CN206203899U

CN206203899U - Multistage hydrogenation apparatus

Info

Publication number: CN206203899U
Application number: CN201621259540.2U
Authority: CN
Inventors: 张云河; 许开华; 郭苗苗
Original assignee: Jingmen GEM New Material Co Ltd
Current assignee: Jingmen GEM New Material Co Ltd
Priority date: 2016-11-23
Filing date: 2016-11-23
Publication date: 2017-05-31
Anticipated expiration: 2026-11-23

Abstract

A kind of multistage hydrogenation apparatus, including multistage hydriding reactor and feeding device, wherein multistage hydriding reactor is main being in series by one-level, two grades ..., N grades of multiple hydriding reactors；Feeding device is used to add CO to hydriding reactors at different levels₂Gas, including high-purity CO₂Storage tank, collection CO₂Storage tank；One-level, two grades ..., N grades of hydriding reactor be respectively mounted hydriding reactor pressure gauge；High-purity CO₂Storage tank is connected by with valvular pipeline with N grades of hydriding reactor, for being passed through high-purity CO to N grades of hydriding reactor₂Gas；Collect CO₂Storage tank is connected respectively by the pipeline with gas compressor with one-level, two grades ..., N grades of hydriding reactor；Collect CO₂Storage tank is also connected by with valvular pipeline with one-level, two grades ..., 1 grade of hydriding reactor of N；High-purity CO₂Storage tank, collection CO₂Storage tank is respectively mounted pressure of storage tank table.The utility model device serves saving high-purity CO₂The purpose of gas, compared to traditional single-stage hydrogenation apparatus, not only saves CO₂Gas usage amount, while allowing the reacting balance to carry out, improves the hydrogenation efficiency of lithium carbonate.

Description

Multistage hydrogenation apparatus

Technical field

The utility model belongs to and prepares battery-level lithium carbonate technical field, specifically a kind of multistage hydrogenation dress Put.

Background technology

Lithium carbonate is more important compound in current lithium salts, be mainly used in new energy car battery, glass ceramics, Alloy and medicine and other fields, especially country advocates Green Travel in recent years, and the principles and policies of low-carbon environment-friendly, New Energy Industry is high Speed development, just includes lithium ion battery among these, and the positive electrode cost in the lithium battery accounts for the 70~80% of whole battery, and The main positive electrode such as including nickle cobalt lithium manganate, cobalt acid lithium, LiFePO4 of the main product of market today, can all use carbonic acid Lithium is prepared from, and as new-energy automobile needs to be continuously increased, produced problem is consequently increased, and especially electrokinetic cell is asked Topic is especially prominent, and this is just related to material purity and material property, therefore to the purity requirement more and more higher of lithium carbonate.

Battery-level lithium carbonate mainly is prepared by raw material of industrial level lithium carbonate at present, mainly including causticizing process, electrolysis, hydrogen Change method etc., wherein causticizing process are primarily referred to as industrial level lithium carbonate and the soluble lithium hydroxide of calcium hydroxide reaction generation, then The lithium hydroxide that will be obtained by resin removal of impurities, then the synthetically prepared LITHIUM BATTERY of carbon dioxide by high-purity lithium carbonate, this Method and step is relatively complicated, and wherein calcium hydroxide just introduces substantial amounts of impurity, extremely disadvantageous removal step later；Electrolysis Method is unfavorable for greatly industrialized production due to power consumption, and hydrogenization method is the most reliable, and hydrogenization method is first to the mixing of lithium carbonate and water High-pureness carbon dioxide is passed through in thing and prepares lithia water, and then decomposed and obtain lithium carbonate and removed with this to be difficult what is be hydrogenated Impurity, then with calcium hydroxide reaction, concentrate and lithium hydroxide solution obtained by the ion exchange resin removal of impurity Ca, Mg etc., most After be passed through high-pureness carbon dioxide gas and prepare battery-level lithium carbonate, but single-stage hydriding reactor being used existing hydrogenation, perhaps more Many carbon dioxide are not utilized completely, too low even with rate, serious waste high-pureness carbon dioxide gas, cause gas raw material Waste and industrial level lithium carbonate reaction is incomplete.

Utility model content

In order to solve the above technical problems, the utility model provides a kind of multistage hydrogenation apparatus, saving is served high-purity Degree CO₂The purpose of gas, compared to traditional single-stage hydrogenation apparatus, not only saves CO₂Gas usage amount, while allowing reacting balance Carry out, improve the hydrogenation efficiency of lithium carbonate.

A kind of multistage hydrogenation apparatus, including multistage hydriding reactor and feeding device, wherein multistage hydriding reactor is main by one Level, two grades ..., N grade multiple hydriding reactors be in series；Feeding device is used to add CO to hydriding reactors at different levels₂Gas, including high-purity CO₂ Storage tank, collection CO₂Storage tank；One-level, two grades ..., N grades of hydriding reactor be respectively mounted hydriding reactor pressure gauge；High-purity CO₂Storage tank is by with valve The pipeline of door is connected with N grades of hydriding reactor, for being passed through high-purity CO to N grades of hydriding reactor₂Gas；Collect CO₂Storage tank is by with gas The pipeline of compressor is connected respectively with one-level, two grades ..., N grades of hydriding reactor, for by one-level, two grades ..., N grades of hydriding reactor CO₂Gas is recycled to collection CO₂In storage tank；Collect CO₂Storage tank also by with valvular pipeline and one-level, two grades ..., N-1 grades Hydriding reactor is connected, for that will collect CO₂The CO that storage tank is reclaimed₂Gas is passed through one-level, two grades ..., N-1 grades of hydriding reactor again；It is high-purity CO₂Storage tank, collection CO₂Storage tank is respectively mounted pressure of storage tank table.

The one-level, two grades ..., N grades of hydriding reactor feed intake according to the discharging opening of previous hydriding reactor and latter hydriding reactor Mouth is connected by way of the pipeline with pump is connected.

The one-level, two grades ..., N grades of hydriding reactor side wall be provided with filler, for adding water.

The one-level, the volume of two grades ..., N grades hydriding reactors are sequentially reduced, and one-level hydriding reactor volume is maximum, N grades of hydriding reactor Volume is minimum.

The N grades of hydriding reactor is three-level hydriding reactor or level Four hydriding reactor.

Working method of the present utility model is：

(1) one-level hydrogenation：The industrial level lithium carbonate and common pure water for weighing certain mass are mixedly configured into slurry, beat Enter in one-level hydriding reactor, temperature control opens the agitating paddle stirring in one-level hydriding reactor at 20~25 DEG C in one-level hydriding reactor；

The CO that will be collected₂Gas adds one-level hydriding reactor, the CO of the collection by gas feeding apparatus₂Gas is from receipts Collection CO₂Storage tank；

According to normal pressure feedback regulation CO in one-level hydriding reactor₂Feed rate, while monitor solution in pH value；Treat solution PH value obtains more muddy lithia water I at 8~8.5, and now hydrogenation reaction rate is slower；

(2) second-stage hydrogenation reaction：

Lithia water I in filtration washing one-level hydriding reactor, obtains filtrate I and filter residue I, while by filter residue I and general Logical pure water is hybridly prepared into slurry and squeezes into second-stage hydrogenation kettle, and second-stage hydrogenation temperature in the kettle is controlled at 20~25 DEG C, opens two Agitating paddle stirring in level hydriding reactor；

The CO that will be collected₂Gas adds second-stage hydrogenation kettle, the CO of the collection by gas feeding apparatus₂Gas is from receipts Collection CO₂Storage tank；

According to normal pressure feedback regulation CO in hydriding reactor₂Feed rate, while monitor solution in pH value；Treat solution ph At 7.5~8, the lithia water II more clarified, now hydrogenation reaction rate is very fast；

(3) three-level hydrogenation：

Lithia water II in filtration washing second-stage hydrogenation reactor, obtains filtrate II and filter residue II, while will filter Slag II and common pure water are hybridly prepared into slurry and squeeze into three-level hydriding reactor, and temperature control is 20~25 in three-level hydriding reactor DEG C, open the agitating paddle stirring in three-level hydriding reactor；

By high-purity CO₂Gas adds three-level hydriding reactor, high-purity CO by gas feeding apparatus₂From high-purity CO₂Storage tank；

According to normal pressure feedback regulation CO in three-level hydriding reactor₂Feed rate, while monitor solution in pH value；Treat solution PH value at 7~7.5, the lithia water III more clarified, now hydrogenation reaction rate is quickly；

Lithia water III in filtration washing three-level hydriding reactor, obtains filtrate III；

The utility model compared with prior art, has the advantages that：

Serve saving high-purity CO₂The purpose of gas, compared to traditional single-stage hydrogenation apparatus, not only saves CO₂Gas Usage amount, while allowing the reacting balance to carry out, improves the hydrogenation efficiency of lithium carbonate.

Brief description of the drawings

Fig. 1 is the structural representation of the utility model embodiment 1.

Reference：1st, one-level hydriding reactor；2nd, second-stage hydrogenation kettle；3rd, three-level hydriding reactor；4th, motor；5th, dog-house；6、 Hydriding reactor pressure gauge；7th, CO is collected₂Storage tank；8th, high-purity CO₂Storage tank；9th, pressure of storage tank table；10th, a CO₂It is passed through pipeline；11st, Two CO₂It is passed through pipeline；12nd, the 3rd CO₂It is passed through pipeline；13 valves；14th, a CO₂Collection conduit；15th, the 2nd CO₂Collection conduit； 16th, the 3rd CO₂Collection conduit；17th, gas compressor；18th, filler；19th, discharging opening.

Specific embodiment

The utility model is described in further detail below in conjunction with the accompanying drawings.

The ＞ of ＜ embodiments 1

Multistage hydrogenation apparatus, including multistage hydriding reactor and feeding device, wherein multistage hydriding reactor is main by one-level hydrogen Change kettle 1, second-stage hydrogenation kettle 2, three-level hydriding reactor 3 to be in series, agitating paddle, motor 4 and stirring are equipped with hydriding reactors at different levels Oar is connected and drives agitating paddle to rotate；Hydriding reactors at different levels top is equipped with dog-house 5, side, and to be equipped with filler 18, bottom equal It is provided with discharging opening 19；The discharging opening 19 of one-level hydriding reactor 1 is connected with the dog-house 5 of second-stage hydrogenation kettle 2 by the pipeline with pump, The discharging opening 19 of second-stage hydrogenation kettle 2 is connected with the dog-house 5 of three-level hydriding reactor 3 by the pipeline with pump again；

One-level hydriding reactor 1, second-stage hydrogenation kettle 2, three-level hydriding reactor 3 are respectively mounted hydriding reactor pressure gauge 6, and each hydrogenation is measured respectively Air pressure in kettle；

Feeding device is used to add CO to hydriding reactors at different levels₂Gas, including high-purity CO₂Storage tank 8, collection CO₂Storage tank 7；The two Storage tank is respectively mounted pressure of storage tank table 9, for measuring the air pressure in storage tank；

High-purity CO₂Storage tank 8 is by the 3rd CO with valve 13₂Pipeline 12 is passed through to be connected with three-level hydriding reactor 3, for Three-level hydriding reactor 3 is passed through high-purity CO₂Gas；

Collect CO₂Storage tank 7 is by the CO with gas compressor 17₂Collection conduit 14, the 2nd CO₂Collection conduit 15, 3rd CO₂Collection conduit 16 is connected respectively with one-level, two grades, three-level hydriding reactor, for by one-level hydriding reactor 1, second-stage hydrogenation kettle 2nd, the CO in three-level hydriding reactor 3₂Gas is recycled to collection CO₂In storage tank 7；

Collect CO₂Storage tank 7 is also by the CO with valve 13₂It is passed through pipeline 10, the 2nd CO₂It is passed through pipeline 11 and Level, second-stage hydrogenation kettle are connected and will collect CO₂The CO that storage tank 7 is reclaimed₂Gas is passed through one-level hydriding reactor 1, second-stage hydrogenation kettle 2 again； In above-mentioned multistage hydrogenation apparatus：One-level, two grades, three-level hydriding reactor side wall be additionally provided with filler 20, for adding water；One-level, Two grades, the volume of three-level hydriding reactor be sequentially reduced, one-level hydriding reactor volume is maximum, and three-level hydriding reactor volume is minimum；Hydriding reactor Series is not limited only to three-level, can also be the multistages such as level Four, Pyatyi.

Claims

1. a kind of multistage hydrogenation apparatus, it is characterised in that：

Including multistage hydriding reactor and feeding device, wherein multistage hydriding reactor is main by one-level, two grades ..., N grades of multiple hydriding reactor string Connection is formed；Feeding device is used to add CO to hydriding reactors at different levels₂Gas, including high-purity CO₂Storage tank, collection CO₂Storage tank；One-level, two Level ..., N grades of hydriding reactor are respectively mounted hydriding reactor pressure gauge；High-purity CO₂Storage tank connects by with valvular pipeline with N grades of hydriding reactor Connect, for being passed through high-purity CO to N grades of hydriding reactor₂Gas；Collect CO₂Storage tank is by the pipeline with gas compressor and one-level, two Level ..., N grades of hydriding reactor are connected respectively, for by the CO in one-level, two grades ..., N grades of hydriding reactor₂Gas is recycled to collection CO₂Storage tank It is interior；Collect CO₂Storage tank is also connected by with valvular pipeline with one-level, two grades ..., N-1 grades of hydriding reactor, for that will collect CO₂ The CO that storage tank is reclaimed₂Gas is passed through one-level, two grades ..., N-1 grades of hydriding reactor again；High-purity CO₂Storage tank, collection CO₂Storage tank is respectively mounted Pressure of storage tank table.

2. multistage hydrogenation apparatus according to claim 1, it is characterised in that：

The one-level, two grades ..., N grades of hydriding reactor it is logical with the latter dog-house of hydriding reactor according to the discharging opening of previous hydriding reactor The mode for crossing the connection of the pipeline with pump is connected.

3. multistage hydrogenation apparatus according to claim 1, it is characterised in that：

4. multistage hydrogenation apparatus according to claim 1, it is characterised in that：

The one-level, the volume of two grades ..., N grades hydriding reactors are sequentially reduced, and one-level hydriding reactor volume is maximum, N grades of hydriding reactor volume It is minimum.

5. multistage hydrogenation apparatus according to any one of claim 1 to 4, it is characterised in that：