CN106946379A - A kind of recycling treatment process of rare earth calcium soap raffinate - Google Patents
A kind of recycling treatment process of rare earth calcium soap raffinate Download PDFInfo
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- CN106946379A CN106946379A CN201710313842.6A CN201710313842A CN106946379A CN 106946379 A CN106946379 A CN 106946379A CN 201710313842 A CN201710313842 A CN 201710313842A CN 106946379 A CN106946379 A CN 106946379A
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- Prior art keywords
- waste water
- rare earth
- raffinate
- technique
- oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/20—Halides
- C01F11/24—Chlorides
- C01F11/32—Purification
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/36—Nitrates
- C01F11/44—Concentrating; Crystallisating; Dehydrating; Preventing the absorption of moisture or caking
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
Abstract
The invention discloses a kind of recycling treatment process of rare earth calcium soap raffinate, pretreated waste water is first carried out oil removal treatment while reducing COD by the technique, then carry out depickling processing and improve pH value, then removing heavy metals are gone by absorption method, the waste water finally given can qualified discharge；Process provides a kind of integrated processing method, the vacancy of rare-earth trade raffinate waste water reclaiming processing is filled up, veritably solve the problems, such as the recovery of efficient resource in calcium soap raffinate waste water, and realize discharged wastewater met the national standard, whole technique is flexible, controllable, rare-earth trade raffinate field of waste water treatment is can be widely applied to, is had a good application prospect.
Description
Technical field
The invention belongs to Sewage advanced treatment field, more particularly to a kind of recycling treatment work of rare earth calcium soap raffinate
Skill.
Background technology
Rare earth element has good physics and chemical characteristic, is widely used in new material and high-tech area, is extremely
Important strategic materials.A not still rare earth resources big country of China, rare earth resources enrich, and are that rare earth extraction separation is big
State, rare earth extraction separation of level occupies first place in the world.
Rare earth extraction is separated, generally using acid solution（Hydrochloric acid, nitric acid or sulfuric acid）Rare earth element is leached from Rare Earth Mine, then
With the extractant after calcium soap（Predominantly P507）The extracting rare-earth element from leachate, metal extraction is mutually dilute with being prepared after acid back extraction
Native produce, and the main component of the raffinate after calcium soap is extracted is calcium chloride or calcium nitrate, in addition to trace rare-earth element, also
Containing the heavy metal such as the organic matters such as extractant, kerosene and Ni, Cd, complicated component, traditional governance approach is exactly to add in lime
And removing heavy metals, activated carbon oil removing, Chinese effluent, have that pure water heavy metal is not up to standard, activated carbon can not realize regeneration, effectively money
Source can not be recycled, the problems such as can not realizing the preparation of high purity product.
With economic fast development and the progressive innovation of abstraction technique, up to now, China's rare earth extraction separation work
The waste water of industry production discharge, directly discharge not only cause the waste of calcium chloride or nitric acid calcium product, and to ecological and ring
Border causes serious influence, and less for the research report of rare earth calcium soap raffinate recycling treatment, it would be highly desirable to solve.
Therefore, inventor is directed to the situation of raffinate complicated component after rare earth calcium soap, looks through a great amount of information and concentrates on studies, opens
A kind of recycling treatment process of rare earth calcium soap raffinate waste water is sent, the technique can be widely applied to what is produced after rare earth calcium soap
Raffinate field of waste water treatment, has a good application prospect.
The content of the invention
Regarding to the issue above, the invention provides a kind of recycling treatment process of rare earth calcium soap raffinate waste water, the technique has
The process problem of calcium soap raffinate is solved to effect, and realizes the recycling of efficient resource in waste water, wastewater to reach standard row
Put, non-secondary pollution is produced, the double benefit with environment-economy.
For up to this purpose, the present invention uses following technical scheme：
A kind of recycling treatment process of rare earth calcium soap raffinate, pretreated waste water is first carried out to oil removal treatment to be reduced simultaneously
COD, then carries out depickling processing and improves pH value, then removes removing heavy metals by absorption method, the discharged wastewater met the national standard finally given.
The absorption method goes the waste water that removing heavy metals are obtained by evaporative crystallization for preparing calcium chloride or nitric acid calcium product,
Recycling condensing water.
The product purity that the evaporative crystallization is obtained is more than 99.5%.
Oil removal treatment uses the oil removing material can to remove oil content to below 1mg/L with a step, COD remove to 50mg/L with
Under, the oil of recovery returns to extraction process.
The depickling processing can be separated acid with diffusion dialysis or sour Retarding resin, and the raffinate pH after depickling is 6 ~ 7, is obtained
To acid solution can be back to the extract technology of Rare Earth Mine.
The acid solution can be hydrochloric acid or nitric acid.
The absorption method is by being loaded with the material Adsorption micro heavy of activated adoption group, water outlet rare earth member
Element, heavy metal concentration are respectively less than 0.1mg/L.
The pretreatment is the solid impurity in removal waste water, suspension.
Compared with prior art, the invention has the advantages that：
1）The invention discloses a kind of recycling treatment process of rare earth calcium soap raffinate waste water, the technique has filled up existing resource
Change the vacancy for the treatment of research, discharged wastewater met the national standard while veritably realizing resource recycling；
2）Present invention process using oil removing material can with a step by oil content remove to while below 1mg/L by COD remove to
Below 50mg/L, substantially, the oil of recovery can equally return to extraction process to effect；
3）Present invention process is a kind of integrated recycling processing method, after absorption removing heavy metals water outlet can also direct evaporative crystallization,
High-purity calcium chloride or nitric acid calcium product are prepared, product purity is flexible, controllable more than 95%, can be widely applied to rare earth calcium soap raffinate
Liquid field of waste water treatment.
Brief description of the drawings
Fig. 1 is a kind of recycling treatment process of rare earth calcium soap raffinate waste water of the invention.
Embodiment
For the present invention is better described, technical scheme is readily appreciated, of the invention is typical but non-limiting
Embodiment is as follows：
As shown in figure 1, a kind of recycling treatment process of rare earth calcium soap raffinate, pretreated waste water is first carried out at oil removing
Reason reduces COD simultaneously, then carries out depickling processing and improves pH value, then removes removing heavy metals by absorption method, the waste water finally given
Qualified discharge can be achieved.
Wherein, absorption method goes the waste water that removing heavy metals are obtained to be produced by evaporative crystallization for preparing calcium chloride or calcium nitrate
Product, recycling condensing water, the product purity obtained through this technique evaporative crystallization is more than 99.5%；
In rare earth calcium soap raffinate organic matter main component be P507 and kerosene, oil removal treatment use oil removing material can with a step general
Oil content is removed to below 1mg/L, and COD is removed to below 50mg/L, and the oil of recovery returns to extraction process；
Rare earth calcium soap raffinate pH is generally less than 2, can be separated acid with diffusion dialysis or sour Retarding resin, the raffinate after depickling
PH is 6 ~ 7, and obtained acid solution can be back to the extract technology of Rare Earth Mine, and acid solution can be hydrochloric acid or nitric acid；
Also containing the heavy metal such as trace rare-earth element, nickel and cadmium in raffinate after depickling, with being loaded with activated adoption group
Material Adsorption micro heavy, water outlet rare earth element, heavy metal concentration are respectively less than 0.1mg/L；
Contain many suspensions in rare earth calcium soap raffinate, need to remove in advance, pre-process to remove the solid impurity in waste water, hang
Float, in case subsequent technique blocks.
Embodiment 1
The praseodymium of certain Rare Earth Enterprises, neodymium calcium soap raffinate, content of hydrochloric acid is 10%, oily 200mg/L, and COD is 2000mg/L, praseodymium, neodymium,
Nickel content is respectively 0.2,10 and 1.5mg/L, and calcium chloride content is 10%.
Step 1：Take the above-mentioned raffinates of 10L, filter and remove suspended substances；
Step 2：Step 1 water outlet enters the adsorption column absorption oil removing for being filled with oil removing material, and water outlet oil content is less than 1mg/L, COD
＜ 50mg/L.Material solvent desorption after adsorption penetration, stripping liquid rectifying recycling design and oil, solvent are recycled, and oil is returned
Return extraction process；
Step 3：Step 2 water outlet enters diffusion dialysis membrane module, water outlet pH=6.5（Scope is 6~7）, the 9% hydrochloric acid return of recovery
Rare Earth Mine extract technology；
Step 4：Step 3 water outlet enters the adsorption column removing heavy metals for being filled with active adsorbing material, and water outlet praseodymium, neodymium, nickel content are small
In 0.1mg/L；
Step 5：Step 4 standard water discharge is discharged, or evaporative crystallization prepares calcium chloride product, and it is 99.5% to obtain purity（Scope >=
99.5%）Calcium chloride product, recycling condensing water is in production technology.
Embodiment 2
The cerium calcium soap raffinate of certain Rare Earth Enterprises, nitric acid content is 1%, oily 10mg/L, and COD is 100mg/L, lanthanum, cerium, content point
Not Wei 0.5,1 mg/L, nitric acid calcium content be 10%.
Step 1：Take the above-mentioned raffinates of 10L, filter and remove suspended substances；
Step 2：Step 1 water outlet enters the adsorption column absorption oil removing for being filled with ORZ oil removing materials, and water outlet oil content is less than 1mg/L,
COD ＜ 50mg/L.Material solvent desorption after adsorption penetration, stripping liquid rectifying recycling design and oil, solvent are recycled, oil
Return to extraction process；
Step 3：Step 2 water outlet enters acid retardance bed, and water outlet pH=7,1% nitric acid of recovery returns to Rare Earth Mine extract technology；
Step 4：Step 3 water outlet enters the adsorption column removing heavy metals for being filled with active adsorbing material, and water outlet cerium content is less than
0.1mg/L；
Step 5：Step 4 standard water discharge is discharged, or evaporative crystallization prepares calcium chloride product, obtains the calcium chloride that purity is 99.7%
Product, recycling condensing water is in production technology.
Embodiment 3
The cerium calcium soap raffinate of certain Rare Earth Enterprises, nitric acid content is 1%, oily 150mg/L, and COD is 1500mg/L, lanthanum, cerium, content
Respectively 0.3,1 mg/L, nitric acid calcium content is 10%.
Step 1：Take the above-mentioned raffinates of 10L, filter and remove suspended substances；
Step 2：Step 1 water outlet enters the adsorption column absorption oil removing for being filled with ORZ oil removing materials, and water outlet oil content is less than 1mg/L,
COD ＜ 50mg/L.Material solvent desorption after adsorption penetration, stripping liquid rectifying recycling design and oil, solvent are recycled, oil
Return to extraction process；
Step 3：Step 2 water outlet enters acid retardance bed, and water outlet pH=6.8,1% nitric acid of recovery returns to Rare Earth Mine extract technology；
Step 4：Step 3 water outlet enters the adsorption column removing heavy metals for being filled with active adsorbing material, and water outlet cerium content is less than
0.1mg/L；
Step 5：Step 4 standard water discharge is discharged, or evaporative crystallization prepares calcium chloride product, obtains the calcium chloride that purity is 99.6%
Product, recycling condensing water is in production technology.
Embodiment 4
The cerium calcium soap raffinate of certain Rare Earth Enterprises, nitric acid content is 9%, oily 100mg/L, and COD is 1000mg/L, lanthanum, cerium, content
Respectively 0.8,1 mg/L, nitric acid calcium content is 10%.
Step 1：Take the above-mentioned raffinates of 10L, filter and remove suspended substances；
Step 2：Step 1 water outlet enters the adsorption column absorption oil removing for being filled with oil removing material, and water outlet oil content is less than 1mg/L, COD
＜ 50mg/L.Material solvent desorption after adsorption penetration, stripping liquid rectifying recycling design and oil, solvent are recycled, and oil is returned
Return extraction process；
Step 3：Step 2 water outlet enters acid retardance bed, and water outlet pH=7,1% nitric acid of recovery returns to Rare Earth Mine extract technology；
Step 4：Step 3 water outlet enters the adsorption column removing heavy metals for being filled with active adsorbing material, and water outlet cerium content is less than
0.1mg/L；
Step 5：Step 4 standard water discharge is discharged, or evaporative crystallization prepares calcium chloride product, obtains the calcium chloride that purity is 99.7%
Product, recycling condensing water is in production technology.
Applicant states that the present invention illustrates the method detailed of the present invention, but not office of the invention by above-described embodiment
It is limited to above-mentioned method detailed, that is, does not mean that the present invention has to rely on above-mentioned method detailed and could implemented.Art
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to each raw material of product of the present invention
Addition, selection of concrete mode etc., within the scope of all falling within protection scope of the present invention and being open.
Claims (8)
1. a kind of recycling treatment process of rare earth calcium soap raffinate, it is characterised in that first removed pretreated waste water
Oil processing reduces COD simultaneously, then carries out depickling processing and improves pH value, then removes removing heavy metals by absorption method, finally gives
Discharged wastewater met the national standard.
2. technique as claimed in claim 1, it is characterised in that the absorption method goes the waste water that removing heavy metals are obtained to pass through evaporation
Crystallize for preparing calcium chloride or nitric acid calcium product, recycling condensing water.
3. technique as claimed in claim 2, it is characterised in that the product purity that the evaporative crystallization is obtained is more than 99.5%.
4. the technique as described in any claim in claim 1-3, it is characterised in that oil removal treatment can using oil removing material
Oil content is removed to below 1mg/L with a step, COD is removed to below 50mg/L, and the oil of recovery returns to extraction process.
5. technique as claimed in claim 4, it is characterised in that the depickling processing can be incited somebody to action with diffusion dialysis or sour Retarding resin
Acid separation, the raffinate pH after depickling is 6 ~ 7, and obtained acid solution can be back to the extract technology of Rare Earth Mine.
6. technique as claimed in claim 5, it is characterised in that the acid solution can be hydrochloric acid or nitric acid.
7. technique as claimed in claim 6, it is characterised in that the absorption method is by being loaded with the material of activated adoption group
Adsorption micro heavy, water outlet rare earth element, heavy metal concentration are respectively less than 0.1mg/L.
8. technique as claimed in claim 1 or 2, it is characterised in that the pretreatment is the solid impurity in removal waste water, hanged
Float.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710313842.6A CN106946379A (en) | 2017-05-05 | 2017-05-05 | A kind of recycling treatment process of rare earth calcium soap raffinate |
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| CN201710313842.6A CN106946379A (en) | 2017-05-05 | 2017-05-05 | A kind of recycling treatment process of rare earth calcium soap raffinate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640331A (en) * | 2018-04-24 | 2018-10-12 | 沈阳建筑大学 | A kind of can-production sewage processing system |
| CN116282118A (en) * | 2022-12-28 | 2023-06-23 | 广西国盛稀土新材料有限公司 | Method for producing industrial calcium chloride by utilizing rare earth smelting high-salt wastewater |
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|---|---|---|---|---|
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| CN108640331B (en) * | 2018-04-24 | 2021-08-17 | 沈阳建筑大学 | System jar effluent disposal system |
| CN116282118A (en) * | 2022-12-28 | 2023-06-23 | 广西国盛稀土新材料有限公司 | Method for producing industrial calcium chloride by utilizing rare earth smelting high-salt wastewater |
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Application publication date: 20170714 |