CN102021337B - Innovative new technology of preparing gallium using ion exchange method - Google Patents

Innovative new technology of preparing gallium using ion exchange method Download PDF

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Publication number
CN102021337B
CN102021337B CN2009101722076A CN200910172207A CN102021337B CN 102021337 B CN102021337 B CN 102021337B CN 2009101722076 A CN2009101722076 A CN 2009101722076A CN 200910172207 A CN200910172207 A CN 200910172207A CN 102021337 B CN102021337 B CN 102021337B
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bed
ion exchange
flow velocity
wind
desorption
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CN102021337A (en
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蔡军
崔欣欣
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses an innovative new technology of preparing gallium using an ion exchange method. The technology applies fixed bed ion exchange separating technology, adds operations of stirring by compressed air at a pressure ranging from 0.25 to 0.30 MPa and extruding, and uses the method of two-stage countercurrent desorption. The process is controlled as following: (1) adsorption: a seed pregnant solution is absorbed by forward flowing, the flow velocity in the bed is in the range from 5 to 6m/h, and counter-current wind is provided when the pressure reaches 150 KPa; (2) washing: wind in counter direction with liquid flows is provided to stir and wash and forward wind is provided to squeeze out impurity liquid, and the washing step is carried out for one or more times; (3) desorption: two-stage countercurrent desorption is carried out, and the flow velocity in the bed is in the range from 4 to 5 m/h in the first stage of desorption and in the range from 3 to 4 m/h in the second stage of desorption; and (4) regeneration: wind in counter direction with liquid flows is regenerated with stirring, then forward liquid is generated, and the flow velocity in the bed is in the range from 4 to 5 m/h. The novel technology is characterized by simple operation, low content of impurities in system, raised production power, reduced raw material consumption and raised production efficiency of apparatuses.

Description

Ion exchange method is produced GALLIUM metal pure technological transformation technology
Technical field
The present invention relates to a kind of ion exchange method and produce GALLIUM metal pure technological transformation novel process, belong to metal wet process smelting technique field.
Background technology
Ion exchange technique has outstanding application in water treatment field and noble metal recovery field, and especially in recent years, utilizing ion exchange technique from Bayer process solution, to extract GALLIUM metal pure has been to be widely used in industrial production.Ion exchange technique mainly is made up of several technological processs such as absorption, washing, desorb, regeneration, and each technological process all has corresponding reaction and unit operation.
What ion exchange technique adopted at present is packed moving bed mostly; Although moving bed technique also can come out the GALLIUM metal pure IX in the Bayer process solution; But in the production process because adsorption liquid viscosity is big and impurity is many; Cause shortcomings such as absorption difficulty, washing are not thorough, desorb is incomplete, system's concentration is low, directly influenced technology production capacity and raw materials consumption.
Summary of the invention
The purpose of this invention is to provide a kind of equipment simple, be convenient to operation, help reducing raw materials consumption again, improve and reclaim liquid concentration, and the technological transformation novel process of impurity in can resolution system.
Ion exchange method of the present invention is produced GALLIUM metal pure technological transformation novel process, is to utilize fixed-bed ion exchange stripping technique, and technological process is controlled as follows:
(1) absorption: seed precipitation solution following current absorption, flow velocity is 5~6m/h in the bed, reverse air feed when pressure reaches 150KPa.
(2) washing: reverse feed liquor wind agitator treating, the forward air feed extrudes impurity liquid, and one or many repeats this operation.
(3) desorb: two sections adverse current desorbs, flow velocity successively is 4~5m/h and 3~4m/h in the bed.
(4) regeneration: at first reverse feed liquor wind stirs regeneration, co-current regeneration then, and a flow velocity is 4~5m/h in the bed.
The present invention adopts fixed-bed ion exchange stripping technique, can be used widely in noble metal hydrometallurgic recovery industry, utilizes the chain control pneumavalve of PLC system, under meter to realize absorption in the ion exchange process, washing, desorb, regenerated full automatic control.
Prove through production practice: it is scientific and reasonable that ion exchange method of the present invention is produced GALLIUM metal pure technological transformation novel process; Simple; Technological process can full-automaticly be implemented; Satisfy extraction each item requirement of GALLIUM metal pure fully, resulting one section stripping liquid concentration has realized improving production capacity, reducing the economic benefit that consumes for the postorder stripping liquid extracts GALLIUM metal pure technology up to 1.5~1.8g/L.
Description of drawings
Fig. 1 ion exchange method of the present invention is produced GALLIUM metal pure technological transformation new technological flow figure.
Embodiment
Ion exchange method of the present invention is produced GALLIUM metal pure technological transformation novel process, utilizes fixed-bed ion exchange stripping technique, increases pressurized air wind and stirs and extrusion process, adopts the way of two sections reverse desorbs.Concrete controlled step is following:
(1) absorbing unit operation: open seed precipitation solution forward feed liquor valve 1 and adsorption tail liquid recovery valve 10 and handling equipment A; Seed precipitation solution gets into from the reactor drum middle part; Flow velocity is 5~6m/h in resin layer, and when pressure in the reactor drum was elevated to 150KPa gradually, seed precipitation solution forward feed liquor valve 1 cut out with adsorption tail liquid recovery valve 10 and handling equipment A automatically; Open the anti-liquid-outlet valve 18 of reverse intake valve 22 and adsorption tail liquid and feed 0.25~0.30MPa pressurized air air feed, reach setting-up time t 1(after 180~240s); The anti-liquid-outlet valve 18 of reverse intake valve 22 and adsorption tail liquid is closed automatically; Open seed precipitation solution forward feed liquor valve 1 and adsorption tail liquid recovery valve 10 and handling equipment A; Proceed absorption, this operation has solved the disadvantage that impurity between the big resin layer of adsorption liquid viscosity causes the absorption difficulty more, sets Q when the absorption cumulative throughflow reaches 1(50~200m 3) after, open forward intake valve 21 air feeds, the seed precipitation solution that reaches between resin layer in the reactor drum is all extruded, absorbing process is accomplished, and gets into next technology.
(2) washing unit operation: open the reverse feed liquor valve 7 of washing composition and anti-liquid-outlet valve 19 of washings and handling equipment B, washing composition gets into from the bottom of reactor drum, when the washing composition cumulative throughflow reaches set(ting)value Q 2(0~20m 3) after, close reverse feed liquor valve 7 of washing composition and handling equipment B, open reverse intake valve 22 air feeds, reach setting-up time t 2(after 120~150s); The anti-liquid-outlet valve 19 of reverse intake valve 22 and washings is closed automatically; Open forward intake valve 21 and washings recovery valve 11, when after reactor pressure P is increased to about 150KPa earlier, being reduced to 135KPa, forward intake valve 21 and washings recovery valve 11 are closed automatically; Open vent valve 23 on the reactor drum, so washing can be removed between resin layer impurity in the impurity and reactor drum fully through one or many.
(3) desorb unit operation: this unit operation divides two sections desorption techniques.
A, one section desorb: open earlier one section strippant feed liquor valve 5 and one section stripping liquid recovery valve 13 and handling equipment E, one section strippant is from the bottom entering of reactor drum, and flow velocity is 4~5m/h in the resin layer, when one section stripping liquid cumulative throughflow reaches Q 3(0~10m 3) after; The liquid in-out valve and the handling equipment of one section desorption technique are closed automatically; Open forward intake valve 21 and one section strippant recovery valve 17, when after reactor pressure P is increased to about 150KPa earlier, being reduced to 135KPa, forward intake valve 21 and one section strippant recovery valve 17 are closed automatically; Open vent valve 23 on the reactor drum, accomplish one section desorption technique.
B, two sections desorbs: at first close vent valve 23; Open two sections strippant feed liquor valves 4 and two sections stripping liquid recovery valves 16 and handling equipment D again; Two sections strippants get into from the bottom of reactor drum, and flow velocity is 3~4m/h in the resin layer, when two sections stripping liquid cumulative throughflows reach Q 4(0~10m 3) after; The liquid in-out valve and the handling equipment of two sections desorption techniques are closed automatically, open forward intake valve 21 and two sections strippant recovery valves 15, when after reactor pressure P is increased to about 150KPa earlier, being reduced to 135KPa; Forward intake valve 21 and two sections strippant recovery valves 15 are closed automatically; Open vent valve on the reactor drum, accomplish whole desorption technique, get into next technology.
(4) regenerative operation unit: this operating unit divided for three steps accomplished.1, regeneration is prepared, and opens the reverse feed liquor valve 8 of regenerator and anti-liquid-outlet valve 20 of regenerated liquid and handling equipment C, and regenerator gets into from the bottom, and the regenerator cumulative throughflow reaches set(ting)value Q 5(0~10m 3) after, close reverse feed liquor valve 8 of regenerator and handling equipment C, open reverse intake valve 22 air feeds, reach setting-up time t 3(after 90~120s); The anti-liquid-outlet valve 20 of reverse intake valve 22 and regenerated liquid is closed automatically; Open forward intake valve 21 and regenerated liquid recovery valve 12; When after reactor pressure P is increased to about 150KPa earlier, being reduced to 135KPa, forward intake valve 21 and regenerated liquid recovery valve 12 are closed automatically, open vent valve 23.2, regenerative process is opened regenerator forward feed liquor valve 3 and regenerated liquid recovery valve 12 and handling equipment C, and regenerator gets into from reactor drum top, and flow velocity is 4~5m/h in the resin layer, and the regenerator cumulative throughflow reaches set(ting)value Q 6(0~10m 3) after, close regenerator forward feed liquor valve 3 and reclaim liquid valve 12 and handling equipment C with regenerated liquid.3, the regeneration postorder is opened forward intake valve 21 and regenerator recovery valve 14, and when after reactor pressure P is increased to about 150KPa earlier, being reduced to 135KPa, forward intake valve 21 and regenerator recovery valve 14 are closed automatically, opens vent valve 23, and regenerative process finishes.Accomplish a complete cycle of IX this moment, prepared the next cycle operation.

Claims (1)

1. an ion exchange method is produced GALLIUM metal pure technological transformation technology, it is characterized in that: utilize fixed-bed ion exchange stripping technique, increase pressurized air wind and stir and extrusion process, adopt the way of two sections adverse current desorbs, technological process is controlled as follows:
(1) absorption: seed precipitation solution following current absorption, flow velocity is 5~6m/h in the bed, reverse air feed when pressure reaches 150KPa;
(2) washing: reverse feed liquor wind agitator treating, the forward air feed extrudes impurity liquid, and one or many repeats this operation;
(3) desorb: two sections adverse current desorbs, flow velocity successively is 4~5m/h and 3~4m/h in the bed;
(4) regeneration: first counter blow stirs regeneration, back co-current regeneration, and flow velocity is 4~5m/h in the bed;
The forward compressed air pressure is 0.14~0.15MPa, and reverse compressed air pressure is 0.25~0.30MPa, confirms that the foundation that forward pressurized air stops is to be reduced to 135KPa after reactor pressure P is increased to 150KPa earlier.
CN2009101722076A 2009-09-09 2009-09-09 Innovative new technology of preparing gallium using ion exchange method Expired - Fee Related CN102021337B (en)

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CN110423902B (en) * 2019-08-29 2021-07-20 赣州有色冶金研究所有限公司 Preparation method and system of high-purity rare earth carbonate
CN115477361B (en) * 2022-05-05 2024-04-05 青岛海尔施特劳斯水设备有限公司 Control method of soft water system and soft water system

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101067165A (en) * 2007-06-05 2007-11-07 冯峰 Ion exchanging method for extracting gallium from alumina production process

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101067165A (en) * 2007-06-05 2007-11-07 冯峰 Ion exchanging method for extracting gallium from alumina production process

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* Cited by examiner, † Cited by third party
Title
JP特开2001-40434A 2001.02.13
JP特开2008-81792A 2008.04.10

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