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A kind of extraction method for separating calcium and extracting lithium from low-temperature calcium-containing brine and its application

A lithium extraction and extraction technology, applied in the field of separating calcium and extracting lithium from low-temperature calcium-containing brine, to achieve the effects of ensuring continuity, large lithium-calcium separation coefficient, and high extraction rate

Active Publication Date: 2022-08-09
GUANGZHOU TINCI MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the solvent extraction method is used to extract lithium from oilfield brine, the low-temperature performance of the extractant and back-extraction agent becomes particularly prominent. It is required that the two phases should not coagulate and precipitate at ambient temperature, and still maintain good extraction performance and flow state. , there is no relevant literature report on this

Method used

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  • A kind of extraction method for separating calcium and extracting lithium from low-temperature calcium-containing brine and its application
  • A kind of extraction method for separating calcium and extracting lithium from low-temperature calcium-containing brine and its application
  • A kind of extraction method for separating calcium and extracting lithium from low-temperature calcium-containing brine and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Li in a calcium-containing brine + , Ca 2+ and Cl - The contents are 3.50, 179.99 and 336.29g / L respectively, the mass ratio of calcium to lithium is 51.42:1, and the density of brine at 0℃ is 1.40g / cm 3 , the pH value of brine is 7.0. Take 24mL N-n-pentyl-3,5,5-trimethylhexanamide as extractant in a 250mL ground conical flask with insulated interlayer, then add 8mL of this brine, the organic phase and the volume of calcium-containing brine. The ratio is 3:1. Put the magnet in the conical flask, insert the ground stopper into the bottle mouth, put it in the DF-101S magnetic stirrer, connect the liquid circulation hose of the DC-3010 low temperature thermostat with the ground cone with the insulating interlayer The inlet and outlet ports of the bottle are connected, and the cooling cycle is performed, and the mixture is mixed and stirred at –0.1°C for 30 minutes. Then, the mixed liquid was transferred to a 100mL plastic test tube after being frozen at the same tempe...

Embodiment 2

[0051] Take 20mL N-n-pentyl-3,5,5-trimethylhexanamide and 4mL N-n-octyl-4-methylpentanamide as extractants in a 250mL ground-top conical flask with insulation sandwich, and then put Wherein 8mL of calcium-containing brine in Example 1 was added, and the volume ratio of the organic phase to the calcium-containing brine was 3:1. Put the magnet in the conical flask, insert the ground stopper into the bottle mouth, put it in the DF-101S magnetic stirrer, connect the liquid circulation hose of the DC-3010 low temperature thermostat with the ground cone with the insulating interlayer The inlet and outlet ports of the bottle were connected, and the cooling cycle was performed, and the mixture was mixed and stirred at –5°C for 30 minutes. Then, the mixed liquid was transferred to a 100mL plastic test tube after being frozen at the same temperature, and centrifuged at 4400r / min for 8min in an LD5-10 desktop centrifuge. The two-phase interface was clear. + , Ca 2+ organic phase. Tran...

Embodiment 3

[0057] Li in a calcium-containing brine + and Ca 2+ The content is 5.56 and 173.79g / L respectively, the mass ratio of calcium and lithium is 31.25:1, of which Na + , K + , Mg 2+ , Cl - and B 2 O 3 The contents are 3.13, 20.51, 1.89, 364.27 and 2.23g / L respectively, and the brine density is 1.40g / cm at 0℃ 3, the pH value of the brine is 4.0, and the ion concentration in the brine is prepared according to the composition of brine in an oilfield in Nanyishan, Qaidam Basin, Qinghai. The brine in the oilfield is pre-oiled with an oil-water separator. Get 3mL of this brine in a 250mL ground-mouth conical flask with insulation interlayer, then add 15mL N-n-pentyl-3,5,5-trimethylhexanamide as extractant and 15mL N,N-di( 1-Methyl)heptylacetamide was used as a co-extracting agent, and the co-extracting agent accounted for 50% of the volume of the organic phase, and the volume ratio of the organic phase to the calcium-containing brine was 10:1. Put the magnet in the conical flask...

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Abstract

The invention discloses an extraction method for separating calcium from low-temperature calcium-containing brine and extracting lithium and its application. A secondary amide solvent or a secondary amide-containing solvent is used as the organic phase, the brine phase consisting of sodium chloride, potassium chloride or a mixture thereof is used as a back-extracting agent, and the freezing point of the organic phase is lower than the temperature at which the extraction is performed, and the brine is in a liquid state. use below. The volume ratio of the organic phase to the calcium-containing brine is 1-10:1, and the brine density is 1.30-1.56g / cm at 0°C 3 , The pH value of brine is 1~7 and the extraction temperature is –20~<0℃ for single-stage extraction or multi-stage countercurrent extraction; the volume ratio of brine phase and loaded organic phase is 1:1~20 and the back extraction temperature is –20~< Single-stage back-extraction or multi-stage counter-current back-extraction is carried out at 0 °C, and a low-calcium-to-lithium ratio lithium-containing brine phase is obtained after two-phase separation. It is transferred to a brine pool, concentrated in the sun, solid-liquid separated and further concentrated, and then a precipitant is added to remove the Ca. 2+ and sulfate radicals and other impurities, and then carry out precipitation and conversion reactions to obtain lithium carbonate, lithium hydroxide, lithium phosphate and lithium dihydrogen phosphate products respectively.

Description

technical field [0001] The invention relates to a method for separating calcium and extracting lithium from calcium-containing brine by a solvent extraction method, in particular to an extraction method for separating calcium and lithium from low-temperature calcium-containing brine with a secondary amide-containing solvent and its application. Background technique [0002] Lithium resources are the material basis for the development of the new energy industry in the 21st century, and can be divided into two types: ore type and brine type. Lithium ores with the most mining applications in the world today are spodumene, lithium feldspar, lepidolite and lepidolite, which are mainly processed by potassium sulfate method, sulfuric acid method, lime method and chlorination roasting method to extract lithium. higher cost. There are many kinds of brine-type lithium resources, which can be divided into chloride-type, sulfate-type and carbonate-type according to Varyashko hydrochemi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C22B3/32C22B26/12C22B3/22
CPCC22B26/12C22B3/22Y02P10/20
Inventor 杨立新李海博田翔邝高龙李娜
Owner GUANGZHOU TINCI MATERIALS TECH