CN110560020A - Method for recycling and utilizing active carbon - Google Patents
Method for recycling and utilizing active carbon Download PDFInfo
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- CN110560020A CN110560020A CN201910905145.9A CN201910905145A CN110560020A CN 110560020 A CN110560020 A CN 110560020A CN 201910905145 A CN201910905145 A CN 201910905145A CN 110560020 A CN110560020 A CN 110560020A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
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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
- B01J20/3416—Regenerating or reactivating of sorbents or filter aids comprising free carbon, e.g. activated carbon
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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
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
- C01B32/36—Reactivation or regeneration
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a method for recycling and utilizing water treatment agent HEDP decolorant activated carbon, which comprises the steps of firstly mixing the recycled activated carbon with pure water in an activated carbon treatment kettle, washing the mixture with water, then performing filter pressing separation, obtaining washing liquid rich in hydroxyethylidene diphosphonic acid, using the washing liquid for HEDP production, mixing the obtained washed activated carbon with a certain amount of hydrogen peroxide water, performing regeneration, filter pressing separation and other steps, using the obtained regenerated activated carbon for decoloring the hydroxyethylidene diphosphonic acid, and using the obtained regenerated liquid for compound product production. The method not only recovers the hydroxyethylidene diphosphonic acid in the recovered activated carbon, improves the resource utilization rate, saves energy, reduces consumption, greatly reduces the usage amount of the activated carbon and the output amount of the recovered activated carbon, does not generate three wastes, and is green and environment-friendly.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for recycling and utilizing activated carbon as a decolorant of a water treatment agent HEDP.
background
The water treatment agent hydroxyethylidene diphosphonic acid (HEDP) has stable C-P bond, high thermal stability and decomposition temperature higher than 250 ℃. And the antioxidant property is good, the effect of inhibiting calcium carbonate, hydrated ferric oxide and calcium phosphate is excellent, and the scale inhibitor is an important scale inhibitor dispersant and is widely applied to industrial water treatment. In the industrial production process, the finished product of the hydroxyethylidene diphosphonic acid can meet the requirement of an application standard after being decolored to reach the standard. A large amount of active carbon is often used for adsorption and decoloration treatment, so that a large amount of hazardous waste solid, namely the waste active carbon, is generated. The waste activated carbon not only needs to consume a large amount of resources for treatment, but also wastes a large amount of attached hydroxyethylidene diphosphonic acid, so that the resource utilization rate is low, the production cost of products is increased, the environmental protection is not facilitated, and the industrial scale development of hydroxyethylidene diphosphonic acid is restricted to a certain extent.
The invention content is as follows:
In order to overcome the defects of the prior art, the invention provides a method for recycling and utilizing activated carbon as a decolorant of a water treatment agent HEDP, which has high resource utilization rate and is green and environment-friendly.
The invention has the advantages of
The invention utilizes a physical method for recycling activated carbon by washing, a chemical method for recycling activated carbon by regenerating aqueous solution of hydrogen peroxide, continuous treatment for recycling activated carbon, and separation to obtain washing solution, regenerated liquid and regenerated activated carbon.
A method for recycling and utilizing activated carbon as a decolorant of a water treatment agent HEDP comprises the following steps:
(1) Putting the reclaimed activated carbon and pure water into an activated carbon treatment kettle according to a certain proportion, stirring and washing for a period of time at a certain temperature, then carrying out filter pressing to separate the activated carbon and water washing liquid by a filter press, transferring the water washing liquid into the activated carbon treatment kettle, stirring and washing, then transferring into the filter press for filter pressing again to separate, transferring the separated water washing liquid into a water washing liquid collection tank, transferring the washed activated carbon into the activated carbon treatment kettle, 2) putting the washed activated carbon, 10% by mass of hydrogen peroxide water solution and pure water into the activated carbon treatment kettle according to a certain proportion, stirring and regenerating for a period of time at a certain temperature, then carrying out filter pressing to separate the activated carbon and regenerated liquid by the filter press, transferring the regenerated liquid into the activated carbon treatment kettle, stirring and washing, then transferring into the filter press for filter pressing again to separate, transferring the regenerated liquid into a regenerated liquid collection tank, collecting the regenerated activated carbon, and compounding with new activated carbon according to a certain, obtaining compound active carbon for later use;
(3) Mixing the hydroxyethylidene diphosphonic acid and compound activated carbon according to a certain proportion for decoloring, diluting the decolored hydroxyethylidene diphosphonic acid with a water washing solution, transferring newly produced recovered activated carbon into an activated carbon treatment kettle, and repeating the step (1) to realize continuity.
wherein the stirring and washing temperature in the activated carbon treatment kettle in the step 1 is 60 ~ 90 ℃, and preferably 80 ~ 90 ℃.
wherein the mass ratio of the recovered activated carbon to the pure water in the step 1 is 1 (2 ~ 5), and preferably 1: 3.
wherein the stirring and water washing time in the step 1 is 30 ~ 120min, preferably 30 ~ 45 min.
wherein the stirring regeneration temperature in the activated carbon treatment kettle in the step 2 is 40 ~ 65 ℃, and preferably 45 ~ 55 ℃.
wherein the mass ratio of the washed activated carbon, 10 mass percent aqueous hydrogen peroxide solution and pure water in the step 2 is 1 (1 ~ 1.5) to (1.5 ~ 2.5), preferably 1: 1.1: 1.9.
wherein the stirring regeneration time in the step 2 is 30 ~ 120min, preferably 40 ~ 60 min.
wherein the regenerated active carbon and the new active carbon in the step 2 are compounded according to the mass ratio of (8 ~ 12) to 1, and the preferable ratio is 10: 1.
the mass ratio of the hydroxyethylidene diphosphonic acid product in the step 3 to the compound activated carbon is 1 (0.3 percent ~ 1%), and the mass ratio of the hydroxyethylidene diphosphonic acid product to the compound activated carbon is preferably 1 (0.3 percent ~ 0.5%).
The water washing liquid obtained by the method can be used for diluting the hydroxyethylidene diphosphonic acid product. The obtained regenerated liquid can be used as a phosphorus or low-phosphorus compound corrosion and scale inhibition water treatment agent monomer, so that the resource utilization rate is improved, the cost is effectively reduced, and the energy conservation and consumption reduction are realized. The obtained regenerated activated carbon is compounded and used for decoloring hydroxyethylidene diphosphonic acid, so that the total amount of the activated carbon used actually is greatly reduced, the annual output of the industrial solid waste recovered activated carbon is reduced to about 10 percent of the original annual output, and the method is free from three wastes and environment-friendly.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The invention is further described below with reference to the description of specific embodiments and the accompanying drawings.
the indexes of partial materials are that the adsorption value of the recovered activated carbon is 6 ~ 7, the adsorption value of the new activated carbon is 15 ~ 16, and the chroma of the undecolored hydroxyethylidene diphosphonic acid is 17 ~ 18.
Note: 1 the requirement of the adsorption value of the qualified new active carbon is more than or equal to 15, and the requirement of the color of the qualified hydroxyethylidene diphosphonic acid is less than 10.
2 the adsorption capacity of the activated carbon in the experiment is measured by a methylene blue adsorption value measuring method.
Example 1
step 1: putting the recovered activated carbon and pure water into an activated carbon treatment kettle according to the mass ratio of 1:3, stirring and washing for 30min at 85 +/-2 ℃, and then performing filter pressing and separation on the activated carbon and the washing liquid by using a filter press. And transferring the water washing solution into an activated carbon treatment kettle, stirring and cleaning, transferring into a filter press, performing filter pressing separation again, transferring the separated water washing solution into a water washing solution collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle.
Step 2: washing activated carbon, 10% by mass of aqueous hydrogen peroxide solution and pure water in a mass ratio of 1: 1.1: 1.9, putting the mixture into an activated carbon treatment kettle, stirring and regenerating the mixture at the temperature of 50 +/-2 ℃ for 50min, then separating the activated carbon and regenerated liquid by using a filter press in a filter pressing way, transferring the regenerated liquid into the activated carbon treatment kettle, stirring and cleaning the activated carbon treatment kettle, transferring the activated carbon treatment kettle into the filter press, carrying out filter pressing separation again, transferring the regenerated liquid obtained by filter pressing into a regenerated liquid collecting tank, collecting the regenerated activated carbon, and compounding the regenerated activated carbon with new activated carbon according to the proportion of 10:1 to obtain compound activated carbon for later use.
and 3, mixing the hydroxyethylidene diphosphonic acid and compound activated carbon according to the mass ratio of 1: 0.3% for decolorization, diluting the decolorized hydroxyethylidene diphosphonic acid with a water washing solution, transferring newly generated recovered activated carbon into an activated carbon treatment kettle, and repeating the step (1) to effectively recover the activated carbon for 10 ~ 11 times.
the detection result is that the adsorption value of the regenerated activated carbon is 12 ~ 13, the chroma of the water washing liquid is 5.6, the content of the hydroxyethylidene diphosphonic acid is 27.46%, and the chroma of the decolorized hydroxyethylidene diphosphonic acid is 7.8.
Example 2
Step 1: putting the recovered activated carbon and pure water into an activated carbon treatment kettle according to the mass ratio of 1:3, stirring and washing for 40min at 82 +/-2 ℃, and then performing filter pressing and separation on the activated carbon and the washing liquid by using a filter press. And transferring the water washing solution into an activated carbon treatment kettle, stirring and cleaning, transferring into a filter press, performing filter pressing separation again, transferring the separated water washing solution into a water washing solution collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle.
Step 2: washing activated carbon, 10% by mass of aqueous hydrogen peroxide solution and pure water in a mass ratio of 1: 1.1: 1.9, putting the mixture into an activated carbon treatment kettle, stirring and regenerating the mixture at the temperature of 47 +/-2 ℃ for 40min, then separating the activated carbon and regenerated liquid by using a filter press in a filter pressing manner, transferring the regenerated liquid into the activated carbon treatment kettle, stirring and cleaning the activated carbon treatment kettle, transferring the activated carbon treatment kettle into the filter press, carrying out filter pressing and separating again, transferring the regenerated liquid obtained by filter pressing into a regenerated liquid collecting tank, collecting the regenerated activated carbon, and compounding the regenerated activated carbon with new activated carbon according to the proportion of 10:1 to obtain compound activated carbon for later use.
and 3, mixing the hydroxyethylidene diphosphonic acid and compound activated carbon according to the mass ratio of 1: 0.3% for decolorization, diluting the decolorized hydroxyethylidene diphosphonic acid with a water washing solution, transferring newly generated recovered activated carbon into an activated carbon treatment kettle, and repeating the step (1) to effectively recover the activated carbon for 10 ~ 11 times.
the detection result is that the adsorption value of the regenerated activated carbon is 11 ~ 12, the chroma of the water washing liquid is 5.5, the content of the hydroxyethylidene diphosphonic acid is 26.89%, and the chroma of the decolorized hydroxyethylidene diphosphonic acid is 8.9.
Example 3
Step 1: putting the recovered activated carbon and pure water into an activated carbon treatment kettle according to the mass ratio of 1:3, stirring and washing for 45min at the temperature of 88 +/-2 ℃, and then performing filter pressing and separation on the activated carbon and the washing liquid by using a filter press. And transferring the water washing solution into an activated carbon treatment kettle, stirring and cleaning, transferring into a filter press, performing filter pressing separation again, transferring the separated water washing solution into a water washing solution collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle.
Step 2: washing activated carbon, 10% by mass of aqueous hydrogen peroxide solution and pure water in a mass ratio of 1: 1.1: 1.9, putting the mixture into an activated carbon treatment kettle, stirring and regenerating the mixture at the temperature of 53 +/-2 ℃ for 60min, then separating the activated carbon and regenerated liquid by using a filter press in a filter pressing way, transferring the regenerated liquid into the activated carbon treatment kettle, stirring and cleaning the activated carbon treatment kettle, transferring the activated carbon treatment kettle into the filter press, carrying out filter pressing separation again, transferring the regenerated liquid obtained by filter pressing into a regenerated liquid collecting tank, collecting the regenerated activated carbon, and compounding the regenerated activated carbon with new activated carbon according to the proportion of 10:1 to obtain compound activated carbon for later use.
and 3, mixing the hydroxyethylidene diphosphonic acid and compound activated carbon according to the mass ratio of 1: 0.5% for decolorization, diluting the decolorized hydroxyethylidene diphosphonic acid with a water washing solution, transferring the newly generated recovered activated carbon into an activated carbon treatment kettle, and repeating the step (1) to effectively recover the activated carbon for 10 ~ 11 times.
the detection result is that the adsorption value of the regenerated activated carbon is 12 ~ 13, the chroma of the water washing liquid is 6.0, the content of the hydroxyethylidene diphosphonic acid is 27.50 percent, and the chroma of the decolorized hydroxyethylidene diphosphonic acid is 8.0.
Comparative example 1
Conventional eluents (methanol is used as an example here)
Step 1: putting the recovered activated carbon and pure water into an activated carbon treatment kettle according to the mass ratio of 1:3, stirring and washing for 45min at the temperature of 88 +/-2 ℃, and then performing filter pressing and separation on the activated carbon and the washing liquid by using a filter press. And transferring the water washing solution into an activated carbon treatment kettle, stirring and cleaning, transferring into a filter press, performing filter pressing separation again, transferring the separated water washing solution into a water washing solution collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle.
Step 2: washing activated carbon with water, and mixing the washed activated carbon with 99% of methanol according to a mass ratio of 1:3, putting the mixture into an activated carbon treatment kettle, stirring and regenerating the mixture for 60min at the temperature of 50 +/-2 ℃, then separating the activated carbon and methanol liquid by using a filter press in a filter press mode, transferring the methanol liquid into the activated carbon treatment kettle, stirring and cleaning the activated carbon treatment kettle, transferring the activated carbon treatment kettle into the filter press, carrying out filter press separation again, transferring the methanol liquid obtained by filter press into a methanol liquid collecting tank, collecting the regenerated activated carbon, and compounding the regenerated activated carbon with new activated carbon according to the proportion of 10:1 to obtain compound activated carbon for later use.
And step 3: the mass ratio of the hydroxyl ethylidene diphosphonic acid to the compound activated carbon is 1: 0.5 percent of the mixture is decolorized, and the decolorized hydroxyethylidene diphosphonic acid is diluted by using a water washing solution.
the detection result is that the adsorption value of the regenerated activated carbon is 9 ~ 10, the chroma of the water washing liquid is 5.7, the content of the hydroxyethylidene diphosphonic acid is 27.21 percent, and the chroma of the decolorized hydroxyethylidene diphosphonic acid is 13.3.
Comparative example 2
Step 1: putting the recovered activated carbon and pure water into an activated carbon treatment kettle according to the mass ratio of 1:3, stirring and washing for 30min at 85 +/-2 ℃, and then performing filter pressing and separation on the activated carbon and the washing liquid by using a filter press. And transferring the water washing solution into an activated carbon treatment kettle, stirring and cleaning, transferring into a filter press, performing filter pressing separation again, transferring the separated water washing solution into a water washing solution collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle.
Step 2: and (3) washing the activated carbon and pure water according to the mass ratio of 1:3, putting the mixture into an activated carbon treatment kettle, stirring and regenerating the mixture for 50min at the temperature of 50 +/-2 ℃, then separating the activated carbon and the regenerated liquid by using a filter press in a filter pressing way, transferring the regenerated liquid into the activated carbon treatment kettle, stirring and cleaning the regenerated liquid, transferring the activated carbon treatment kettle into the filter press, carrying out filter pressing separation again, transferring the regenerated liquid obtained by filter pressing into a regenerated liquid collecting tank, collecting the regenerated activated carbon, and compounding the regenerated activated carbon with new activated carbon according to the proportion of 10:1 to obtain compound activated carbon for later use.
And step 3: the mass ratio of the hydroxyl ethylidene diphosphonic acid to the compound activated carbon is 1: 0.3 percent of the mixture is decolorized, and the decolorized hydroxyethylidene diphosphonic acid is diluted by using a water washing solution.
the detection result is that the adsorption value of the regenerated activated carbon is 7 ~ 8, the chroma of the water washing liquid is 5.5, the content of the hydroxyethylidene diphosphonic acid is 26.21 percent, and the chroma of the decolorized hydroxyethylidene diphosphonic acid is 16.8.
The above examples only express the patented embodiments of the invention, and the description is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present patent. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The method for recycling and utilizing the activated carbon is characterized in that the activated carbon is used as a water treatment agent HEDP decolorant, and specifically comprises the following steps:
Putting the recovered activated carbon and pure water into an activated carbon treatment kettle, stirring and washing, separating the activated carbon from a washing liquid, transferring the separated washing liquid into a washing liquid collecting tank, and transferring the washed activated carbon into the activated carbon treatment kettle;
(2) Putting aqueous hydrogen peroxide and pure water into an activated carbon treatment kettle, stirring and regenerating, separating activated carbon from regenerated liquid, transferring the separated regenerated liquid into a regenerated liquid collecting tank, collecting regenerated activated carbon, and compounding with new activated carbon to obtain compound activated carbon for later use;
(3) The compound active carbon is directly used as a decolorant of the water treatment agent HEDP.
2. The method according to claim 1, characterized in that in the step (1), the activated carbon and the pure water are separated by stirring and water washing for 2-3 times; and (3) stirring, washing and separating the regenerated liquid and the activated carbon in the step (2) for 2-3 times.
3. The method according to claim 1, wherein the temperature of the stirring water washing in the step (1) is 60-90 ℃; the mass ratio of the activated carbon to the pure water is 1: 2-5; stirring and washing for 30-120 min.
4. The method according to claim 1, wherein the temperature of the stirring water washing in the step (2) is 40-65 ℃; stirring and regenerating for 30-120 min.
5. The method according to claim 1, characterized in that the aqueous hydrogen peroxide solution has a mass fraction of 10%.
6. the method according to claim 5, wherein the mass ratio of the activated carbon, 10% by mass of aqueous hydrogen peroxide solution and pure water is 1 (1 ~ 2) to (1 ~ 3).
7. the method according to claim 1, wherein the compound activated carbon is prepared by mixing regenerated activated carbon and new activated carbon according to the mass ratio of 8-12: 1.
8. The method of claim 7, wherein the hydroxyethylidene diphosphonic acid product and the compounded activated carbon are mixed in a mass ratio of 1: 0.1 to 1 percent.
9. The process of claim 1 wherein the regenerated activated carbon has an adsorption value of 10 to 15 and can be recovered 10 to 12 times using the process.
10. the method as claimed in claim 1, wherein the water washing solution in the step (2) can be used for diluting a water treatment agent HEDP to prepare a water treatment agent HEDP aqueous solution product; the regenerated liquid in the step (3) can be used for producing phosphorus or low-phosphorus compound corrosion and scale inhibition water treatment agent monomers.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113000041A (en) * | 2021-02-26 | 2021-06-22 | 上海大学材料基因组工程(萍乡)研究院 | Regeneration method of waste activated carbon by using biomass |
| CN117486721A (en) * | 2023-09-06 | 2024-02-02 | 武汉椿岭科技有限公司 | Decoloring technology of diethylene glycol bis (allyl carbonate) and oligomer optical resin thereof |
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| CN117486721A (en) * | 2023-09-06 | 2024-02-02 | 武汉椿岭科技有限公司 | Decoloring technology of diethylene glycol bis (allyl carbonate) and oligomer optical resin thereof |
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| CN110560020B (en) | 2022-03-04 |
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