CN112403029A - Novel resin decoppering process flow - Google Patents
Novel resin decoppering process flow Download PDFInfo
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- CN112403029A CN112403029A CN202011298190.1A CN202011298190A CN112403029A CN 112403029 A CN112403029 A CN 112403029A CN 202011298190 A CN202011298190 A CN 202011298190A CN 112403029 A CN112403029 A CN 112403029A
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- China
- Prior art keywords
- resin column
- copper
- regenerated
- process flow
- water
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- 239000011347 resin Substances 0.000 title claims abstract description 63
- 229920005989 resin Polymers 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims abstract description 26
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 44
- 229910052802 copper Inorganic materials 0.000 claims abstract description 44
- 239000010949 copper Substances 0.000 claims abstract description 44
- 239000000463 material Substances 0.000 claims abstract description 27
- 238000001179 sorption measurement Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 230000008929 regeneration Effects 0.000 claims abstract description 14
- 238000011069 regeneration method Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 230000001681 protective effect Effects 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 3
- 238000003860 storage Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000006227 byproduct Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000011010 flushing procedure Methods 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 p-methylsulfonylphenylserine ethyl ester sulfate Chemical compound 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical class [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a novel resin decoppering process flow, which comprises the following steps: step 1: pumping the reaction materials into a cooler by a circulating pump, cooling and circulating by circulating water, and performing step 2: and (3) controlling the pH value of the reaction material cooled in the step (1) to be 2-3, and conveying the reaction material to a regenerated resin column from the lower part. Has the advantages that: according to the invention, the copper removal operation of the L-ethyl ester production waste liquid is realized by adopting ammonia water, water and sulfuric acid solution for multiple times of flushing, so that the device can continuously remove copper on line, the copper removal efficiency can reach more than 95%, and when the concentration of the regenerated liquid ammonia water is lower than 5%, the copper content is about 6 mg/L; when the concentration of the regenerated liquid ammonia water is higher than 5% and lower than 10%, the copper content is about 15 mg/L; the adsorption temperature is 20 ℃, the adsorption flow rate is 5BV/h, the copper content in the regeneration liquid is about 10mg/L, the copper removing method has high copper removing efficiency and good copper removing quality, and meanwhile, through automatic control in the copper removing process, errors generated by manual control are effectively avoided, and the generation of byproducts is avoided.
Description
Technical Field
The invention relates to the technical field of novel copper removal of an L-ethyl ester production device, in particular to a novel resin copper removal process flow.
Background
At present, the batch production process adopts kettle type equipment to remove copper. Adding deionized water into a stirring kettle, adding p-methylsulfonylphenylserine ethyl ester sulfate while stirring, dropwise adding saturated sodium sulfide solution after complete dissolution to remove copper ions, adding activated carbon, heating to 45 ℃, keeping the temperature for 1h, and filtering while the solution is hot.
However, in the copper removing method, the copper removing process is discontinuous, so that the final copper removing efficiency is low, the copper content reaches 30mg/L after the primary copper removing, the copper content reaches 20mg/L after the secondary copper removing, and byproducts are generated in the secondary copper removing process, so that the copper removing quality is poor.
Disclosure of Invention
The invention aims to solve the problems and provide a novel resin copper removal process flow.
The invention realizes the purpose through the following technical scheme:
a novel resin decoppering process flow comprises the following steps:
step 1: pumping the reaction materials into a cooler by a circulating pump, and cooling and circulating by circulating water;
step 2: controlling the pH value of the reaction material cooled in the step 1 to be 2-3, conveying the reaction material to a regenerated resin column from the lower part, feeding a water belt material from the lower part to the upper part of the regenerated resin column, feeding the material from the lower part of the regenerated resin column, and discharging the material from the upper part to a protective resin column;
and step 3: after the materials enter the protective resin column, ammonia water is adopted again to enter the regenerated resin column from top to bottom to remove water in the regenerated resin column, and after the ammonia water replacement is finished, the solution is discharged from the regenerated resin column to an external storage tank to achieve the purpose of copper removal;
and 4, step 4: after the water washing is finished, the regenerated resin column is washed by sulfuric acid again, the regenerated liquid is discharged from the upper part, and continuous copper removal operation can be carried out by repeated circulation.
Furthermore, in the step 1, the temperature of the reaction materials is maintained below 45 ℃ in the cooling circulation process, and the time of the whole copper removal process flow is 8-10H.
Furthermore, the regenerated resin column, the adsorption resin column and the protection resin column are all automatically controlled, so that errors caused by manual control can be avoided.
Furthermore, the model of the regenerated resin column is MY-01, the model of the adsorption resin column is MY-02, and the model of the protective resin column is MY-03, so that the effect of copper removal can be ensured.
The invention has the beneficial effects that:
according to the invention, the copper removal operation of the L-ethyl ester production waste liquid is realized by adopting ammonia water, water and sulfuric acid solution for multiple times of flushing, so that the device can continuously remove copper on line, the copper removal efficiency can reach more than 95%, and when the concentration of the regenerated liquid ammonia water is lower than 5%, the copper content is about 6 mg/L; when the concentration of the regenerated liquid ammonia water is higher than 5% and lower than 10%, the copper content is about 15 mg/L; the adsorption temperature is 20 ℃, the adsorption flow rate is 5BV/h, the copper content in the regeneration liquid is about 10mg/L, the copper removal efficiency is high, the copper removal quality is good, meanwhile, through the automatic control in the copper removal process, the error generated by manual control is effectively avoided, and the generation of byproducts is avoided.
Drawings
FIG. 1 is a schematic diagram of a novel resin decoppering process according to the present invention.
The reference numerals are explained below:
1. regenerating the resin column; 2. adsorbing a resin column; 3. and (4) protecting the resin column.
Detailed Description
A novel resin decoppering process flow comprises the following steps:
step 1: pumping the reaction materials into a cooler by a circulating pump, and cooling and circulating by circulating water;
step 2: controlling the pH value of the reaction material cooled in the step 1 to be 2-3, conveying the reaction material to a regenerated resin column from the lower part, feeding a water belt material from the lower part to the upper part of the regenerated resin column, feeding the material from the lower part of the regenerated resin column, and discharging the material from the upper part to a protective resin column;
and step 3: after the materials enter the protective resin column, ammonia water is adopted again to enter the regenerated resin column from top to bottom to remove water in the regenerated resin column, and after the ammonia water replacement is finished, the solution is discharged from the regenerated resin column to an external storage tank to achieve the purpose of copper removal;
and 4, step 4: after the water washing is finished, the regenerated resin column is washed by sulfuric acid again, the regenerated liquid is discharged from the upper part, and continuous copper removal operation can be carried out by repeated circulation.
In this embodiment, in the step 1, the temperature of the reaction material is maintained below 45 ℃ in the cooling circulation process, and the time of the whole copper removal process is 8-10H.
In this embodiment, the regenerated resin column, the adsorption resin column, and the protection resin column are all controlled automatically, so that errors caused by manual control can be avoided.
In the embodiment, the type of the regenerated resin column is MY-01, the type of the adsorption resin column is MY-02, and the type of the protective resin column is MY-03, so that the effect of copper removal can be ensured.
The concentration of the regeneration liquid of the copper removing process at different adsorption temperatures and regeneration temperatures is as follows:
the adsorption temperature is controlled at 20 ℃, the regeneration temperature is 20 ℃, the adsorption flow rate is 10BV/h, and the concentration of the regeneration liquid is 12 percent;
the adsorption temperature is controlled at 20 ℃, the regeneration temperature is 40 ℃, the adsorption flow rate is 10BV/h, and the concentration of the regeneration liquid is 15 percent;
the adsorption temperature is controlled at 5 ℃, the regeneration temperature is 50 ℃, the adsorption flow rate is 10BV/h, and the concentration of the regeneration liquid is 15 percent.
If the adsorption resin column and the regeneration resin column are added, the concentration of the regeneration liquid is increased by less than 2 percent and is increased to 3 groups in series, and the concentration of the regeneration liquid is increased by less than 2 percent.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A novel resin decoppering process flow is characterized in that: it comprises the following steps:
step 1: pumping the reaction materials into a cooler by a circulating pump, and cooling and circulating by circulating water;
step 2: controlling the pH value of the reaction material cooled in the step 1 to be 2-3, conveying the reaction material to a regenerated resin column from the lower part, feeding a water belt material from the lower part to the upper part of the regenerated resin column, feeding the material from the lower part of the regenerated resin column, and discharging the material from the upper part to a protective resin column;
and step 3: after the materials enter the protective resin column, ammonia water is adopted again to enter the regenerated resin column from top to bottom to remove water in the regenerated resin column, and after the ammonia water replacement is finished, the solution is discharged from the regenerated resin column to an external storage tank to achieve the purpose of copper removal;
and 4, step 4: after the water washing is finished, the regenerated resin column is washed by sulfuric acid again, the regenerated liquid is discharged from the upper part, and continuous copper removal operation can be carried out by repeated circulation.
2. The novel resin decoppering process flow according to claim 1, characterized in that: in the step 1, the temperature of the reaction materials is maintained below 45 ℃ in the cooling circulation process, and the time of the whole copper removal process flow is 8-10H.
3. The novel resin decoppering process flow according to claim 1, characterized in that: the regeneration resin column, the adsorption resin column and the protection resin column are all automatically controlled.
4. The novel resin decoppering process flow according to claim 1, characterized in that: the model of the regenerated resin column is MY-01, the model of the adsorption resin column is MY-02, and the model of the protective resin column is MY-03.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011298190.1A CN112403029A (en) | 2020-11-18 | 2020-11-18 | Novel resin decoppering process flow |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011298190.1A CN112403029A (en) | 2020-11-18 | 2020-11-18 | Novel resin decoppering process flow |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112403029A true CN112403029A (en) | 2021-02-26 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011298190.1A Pending CN112403029A (en) | 2020-11-18 | 2020-11-18 | Novel resin decoppering process flow |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320482A (en) * | 2001-01-05 | 2001-11-07 | 南京大学 | Operating technology for ion-exchange or adsorption parametric pump |
| JP2011214132A (en) * | 2010-03-17 | 2011-10-27 | Jx Nippon Mining & Metals Corp | Recovery method for cobalt |
| CN103241803A (en) * | 2013-05-14 | 2013-08-14 | 广东新大禹环境工程有限公司 | Electroplating wastewater separating process |
| CN106757150A (en) * | 2016-11-16 | 2017-05-31 | 天津碧水源膜材料有限公司 | A kind of method that copper in contained waste liquid is reclaimed using absorption and electro-deposition group technology |
| CN111004926A (en) * | 2018-10-08 | 2020-04-14 | 金川集团股份有限公司 | Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin |
-
2020
- 2020-11-18 CN CN202011298190.1A patent/CN112403029A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320482A (en) * | 2001-01-05 | 2001-11-07 | 南京大学 | Operating technology for ion-exchange or adsorption parametric pump |
| JP2011214132A (en) * | 2010-03-17 | 2011-10-27 | Jx Nippon Mining & Metals Corp | Recovery method for cobalt |
| CN103241803A (en) * | 2013-05-14 | 2013-08-14 | 广东新大禹环境工程有限公司 | Electroplating wastewater separating process |
| CN106757150A (en) * | 2016-11-16 | 2017-05-31 | 天津碧水源膜材料有限公司 | A kind of method that copper in contained waste liquid is reclaimed using absorption and electro-deposition group technology |
| CN111004926A (en) * | 2018-10-08 | 2020-04-14 | 金川集团股份有限公司 | Method for extracting nickel and cobalt from low-grade laterite-nickel ore leaching solution by resin |
Non-Patent Citations (1)
| Title |
|---|
| 宋永辉等编著: "《提金氰化废水处理理论与方法》", 31 March 2015, 北京：冶金工业出版社 * |
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Application publication date: 20210226 |