CN103318925B - Method for producing high-purity lithium carbonate by using lithium concentrate - Google Patents
Method for producing high-purity lithium carbonate by using lithium concentrate Download PDFInfo
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Abstract
The invention relates to a method for producing high-purity lithium carbonate by using lithium concentrate. The method is characterized by comprising the following steps of: preparing an acid clinker, preparing a mixing size, preparing a lithium sulfate leaching solution, preparing a lithium sulfate purification liquid, preparing a lithium sulfate finishing solution, preparing a sodium carbonate solution, performing primary lithium deposition reaction, preparing a sodium separating mother liquor, preparing excellent lithium carbonate in a sweating manner, and preparing 99.99% of high-purity lithium carbonate. By adopting the method, the principle of removing calcium and magnesium ions is ingeniously utilized in preparation of common lithium carbonate; a fussy procedure of removing calcium and magnesium by ion exchange resin is avoided when the common lithium carbonate is purified to prepare the high-purity lithium carbonate; a method of recycling after separating out sodium sulfate in a freezing manner is adopted to process the primary lithium settling mother liquor; the high-purity lithium carbonate mother liquor in precipitation of the high-purity lithium carbonate is used as an optimal lithium carbonate washing liquor for primary lithium sedimentation after being recycled for a plurality of times. Thus, the method has the characteristics of simple process, high production efficiency, high recovery rate and low production cost.
Description
Technical field
The present invention relates to a kind of preparation method of pure Lithium Carbonate, particularly relate to a kind of method of lithium concentrate production pure Lithium Carbonate.
Background technology
The preparation method of 99.99% traditional pure Lithium Carbonate has two kinds:
One is that raw material is first prepared into ordinary hydrogen Lithium Oxide 98min after roasting, acidifying, leaching with lithium concentrate, again recrystallization purification is carried out to ordinary hydrogen Lithium Oxide 98min, then the lithium hydroxide after purifying is dissolved in pure water and passes into carbonic acid gas and carry out carbonization and become pure Lithium Carbonate, the method lithium hydroxide amount remaining in mother liquor when carrying out recrystallization to ordinary hydrogen Lithium Oxide 98min and purifying is larger, and yield is low.
Another kind is raw material with lithium concentrate or salt lake brine, the lithium extracted first is obtained by reacting sinker mother liquor and common Quilonum Retard with sodium carbonate, sinker mother liquor adopts evaporation process, common Quilonum Retard is put into logical carbonic acid gas in pure water as the raw material of pure Lithium Carbonate and is carried out carbonization and be dissolved into lithium bicarbonate, and then lithia water is removed calcium ions and magnesium ions through ion exchange resin, again intensification is carried out to the solution after calcium-magnesium removing and separate out pure Lithium Carbonate, the method will use the high ion exchange resin calcium-magnesium removing ion of use cost, and prepare common Quilonum Retard time steam consumption quantity and sodium carbonate consumption all higher, ion exchange resin carries out manipulation of regeneration also can lose part lithium, and also can produce comparative quantity large waste water during bronsted lowry acids and bases bronsted lowry process resin.
Summary of the invention
The object of the present invention is to provide and a kind ofly produce simple, that the rate of recovery is high, energy-conservation method of producing 99.99% pure Lithium Carbonate with lithium concentrate.
The technical solution used in the present invention is:
A method for lithium concentrate production pure Lithium Carbonate, comprises the steps:
(1) sour grog step is prepared: the lithium concentrate of 2000 mass parts is first processed into roasting material through 1000-1150 DEG C of calcining transformation in rotary kiln, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% after cooler is cooled to 80-145 DEG C, and then roasting material is mixed through worm conveyor with the vitriol oil of 500-600 mass parts, and be warming up to 220-280 DEG C of constant temperature 20-30 minute and arrive to obtain sour grog, the remaining sulfuric acid mass percentage controlling sour grog is 3-6%;
(2) adjusting slurry step is prepared: stirring condition adds 1600-2400 mass parts slag washing water and 1600-800 mass parts sweat mother liquor limit below and adds 2500 mass parts acid grogs and carry out sizing mixing obtaining adjusting slurry in surge tank;
(3) prepare Lithium Sulphate leach liquor step: adjusting slurry Paris white carries out being neutralized to pH=5-6, then with scavenging solution filter residue, slurries pH is adjusted to 6.5-8, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water;
(4) Lithium Sulphate scavenging solution step is prepared: in Lithium Sulphate leach liquor, add quality than sodium carbonate: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 9.5-11.5 of lithium sulfate solution, then carry out filtration to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue;
(5) prepare Lithium Sulphate and complete liquid step: it is 52-60g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration and obtain Lithium Sulphate and complete liquid;
(6) sodium carbonate solution step is prepared: sodium carbonate is dissolved in sweat mother liquor, and obtains sodium carbonate solution after filtering, the concentration of sodium carbonate of sodium carbonate solution is 200-300g/L;
(7) elementary sinker reactions steps: sodium carbonate solution is transferred in sinker reactor, open and stir, and in reactor, add the additive accounting for sodium carbonate solution quality 0.02%--0.1%, then sodium carbonate solution is warming up to 80-98 DEG C, and keep 80-98 DEG C slowly to add Lithium Sulphate completing liquid, control the excessive 5%-25% of sodium carbonate, Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtains that calcium contents is less than 0.0005%, Mg content is less than the top grade Quilonum Retard of 0.0003% and elementary sinker mother liquor;
(8) mother liquid of sodium preparation process is analysed: elementary sinker mother liquor is isolated sodium sulfate after carrying out being refrigerated to-3-5 DEG C and obtained analysing mother liquid of sodium;
(9) top grade Quilonum Retard step is prepared in sweat: join analyse mother liquid of sodium in reactor, and be incorporated as the additive of analysing mother liquid of sodium quality 0.002%-0.05% and measuring, then be warming up to 90 DEG C-98 DEG C and separate out precipitation, the top grade Quilonum Retard that calcium contents is less than 0.0005%, Mg content is less than 0.0003% is obtained through solid-liquid separation washing, and obtaining sweat mother liquor, Lithium Oxide 98min concentration remaining in sweat mother liquor controls as Li
2o≤4g/L; Gained sweat mother liquid recycling is in preparation sodium carbonate solution and to size mixing leaching Lithium Sulphate for sour grog on a small quantity;
(10) pure Lithium Carbonate preparation process: top grade Quilonum Retard is joined in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 14-19g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 90-98 DEG C, then carry out centrifugation and washing, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate; Carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after cooling, and the content controlling Lithium Oxide 98min in lithia water is 14-19g/L, be warming up to after filtering 90-98 DEG C separate out precipitation and solid-liquid separation, washing obtain 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally; Carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
Additive in step (7) and step (9) is at least one in EDTA and citric acid.
In step (10), top grade Quilonum Retard joins in pure water and carries out logical carbon dioxide solubility, is: the Ca < 0.00005% in pure water, the Mg < 0.00005% in pure water to the purity requirement of pure water; Carbonization mother liquor is cooled, require carbonization mother liquor temperature be cooled to≤38 DEG C.
The present invention make use of dexterously and just eliminates calcium ions and magnesium ions when preparing common Quilonum Retard, avoid and adopt loaded down with trivial details ion exchange resin calcium-magnesium removing operation when carrying out synthesis pure Lithium Carbonate to common Quilonum Retard, and to the method that the process of elementary sinker mother liquor adopts freezing precipitation sodium sulfate Posterior circle to utilize, this has not only saved traditional technology carries out evaporation process steam energy consumption to elementary sinker mother liquor, and also remaining sodium carbonate excessive in mother liquor has been recycled for preparing sodium carbonate solution after primary mother liquor precipitation sodium sulfate, sodium carbonate consumption is low, and the mother liquor after separating out sodium sulfate is for before the preparation sodium carbonate solution that heats up, Quilonum Retard is first utilized to raise the characteristic of solubleness reduction with temperature, intensification is carried out to mother liquor after analysing sodium sulfate and separates out precipitation, do not consume sodium carbonate like this and just directly obtain a certain amount of top grade Quilonum Retard, and then sweat mother liquor while hot for preparing sodium carbonate solution, additionally consumption sodium carbonate and steam just do not obtain a certain amount of top grade Quilonum Retard dexterously, and pure Lithium Carbonate mother liquor during precipitation pure Lithium Carbonate serves as the use of the top grade Quilonum Retard wash water of elementary sinker after several recycle, fully ensure that the rate of recovery of lithium.
The present invention has the advantages that technique is simple, production efficiency is high, the rate of recovery is high, various consumption is low, constant product quality, superior product quality, production cost are low.
Embodiment
Below in conjunction with embodiment, the present invention will be further described.
Embodiment 1:
Get 2 tons of Lithium Oxide 98min content be 6% lithium concentrate first in rotary kiln, be processed into roasting material through 1000 DEG C of calcining transformations, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% after cooler is cooled to 145 DEG C, and then roasting material is mixed through worm conveyor with 500 kilograms of vitriol oils, and be warming up to 220 DEG C of constant temperature and within 30 minutes, arrive to obtain sour grog, the residual sulfur acid content controlling sour grog is 3%, then in surge tank, whipped state adds 2.4 tons of slag washing water and 0.8 ton of sweat mother liquor limit below and adds 2500 kilograms of sour grogs and carry out sizing mixing obtaining adjusting slurry, adjusting slurry Paris white carries out being neutralized to pH=5, with scavenging solution filter residue, slurries pH is adjusted to 6.5 again, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water, mass percent sodium carbonate is added: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 9.5 of lithium sulfate solution in Lithium Sulphate leach liquor, then filtration is carried out to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue, it is 60g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration to obtain Lithium Sulphate and complete liquid 1.9M
3, then to become concentration of sodium carbonate to be the sodium carbonate solution 2.52M of 200g/L with sweat mother liquor with sodium carbonate
3, and sodium carbonate solution is transferred to 5M
3sinker reactor in, open and stir, and in still, add 504 grams of EDTA, then sodium carbonate solution is warming up to 80 DEG C, and keeps 80 DEG C slowly to add Lithium Sulphate completing liquid, sodium carbonate is excessive is 25%, Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtains top grade Quilonum Retard and elementary sinker mother liquor, and elementary sinker mother liquor is isolated sodium sulfate and obtained analysing mother liquid of sodium 3.4M after carrying out being refrigerated to-3 DEG C
3, analyse mother liquid of sodium and proceed to 5M
3sweat still in, open sweat still and stir and add 1700 grams of EDTA, be then warming up to 98 DEG C of precipitation Quilonum Retards, then carry out centrifugation and washing obtains top grade Quilonum Retard, obtain sweat mother liquor simultaneously, top grade Quilonum Retard is added in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 14g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 90 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor is cooled to 37 DEG C of recycles through cooling tower, top grade Quilonum Retard is added in the carbonization mother liquor through cooling, then logical carbon dioxide solubility becomes lithia water, the Lithium Oxide 98min content controlled wherein is 19g/L, transfer in high-purity sinker still after filtering again, open and stir and be warmed up to 90 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after being cooled to 37 DEG C, and the content controlling Lithium Oxide 98min in lithia water is 14g/L, be warming up to 90 DEG C after filtering and separate out precipitation and solid-liquid separation, washing obtains 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally, carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
Embodiment 2:
Get 2 tons of Lithium Oxide 98min content be 6% lithium concentrate first in rotary kiln, be processed into roasting material through 1150 DEG C of calcining transformations, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% when cooler is cooled to 120 DEG C, and then roasting material is mixed through worm conveyor with 600 kilograms of vitriol oils, and be warming up to 280 DEG C of constant temperature and within 20 minutes, arrive to obtain sour grog, the residual sulfur acid content controlling sour grog is 6%, then in surge tank, whipped state adds 1.6 tons of slag washing water and 1.6 tons of sweat mother liquor limits below and adds 2500 kilograms of sour grogs and carry out sizing mixing obtaining adjusting slurry, adjusting slurry Paris white carries out being neutralized to pH=6, with scavenging solution filter residue, slurries pH is adjusted to 8 again, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water, mass percent sodium carbonate is added: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 11.5 of lithium sulfate solution in Lithium Sulphate leach liquor, then filtration is carried out to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue, it is 52g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration to obtain Lithium Sulphate and complete liquid 2.2M
3, then to become concentration of sodium carbonate to be the sodium carbonate solution 1.41M of 300g/L with sweat mother liquor with sodium carbonate
3, and sodium carbonate solution is transferred to 5M
3sinker reactor in, open and stir, and in still, add 1410 grams of EDTA, then sodium carbonate solution is warming up to 98 DEG C, and keep 98 DEG C slowly to add Lithium Sulphate completing liquid, sodium carbonate is excessive is 5%, and Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtain top grade Quilonum Retard and elementary sinker mother liquor, elementary sinker mother liquor is isolated sodium sulfate and is obtained analysing mother liquid of sodium 2.4M after carrying out being refrigerated to 5 DEG C
3, analyse mother liquid of sodium and proceed to 5M
3sweat still in, open sweat still and stir and add 48 grams of EDTA, be then warming up to 90 DEG C of precipitation Quilonum Retards, then carry out centrifugation and washing obtains top grade Quilonum Retard, obtain sweat mother liquor simultaneously, top grade Quilonum Retard is added in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 19g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 98 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor is cooled to 36 DEG C of recycles through cooling tower, top grade Quilonum Retard is added in the carbonization mother liquor through cooling, then logical carbon dioxide solubility becomes lithia water, the Lithium Oxide 98min content controlled wherein is 16g/L, transfer in high-purity sinker still after filtering again, open and stir and be warmed up to 95 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after being cooled to 30 DEG C, and the content controlling Lithium Oxide 98min in lithia water is 17g/L, be warming up to 95 DEG C after filtering and separate out precipitation and solid-liquid separation, washing obtains 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally, carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
Embodiment 3:
Get 2 tons of Lithium Oxide 98min content be 6% lithium concentrate first in rotary kiln, be processed into roasting material through 1100 DEG C of calcining transformations, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% when cooler is cooled to 100 DEG C, and then roasting material is mixed through worm conveyor with 550 kilograms of vitriol oils, and be warming up to 250 DEG C of constant temperature and within 25 minutes, arrive to obtain sour grog, the residual sulfur acid content controlling sour grog is 4%, then in surge tank, whipped state adds 2 tons of slag washing water and 1.2 tons of sweat mother liquor limits below and adds 2500 sour grogs and carry out sizing mixing obtaining adjusting slurry, adjusting slurry Paris white carries out being neutralized to pH=5.5, with scavenging solution filter residue, slurries pH is adjusted to 7 again, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water, mass percent sodium carbonate is added: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 10.5 of lithium sulfate solution in Lithium Sulphate leach liquor, then filtration is carried out to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue, it is 55g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration to obtain Lithium Sulphate and complete liquid 2.0M
3, then to become concentration of sodium carbonate to be the sodium carbonate solution 1.71M of 250g/L with sweat mother liquor with sodium carbonate
3, and sodium carbonate solution is transferred to 5M
3sinker reactor in, open and stir, and in still, add 1710 grams of citric acids, then sodium carbonate solution is warming up to 90 DEG C, and keep 90 DEG C slowly to add Lithium Sulphate completing liquid, sodium carbonate is excessive is 10%, and Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtain top grade Quilonum Retard and elementary sinker mother liquor, elementary sinker mother liquor is isolated sodium sulfate and is obtained analysing mother liquid of sodium 2.6M after carrying out being refrigerated to 0 DEG C
3, analyse mother liquid of sodium and proceed to 5M
3sweat still in, open sweat still and stir and add 52 grams of citric acids, be then warming up to 95 DEG C of precipitation Quilonum Retards, then carry out centrifugation and washing obtains top grade Quilonum Retard, obtain sweat mother liquor simultaneously, top grade Quilonum Retard is added in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 18g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 95 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor is cooled to 35 DEG C of recycles through cooling tower, top grade Quilonum Retard is added in the carbonization mother liquor through cooling, then logical carbon dioxide solubility becomes lithia water, the Lithium Oxide 98min content controlled wherein is 17g/L, transfer in high-purity sinker still after filtering again, open and stir and be warmed up to 94 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after being cooled to 20 DEG C, and the content controlling Lithium Oxide 98min in lithia water is 14g/L, be warming up to 94 DEG C after filtering and separate out precipitation and solid-liquid separation, washing obtains 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally, carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
Embodiment 4:
Get 2 tons of Lithium Oxide 98min content be 6% lithium concentrate first in rotary kiln, be processed into roasting material through 1050 DEG C of calcining transformations, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% when cooler is cooled to 80 DEG C, and then roasting material is mixed through worm conveyor with 560 kilograms of vitriol oils, and be warming up to 260 DEG C of constant temperature and within 20 minutes, arrive to obtain sour grog, the residual sulfur acid content controlling sour grog is 5%, then in surge tank, whipped state adds 2.0 tons of slag washing water and 1.2 tons of sweat mother liquor limits below and adds 2500 kilograms of sour grogs and carry out sizing mixing obtaining adjusting slurry, adjusting slurry Paris white carries out being neutralized to pH=6, with scavenging solution filter residue, slurries pH is adjusted to 6.5 again, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water, mass percent sodium carbonate is added: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 10 of lithium sulfate solution in Lithium Sulphate leach liquor, then filtration is carried out to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue, it is 58g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration to obtain Lithium Sulphate and complete liquid 1.95M
3, then to become concentration of sodium carbonate to be the sodium carbonate solution 1.71M of 280g/L with sweat mother liquor with sodium carbonate
3, and sodium carbonate solution is transferred to 5M
3sinker reactor in, open and stir, and in still, add 400 grams of EDTA and 400 gram citric acids, then sodium carbonate solution is warming up to 92 DEG C, and keep 92 DEG C slowly to add Lithium Sulphate completing liquid, sodium carbonate is excessive is 15%, and Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtain top grade Quilonum Retard and elementary sinker mother liquor, elementary sinker mother liquor is isolated sodium sulfate and is obtained analysing mother liquid of sodium 2.6M after carrying out being refrigerated to 2 DEG C
3, analyse mother liquid of sodium and proceed to 5M
3sweat still in, open sweat still and stir and add 400 grams of EDTA and 200 gram citric acids, be then warming up to 94 DEG C of precipitation Quilonum Retards, then carry out centrifugation and washing obtains top grade Quilonum Retard, obtain sweat mother liquor simultaneously, top grade Quilonum Retard is added in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 18g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 96 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor is cooled to 34 DEG C of recycles through cooling tower, top grade Quilonum Retard is added in the carbonization mother liquor through cooling, then logical carbon dioxide solubility becomes lithia water, the Lithium Oxide 98min content controlled wherein is 16g/L, transfer in high-purity sinker still after filtering again, open and stir and be warmed up to 93 DEG C, then centrifugation and washing is carried out, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate, carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after being cooled to 25 DEG C, and the content controlling Lithium Oxide 98min in lithia water is 19g/L, be warming up to 93 DEG C after filtering and separate out precipitation and solid-liquid separation, washing obtains 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally, carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
Claims (3)
1. by a method for lithium concentrate production pure Lithium Carbonate, it is characterized in that, comprise the steps:
(1) sour grog step is prepared: the lithium concentrate of 2000 mass parts is first processed into roasting material through 1000-1150 DEG C of calcining transformation in rotary kiln, roasting material is less than 80 orders with the grain diameter that ball mill carries out being milled to 95% after cooler is cooled to 80-145 DEG C, and then roasting material is mixed through worm conveyor with the vitriol oil of 500-600 mass parts, and be warming up to 220-280 DEG C of constant temperature 20-30 minute and arrive to obtain sour grog, the remaining sulfuric acid mass percentage controlling sour grog is 3-6%;
(2) adjusting slurry step is prepared: stirring condition adds 1600-2400 mass parts slag washing water and 1600-800 mass parts sweat mother liquor limit below and adds 2500 mass parts acid grogs and carry out sizing mixing obtaining adjusting slurry in surge tank;
(3) prepare Lithium Sulphate leach liquor step: adjusting slurry Paris white carries out being neutralized to pH=5-6, then with scavenging solution filter residue, slurries pH is adjusted to 6.5-8, then carry out filtering and washing with filter, obtain Lithium Sulphate leach liquor and slag washing water;
(4) Lithium Sulphate scavenging solution step is prepared: in Lithium Sulphate leach liquor, add quality than sodium carbonate: the sodium carbonate of sodium hydroxide=1:1 and sodium hydroxide mixing solutions regulate the pH to 9.5-11.5 of lithium sulfate solution, then carry out filtration to it and obtain Lithium Sulphate scavenging solution and scavenging solution filter residue;
(5) prepare Lithium Sulphate and complete liquid step: it is 52-60g/L that Lithium Sulphate scavenging solution is carried out evaporation concentration to Lithium Oxide 98min content, then carry out filtration and obtain Lithium Sulphate and complete liquid;
(6) sodium carbonate solution step is prepared: sodium carbonate is dissolved in sweat mother liquor, and obtains sodium carbonate solution after filtering, the concentration of sodium carbonate of sodium carbonate solution is 200-300g/L;
(7) elementary sinker reactions steps: sodium carbonate solution is transferred in sinker reactor, open and stir, and in reactor, add the additive accounting for sodium carbonate solution quality 0.02%--0.1%, then sodium carbonate solution is warming up to 80-98 DEG C, and keep 80-98 DEG C slowly to add Lithium Sulphate completing liquid, control the excessive 5%-25% of sodium carbonate, Lithium Sulphate completes after liquid adds and carries out centrifugation and washing, obtains that calcium contents is less than 0.0005%, Mg content is less than the top grade Quilonum Retard of 0.0003% and elementary sinker mother liquor;
(8) mother liquid of sodium preparation process is analysed: elementary sinker mother liquor is isolated sodium sulfate after carrying out being refrigerated to-3-5 DEG C and obtained analysing mother liquid of sodium;
(9) top grade Quilonum Retard step is prepared in sweat: join analyse mother liquid of sodium in reactor, and be incorporated as the additive of analysing mother liquid of sodium quality 0.002%-0.05% and measuring, then be warming up to 90 DEG C-98 DEG C and separate out precipitation, the top grade Quilonum Retard that calcium contents is less than 0.0005%, Mg content is less than 0.0003% is obtained through solid-liquid separation washing, and obtaining sweat mother liquor, Lithium Oxide 98min concentration remaining in sweat mother liquor controls as Li
2o≤4g/L; Gained sweat mother liquid recycling is in preparation sodium carbonate solution and to size mixing leaching Lithium Sulphate for sour grog on a small quantity;
(10) pure Lithium Carbonate preparation process: top grade Quilonum Retard is joined in pure water and passes into carbon dioxide solubility and become lithia water, and the content controlling Lithium Oxide 98min in lithia water is 14-19g/L, then filter, filtrate is transferred in high-purity sinker still, open and stir and be warmed up to 90-98 DEG C, then carry out centrifugation and washing, obtain carbonization mother liquor and 99.99% pure Lithium Carbonate; Carbonization mother liquor carries out recycle and continues on for carbonization and dissolve top grade Quilonum Retard and become lithia water after cooling, and the content controlling Lithium Oxide 98min in lithia water is 14-19g/L, be warming up to after filtering 90-98 DEG C separate out precipitation and solid-liquid separation, washing obtain 99.99% pure Lithium Carbonate, obtain carbonization mother liquor equally; Carbonization mother liquor after several times recycle is used as the bath water of top grade Quilonum Retard.
2. the method for a kind of lithium concentrate production pure Lithium Carbonate according to claim 1, is characterized in that, the additive in step (7) and step (9) is at least one in EDTA and citric acid.
3. the method for a kind of lithium concentrate production pure Lithium Carbonate according to claim 1, it is characterized in that, in step (10), top grade Quilonum Retard joins in pure water and carries out logical carbon dioxide solubility, to the purity requirement of pure water be: the Ca < 0.00005% in pure water, the Mg < 0.00005% in pure water; Carbonization mother liquor is cooled, require carbonization mother liquor temperature be cooled to≤38 DEG C.
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