon by covering so that
Activated carbon specific surface area reduction, causing the adsorption capacity of activated carbon reduce, in turn result in mercury catalyst mercury chloride composition volatilize,
Scatter and disappear so that turn into useless mercury catalyst after mercury catalyst loss of activity；And as described above, mercury catalyst is the preparation work for polyvinyl chloride
As catalyst in skill, and polyvinyl chloride (PVC) have excellent heat resistance, wearability, resistance to chemical corrosion the features such as, when
In process of production, polyvinyl chloride will be covered in the surface of mercury catalyst, and then so that after mercury chloride volatilization, polyvinyl chloride is just
It is covered in the surface of activated carbon, or even reveals among the space of activated carbon, blocks the space of activated carbon, in turn result in activated carbon
Loss of activity, therefore, while activated carbon is recycled, it is necessary to handle activated carbon after so that activated carbon
The PVC compositions on space or surface disappear, and could cause the activity of the activated carbon recycled and be strengthened, and then contribute to system
The activity raising of standby new mercury catalyst；Therefore, there is substantial amounts of researcher to engage in the research of the technology, such as Patent No.
201410034603.3《A kind of method for recycling useless mercury catalyst》Useless mercury catalyst is added to the water, control temperature 70 C~
95 DEG C, the lower thermosol pretreatment of stirring adjusts pH value 1~3, through 10min~60min it is ultrasonically treated after take advantage of a favourable situation filtering, or in ultrasound
Filtered in, the mercury chloride and phosphorus, sulphur impurity that depart from from activated carbon surface is separated in time with activated carbon.After filtering, obtain
Activated carbon is scrubbed, screening, the preparation for mercury catalyst；Obtained mercurous filtrate, controls temperature 50 C~90 DEG C, adds and neutralizes
Agent adjusts pH value to 6~8, reacts mercury ion in 30min~90min, solution and is fully converted into mercury oxide precipitation, mercury catalyst poisoning
Thing phosphorus, sulphur are still remained in solution.Although this method improves the active component of activated carbon to a certain extent, but is difficult to
The space of activated carbon is reached complete exposed, in turn resulting in the active component of activated carbon can not still maximize；And at place
Substantial amounts of discharging of waste liquid can be also produced during reason, the pollution of environment is in turn resulted in；For another example Patent No. 201210287604.X
's《Waste active carbon mercury catalyst recovery process》, waste active carbon mercury catalyst recovery process, it comprises the following steps：A, by waste active carbon
Mercury catalyst removes residue through vibratory sieve；B, using the above-mentioned waste active carbon mercury catalyst by removing residue as activated carbon raw material, with
Technique afterwards is as the technique with new Activated Carbon Production mercury catalyst；The technique is only by physical can take off in activated carbon
From composition depart from fall, cause activated carbon space and stick to activated carbon surface chemical composition depart from fall, and then
The active situation of activated carbon is caused still to be difficult to ensure that；For another example Patent No. 201410741444.0《It is a kind of from useless mercury catalyst
The equipment and recovery method of mercury and activated carbon are reclaimed in environmental protection in multicomponent》Be by material to the material trough on chain transfer；
Electroreduction is carried out to fully loaded material trough；Ultrasonic oscillator is cleaned；Second material trough enters electroreduction station, electricity also simultaneously
It is former；Discharging, return；Material enters active carbon regenerating unit, produces regenerated carbon；Periodically open and put mercury valve.This method its
Energy consumption is relatively low, complex operation, and is also difficult to eliminate in PVC adsorbents, causes the activity of activated carbon to be difficult to
To comprehensive raising.
It can be seen that, above-mentioned technique in the prior art, in the recovery processing technique of activated carbon, exist be difficult to by
PVC material is exposed from the space of activated carbon to be come, and then causes still to exist and fill out in the space of the activated carbon recycled
The state filled so that the activity of activated carbon is difficult to be improved, and in the prior art for the waste liquid that is produced after processing not
Further to be handled so that the discharge capacity of waste liquid is larger, solution causes the energy in the pollution of environment, and processing removal process
Consumption is larger, and technological process is complex, causes recycling cost higher.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides activated carbon in a kind of useless mercury catalyst and followed
Ring recoverying and utilizing method.
It is achieved particular by following technical scheme：
Activated carbon recycling method, comprises the following steps in a kind of useless mercury catalyst：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 10-30min, adjustment temperature is 110-
130 DEG C of stir process 10-30min, then pH value is adjusted for 3.5-4.3, then be placed in ultrasonic filters, filtration treatment is obtained
Obtain filter cake and filtrate；
(2) by filter cake after washing, screening process, then it is placed on distillation in the retort that temperature is 850-900 DEG C
20-30min is handled, activated carbon, the preparation for mercury catalyst is obtained；The temperature of filtrate is adjusted to 70-85 DEG C, adjustment pH value is
6.9-7.3, reaction treatment 10-25min, then be placed in ultrasonic filters, filtration treatment, obtain mercurous filter cake and waste liquid；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is (3-5) by waste liquid and water：(0.9-1.3) is mixed
After conjunction, then use it for step 1) used with useless mercury catalyst mixing circulation, treat that the mercury content in final waste liquid is less than 0.01%
When, the production of the production technology progress fertilizer containing phosphatic manure will be sent into after its concentration.
Described useless mercury catalyst, its mixing ratio with water, is by quality ratio 1：(5-7).
Described ultrasonic processor, it uses ultrasonically treated frequency for 10-3000Hz.
Described ultrasonic filters, its supersonic frequency used in filter process is 25-47Hz.
Described step 1), it adjusts pH value and uses sodium carbonate, sodium bicarbonate solid or liquid.
Described step 2) it adjusts pH value and uses disodium hydrogen phosphate, sodium dihydrogen phosphate.
Compared with prior art, technique effect of the invention is embodied in：
After useless mercury catalyst is first mixed with water, then used ultrasonic processor to handle, adjustment pH value, then by its
Filtered under ultrasound environments, so cause the PVC compositions in activated carbon space obtain it is ultrasonically treated come off, and be shed to solution
In；Pass it through again after washing, screening process so that exposed PVC compositions and other impurities in activated carbon surface is taken off
From, then it is calcination processing at 850-900 DEG C to be placed on temperature, and then cause the gap of activated carbon to obtain comprehensively exposed, enter
And the activity of activated carbon is enhanced, then the preparation of mercury catalyst is used it for, reduction mercury catalyst prepares cost, also reduces useless mercury and touches
The probability of matchmaker's exhaust emission environment.
The present invention especially reacts by filtrate is carried out into pH adjustment, and the filtration treatment in ultrasonic filters so that filter
Mercurous composition in liquid is precipitated in neutral environment, and other impurities are dissolved in filtrate, so reach isolate it is mercurous into
Point, and mercurous composition is used for the preparation of mercury catalyst, the cost of mercury catalyst preparation is reduced, environmental pollution rate is also reduced；
Also, it is of the invention further by waste liquid progress return processing so that the composition such as phosphorus, sulphur in waste liquid obtains richness
Collection, the relative amount of mercury composition is reduced, and then cause mercury composition obtained in follow-up discharge process constantly reduction and
Reduce, so whne its by it to less than 0.01% when, then use it for the production containing phosphatic manure, and then reduce the discharge of waste liquid
Amount, adds the added value of product of technique, improves the additional profit of technique, reduces the place to the mercury catalyst recovered carbon that gives up
Cost is managed, the pollution rate of mercury composition discharge in the environment is also reduced.
The further activated carbon for preparing such scheme of the invention carries out the processing of activity experiment, by it to coloring matter
Absorption and fresh activated carbon and Patent No. 201410034603.3《A kind of method for recycling useless mercury catalyst》
The activated carbon of preparation carries out the test experience of input ratio, and specific experimental method is：
Coloured waste liquid 1000g is weighed, and the coloured waste liquids of the 1000g are divided into 50 groups, every group of 20g；Wherein using the present invention
Embodiment 1 (10 groups), embodiment 2 (10 groups), embodiment 3 (10 groups), embodiment 4 (10 groups) and Patent No.
201410034603.3 activated carbons (5 groups) prepared absorb coloured waste liquid with fresh (5 groups) inputs of activated carbon, and record input
The contrast test of amount, its result is that 1- of embodiment of the present invention embodiments 4 prepare activated carbon and are used for being higher by than fresh activity charcoal respectively
1.3-2.1%, 1.7-1.9%, 2.1-2.5%, 1.5-2.4%, activated carbon ratio prepared by Patent No. 201410034603.3
Fresh activity charcoal is higher by 18.3-25.7%, it can thus be seen that the activity of activated carbon product prepared by the present invention obtains larger journey
The raising of degree, and cause the activity of activated carbon to tend to fresh activity charcoal；Also, the present invention is by the technique in preparation technology again
The different controls of parameter, and then make it that the functional component of the activated carbon of recycling is more excellent under different conditions, especially
The change of temperature parameter and ultrasonically treated degree in processing procedure so that the deployment conditions and mistake of activated carbon in the solution
The deployment conditions of PVC leachables during filter are differed, and then the level of activity of the activated carbon recycled is differed.
Embodiment
Limited with reference to specific embodiment technical scheme is further, but claimed
Scope is not only limited to made description.
Embodiment 1
Activated carbon recycling method, comprises the following steps in a kind of useless mercury catalyst：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 10min, adjustment temperature is 110 DEG C of stirrings
10min is handled, then it is 3.5 to adjust pH value, then be placed in ultrasonic filters, filtration treatment, obtain filter cake and filtrate；
(2) by filter cake after washing, screening process, then it is placed on distillation processing in the retort that temperature is 850 DEG C
20min, obtains activated carbon, the preparation for mercury catalyst；The temperature of filtrate is adjusted to 70 DEG C, adjustment pH value is at 6.9, reaction
10min is managed, then is placed in ultrasonic filters, filtration treatment, mercurous filter cake and waste liquid is obtained；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is 3 by waste liquid and water：After 0.9 mixing, then will
It is used for step 1) used with useless mercury catalyst mixing circulation, it is when the mercury content in final waste liquid is less than 0.01%, its is dense
The production that the production technology containing phosphatic manure carries out fertilizer is sent into after contracting processing.
Described useless mercury catalyst, its mixing ratio with water, is by quality ratio 1：5.
Described ultrasonic processor, it uses ultrasonically treated frequency for 10Hz.
Described ultrasonic filters, its supersonic frequency used in filter process is 25Hz.
Described step 1), it adjusts pH value and uses sodium carbonate solid.
Described step 2) it adjusts pH value and uses disodium hydrogen phosphate.
Embodiment 2
Activated carbon recycling method, comprises the following steps in a kind of useless mercury catalyst：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 30min, adjustment temperature is 130 DEG C of stirrings
30min is handled, then it is 4.3 to adjust pH value, then be placed in ultrasonic filters, filtration treatment, obtain filter cake and filtrate；
(2) by filter cake after washing, screening process, then it is placed on distillation processing in the retort that temperature is 900 DEG C
30min, obtains activated carbon, the preparation for mercury catalyst；The temperature of filtrate is adjusted to 85 DEG C, adjustment pH value is at 7.3, reaction
25min is managed, then is placed in ultrasonic filters, filtration treatment, mercurous filter cake and waste liquid is obtained；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is 5 by waste liquid and water：After 1.3 mixing, then will
It is used for step 1) used with useless mercury catalyst mixing circulation, it is when the mercury content in final waste liquid is less than 0.01%, its is dense
The production that the production technology containing phosphatic manure carries out fertilizer is sent into after contracting processing.
Described useless mercury catalyst, its mixing ratio with water, is by quality ratio 1：7.
Described ultrasonic processor, it uses ultrasonically treated frequency for 3000Hz.
Described ultrasonic filters, its supersonic frequency used in filter process is 47Hz.
Described step 1), it adjusts pH value and uses sodium bicarbonate solid.
Described step 2) it adjusts pH value and uses sodium dihydrogen phosphate.
Embodiment 3
Activated carbon recycling method, comprises the following steps in a kind of useless mercury catalyst：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 20min, adjustment temperature is 120 DEG C of stirrings
20min is handled, then it is 3.9 to adjust pH value, then be placed in ultrasonic filters, filtration treatment, obtain filter cake and filtrate；
(2) by filter cake after washing, screening process, then it is placed on distillation processing in the retort that temperature is 890 DEG C
25min, obtains activated carbon, the preparation for mercury catalyst；The temperature of filtrate is adjusted to 78 DEG C, adjustment pH value is at 7.1, reaction
15min is managed, then is placed in ultrasonic filters, filtration treatment, mercurous filter cake and waste liquid is obtained；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is 4 by waste liquid and water：1 mixing after, then by its
For step 1) used with useless mercury catalyst mixing circulation, when the mercury content in final waste liquid is less than 0.01%, concentrated
The production that the production technology containing phosphatic manure carries out fertilizer is sent into after processing.
Described useless mercury catalyst, its mixing ratio with water, is by quality ratio 1：:6.
Described ultrasonic processor, it uses ultrasonically treated frequency for 1000Hz.
Described ultrasonic filters, its supersonic frequency used in filter process is 29Hz.
Described step 1), it adjusts pH value and uses sodium carbonate liquid.
Described step 2) it adjusts pH value and uses disodium hydrogen phosphate, sodium dihydrogen phosphate according to 1:1:Mixture.
Embodiment 4
Activated carbon recycling method, comprises the following steps in a kind of useless mercury catalyst：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 15min, adjustment temperature is 125 DEG C of stirrings
25min is handled, then it is 4.1 to adjust pH value, then be placed in ultrasonic filters, filtration treatment, obtain filter cake and filtrate；
(2) by filter cake after washing, screening process, then it is placed on distillation processing in the retort that temperature is 860 DEG C
29min, obtains activated carbon, the preparation for mercury catalyst；The temperature of filtrate is adjusted to 73 DEG C, adjustment pH value is at 7.1, reaction
20min is managed, then is placed in ultrasonic filters, filtration treatment, mercurous filter cake and waste liquid is obtained；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is 5 by waste liquid and water：After 0.9 mixing, then will
It is used for step 1) used with useless mercury catalyst mixing circulation, it is when the mercury content in final waste liquid is less than 0.01%, its is dense
The production that the production technology containing phosphatic manure carries out fertilizer is sent into after contracting processing.
Described useless mercury catalyst, its mixing ratio with water, is by quality ratio 1：7.
Described ultrasonic processor, it uses ultrasonically treated frequency for 500Hz.
Described ultrasonic filters, its supersonic frequency used in filter process is 28Hz.
Described step 1), it adjusts pH value and uses sodium acid carbonate liquid.
Described step 2) it adjusts pH value and uses sodium dihydrogen phosphate solid.
Claims (6)
1. a kind of activated carbon recycling method in useless mercury catalyst, it is characterised in that comprise the following steps：
(1) useless mercury catalyst is added to the water, and handled using ultrasonic processor after 10-30min, adjustment temperature is 110-130 DEG C
Stir process 10-30min, then pH value is adjusted for 3.5-4.3, then be placed in ultrasonic filters, filtration treatment, obtain filter cake
With filtrate；
(2) by filter cake after washing, screening process, then it is placed on calcination processing in the retort that temperature is 850-900 DEG C
20-30min, obtains activated carbon, the preparation for mercury catalyst；The temperature of filtrate is adjusted to 70-85 DEG C, adjustment pH value is 6.9-
7.3, reaction treatment 10-25min, then be placed in ultrasonic filters, filtration treatment, obtain mercurous filter cake and waste liquid；
(3) mercurous filter cake is used for the preparation of mercury catalyst, according to mass ratio is (3-5) by waste liquid and water：(0.9-1.3) is mixed
Afterwards, then use it for step 1) used with useless mercury catalyst mixing circulation, when the mercury content in final waste liquid is less than 0.01%,
The production of the production technology progress fertilizer containing phosphatic manure will be sent into after its concentration.
2. activated carbon recycling method in the mercury catalyst that gives up as claimed in claim 1, it is characterised in that described useless mercury
Catalyst, its mixing ratio with water, is by quality ratio 1：(5-7).
3. activated carbon recycling method in the mercury catalyst that gives up as claimed in claim 1, it is characterised in that described ultrasound
Processor, it uses ultrasonically treated frequency for 10-3000Hz.
4. activated carbon recycling method in the mercury catalyst that gives up as claimed in claim 1, it is characterised in that described ultrasound
Filter, its supersonic frequency used in filter process is 25-47Hz.
5. activated carbon recycling method in the mercury catalyst that gives up as claimed in claim 1, it is characterised in that described step
1), it adjusts pH value and uses sodium carbonate, sodium bicarbonate solid or liquid.
6. activated carbon recycling method in the mercury catalyst that gives up as claimed in claim 1, it is characterised in that described step
2) it adjusts pH value and uses disodium hydrogen phosphate, sodium dihydrogen phosphate.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773087A (en) * | 2012-08-02 | 2012-11-14 | 长葛市九州化工有限公司 | Method for recycling wastewater from preparation of mercury catalyst |
| CN102814173A (en) * | 2012-08-03 | 2012-12-12 | 长葛市九州化工有限公司 | Waste active carbon mercury catalyst recovery process |
| CN102962033A (en) * | 2012-11-23 | 2013-03-13 | 那风换 | Method for synchronously recovering mercuric chloride, metal salt and active carbon in spent catalyst |
| CN103693676A (en) * | 2013-12-12 | 2014-04-02 | 毛振华 | Waste mercury catalyst recovery technology and waste mercury catalyst recovery device |
| CN103803638A (en) * | 2014-01-25 | 2014-05-21 | 中南大学 | Method for recycling waste mercury catalyst |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7507736B2 (en) * | 2007-02-07 | 2009-03-24 | Hoffmann-La Roche Inc. | Indol-2-yl-piperazin-1-yl-methanone derivatives |
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- 2015-08-03 CN CN201510481291.5A patent/CN105148896B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102773087A (en) * | 2012-08-02 | 2012-11-14 | 长葛市九州化工有限公司 | Method for recycling wastewater from preparation of mercury catalyst |
| CN102814173A (en) * | 2012-08-03 | 2012-12-12 | 长葛市九州化工有限公司 | Waste active carbon mercury catalyst recovery process |
| CN102962033A (en) * | 2012-11-23 | 2013-03-13 | 那风换 | Method for synchronously recovering mercuric chloride, metal salt and active carbon in spent catalyst |
| CN103693676A (en) * | 2013-12-12 | 2014-04-02 | 毛振华 | Waste mercury catalyst recovery technology and waste mercury catalyst recovery device |
| CN103803638A (en) * | 2014-01-25 | 2014-05-21 | 中南大学 | Method for recycling waste mercury catalyst |
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