CN106904784A - A kind of recycling treatment process of rare earth soda soap raffinate - Google Patents
A kind of recycling treatment process of rare earth soda soap raffinate Download PDFInfo
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- CN106904784A CN106904784A CN201710313841.1A CN201710313841A CN106904784A CN 106904784 A CN106904784 A CN 106904784A CN 201710313841 A CN201710313841 A CN 201710313841A CN 106904784 A CN106904784 A CN 106904784A
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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
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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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
- 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
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
- C02F1/4693—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electrodialysis
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of recycling treatment process of rare earth soda soap raffinate, pretreated waste water is first carried out oil removal treatment while reducing COD by the technique, then carry out depickling treatment and improve pH value, removing heavy metals are gone by absorption method again, the further evaporative crystallization of waste water for finally giving prepares sodium salt product, recycling condensing water；Process provides a kind of integrated processing method, the vacancy of rare-earth trade raffinate waste water reclaiming treatment is filled up, veritably solve the problems, such as the recovery of efficient resource in soda 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 soda 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 it is big to be that rare earth extraction is separated
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 soda 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 be sodium salt by the main component of the raffinate after soda soap extraction, in addition to trace rare-earth element, also contain extraction
The organic matters such as agent, kerosene and heavy metal, complicated component, traditional governance approach be exactly plus lime in and removing heavy metals, activity
Charcoal oil removing, Chinese effluent, it is not up to standard to there is pure water heavy metal, and activated carbon cannot realize regeneration, and efficient resource cannot be recycled,
The problems such as preparation of high purity product can not be realized.
With economic fast development and the progressive innovation of abstraction technique, up to now, China's rare earth extraction separates work
The waste water of industry production discharge, directly discharge not only causes the waste of sodium salt product, and ecological and environment caused sternly
The influence of weight, and it is less for the research report of rare earth soda soap raffinate recycling treatment, it would be highly desirable to solve.
Therefore, inventor looks through a great amount of information and concentrates on studies for the situation of raffinate complicated component after rare earth soda soap, opens
Send a kind of recycling treatment process of rare earth soda soap raffinate waste water, the technique can be widely applied to what is produced after rare earth soda 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 soda soap raffinate waste water, the technique has
The process problem of soda 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.
It is that, up to this purpose, the present invention uses following technical scheme：
A kind of recycling treatment process of rare earth soda soap raffinate, pretreated waste water is first carried out oil removal treatment to be reduced simultaneously
COD, then carries out depickling treatment and improves pH value, then removes removing heavy metals by absorption method, and the waste water for finally giving further evaporates
Crystallization prepares sodium salt product.
The absorption method goes the waste water that removing heavy metals are obtained to pass through bipolar membrane electrodialysis acid-alkali regeneration, the acid solution for obtaining and alkali
Liquid returns to technique and uses, fresh water reuse or discharge.
The acid-alkali regeneration obtains acid solution and alkali lye, fresh water reuse or discharge by bipolar membrane electrodialysis.
The sodium salt product purity that the evaporative crystallization is obtained is more than 99.5%, recycling condensing water.
The sodium salt product is sodium sulphate or sodium chloride product.
Oil removal treatment uses the oil removing material can to remove to below 1mg/L oil content with a step, COD remove to 50mg/L with
Under, the oil of recovery returns to extraction process.
The depickling treatment 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 unit
Element, heavy metal concentration are respectively less than 0.1mg/L.
The pretreatment is solid impurity, the suspension in removal waste water.
Compared with prior art, the invention has the advantages that：
1）The invention discloses a kind of recycling treatment process of rare earth soda soap raffinate waste water, the technique has filled up existing soda soap
The vacancy of raffinate recycling treatment 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, except evaporative crystallization prepares high pure sodium of the purity more than 95%
Outside product salt, also disclose bipolar membrane electrodialysis and realize acid-alkali regeneration, acid solution and alkali lye return to technique and uses, whole technique spirit
It is living, controllable, can be widely applied to rare earth soda soap raffinate field of waste water treatment.
Brief description of the drawings
Fig. 1 is a kind of recycling treatment process of rare earth soda soap raffinate waste water of the invention.
Specific embodiment
For the present invention is better described, technical scheme is readily appreciated, it is of the invention typical but non-limiting
Embodiment is as follows：
As shown in figure 1, a kind of recycling treatment process of rare earth soda soap raffinate, pretreated waste water is first carried out at oil removing
Reason reduces COD simultaneously, then carries out depickling treatment and improves pH value, then removes removing heavy metals by absorption method, the waste water for finally giving
Further evaporative crystallization prepares sodium salt product.
Wherein, absorption method goes the waste water that removing heavy metals are obtained by evaporative crystallization for preparing sodium salt product（Sodium chloride and
Sodium sulphate）, recycling condensing water, the product purity obtained through this technique evaporative crystallization is more than 99.5%；
In addition, absorption method goes the waste water that removing heavy metals are obtained can also be by acid-alkali regeneration（Bipolar membrane electrodialysis）Realize acid solution and
The recycling of alkali lye, returns to technique and uses.
Organic matter main component is P507 and kerosene in rare earth soda soap raffinate, and oil removal treatment uses the oil removing material can be with one
Step removes to below 1mg/L oil content, and COD is removed to below 50mg/L, and the oil of recovery returns to extraction process；
Rare earth soda 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 the acid solution for obtaining 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 soda soap raffinate, need to remove in advance, pre-process as the solid impurity in removal waste water, hang
Float, in case subsequent technique blocks.
Embodiment 1
The praseodymium of certain Rare Earth Enterprises, neodymium soda soap raffinate, content of hydrochloric acid is 10%, oily 200mg/L, and COD is 1950mg/L, praseodymium, neodymium,
Nickel content is respectively 10,5 and 0.2mg/L, and sodium 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 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 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 sodium chloride product, obtains the sodium chloride that purity is 99.5%
Product, recycling condensing water is in production technology.
Embodiment 2：
The cerium soda soap raffinate of certain Rare Earth Enterprises, sulfuric acid content is 1%, oily 20mg/L, and COD is 150mg/L, lanthanum, cerium, content point
Not Wei 0.5,1 mg/L, sodium sulphate 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=7,1% sulfuric 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 sodium sulphate product, obtains the sodium sulphate that purity is 99.7%
Product, recycling condensing water is in production technology.
Embodiment 3：
The lanthanum soda soap raffinate of certain Rare Earth Enterprises, nitric acid content 6.3%, oily 49mg/L, COD are 560mg/L, lanthanum, cerium content difference
It is 2 and 8mg/L, nitric acid sodium content is 8%.
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 diffusion dialysis membrane module depickling, and water outlet pH=6,6% nitric acid for obtaining returns to Rare Earth Mine and leaches
Technique；
Step 4：Step 3 water outlet enters the adsorption column for being filled with active adsorbing material, and water outlet lanthanum, cerium content are respectively less than 0.1mg/L；
Step 5：Step 4 water outlet is mainly 8% sodium nitrate solution, into bipolar membrane electrodialysis acid-alkali regeneration, 7% nitric acid for obtaining
Leaching is returned respectively with 7% NaOH and saponifying process is used, fresh water（0.6%）Returned after being further concentrated into 8% through electrodialysis
Bipolar membrane electrodialysis, electrodialysis fresh water is back to production technology.
Applicant states that the present invention illustrates method detailed of the invention by above-described embodiment, but the present invention not office
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 implement.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 disclosing.
Claims (10)
1. a kind of recycling treatment process of rare earth soda soap raffinate, it is characterised in that first removed pretreated waste water
Oil processing reduces COD simultaneously, then carries out depickling treatment and improves pH value, then removes removing heavy metals by absorption method, finally gives
The further evaporative crystallization of waste water prepares sodium salt product.
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 soda acid
Regeneration, the acid solution and alkali lye that obtain return to technique and use, fresh water reuse or discharge.
3. technique as claimed in claim 2, it is characterised in that the acid-alkali regeneration by bipolar membrane electrodialysis obtain acid solution and
Alkali lye, fresh water reuse or discharge.
4. technique as claimed in claim 1, it is characterised in that the sodium salt product purity that the evaporative crystallization is obtained is more than
99.5%, recycling condensing water.
5. technique as claimed in claim 4, it is characterised in that the sodium salt product is sodium sulphate or sodium chloride product.
6. the technique as described in any claim in claim 1-5, 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.
7. technique as claimed in claim 6, it is characterised in that the depickling treatment can will with diffusion dialysis or sour Retarding resin
Acid is separated, and the raffinate pH after depickling is 6 ~ 7, and the acid solution for obtaining can be back to the extract technology of Rare Earth Mine.
8. technique as claimed in claim 7, it is characterised in that the acid solution can be hydrochloric acid or nitric acid.
9. technique as claimed in claim 8, 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.
10. technique as claimed in claim 1 or 2, it is characterised in that the pretreatment be remove solid impurity in waste water,
Suspension.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188358A (en) * | 2017-07-19 | 2017-09-22 | 北京中科康仑环境科技研究院有限公司 | A kind of recycling treatment system, processing method and the application of high-concentration ammonium salt waste water |
| CN107215996A (en) * | 2017-07-19 | 2017-09-29 | 北京中科康仑环境科技研究院有限公司 | A kind of recycling treatment system, processing method and the application of high concentration sodium salt waste water |
| CN109052800A (en) * | 2018-08-16 | 2018-12-21 | 天津中科拓新科技有限公司 | A kind of sodium sulfate wastewater containing phenol cleans circulation utilization method |
| CN109292884A (en) * | 2018-10-24 | 2019-02-01 | 云南同硕环保科技有限公司 | Preprocess method before a kind of film of non-ferrous metal extraction extraction raffinate |
| CN111777082A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN111777245A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from nickel sulfate raffinate |
| CN112575186A (en) * | 2020-12-14 | 2021-03-30 | 江苏卓博环保科技有限公司 | Resourceful treatment device and method for raffinate from vanadium extraction from stone coal |
| CN113716779A (en) * | 2021-09-01 | 2021-11-30 | 珠海市科立鑫金属材料有限公司 | Treatment process of high-salinity wastewater |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107188358A (en) * | 2017-07-19 | 2017-09-22 | 北京中科康仑环境科技研究院有限公司 | A kind of recycling treatment system, processing method and the application of high-concentration ammonium salt waste water |
| CN107215996A (en) * | 2017-07-19 | 2017-09-29 | 北京中科康仑环境科技研究院有限公司 | A kind of recycling treatment system, processing method and the application of high concentration sodium salt waste water |
| CN109052800A (en) * | 2018-08-16 | 2018-12-21 | 天津中科拓新科技有限公司 | A kind of sodium sulfate wastewater containing phenol cleans circulation utilization method |
| CN109292884A (en) * | 2018-10-24 | 2019-02-01 | 云南同硕环保科技有限公司 | Preprocess method before a kind of film of non-ferrous metal extraction extraction raffinate |
| CN111777082A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN111777245A (en) * | 2019-04-04 | 2020-10-16 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from nickel sulfate raffinate |
| CN111777082B (en) * | 2019-04-04 | 2021-11-23 | 中国科学院过程工程研究所 | Method for recovering sodium sulfate from raffinate of waste battery recovery liquid |
| CN112575186A (en) * | 2020-12-14 | 2021-03-30 | 江苏卓博环保科技有限公司 | Resourceful treatment device and method for raffinate from vanadium extraction from stone coal |
| CN112575186B (en) * | 2020-12-14 | 2024-06-14 | 江苏卓博环保科技有限公司 | Resourceful treatment device and method for stone coal vanadium extraction raffinate |
| CN113716779A (en) * | 2021-09-01 | 2021-11-30 | 珠海市科立鑫金属材料有限公司 | Treatment process of high-salinity wastewater |
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Application publication date: 20170630 |