CN107827168B - A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate - Google Patents

A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate Download PDF

Info

Publication number
CN107827168B
CN107827168B CN201711147991.6A CN201711147991A CN107827168B CN 107827168 B CN107827168 B CN 107827168B CN 201711147991 A CN201711147991 A CN 201711147991A CN 107827168 B CN107827168 B CN 107827168B
Authority
CN
China
Prior art keywords
waste solution
copper electrolysis
absorbent
container
copper
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201711147991.6A
Other languages
Chinese (zh)
Other versions
CN107827168A (en
Inventor
杨晓亮
王文龙
董开拓
郭雅博
孙莉
纪小平
陈芋霞
季婷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinchuan Group Copper Gui Co ltd
Original Assignee
Jinchuan Group Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jinchuan Group Co Ltd filed Critical Jinchuan Group Co Ltd
Priority to CN201711147991.6A priority Critical patent/CN107827168B/en
Publication of CN107827168A publication Critical patent/CN107827168A/en
Application granted granted Critical
Publication of CN107827168B publication Critical patent/CN107827168B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00Compounds of nickel
    • C01G53/10Sulfates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/0082Regulation; Control
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • B01D1/30Accessories for evaporators ; Constructional details thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0018Evaporation of components of the mixture to be separated
    • B01D9/0031Evaporation of components of the mixture to be separated by heating

Abstract

The invention discloses a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate, extraction process are as follows: the waste solution of copper electrolysis being concentrated and moisture absorber will be needed to be contained in two containers respectively;Increase the contact area of water vapour and liquid level with proper method;It is two container headspaces are closed and be interconnected;Take the air in ullage space away with vacuum system;The temperature that waste solution of copper electrolysis is properly increased in a manner of heating, increases vapour pressure, and moisture forms steam with faster speed;Moisture absorber absorbs the water vapour in space with faster speed;Solid sulphuric acid nickel is crystallized out when waste solution of copper electrolysis is concentrated into a certain degree.The entire production process of the present invention can realize closed operation, and no acid mist generates, and environment is good;Energy consumption is controllable, and production cost is low.

Description

A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate
Technical field
A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate is related to a kind of method for concentration of aqueous solution.
Background technique
At present, the method for nickel mainly uses crystallisation, extraction and ion-exchange in purification removing copper electrolyte.State Interior majority producer uses crystallisation output crude nickle sulphate, mainly has electric heating evaporation method, freeze crystallization, steam indirect heating dense Contracting, straight fiery concentration method, evaporator with submerged combustion production crude nickle sulphate etc..There is electric heating evaporation method high degree of automation, nickel removal to imitate The advantages that rate is high, but power consumption is high, and ability is low, and environmental protection investments and operating cost are higher, is restricted in application.Freeze crystallization Due to needing the factors such as equipment is more, take up a large area, nickel removal low efficiency not to be widely adopted always.Straight fire concentration method, which has, to be set The advantages that standby simple, nickel direct yield is high, was once widely used in small-sized copper smelting plant, but its burning is not closed, sour with evaporation equipment It volatilizees the disadvantages of more, energy consumption is high, environmental pollution is serious, severe operational environment, large labor intensity.The concentration of steam indirect heating uses Steam indirect heating evaporates solution, due to solution containing acid high, seriously corroded, to being evaporated in vacuo, material is more demanding, using warding off Porcelain reaction kettle has the characteristics such as high temperature resistant, peracid, but its heat transfer efficiency is low, and percent crystallization in massecuite is low, and nickel direct yield is relatively low, evaporation rate Slowly, the factory for being relatively suitble to treating capacity small.
Summary of the invention
The purpose of the present invention is to above-mentioned problem, provide that a kind of concentrate solution power consumption is low, environment is good The method that good, good product quality, concentration copper electrolyte at low cost extract nickel.
What the purpose of the present invention was achieved through the following technical solutions: a kind of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate Method, specifically includes the following steps:
(1) absorbent for absorbing moisture and the waste solution of copper electrolysis of concentration to be evaporated are contained in respectively in two containers, two Container top is connected, and two containers is made to form the same confined space of inverted U shape, and the connectivity part of two container tops is shared sky Between be used as steam flow channel, at this with vacuumize interface and connect;
(2) confined space is vacuumized, takes the air in confined space away, vacuum degree is that 10-101 KPa stops It only vacuumizes, the saturated vapor pressure in two containers is made difference occur, waste solution of copper electrolysis starts to evaporate, and the vapor of evaporation is spontaneous It is shifted by steam flow channel to the small container equipped with absorbent of vapour pressure, absorbent absorbs water vapour;
(3) absorbent constantly absorbs the vapor that waste solution of copper electrolysis evaporates, and waste solution of copper electrolysis is concentrated into certain journey Solid sulphuric acid nickel is started crystallizing out when spending, and nickel sulfate crystallization is obtained by filtration.
The absorbent is the substance that the concentrated sulfuric acid or other vapour pressures are less than upper space vapour pressure.
Waste solution of copper electrolysis of the invention changes the temperature of waste solution of copper electrolysis in a manner of heating, and makes to hold equipped with waste solution of copper electrolysis Vapour pressure in device increases.
After the present invention vacuumizes stopping, being pumped by two spray cycles and keep the vacuum degree in confined space constant, wherein one Spray cycle pump, which is mounted in, to be filled between the upper vessel portion of waste solution of copper electrolysis and lower part, by waste solution of copper electrolysis constantly from the container Portion carries out sprinkling and accelerates evaporation;Another spray cycle pump is mounted in filling between the upper vessel portion of absorbent and lower part, by absorbent The vapor that sprinkling absorbs waste solution of copper electrolysis evaporation is constantly carried out from the upper vessel portion.
The bottom of the container equipped with absorbent and the container equipped with waste solution of copper electrolysis is respectively equipped with corresponding storage tank, Storage tank is communicated with the outlet of corresponding container, while the storage tank is communicated by circulating pump with the entrance of corresponding container.
The beneficial effects of the present invention are:
1. the present invention is pressed with difference according to the saturated vapor of different solutions, the water in solution can be as a vapor from steaming The big solution of vapour pressure shares two container headspaces from the principle for being sent to the small solution transfer of vapour pressure, makes above two containers altogether The vapor in the flow of water vapor channel for using the same space to evaporate as waste liquid, evaporation can flow freely;Gas in confined space Press 10-101 KPa, it can be normal pressure or have certain vacuum degree, the saturated vapor of two media is pressed with difference in container, makes water Part is freely shifted from the big substance of vapour pressure to the small substance of vapour pressure;The present invention passes through pressure, the temperature in the control communal space The surface area of degree, electrolyte and moisture absorption agent, control moisture content transmits between solution and moisture absorption agent as a vapor, whole A production process realizes closed operation, and no acid mist generates, and environment is good;Energy consumption is controllable, and production cost is low;Production system can be with Increase multiple containers according to the requirement of production capacity, realizes that space locating for multiple water vapour evaporations and absorption interface is shared.
By installing spray cycle pump respectively to two containers, the form for making solution and absorbent sprinkle water is presented the present invention Raindrop shape, is circulated, and is increased the surface area of waste solution of copper electrolysis by circulation sprinkling waste solution of copper electrolysis, is made in solution Water vapour is uniform, is rapidly performed by evaporation, and reinforced solution flow rate strengthens steam flowing velocity;Increased by sprinkling absorbent The big contact area with the vapor of waste solution of copper electrolysis evaporation, accelerates absorption rate.
The present invention is by installing the independent circulatory system: i.e. storage tank and circulating pump to waste solution of copper electrolysis and moisture absorber; It is continuously replenished or is taken away, the water transport for evaporating waste solution of copper electrolysis is carried out continuously, and whole system realizes continuous processing Purpose.Meanwhile waste solution of copper electrolysis crystallizes out solid sulphuric acid nickel when being concentrated into a certain degree, is taken out of by its corresponding circulatory system Nickel sulfate crystallization is obtained by filtration after container.
Detailed description of the invention
The structural schematic diagram of Fig. 1 embodiment of the present invention.
In figure: 1. vacuumize interface, 2. communal spaces, 3. waste solution of copper electrolysis, 4. absorbents, 5. spray solution circulating pumps, 6. absorbing liquid spray cycle pump, 7. solution circulation pumps, 8. absorbing liquid circulating pumps, 9. solution storage troughs, 10. absorbing liquid storage tanks, 11. molten Liquid water level detector, 12. absorbing liquid water level detectors.
Specific embodiment
A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate, extraction process is under normal temperature conditions, to incite somebody to action Waste solution of copper electrolysis and moisture absorber agent are contained in respectively in two containers, and two reservoirs are in same confined air Between inverted u-shaped shape, upper space is shared, and the communal spaces 2 are used as flow of water vapor channel above two containers, and the communal space 2 connects Be connected to and vacuumize interface 1, a sprinkling system is installed between the top and the bottom of two containers respectively, it may be assumed that spray cycle pump, the pump it is defeated Enter end to communicate with the lower part of corresponding container, the output end of the pump installs sprinkler head, and sprinkler head is located at the top in corresponding container, makes Two solution are spilt with raindrop shape point circulate respectively.Take the air in ullage space, copper electricity away by way of vacuumizing Water in liquid waste solution is shifted since be sent to the small absorbent of vapour pressure from the big waste liquid of vapour pressure in the form of water vapour, is passed through The moisture absorber of sprinkling absorbs, and vapour pressure reduces in space, and the water in waste solution of copper electrolysis accelerates evaporation, and water vapour continues to flow to Moisture absorber is absorbed, and waste solution of copper electrolysis crystallizes out nickel sulfate after being concentrated by evaporation to nickel sulfate solubility supersaturation, is filtered It is crystallized to nickel sulfate.
The above-mentioned temperature that waste solution of copper electrolysis can be properly increased by way of heating, from 15 DEG C to 180 DEG C, temperature is higher, The vapour pressure of waste solution of copper electrolysis is bigger, and moisture content transfer velocity is faster.Or keep the air pressure in the communal space 2 smaller, waste solution of copper electrolysis Evaporation rate it is faster.
The absorbent that the present invention uses is the substance of the small vapour pressure of side space thereon of vapour pressure, can be liquid, such as dense Sulfuric acid is also possible to solid, such as calcium oxide, phosphorus pentoxide.Raindrop shape is presented in the form sprinkled water in absorbent to be followed Water vapour in space is absorbed with faster speed when circulation is dynamic.
Above-mentioned waste solution of copper electrolysis and moisture absorber can install the independent circulatory system, it may be assumed that respective circulating pump and Storage tank, is constantly added to corresponding container for the liquid in storage tank by circulating pump or the liquid of taking away in corresponding container is discharged into pair In the storage tank answered, the transfer continuities of the moisture in whole container is made to carry out the purpose, it can be achieved that continuous processing;Work as waste solution of copper electrolysis Solid sulphuric acid nickel is crystallized out when being concentrated into certain density level, and container is taken out of by the corresponding circulatory system, sulfuric acid is obtained by filtration Nickel crystallization.
In order to preferably control installation detecting devices perception separately detects density case and the moisture absorption agent of electrolyte Aqueous situation, automatic monitoring and processing are realized, when density of electrolyte and moisture absorption agent water content reach moisture content transfer It is replaced automatically when critical point.
When being pressed with difference with the saturated vapor that the principle of the present invention is different solutions, in two containers not because of saturated vapor pressure Together, the moisture in solution can be realized and be produced as a vapor from the big solution of vapour pressure from the small solution transfer of vapour pressure is sent to Object is crude nickle sulphate crystal purpose out.
Embodiment 1
By the waste solution of copper electrolysis of cupric 0.3g/l, 10m3 containing sour 280g/l, nickeliferous 35g/l be passed through it is as shown in Figure 1 to Liquid zone domain is evaporated, absorbent uses 98% concentrated sulfuric acid of 10m3, and suction reaches -70kPa under normal temperature conditions, and starting is each Self-corresponding circulating pump and spray cycle pump, keep vacuum of space constant, after 4 hours, the liquor capacity in liquid zone domain to be evaporated It reduces to 3 m3, absorbent volume reaches 17 m3, corresponding two circulating pump of each container out of service, by liquid after the evaporation of 3 m3 It is filtered, obtains 2.1 m3 of acid solution containing sour 930g/l, nickeliferous 3g/l, crude nickle sulphate crystallizes 1.5 tons.The concentrated sulfuric acid absorbs moisture Concentration is down to 75% afterwards, is applied to production as production reagent.

Claims (5)

1. a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate, it is characterised in that: specifically includes the following steps:
(1) absorbent for absorbing moisture and the waste solution of copper electrolysis of concentration to be evaporated are contained in respectively in two containers, two containers Top is connected, and two containers is made to form the confined space of inverted U shape, and the connectivity part of two container tops is the communal space as steam Flow channel, at this with vacuumize interface and connect;
(2) confined space is vacuumized, takes the air in confined space away, vacuum degree is that 10-101 KPa stops taking out Vacuum makes the saturated vapor pressure in two containers difference occur, and waste solution of copper electrolysis starts to evaporate, and the vapor of evaporation is spontaneous to be passed through Steam flow channel is shifted to the small container equipped with absorbent of vapour pressure, and absorbent absorbs water vapour;
(3) absorbent constantly absorbs the vapor that waste solution of copper electrolysis evaporates, when waste solution of copper electrolysis is concentrated into a certain degree Existing solid sulphuric acid nickel is started crystallizing out, nickel sulfate crystallization is finally obtained by filtration.
2. a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate as described in claim 1, it is characterised in that: institute Stating absorbent is the concentrated sulfuric acid.
3. a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate as described in claim 1, it is characterised in that: copper Electrolysis waste solution increases the vapour pressure in waste solution of copper electrolysis container in a manner of heating.
4. a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate as described in claim 1, it is characterised in that: take out It after vacuum stops, being pumped by two spray cycles and keeps the vacuum degree in confined space constant, wherein spray cycle pump, which is mounted in, to be contained Have between the upper vessel portion of waste solution of copper electrolysis and lower part, waste solution of copper electrolysis is constantly subjected to sprinkling from the upper vessel portion and accelerates to steam Hair;Another spray cycle pump, which is mounted in, to be filled between the upper vessel portion of absorbent and lower part, and absorbent is continuous from the upper vessel portion Carry out the vapor that sprinkling absorbs waste solution of copper electrolysis evaporation.
5. a kind of method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate as described in claim 1, it is characterised in that: dress There are the container of absorbent and the container bottom equipped with waste solution of copper electrolysis to be respectively equipped with corresponding storage tank, storage tank and corresponding container Outlet communicates, while the storage tank is communicated by circulating pump with the entrance of corresponding container.
CN201711147991.6A 2017-11-17 2017-11-17 A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate Active CN107827168B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201711147991.6A CN107827168B (en) 2017-11-17 2017-11-17 A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201711147991.6A CN107827168B (en) 2017-11-17 2017-11-17 A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate

Publications (2)

Publication Number Publication Date
CN107827168A CN107827168A (en) 2018-03-23
CN107827168B true CN107827168B (en) 2019-03-08

Family

ID=61652936

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201711147991.6A Active CN107827168B (en) 2017-11-17 2017-11-17 A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate

Country Status (1)

Country Link
CN (1) CN107827168B (en)

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049979A (en) * 2007-05-16 2007-10-10 梅州市金雁铜业公司 Method for extracting nickel sulfate from waste solution of copper electrolysis
CN102557154A (en) * 2011-12-23 2012-07-11 江门市芳源环境科技开发有限公司 Negative pressure evaporation and step-by-step feeding method of nickel sulfate solution
CN102627333A (en) * 2012-04-24 2012-08-08 中南大学 Method for refined nickel sulfate
JP2014159633A (en) * 2014-02-03 2014-09-04 Pan Pacific Copper Co Ltd Method for recovering nickel from copper electrolyte
CN104229906A (en) * 2014-09-28 2014-12-24 梅州环保设备有限公司 Method and equipment for preparing electroplating-grade nickel sulfate from nickel-containing wastewater produced in surface treatment process
CN204058135U (en) * 2014-09-28 2014-12-31 梅州环保设备有限公司 Nickel-containing waste water is utilized to prepare the equipment of plating level single nickel salt
JP2016029017A (en) * 2015-10-29 2016-03-03 住友金属鉱山株式会社 Facility and method for crystallizing nickel sulfate

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101049979A (en) * 2007-05-16 2007-10-10 梅州市金雁铜业公司 Method for extracting nickel sulfate from waste solution of copper electrolysis
CN102557154A (en) * 2011-12-23 2012-07-11 江门市芳源环境科技开发有限公司 Negative pressure evaporation and step-by-step feeding method of nickel sulfate solution
CN102627333A (en) * 2012-04-24 2012-08-08 中南大学 Method for refined nickel sulfate
JP2014159633A (en) * 2014-02-03 2014-09-04 Pan Pacific Copper Co Ltd Method for recovering nickel from copper electrolyte
CN104229906A (en) * 2014-09-28 2014-12-24 梅州环保设备有限公司 Method and equipment for preparing electroplating-grade nickel sulfate from nickel-containing wastewater produced in surface treatment process
CN204058135U (en) * 2014-09-28 2014-12-31 梅州环保设备有限公司 Nickel-containing waste water is utilized to prepare the equipment of plating level single nickel salt
JP2016029017A (en) * 2015-10-29 2016-03-03 住友金属鉱山株式会社 Facility and method for crystallizing nickel sulfate

Also Published As

Publication number Publication date
CN107827168A (en) 2018-03-23

Similar Documents

Publication Publication Date Title
CN101786754A (en) Zero-emission treatment process for salt-containing wastewater
CN110171900B (en) High-temperature salt-containing wastewater concentration and crystallization device and application
CN102101019A (en) Membrane distillation and cleaning method
CN103657136B (en) Method and equipment for evaporative crystallization of aluminium chloride
CN107674012A (en) A kind of NMP dewatering membranes are impregnated with gasification purifying plant
CN103253819A (en) Device and production technology for treating ternary-monomer wastewater and extracting sodium sulfate
CN107827168B (en) A method of concentration waste solution of copper electrolysis crystallization production crude nickle sulphate
CN112028371B (en) System for utilize BOE waste liquid preparation ammonium bifluoride
US4420318A (en) Vacuum freezing process with multiple phase transformations of low pressure vapor
CN103708993B (en) A kind of vinylidene is thick cracking gas alkali cleaning and dehydrating process in producing
RU2016103702A (en) A method of obtaining lithium hydroxide monohydrate from brines and installation for its implementation
CN104524806B (en) A kind of hexamethylenamine complete continuous crystallisation production technology and equipments
CN103466658A (en) Sodium cyanide evaporation and concentration device and method
CN114436293B (en) Method for directly producing sodium bromide from low-concentration brine
CN208362100U (en) A kind of glycerol production waste liquid recovery apparatus
CN205023891U (en) Crystallizing evaporator
CN204428875U (en) The complete continuous crystallisation production process equipment of a kind of methenamine
CN203959827U (en) Tripping device for process for preparation of CS 2 molten sulfur
CN215855206U (en) Dehumidifying device suitable for brine desalination treatment
CN210287045U (en) System membrane waste water evaporation concentration system
CN203558867U (en) Sodium cyanide evaporation concentration device
CN214192635U (en) Concentrated solution drying machine
CN103213953B (en) A kind of technique being extracted ammonium thiosulfate, ammonium thiocyanate by desulfurization waste liquor
CN207552215U (en) A kind of NMP dewatering membranes are impregnated with gasification purifying plant
CN207566897U (en) A kind of Adlerika rapid crystallization processing system

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20240315

Address after: 737199 No. 2 Jianshe Road, Jinchuan District, Jinchang City, Gansu Province (east of Beijing Road, west of Heya Road, south of Guiyang Road)

Patentee after: Jinchuan Group Copper Gui Co.,Ltd.

Country or region after: China

Address before: 737103 No. 98, Jinchuan Road, Jinchang, Gansu

Patentee before: JINCHUAN GROUP Co.,Ltd.

Country or region before: China