CN205074014U - Device of cobalt manganese catalyst is retrieved to wet process - Google Patents
Device of cobalt manganese catalyst is retrieved to wet process Download PDFInfo
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- CN205074014U CN205074014U CN201520158732.3U CN201520158732U CN205074014U CN 205074014 U CN205074014 U CN 205074014U CN 201520158732 U CN201520158732 U CN 201520158732U CN 205074014 U CN205074014 U CN 205074014U
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Abstract
The utility model discloses a device of cobalt manganese catalyst is retrieved to wet process comprises with precipitation separation system two parts in with the extraction piece -rate system, wherein: making beating jar that the extraction piece -rate system set up including order in proper order, extract filter, one -level liquid -liquid separation ware, aqueous phase storage tank, static mixer and second grade liquid -liquid separation ware elementarily, in indisputable gunbarrel, metal seizure filter, cobalt manganese gunbarrel, the cobalt manganese connected including order in proper order with the precipitation separation system precipitate filter and cobalt manganese dissolving tank. The utility model discloses a wet process retrieves that the apparatus and method for environmental protection of catalyst is clean, degree of automation is high, regeneration efficiency is high, greatly reduced organic pollutant's emission, solved the long -term problem of stabilizing the reclaiming of cobalt manganese composite catalyst, guarantee effective retrieval and utilization of cobalt manganese composite catalyst and organic matter, effectively realize the pollutant reduction of discharging.
Description
Technical field
The utility model belongs to chemical field, specifically, be about in a kinds of oxidation reaction technique from oxidation residua the device of hydrometallurgic recovery cobalt-manganese catalyst.
Background technology
Cobalt-manganese catalyst, as a kind of composite catalyst, is widely used in the oxidation reaction of organic compound with its good catalytic stability and activity.But because cobalt manganese composite catalyst is expensive, change greatly must increase operating cost if frequent, also can cause heavy metal pollution simultaneously, increase the burden of post processing.Therefore, need the cobalt manganese composite catalyst after to participation oxidation reaction to carry out recycling, thus reach the object of Footwall drift catalyst, reduce production run cost, reduce downstream contamination.
At present, the recovery of cobalt manganese composite catalyst mainly adopts control ph, cobalt and manganese is carried out to the mode of precipitate and separate, but prior art exists following shortcoming:
1, the organic solid of oxidation residua is separated and adopts plate and frame filter press to carry out separating treatment, and separative efficiency is low, and often need manual cleaning to safeguard, working environment is poor.
2, cobalt-manganese catalyst regeneration efficiency is not high, and return rate is low;
3, the organic matter in oxidation residua can not effectively reclaim, and causes very large waste, and can cause environmental pollution, increases post-processing difficulty.
Therefore, need a kind of better means, effectively can be recycled the cobalt-manganese catalyst in oxidation residua, the organic matter in oxidation residua can be reclaimed again simultaneously.
Utility model content
The purpose of this utility model, be the device that hydrometallurgic recovery cobalt-manganese catalyst from oxidation residua in a kind of oxidation of organic compounds reaction process is provided, to solve the problem of the long-acting stable reclaiming of cobalt manganese composite catalyst, ensure oxidation panel cobalt manganese composite catalyst and organic effective reuse, effectively realize pollution reduction.
For achieving the above object, the device of hydrometallurgic recovery catalyst of the present utility model is made up of extract and separate system and neutralization precipitation piece-rate system two parts, wherein:
Described extract and separate system comprises making beating tank, elementary extraction filter, one-level Liquid liquid Separation device, aqueous phase storage tank, static mixer and the secondary Liquid liquid Separation device that order is successively arranged;
Described neutralization precipitation piece-rate system comprises the iron settling tank, metal capture filter device, cobalt manganese settling tank, cobalt manganese deposition filter and the cobalt manganese dissolving tank that are linked in sequence successively.
According to the utility model, described making beating tank, cobalt manganese settling tank and cobalt manganese dissolving tank are equipped with agitator.
According to a preferred embodiment of the present utility model, the rear end of described one-level Liquid liquid Separation device is also connected with a solvent tank.
According to the utility model, between described making beating tank and elementary extraction filter, between aqueous phase storage tank and static mixer, between iron settling tank and metal capture filter device and between cobalt manganese settling tank and cobalt manganese deposition filter, be equipped with solution feed pump.
According to a preferred embodiment, described metal capture filter device is one or arranged side by side multiple.
According to another preferred embodiment, described elementary extraction filter adopts outside filtering type cluster type filter, filter interior filter element adopts the metallic support skeleton of 6+1 formula, the runner pipe comprising a central tube of not holing and hole around the six roots of sensation of central tube, outside is the filter cloth being wrapped in six roots of sensation runner pipe periphery.
Further, the inside of described outside filtering type cluster type filter is provided with spray equipment, for carrying out spray washing to filter cake.
According to the utility model, described one-level Liquid liquid Separation device and secondary Liquid liquid Separation device adopt tilting corrugated plating as coalescing element.
According to the utility model, described metal capture filter device and cobalt manganese deposition filter adopt inward flow filtration-type core type filter, and filter interior filter element adopts the powder sintered filter core of high-precision metal, and filtering accuracy is 0.5 μm.
Compared with prior art, the utility model has following beneficial effect:
1, the utility model adopts the dissolved organic matter in organic phase solvent extraction and recovery aqueous phase, greatly reduce the burden of waste water downstream process, the renewable reuse of dissolved organic matter, improves the recycle value of accessory substance and the recovery utilization rate of cobalt-manganese catalyst simultaneously.
2, the utility model adopts Full-automatic reverse cleaning cluster type filter and Full-automatic reverse clean metal core type filter to carry out Separation of Solid and Liquid, is separated by metallic catalyst from liquid phase.Whole service process can adopt totally-enclosed to operate, PLC Automatic Control, and filter plant is counter online to be cleaned, and greatly reduces manual operation intensity and operation and maintenance cost, improves equipment operating environment, clean environment firendly.
3, the utility model adopts tilting corrugated plating separator to be separated with aqueous phase organic phase, make use of the principle of the differential tension of material, and the efficiency that makes to be separated is higher, and stability is better.
4, the utility model adopts outside filtering type cluster type filter to be separated organic solid impurity, adopt and add the mode of calming the anger and being combined with shower water, washing drying is carried out to the filter cake that organic solid is formed, greatly reduce the content of cobalt and manganese in organic solid to be recycled, and can dry residue emission be realized, effectively reclaim organic solid.
5, the utility model adopts the powder sintered filter core of high porosity metal to be separated with cobalt manganese sediment iron system sediment, and separating effect is better, and filtering accuracy is high, and compressive resistance is good, has good cleaning and regeneration effect.
Accompanying drawing explanation
Fig. 1 is the process unit flow chart of the device of hydrometallurgic recovery catalyst of the present utility model.
Fig. 2 is the structural representation of the inner filter element of outside filtering type cluster type filter.
Fig. 3 is the operating process schematic diagram of the device of hydrometallurgic recovery catalyst of the present utility model.
Figure number illustrates:
1, making beating tank; 2, agitator; 3, separation solution feed pump is just carried; 4, elementary extraction filter;
5, one-level Liquid liquid Separation device; 6, solvent tank; 7, aqueous phase storage tank; 8, secondary extraction solution feed pump;
9, static mixer; 10, secondary Liquid liquid Separation device; 11, iron settling tank;
12, iron precipitation solution feed pump; 13, metal capture filter device; 14, cobalt manganese settling tank;
15, cobalt manganese precipitation solution feed pump; 16, cobalt manganese deposition filter; 17, cobalt manganese dissolving tank;
20, central tube; 21, runner pipe; 22, filter cloth.
Detailed description of the invention
Below in conjunction with accompanying drawing, be described in further detail with the device of specific embodiment to hydrometallurgic recovery catalyst of the present utility model.Should be understood that following examples only for illustration of the utility model but not for limiting scope of the present utility model.
As shown in Figure 1, be the process unit flow chart of the device of hydrometallurgic recovery catalyst of the present utility model, in oxidation of organic compounds reaction process from oxidation residua hydrometallurgic recovery cobalt-manganese catalyst.As shown in the figure, device of the present utility model is made up of extract and separate system and neutralization precipitation piece-rate system two parts, wherein:
Described extract and separate system comprises making beating tank 1, elementary extraction filter 4, one-level Liquid liquid Separation device 5, aqueous phase storage tank 7, static mixer 9, the secondary Liquid liquid Separation device 10 that order is successively arranged, wherein:
Making beating tank 1, for being mixed with water and organic solvent by oxidation residua, to carry out elementary extraction to oxidation residua, removes the part organic solute in oxidation residua and water soluble compound;
Elementary extraction filter 4 removes the insoluble sludge after elementary extraction for filtering;
One-level Liquid liquid Separation device 5 for carrying out Liquid liquid Separation to elementary extract, to remove organic phase;
Aqueous phase storage tank 7 is for receiving from the isolated aqueous phase of one-level Liquid liquid Separation device 5;
Static mixer 9 will be for mixing from the isolated aqueous phase of one-level Liquid liquid Separation device 5 with external clean organic solvent;
Secondary Liquid liquid Separation device 10 is for carrying out Liquid liquid Separation to the aqueous phase after secondary extract.
Preferably, described making beating tank 1 is provided with agitator 2, fully mixes with water and organic solvent to be made oxidation residua by stirring; The rear end of one-level Liquid liquid Separation device 5 is also connected with a solvent tank 6, for receiving isolated organic phase in one-level Liquid liquid Separation device 5; Making beating tank 1 is separated solution feed pump 3 with being provided with between elementary extraction filter 4 just to carry, and is provided with secondary extraction solution feed pump 8 between aqueous phase storage tank 7 and static mixer 9.
Described neutralization precipitation piece-rate system comprises the iron settling tank 11, metal capture filter device 13, cobalt manganese settling tank 14, cobalt manganese deposition filter 16 and the cobalt manganese dissolving tank 17 that are linked in sequence successively, wherein:
Iron settling tank 11 for receiving the aqueous phase from secondary Liquid liquid Separation device 10, and is provided with the pipeline passing into alkali lye, to obtain iron system sediment by passing in alkali lye with the mode of aqueous phase;
Metal capture filter device 13 is for removing iron system sediment;
Cobalt manganese settling tank 14 for receiving except the sedimentary aqueous phase of de-iron system, and is provided with the pipeline passing into alkali lye equally, with the Two-step neutralization by aqueous phase and alkali lye, obtains cobalt manganese sediment;
Cobalt manganese deposition filter 16 obtains cobalt manganese sediment for filtering, and filtrate is then delivered to sewage disposal further;
Cobalt manganese dissolving tank 17 is for dissolving to carry out regeneration to cobalt manganese sediment.
Preferably, between described iron settling tank 11 and metal capture filter device 13, be provided with iron precipitation solution feed pump 12, between cobalt manganese settling tank 14 and cobalt manganese deposition filter 16, be provided with cobalt manganese precipitation solution feed pump 15; In addition, metal capture filter device 13 can be one or arranged side by side multiple; Cobalt manganese settling tank 14 can be provided with agitator 2, fully mix with alkali lye to make aqueous phase; Cobalt manganese dissolving tank 17 is also provided with agitator 2, so that the sedimentary abundant dissolving of cobalt manganese.
Further, elementary extraction filter 4 adopts outside filtering type cluster type filter, as shown in Figure 2, the inner filter element (see CN200720046612.X) of described filter adopts the metallic support skeleton of 6+1 formula, the runner pipe 21 comprising a central tube of not holing 20 and hole around the six roots of sensation of central tube, outside is the filter cloth 22 being wrapped in six roots of sensation runner pipe 21 periphery; Cluster type filter interior can arrange spray equipment (not shown) further, to realize the spray washing to filter cake.
In device of the present utility model, one-level Liquid liquid Separation device 5 and secondary Liquid liquid Separation 10 adopt tilting corrugated plating separator (CN201320756856.2).
In device of the present utility model, metal capture filter device 13 and cobalt manganese deposition filter 16 adopt inward flow filtration-type core type filter, and filter interior filter element adopts the powder sintered filter core of high-precision metal, and filtering accuracy is 0.5 μm.
Adopt above device, in extract and separate link (extract and separate system), first oxidation residua carries out elementary extraction with organic solvent and water, removes organic solute wherein and water soluble compound, carry out Separation of Solid and Liquid subsequently, remove undissolved oxidation residua; Then carry out Liquid liquid Separation, removing organic phase wherein, aqueous phase then carries out reextraction by clean organic phase, and extract carries out Liquid liquid Separation again, and the organic phase after separation returns elementary extraction step, and aqueous phase then enters neutralization precipitation piece-rate system;
Be separated link (neutralization precipitation piece-rate system) at neutralization precipitation, first in aqueous phase, pass into alkali lye and neutralize, obtain iron system sediment; After filtration except after de-iron system sediment, again pass into alkali lye in aqueous phase and carry out Two-step neutralization, obtain cobalt manganese sediment; Then filter and obtain cobalt manganese sediment, regeneration after being dissolved further.
In extract and separate link, the organic phase of elementary extract after Liquid liquid Separation is reclaimed further, to recycle dissolved organic matter wherein.
Be separated link at neutralization precipitation, the aqueous phase filtered out after cobalt manganese sediment enters sewage disposal link further, in order to avoid to environment.
Fig. 3 shows the technological process adopting device of the present utility model to reclaim the cobalt-manganese catalyst in oxidation residua, comprises the following steps:
A, elementary extraction: the oxidation residua after oxidation reaction is fully uniformly mixed with organic phase and water in making beating tank, the dissolved organic matter in extraction oxidation residua;
B, elementary extract and separate: organic phase, water and organic solid mixture enter elementary extraction filter 4 and carry out Separation of Solid and Liquid after just carrying and being separated solution feed pump 3 supercharging, organic solid is filtered element interception and is separated, and the mixed phase of organic phase and water enters one-level Liquid liquid Separation device 5;
C, one-level Liquid liquid Separation: organic phase and aqueous mixtures carry out primary separation in one-level Liquid liquid Separation device 4, and organic phase enters solvent tank 6 mutually, and aqueous phase enters aqueous phase storage tank 7;
D, reextraction: aqueous phase is through the supercharging of secondary extraction solution feed pump 8, and mix mutually with external clean organic phase in static mixer 9, organic phase carries out reextraction to the part dissolved organic matter in aqueous phase;
E, secondary Liquid liquid Separation: organic phase and aqueous mixtures carry out secondary Liquid liquid Separation in secondary Liquid liquid Separation device 10, organic phase enters making beating tank 1, and aqueous phase enters iron settling tank 11;
F, once neutralize: aqueous phase solution iron settling tank 11 in alkali in and, make the iron ion in aqueous phase be converted into ferric hydroxide precipitate precipitation;
G, iron system sediment Separation of Solid and Liquid: aqueous phase solution is after aqueous slkali once neutralizes, aqueous phase solution containing ferric hydroxide precipitate is delivered to metal capture filter device 13 through iron precipitation solution feed pump 12 and carries out Separation of Solid and Liquid, ferric hydroxide precipitate is filtered element interception and is separated, and after filter, liquid enters cobalt manganese settling tank 14;
H, Two-step neutralization: filter after aqueous phase solution cobalt manganese settling tank 14 in alkali in and, make the cobalt and manganese in aqueous phase be converted into carbonate deposition precipitation;
I, cobalt manganese sediment Separation of Solid and Liquid: the aqueous phase solution containing cobalt manganese carbonate deposition is delivered to cobalt manganese deposition filter 16 through cobalt manganese deposition filter solution feed pump 15, cobalt manganese carbonate deposition is filtered element interception and is separated, after filter, liquid enters sewage-treatment plant, the cobalt manganese be blocked precipitates the cobalt manganese dissolving tank 17 entered below filter, through acetic acid and water making beating, can reuse after allocating with fresh catalyst;
In above-mentioned steps, described alkali is NaOH or aqueous sodium carbonate.
Adopt device of the present utility model, by above technological operation, cobalt-manganese catalyst reclaims conversion ratio can reach more than 85%.
Claims (9)
1. a device for hydrometallurgic recovery cobalt-manganese catalyst, for the recovery of cobalt manganese composite catalyst, is characterized in that, described device is made up of extract and separate system and neutralization precipitation piece-rate system two parts, wherein:
Described extract and separate system comprises making beating tank, elementary extraction filter, one-level Liquid liquid Separation device, aqueous phase storage tank, static mixer and the secondary Liquid liquid Separation device that order is successively arranged;
Described neutralization precipitation piece-rate system comprises the iron settling tank, metal capture filter device, cobalt manganese settling tank, cobalt manganese deposition filter and the cobalt manganese dissolving tank that are linked in sequence successively.
2. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, is characterized in that, described making beating tank, cobalt manganese settling tank and cobalt manganese dissolving tank are equipped with agitator.
3. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, it is characterized in that, the rear end of described one-level Liquid liquid Separation device is also connected with a solvent tank.
4. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, it is characterized in that, between described making beating tank and elementary extraction filter, between aqueous phase storage tank and static mixer, between iron settling tank and metal capture filter device and between cobalt manganese settling tank and cobalt manganese deposition filter, be equipped with solution feed pump.
5. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, is characterized in that, described metal capture filter device is one or arranged side by side multiple.
6. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, it is characterized in that, described elementary extraction filter adopts outside filtering type cluster type filter, filter interior filter element adopts the metallic support skeleton of 6+1 formula, the runner pipe comprising a central tube of not holing and hole around the six roots of sensation of central tube, outside is the filter cloth being wrapped in six roots of sensation runner pipe periphery.
7. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 6, it is characterized in that, the inside of described outside filtering type cluster type filter is provided with spray equipment, for carrying out spray washing to filter cake.
8. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, is characterized in that, described one-level Liquid liquid Separation device and secondary Liquid liquid Separation device adopt tilting corrugated plating as coalescing element.
9. the device of hydrometallurgic recovery cobalt-manganese catalyst as claimed in claim 1, it is characterized in that, described metal capture filter device and cobalt manganese deposition filter adopt inward flow filtration-type core type filter, and filter interior filter element adopts the powder sintered filter core of high-precision metal, and filtering accuracy is 0.5 μm.
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CN106031883A (en) * | 2015-03-19 | 2016-10-19 | 北京飞潮世辰环境工程技术有限公司 | Recovery apparatus and recovery method of cobalt-manganese catalyst by wet method |
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Effective date of registration: 20180725 Address after: 214191 Rong Road 71, Xishan economic and Technological Development Zone, Wuxi, Jiangsu Patentee after: Feature-Tec (Wuxi) Filtration Technology Co., Ltd. Address before: 100083 room 506, block B, science and technology mansion, 30 Xueyuan Road, Haidian District, Beijing. Patentee before: BEIJING FEATURE ENVIRONMENT ENGINEERING TECHNOLOGY CO., LTD. |
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