CN109453754A - A kind of regeneration method of useless antichlor - Google Patents
A kind of regeneration method of useless antichlor Download PDFInfo
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- CN109453754A CN109453754A CN201710797464.3A CN201710797464A CN109453754A CN 109453754 A CN109453754 A CN 109453754A CN 201710797464 A CN201710797464 A CN 201710797464A CN 109453754 A CN109453754 A CN 109453754A
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- antichlor
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
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Abstract
The invention discloses a kind of regeneration methods of useless antichlor, the following steps are included: (1) impregnates 0~100 DEG C of water of useless antichlor 1~10 time, it is every to complete a dip operation 0.1~10h of needs, it impregnates need to change 0~100 DEG C fresh of water every time；(2) it is drained after taking out the antichlor of step (1), it is spare after 100 ± 5 DEG C of dry 10h；(3) by antichlor to the saturated extent of adsorption of alkali metal, aqueous solution containing alkali metal compound is sprayed on the antichlor of step (2), then dry 10 ± 1h, 4 ± 1h of roasting at 200~700 DEG C at 100 ± 5 DEG C, obtain regeneration antichlor.The regeneration method of the useless antichlor of the present invention, the regeneration effect for the antichlor that gives up is significant, and the chlorosity for regenerating antichlor can be restored to 20~40%；The regeneration method of useless antichlor is simple, it is environmentally protective, it can be achieved that useless antichlor secondary use.
Description
Technical field
The present invention relates to a kind of regeneration methods of useless antichlor, belong to the regeneration field of useless antichlor.
Background technique
Chlorine is the poisonous substance of the common catalyst and adsorbent of industry, will also result in pollution to environment.Since chlorine is with very high
Electron affinity and migration, easily reacted with metal ion, and often migrated downward into process fluid, cause the permanent of catalyst
Property poisoning, and often full bed.
The country puts into more strength in terms of the research of antichlor, and various patented technologies and report emerge one after another, have low
Temperature, room temperature and high temperature modification, the product for some different properties that the country has developed in succession, as T401 series, NC2301 series,
KT407 series, NC series, WDL series, WGL series etc..From the point of view of reported in literature, presently mainly naphtha, light liquid
HCl is removed in hydrocarbon, liquefied petroleum gas.
The development and application of external antichlor is earlier than the country, and there are many foreign countries' antichlor trade mark at present, mainly there is Britain
ICI, the BASF of Germany, the U.S. the companies such as UCI product.For ICI59-3 using aluminium oxide as carrier, sodium oxide molybdena is that active component can
For natural gas or naphtha dechlorination；For the G32-W of UCI company using active carbon as carrier, copper chromium is that active component is used for liquid third
The dechlorination of dilute raw material.Foreign countries have done more in the developmental research field for widening antichlor in recent years other than industrialized antichlor
Further work, the active component research of antichlor have also been expanded to Fe2O3、K2O, Cu, Mn, Mg, V, Ni etc..Meanwhile it is right
Antichlor reaction mechanism has also carried out the research of the removing hydrogen chloride in in-depth study, especially coal gas of high temperature and flue gas more
It is active.
Typically, when entire antichlor bed penetrates, saturation is had not been reached yet in the antichlor of lower part, in order to improve lower part
The utilization rate of antichlor, Chinese patent CN101724435 will first contain fluorocarbon oil product or gas is passed through one and satisfies equipped with not up to absorption
The upstream dechlorination tank of the antichlor bed of sum, then pass through a downstream dechlorination contacted with upstream dechlorination tank and new antichlor is housed
Tank.This method can efficiently use the absorption chlorosity of antichlor, saturation chlorosity be reached or approach, to greatly improve antichlor
Utilization rate.When the dechlorination tank for carrying out dechlorination operation penetrates, feed change flow direction makes raw material first pass through the dechlorination that bed penetrates
Tank, then it is passed through the dechlorination tank for more renewing antichlor for being serially connected with downstream, when it will reach penetrate chlorosity again, repeat above-mentioned
Operation.This method is to extend the service life of antichlor, and there is no the processing for fundamentally solving the problems, such as antichlor.
And for the processing of useless antichlor, landfill method is generallyd use at present, and processing cost is higher, mishandling easily to underground
Water body pollutes.The regeneration of useless antichlor is also in blank stage.
Summary of the invention
In order to solve the defects of antichlor can not regenerate in the prior art, the present invention provides a kind of regeneration side of useless antichlor
Method.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows:
A kind of regeneration method of useless antichlor, comprising the following steps:
(1) 0~100 DEG C of water of useless antichlor is impregnated 1~10 time, dip operation needs 0.1 of every completion~
10h impregnates need to change 0~100 DEG C fresh of water every time；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 ± 5 DEG C of dry 10h；
(3) step is sprayed on by the aqueous solution containing alkali metal compound to the saturated extent of adsorption of alkali metal by antichlor
(2) on antichlor, then dry 10 ± 1h, 4 ± 1h of roasting at 200~700 DEG C at 100 ± 5 DEG C, obtain regeneration dechlorination
Agent.
The present invention is eluted the chlorine in useless antichlor using the method for washing, then pass through by control regeneration condition
The method for spraying the aqueous solution containing alkali metal compound introduces alkali metal compound, to improve the chlorosity of regeneration antichlor.
In order to further increase chlorosity, in step (1), the temperature of water is 10~70 DEG C.Further preferably 20~40 DEG C.
In order to further increase regeneration efficiency, while energy saving, the matter of the water of each dip operation described in step (1)
Amount is 0.5~5 times of useless antichlor quality, is preferably 1~2 times.
In order to further increase regeneration efficiency, the soaking time in step (1) is 0.5~5h.Preferably soaking time is 1
~2h.
In order to further increase regeneration efficiency, at the same it is energy saving, and immersion number described in step (1) is 2~7 times.Compared with
Excellent immersion number is 3~5 times.
In order to further increase regeneration efficiency, in step (3), alkali metal compound KOH, KNO3、K2CO3, potassium acetate,
NaOH、NaNO3、Na2CO3, at least one of sodium acetate.
In order to improve the chlorosity after useless antichlor regeneration, the quality of the aqueous solution of alkali metal compound described in step (3)
Concentration is 5~40%.Preferably mass concentration is 10~20%.
In order to further increase the chlorosity after useless antichlor regeneration, maturing temperature described in step (3) is 300~600 DEG C.
Preferably temperature is 400~500 DEG C.
The chlorosity of the resulting regeneration antichlor of above-mentioned steps (4) is 20~40%.
The unmentioned technology of the present invention is referring to the prior art.
The regeneration method of the useless antichlor of the present invention, the regeneration effect for the antichlor that gives up is significant, and the chlorosity for regenerating antichlor can be extensive
Again to 20~40%；The regeneration method of useless antichlor is simple, it is environmentally protective, it can be achieved that useless antichlor secondary use.
Specific embodiment
For a better understanding of the present invention, below with reference to the embodiment content that the present invention is furture elucidated, but it is of the invention
Content is not limited solely to the following examples.
Embodiment 1
(1) 0 DEG C of tap water of the spherical useless antichlor of 100g is impregnated 1 time, completes 1 dip operation and needs 0.1h, from
The quality of water is 0.5 times of useless antichlor；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to the saturated extent of adsorption of KOH (namely the quality dosage of KOH aqueous solution be saturated extent of adsorption divided by
Concentration), the aqueous solution by mass concentration for 5% KOH is sprayed on the antichlor of step (2), through 100 DEG C of dry 10h, 200
DEG C roasting 4h after obtain regeneration antichlor.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 2
(1) 100g strip is given up into antichlor with tap water immersion 10 times of 100 DEG C, every dip operation of completion needs 10
H impregnates replace fresh 100 DEG C of tap water every time, and the quality of the tap water that each dip operation uses is the 5 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to KNO3Saturated extent of adsorption, by mass concentration be 40% KNO3Aqueous solution be sprayed on step
(2) on antichlor, regeneration antichlor is obtained after 100 DEG C of dry 10h, 700 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 3
(1) 10 DEG C of tap water of the spherical useless antichlor of 100g is impregnated 2 times, it is every to complete a dip operation needs
0.5h impregnates replace 10 DEG C fresh of tap water every time, and the quality for the tap water that each dip operation uses is the antichlor that gives up
1 times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to K2CO3Saturated extent of adsorption, by mass concentration be 10% K2CO3Aqueous solution be sprayed on step
Suddenly on the antichlor of (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 300 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 4
(1) 70 DEG C of tap water of the spherical useless antichlor of 100g to be impregnated 7 times, dip operation of every completion needs 5h,
It impregnates every time and replaces fresh 70 DEG C of tap water, the quality of the tap water that each dip operation uses is the 2 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) saturated extent of adsorption for pressing antichlor Dichlorodiphenyl Acetate potassium, by the aqueous solution spraying for the potassium acetate that mass concentration is 20%
On the antichlor of step (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 600 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 5
(1) 20 DEG C of tap water of the spherical useless antichlor of 100g to be impregnated 3 times, dip operation of every completion needs 1h,
It impregnates every time and replaces fresh 20 DEG C of tap water, the quality of the tap water that each dip operation uses is the 1 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to the saturated extent of adsorption of NaOH, the aqueous solution by mass concentration for 15% NaOH is sprayed on step
Suddenly on the antichlor of (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 400 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 6
(1) 40 DEG C of tap water of the spherical useless antichlor of 100g to be impregnated 5 times, dip operation of every completion needs 2h,
It impregnates every time and replaces fresh 40 DEG C of tap water, the quality of the tap water that each dip operation uses is the 2 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to NaNO3Saturated extent of adsorption, by mass concentration be 15% NaNO3Aqueous solution be sprayed on step
Suddenly on the antichlor of (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 500 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 7
(1) 30 DEG C of tap water of the spherical useless antichlor of 100g is impregnated 3 times, it is every to complete a dip operation needs
1.5h impregnates replace 30 DEG C fresh of tap water every time, and the quality for the tap water that each dip operation uses is the antichlor that gives up
1 times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to Na2CO3Saturated extent of adsorption, by mass concentration be 20% Na2CO3Aqueous solution be sprayed on
On the antichlor of step (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 450 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 8
(1) 40 DEG C of tap water of the spherical useless antichlor of 100g is impregnated 3 times, it is every to complete a dip operation needs
1.5h impregnates replace 40 DEG C fresh of tap water every time, and the quality for the tap water that each dip operation uses is the antichlor that gives up
1 times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) saturated extent of adsorption for pressing antichlor Dichlorodiphenyl Acetate sodium, by the aqueous solution spraying for the sodium acetate that mass concentration is 18%
On the antichlor of step (2), regeneration antichlor is obtained after 100 DEG C of dry 10h, 500 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 9
(1) 100g strip is given up into antichlor with tap water immersion 4 times of 40 DEG C, dip operation of every completion needs 2h,
It impregnates every time and replaces fresh 40 DEG C of tap water, the quality of the tap water that each dip operation uses is the 1 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to NaOH and Na2CO3Saturated extent of adsorption, by mass concentration be 20% NaOH and Na2CO3's
(concentration of NaOH is 5%, Na to aqueous solution2CO3Concentration be 15%) be sprayed on the antichlor of step (2), through 100 DEG C of dryings
Regeneration antichlor is obtained after 10h, 500 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Embodiment 10
(1) 30 DEG C of tap water of the spherical useless antichlor of 100g to be impregnated 5 times, dip operation of every completion needs 1h,
It impregnates every time and replaces fresh 30 DEG C of tap water, the quality of the tap water that each dip operation uses is the 1 of useless antichlor
Times；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 DEG C of dry 10h；
(3) by antichlor to KOH and Na2CO3Saturated extent of adsorption, by mass concentration be 20% KOH and Na2CO3Water
(concentration of KOH is 10%, Na to solution2CO3Concentration be 10%) be sprayed on the antichlor of step (2), through 100 DEG C of dryings
Regeneration antichlor is obtained after 10h, 450 DEG C of roasting 4h.
The regeneration condition of the present embodiment and the chlorosity for regenerating antichlor are shown in Table 1.
Comparative example 1
Compared with Example 7, only with 3 tap water dip operations, but without the Na of spraying 20%2CO3Aqueous solution.
(1) 30 DEG C of tap water of the spherical useless antichlor of 100g is impregnated 3 times, it is every to complete a dip operation needs
1.5h impregnates replace 30 DEG C fresh of tap water every time, and the quality for the tap water that each dip operation uses is the antichlor that gives up
1 times；
(2) it is drained after taking out the antichlor of step (1), it is de- that regeneration is obtained after 100 DEG C of dry 10h, 450 DEG C of roasting 4h
Chlorine agent.
The regeneration condition of this comparative example and the chlorosity for regenerating antichlor are shown in Table 1.
Comparative example 2
Compared with Example 7, only with the Na of spraying 20%2CO3Aqueous solution operation, but impregnated without 3 tap water
Operation.
(1) the spherical useless antichlor of 100g is spare after 100 DEG C of dry 10h；
(2) by antichlor to Na2CO3Saturated extent of adsorption, by mass concentration be 20% Na2CO3Aqueous solution be sprayed on
On above-mentioned useless antichlor, regeneration antichlor is obtained after 100 DEG C of dry 10h, 450 DEG C of roasting 4h.
The regeneration condition of this comparative example and the chlorosity for regenerating antichlor are shown in Table 1.
Comparative example 3
According to a kind of antichlor of Chinese patent CN103386244A (antichlor and preparation method thereof) report and its preparation
Method, the antichlor are prepared by following material: carrier 15~70%；Active component 15~60%；Pore creating material 1~
10%；Extrusion aid 1~5%；Binder 2~10%；Carrier is salt of weak acid, kaolin, boehmite or Al2O3In at least
It is a kind of；Above-mentioned material is mixed, water kneading, extrusion, drying and roasting are added.
The antichlor is high to high concentration or low concentration HCl adsorption efficiency at normal temperature, and removal precision is high, chlorosity is up to
30% or more.
From the point of view of the comparison of embodiment and comparative example, the present invention is eluted the chlorine in useless antichlor using the method first washed
Get off, then the method by introducing alkali metal compound, improve the chlorosity of regeneration antichlor, the regeneration effect for the antichlor that gives up is aobvious
It writes, the chlorosity for regenerating antichlor can be restored to 20~40%, can achieve the level of the fresh antichlor of existing patent report.
Table 1 give up antichlor regeneration condition and regenerate antichlor chlorosity
Claims (9)
1. a kind of regeneration method of useless antichlor, it is characterised in that: the following steps are included:
(1) 0~100 DEG C of water of useless antichlor is impregnated 1~10 time, it is every to complete a dip operation 0.1~10h of needs, often
Secondary immersion needs to change 0~100 DEG C fresh of water；
(2) it is drained after taking out the antichlor of step (1), it is spare after 100 ± 5 DEG C of dry 10h；
(3) step (2) is sprayed on by the aqueous solution containing alkali metal compound to the saturated extent of adsorption of alkali metal by antichlor
On antichlor, then dry 10 ± 1h, 4 ± 1h of roasting at 200~700 DEG C at 100 ± 5 DEG C, obtain regeneration antichlor.
2. the regeneration method of useless antichlor described in accordance with the claim 1, it is characterised in that: in step (1), the temperature of water is 10
~70 DEG C.
3. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: each leaching described in step (1)
The quality for steeping the water of operation is 0.5~5 times of useless antichlor.
4. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: when immersion described in step (1)
Between be 0.5~5h.
5. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: immersion described in step (1) time
Number is 2~7 times.
6. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: in step (3), alkali metal
Closing object is KOH, KNO3、K2CO3, potassium acetate, NaOH, NaNO3、Na2CO3Or at least one of sodium acetate.
7. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: alkali metal described in step (3)
The mass concentration of the aqueous solution of compound is 5~40%.
8. the regeneration method of useless antichlor according to claim 1 or 2, it is characterised in that: roasting temperature described in step (3)
Degree is 300~600 DEG C.
9. regeneration antichlor according to claim 1 or 2, it is characterised in that: the chlorine of the resulting regeneration antichlor of step (4)
Hold is 20~40%.
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| CN201710797464.3A CN109453754A (en) | 2017-09-06 | 2017-09-06 | A kind of regeneration method of useless antichlor |
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| CN201710797464.3A CN109453754A (en) | 2017-09-06 | 2017-09-06 | A kind of regeneration method of useless antichlor |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101116807A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Gas dechlorinating agent and its preparing method |
| CN102851494A (en) * | 2012-08-29 | 2013-01-02 | 江西自立资源再生有限公司 | Chlorine removal method for recycle use |
| CN103272410A (en) * | 2013-05-31 | 2013-09-04 | 青海华信冶炼有限公司 | Circular removal process for chloride ions in manganese sulfate electrolyte and application of cuprous hydroxide as dechlorinating agent |
| CN103328095A (en) * | 2011-06-27 | 2013-09-25 | 雪佛龙美国公司 | Recovery of alkyl chloride adsorbtion capacity by basic solution treatment of spent adsorbent |
| CN105498682A (en) * | 2015-12-07 | 2016-04-20 | 上海绿强新材料有限公司 | Mesoporous chloride scavenging agent and preparation method thereof |
-
2017
- 2017-09-06 CN CN201710797464.3A patent/CN109453754A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101116807A (en) * | 2006-07-31 | 2008-02-06 | 中国石油化工股份有限公司 | Gas dechlorinating agent and its preparing method |
| CN103328095A (en) * | 2011-06-27 | 2013-09-25 | 雪佛龙美国公司 | Recovery of alkyl chloride adsorbtion capacity by basic solution treatment of spent adsorbent |
| CN102851494A (en) * | 2012-08-29 | 2013-01-02 | 江西自立资源再生有限公司 | Chlorine removal method for recycle use |
| CN103272410A (en) * | 2013-05-31 | 2013-09-04 | 青海华信冶炼有限公司 | Circular removal process for chloride ions in manganese sulfate electrolyte and application of cuprous hydroxide as dechlorinating agent |
| CN105498682A (en) * | 2015-12-07 | 2016-04-20 | 上海绿强新材料有限公司 | Mesoporous chloride scavenging agent and preparation method thereof |
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