CN104229837A - Method for improving carbonization efficiency of lithium carbonate by controlling feeding speed - Google Patents
Method for improving carbonization efficiency of lithium carbonate by controlling feeding speed Download PDFInfo
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- CN104229837A CN104229837A CN201410490256.5A CN201410490256A CN104229837A CN 104229837 A CN104229837 A CN 104229837A CN 201410490256 A CN201410490256 A CN 201410490256A CN 104229837 A CN104229837 A CN 104229837A
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- packed bed
- lithium carbonate
- quilonum retard
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Abstract
The invention relates to the technical field of chemical separation and purification, in particular to a method for improving the carbonization efficiency of lithium carbonate by controlling the feeding speed. The method comprises the following steps: dissolving lithium carbonate rough products in high-purity water, so as to prepare lithium carbonate slurry with the material concentration being 30 to 90 g/L, feeding the slurry into a rotating packed bed, feeding CO2 gas into the rotating packed bed, obtaining feed liquid after carbonization reaction is performed for 40 to 150min, controlling the feeding speed of the slurry to be 100 to 400ml/min, controlling the rotation speed of the rotating packed bed to be not higher than 50Hz, controlling the flow of the CO2 gas to be 0.02 to 0.20 m<3>/L, performing solid-liquid separation on the feed liquid, and obtaining lithium hydrogencarbonate solution. The method adopts the high gravity technology, adopts the high-speed rotating packed bed as reaction equipment, and adjusts the reaction condition of the carbonization process of lithium carbonate, and compared with the prior art, the method has the advantages that the efficiency of converting lithium carbonate into lithium hydrogencarbonate is greatly improved, and simultaneously the reaction time is shortened.
Description
Technical field
The present invention relates to chemical separation and purification technical field, particularly relate to a kind of carbonization method of Quilonum Retard.
Background technology
The preparation of pure Lithium Carbonate usually with the thick product slip of Quilonum Retard for raw material, by passing into CO wherein
2there is carburizing reagent and obtain lithia water, then through ion exchange resin removal step, obtain pure Lithium Carbonate product by pyrolytic reaction afterwards.Therefore, the preparation of lithia water is that preparation one of pure Lithium Carbonate must through process.How to improve the transformation efficiency of Crude lithium Carbonate to lithium bicarbonate process, and to shorten this transformation time be the problem that must consider preparing lithia water.
Dai Zhifeng shows in " in pure Lithium Carbonate preparation process the optimization of carburizing reagent and the research of calcium-magnesium removing " the Master degree candidate's Diplomarbeit to deliver for 2005: when carbonization temperature is at 20 DEG C, the carburizing reagent time when 90min, CO
2the flows per unit time of gas controls at 2.667L/min (0.16m
3/ h) time the speed of carburizing reagent can be made to reach maximum, carbonization most effective, the transformation efficiency of Quilonum Retard reaches 78.7%.Even if when the prolongation reaction times is to 150min, the transformation efficiency of Quilonum Retard is also only 79.2%.
Chemical process intensifying technology refers to and can significantly reduce chemical industry equipment volume, reduction device quantity, and simplification of flowsheet, strengthening chemical process, the chemical industry new technology of energy-conserving and environment-protective, meet society energy-saving and emission-reduction, environment amenable demand for development, be therefore considered to the effective technology means solving chemical industry " high energy consumption, high pollution and high material-consumption " problem.High-gravity technology is one of technology having development prospect in chemical process intensifying technology.It has equipment microminiaturization, efficiency is high, energy consumption is low, easy running, the safe and reliable and advantage such as suitability widely, therefore have broad application prospects in fields such as chemical industry, material, biology and environmental protection.
The centrifugal force that high-gravity technology is produced by high speed rotating just increases universal gravity constant, simulation Elevated Gravity, realizes the technology of the mixing of strengthening microcosmic and mass transfer process.The equipment of simulation Elevated Gravity is called high speed rotating bed of packings.Gas liquid reaction many employings adverse current high speed rotating bed of packings, such as, its structure can see old peak of building in 2002 Chemical Industry Press, shown in " high-gravity technology and the application " delivered.
People urgently wish high-gravity technology to be bonded to Quilonum Retard in the middle of the Transformation Application of lithium bicarbonate.
Summary of the invention
For overcoming the deficiencies in the prior art, the invention provides a kind of method improving Quilonum Retard carbonization efficiency by controlling input speed, it comprises the steps:
Step one: get the thick product of Quilonum Retard and be dissolved in distilled water and be mixed with the Quilonum Retard slip that material concentration is 30 ~ 90g/L;
Step 2: make described slip enter rotary packed bed in, and to described rotary packed bed in pass into CO
2gas, obtains feed liquid after carrying out the carburizing reagent of 40 ~ 150min; Wherein, the input speed controlling described slip is 100 ~ 400mL/min, rotary packed bed rotating speed is not higher than 50Hz; And CO
2gas flow is 0.02 ~ 0.20m
3/ L;
Step 3: carry out solid-liquid separation to described feed liquid, obtains lithia water.
Further, described feeding rate is 250 ~ 350mL/min.
Further, described material concentration is 50 ~ 70g/L; Described CO
2gas flow is 0.04 ~ 0.12m
3/ L; Described rotary packed bed rotating speed is 30 ~ 50Hz.
Further, the described carburizing reagent time is 50 ~ 90min.
Beneficial effect:
The present invention is in conjunction with high-gravity technology, adopt high speed rotating bed of packings as conversion unit, optimized the reaction conditions of Quilonum Retard carbonization process by adjustment input speed, substantially increase than prior art the transformation efficiency that Quilonum Retard is converted into lithium bicarbonate, also shorten the reaction times simultaneously.
Accompanying drawing explanation
The trend map that Fig. 1 (a) ~ (d) is each influence factor of the present invention and transformation efficiency.
Fig. 2 (a) ~ (d) is each influence factor of the present invention and the trend map in reaction times.
Embodiment
Below, embodiments of the invention are described in detail with reference to the accompanying drawings.But, the present invention can be implemented in many different forms, and the present invention should not be interpreted as being limited to the specific embodiment of setting forth here.On the contrary, provide these embodiments to be to explain principle of the present invention and practical application thereof, thus enable others skilled in the art understand various embodiment of the present invention and be suitable for the various amendments of certain expected application.
The present invention for raw material, prepares lithia water by high-gravity technology with the thick product slip of Quilonum Retard.By the investigation to material concentration, gas flow, high speed rotating bed of packings rotating speed, feeding rate, obtain the preparation method of lithia water rapidly and efficiently.
The present invention adopts and oldly builds adverse current high speed rotating bed of packings that peak provides as conversion unit, and during the work of adverse current high speed rotating bed of packings, environmental liquids under peristaltic pump is assisted, can enter rotor internal cavity from liquid-inlet.Under the effect of filler, circumferential speed increases, and the centrifugal force produced pushes it against rotor periphery.Gas phase tangentially enters rotor periphery through gas feed, enters in filler under the effect of gaseous tension.Liquid more contacts so that great speed of relative movement is reverse with gas under news rapidly at high dispersive, high turbulence, strong mixing and interface, greatly enhances mass transfer process.Afterwards, liquid is thrown to after shell collects by rotor and discharges through liquid exit.Gas leaves rotor from rotor center, is drawn by pneumatic outlet, completes whole mass transfer or reaction process.
The concrete implementation step of the present invention is as follows:
Step one: get the thick product m of Quilonum Retard
x1(purity is more than 99.5%) is dissolved in 1L distilled water, stirs and obtains the thick product slip of Quilonum Retard with default material concentration (unit, g/L), then pour in four-necked bottle, continues to stir.
Step 2: described slip is sent in high speed rotating bed of packings by peristaltic pump, and to described rotary packed bed in pass into CO
2gas, carries out carbonization to described slip.Wherein, the input speed (unit, mL/min) of described slip, rotary packed bed rotating speed (unit, Hz) and CO is controlled
2flow (unit, the m of gas
3/ L) to preset range.
Wherein, in order to accurately judge reaction end, in whole carbonization process, preferably measuring solution ph every 5 minutes, until the variation range of pH is no more than 0.02, determining that this moment is reaction end.Record whole reaction times t
x(min).
Step 3: after question response is complete, be converted into lithium bicarbonate feed liquid (abbreviation carbonization process) after the carbonization of described Quilonum Retard slip.Described feed liquid is analyzed, calculates the transformation efficiency of carbonization process.
Then the feed liquid obtained after reacting completely is carried out suction filtration, obtain the filtrate of clarifying and filter cake.Wherein, carry out inductively coupled plasma atomic emission spectrum test after described filtrate sampling, measure lithium concentration C in filtrate
x; Described filter cake is dried, and weighs, recording quality m
x2.
Finally in conjunction with above-mentioned obtained data, calculate the efficiency of conversion ω of carbonization process according to formula 1
x(%).
Wherein, C
x(Li
+) be lithium concentration in filtrate, unit g/L;
V
xfor the material liquid volume obtained after carburizing reagent, unit L;
M (Li
2cO
3) be the molar mass of Quilonum Retard, unit is g/mol;
M (Li
+) be the molar mass of lithium ion, unit is g/mol;
M
x1for the quality of Quilonum Retard crude product before carburizing reagent, unit is g;
M
x2for the quality of filter cake described after carburizing reagent, unit is g.
Particularly, in order to carry out described carbonization process four large influence factors: material concentration (A), gas flow (B), rotary packed bed rotating speed (C), feeding rate (D) influence degree to technique are analyzed, to finding out more preferred implementation condition further.The present invention through a large amount of embodiment surface, by high-gravity technology under following implementation condition obtain transformation efficiency all higher than the carbonization process transformation efficiency of prior art:
Material concentration: 40 ~ 80g/L; Gas flow: 0.02 ~ 0.15m
3/ L; High speed rotating bed of packings rotating speed: 10 ~ 50Hz; Feeding rate: 100 ~ 400mL/min.
Wherein, in order to more a step selects better implementation condition, selecting several numerical point in the corresponding scope of ABCD, to be set to the preset value of embodiment as shown in table 1.
The each influence factor preset value of table 1ABCD
The present invention is provided with 9 embodiments, and the implementation condition of this embodiment 1 ~ 9 is as shown in table 2 respectively, and it is as shown in table 3 to obtain respective reaction result according to this implementation condition.Choose transformation efficiency ω
xfor principal reaction index, carry out extreme difference R analysis, result is as shown in table 4.
The each embodiment reaction conditions of table 2
| Embodiment | A(g/L) | B(m 3/h) | C(Hz) | D(mL/min) |
| 1 | 50 | 0.04 | 30 | 150 |
| 2 | 50 | 0.08 | 40 | 250 |
| 3 | 50 | 0.12 | 50 | 350 |
| 4 | 60 | 0.04 | 40 | 350 |
| 5 | 60 | 0.08 | 50 | 150 |
| 6 | 60 | 0.12 | 30 | 250 |
| 7 | 70 | 0.04 | 50 | 250 |
| ? | ? | ? | ? | ? |
| 8 | 70 | 0.08 | 30 | 350 |
| 9 | 70 | 0.12 | 40 | 150 |
The each embodiment reaction result of table 3
| Embodiment | t x(min) | C x(g/L) | m x2(g) | ω x(％) |
| 1 | 102 | 7.233 | 6.9 | 90.2 |
| 2 | 68 | 8.155 | 3.9 | 94.1 |
| 3 | 55 | 8.335 | 5.1 | 98.9 |
| 4 | 53 | 7.881 | 12.3 | 88 |
| 5 | 73 | 7.773 | 14.2 | 90.3 |
| 6 | 58 | 7.929 | 14.3 | 92.4 |
| 7 | 57 | 8.090 | 22.9 | 91.4 |
| 8 | 50 | 7.834 | 21.6 | 86 |
| 9 | 87 | 7.065 | 25 | 83 |
Corresponding k (ω x) value of each influence factor of table 4 and R value
| ? | A(g/L) | B(m 3/h) | C(Hz) | D(mL/min) |
| k 1(ω x) | 94.400 | 89.867 | 89.533 | 87.833 |
| k 2(ω x) | 90.233 | 90.133 | 88.367 | 92.633 |
| k 3(ω x) | 86.800 | 91.433 | 93.533 | 90.967 |
| R | 7.600 | 1.566 | 5.166 | 4.800 |
As shown in Table 3, under the four kinds of influence factor conditions preset, embodiment 1 ~ 9 just reacts completely in 50 ~ 102min, can obtain the high transformation efficiency of 83% ~ 98.9%.Quilonum Retard is obtained much higher less than the transformation efficiency of 80% than the carburizing reagent 90 ~ 150min of prior art.
Below, judge that each influence factor affects primary and secondary to indicator reaction by range analysis, obtain best implementation condition further with this.Extreme difference R value is larger, and represent that the impact of influence factor on indicator reaction is larger, influence factor is more important; On the contrary, the impact of the influence factor that extreme difference R value is little is less.Each R value size in comparison sheet 4, finds that R value is R from big to small successively
a> R
c> R
d> R
b, namely to test, transformation efficiency has the greatest impact is material concentration, is secondly rotating speed and feeding rate, and affecting minimum is CO
2gas flow.
With each influence factor level for X-coordinate, the mean value of indicator reaction is ordinate zou, draws influence factor and indicator reaction trend map.As shown in Fig. 1 (a), Fig. 1 (b), Fig. 1 (c), Fig. 1 (d).Can be found out more intuitively by influence factor and indicator reaction trend map, the trend that test index changes along with the change of influence factor level.Therefore can judge: when with transformation efficiency ω
xduring main experimental results, excellent level is A
1, B
3, C
3, D
2; Excellently be combined as A
1b
3c
3d
2; I.e. material concentration 50g/L, CO
2gas flow 0.12m
3/ h, high speed rotating bed of packings rotating speed 50Hz, feeding rate 250mL/min are the Optimal technique process combination of experiment.
If choose t
xfor main result, carry out range analysis, result is as shown in table 5.
Corresponding k (the t of each influence factor of table 5
x) value and R value
| ? | A(g/L) | B(m 3/h) | C(Hz) | D(mL/min) |
| k 1(t x) | 75.000 | 70.667 | 70.000 | 87.333 |
| k 2(t x) | 61.333 | 63.667 | 69.333 | 61.000 |
| k 3(t x) | 64.667 | 66.667 | 61.667 | 52.667 |
| R | 13.667 | 7.000 | 8.333 | 34.666 |
Each R value size in comparison sheet 5, finds that R value is R from big to small successively
d> R
a> R
c> R
b, what namely have the greatest impact to the reaction times is feeding rate, and it is particularly remarkable to affect comparatively other influences factor.Next is material concentration and rotating speed, and affecting minimum is CO
2gas flow.
With each influence factor level for X-coordinate, the mean value of test index is ordinate zou, draws influence factor and index sign trend.As shown in Fig. 2 (a), Fig. 2 (b), Fig. 2 (c), Fig. 2 (d).Can be found out more intuitively by influence factor and index sign trend, the trend that test index changes along with the change of influence factor level.It can thus be appreciated that, when with t
xfor main result can be chosen: excellent level is A
2, B
2, C
3, D
3, be excellently combined as A
2b
2c
3d
3, i.e. material concentration 60g/L, gas flow 0.08m
3/ h, high speed rotating bed of packings rotating speed 50Hz, feeding rate 350mL/min are the Optimal technique process combination of experiment.
With ω
xand t
xfor indicator reaction, analyze each influence factor preferably span.
Analyze shown in associative list 6 for influence factor A: if choose ω
xfor the excellent level of principal reaction index chooses A
1if choose t
xfor the excellent level of principal reaction index chooses A
2, i.e. the desirable A of the preferable range of material concentration A
1~ A
2between.
Analyze shown in associative list 6 for influence factor B: if choose ω
xfor the excellent level of principal reaction index chooses B
3if choose t
xfor the excellent level of principal reaction index chooses B
2, i.e. the desirable B of the preferable range of gas flow B
2~ B
3between.
Analyze shown in associative list 6 for influence factor C: if choose ω
xfor the excellent level of principal reaction index chooses C
3if choose t
xfor the excellent level of principal reaction index chooses C equally
3, namely the implementation condition of bed of packings rotating speed C the best is C
3, but bed of packings rotating speed C only this value can not be limited thus, in the embodiment 1 ~ 9 cited by the present invention, bed of packings rotating speed is from C
1~ C
3span all can realize the object of the invention.
Analyze shown in associative list 6 for influence factor D: if choose ω
xfor the excellent level of principal reaction index chooses D
2if choose t
xfor the excellent level of principal reaction index chooses D
3, i.e. the desirable D of the preferable range of input speed D
2~ D
3between.
Each influence factor of table 6 is on the Comprehensive Correlation of the impact of differential responses index
| ? | A(g/L) | B(m 3/h) | C(Hz) | D(mL/min) |
| k 1(ω x) | 94.400 | 89.867 | 89.533 | 87.833 |
| k 2(ω x) | 90.233 | 90.133 | 88.367 | 92.633 |
| k 3(ω x) | 86.800 | 91.433 | 93.533 | 90.967 |
| k 1(t x) | 75.000 | 70.667 | 70.000 | 87.333 |
| k 2(t x) | 61.333 | 63.667 | 69.333 | 61.000 |
| k 3(t x) | 64.667 | 66.667 | 61.667 | 52.667 |
Can show that the transformation efficiency that each factor of influence of control obtains in suitable scope will be the selection optimized further, i.e. material concentration 50 ~ 60g/L, gas flow 0.08 ~ 0.12m
3/ h, high speed rotating bed of packings rotating speed 30 ~ 50Hz, feeding rate 250 ~ 350mL/min are the most preferred processing condition of the present invention.
Although illustrate and describe the present invention with reference to specific embodiment, but it should be appreciated by those skilled in the art that: when not departing from the spirit and scope of the present invention by claim and equivalents thereof, the various changes in form and details can be carried out at this.
Claims (4)
1. improving a method for Quilonum Retard carbonization efficiency by controlling input speed, it is characterized in that, comprise the steps:
Step one: get the thick product of Quilonum Retard and be dissolved in distilled water and be mixed with the Quilonum Retard slip that material concentration is 30 ~ 90g/L;
Step 2: make described slip enter rotary packed bed in, and to described rotary packed bed in pass into CO
2gas, obtains feed liquid after carrying out the carburizing reagent of 40 ~ 150min; Wherein, the input speed controlling described slip is 100 ~ 400mL/min, rotary packed bed rotating speed is not higher than 50Hz; And CO
2gas flow is 0.02 ~ 0.20m
3/ L;
Step 3: carry out solid-liquid separation to described feed liquid, obtains lithia water.
2. improve the method for Quilonum Retard carbonization efficiency according to claim 1, it is characterized in that, described feeding rate is 250 ~ 350mL/min.
3. according to claim 1 or 2, improve the method for Quilonum Retard carbonization efficiency, it is characterized in that, described material concentration is described material concentration is 50 ~ 70g/L; Described CO
2gas flow is 0.04 ~ 0.12m
3/ L; Described rotary packed bed rotating speed is 30 ~ 50Hz.
4. improve the method for Quilonum Retard carbonization efficiency according to claim 1, it is characterized in that, the described carburizing reagent time is 50 ~ 90min.
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975357A (en) * | 2018-08-31 | 2018-12-11 | 北京化工大学 | A kind of hypergravity purifying industrial level lithium carbonate system and method |
| CN110902702A (en) * | 2019-12-23 | 2020-03-24 | 天齐锂业（江苏）有限公司 | Automatic design method and control method for lithium carbonate continuous carbonization process |
| CN114933105A (en) * | 2022-05-10 | 2022-08-23 | 海南省智慧环境投资控股有限公司 | Domestic waste separation and concentration treatment device |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180488A (en) * | 2010-04-09 | 2011-09-14 | 清华大学 | Method for preparing nano lithium carbonate |
| CN102531002A (en) * | 2011-12-23 | 2012-07-04 | 四川天齐锂业股份有限公司 | Method for purifying lithium carbonate |
-
2014
- 2014-09-23 CN CN201410490256.5A patent/CN104229837B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180488A (en) * | 2010-04-09 | 2011-09-14 | 清华大学 | Method for preparing nano lithium carbonate |
| CN102531002A (en) * | 2011-12-23 | 2012-07-04 | 四川天齐锂业股份有限公司 | Method for purifying lithium carbonate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108975357A (en) * | 2018-08-31 | 2018-12-11 | 北京化工大学 | A kind of hypergravity purifying industrial level lithium carbonate system and method |
| CN110902702A (en) * | 2019-12-23 | 2020-03-24 | 天齐锂业（江苏）有限公司 | Automatic design method and control method for lithium carbonate continuous carbonization process |
| CN110902702B (en) * | 2019-12-23 | 2022-01-25 | 天齐锂业（江苏）有限公司 | Automatic design method and control method for lithium carbonate continuous carbonization process |
| CN114933105A (en) * | 2022-05-10 | 2022-08-23 | 海南省智慧环境投资控股有限公司 | Domestic waste separation and concentration treatment device |
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