CN1693512A - High sodium metal lithium and its manufacturing method - Google Patents

Abstract

A high-Na metal lithium with high content of Na and activity for the catalysis process contains metal lithium and trace elements, in which Na content is 1.5-3.5 mass%. Its preparing process includes such steps as mixing lithium carbonate, hydrochloric acid and Na salt, stirring while reacting, press filtering, concentrating, baking, electrolyzing, smelting and casting.

Description

High sodium metal lithium and manufacture method thereof

Technical field

The invention belongs to field of metallurgy, relate in particular to higher metallic lithium of sodium content and manufacture method thereof.

Background technology

Metallic lithium has crucial effect in modern industry, molar mass is little, electronegativity is low and the chemically reactive advantages of higher because it has, and all is widely used in industry such as lithium cell, lithium alloy, atomic reactor, pharmacy, chemical fibre, pottery, plastics, metallurgy, organolithium.Industrial purity requirement to metallic lithium differs, and the purity of general industry level metallic lithium reaches 98.5%.For a long time, low sodium lithium is the main product in market always, and the sodium content of electrolysis lithium is lower than 1% usually; And high sodium metal lithium is mainly used in the catalytic process of industries such as medicine, petrochemical industry, rubber, and sodium content is high more, and dispersiveness is good more, reacts fast more, and the production cycle is short more, and energy consumption is low more.

Summary of the invention

Purpose of the present invention provides a kind of high sodium metal lithium and manufacture method thereof.

The present invention is achieved by the following technical solution: a kind of high sodium metal lithium and manufacture method thereof, described high sodium metal lithium comprises metallic lithium and trace element, the quality of metallic lithium accounts for more than 96.5% of product total mass, and the quality of sodium accounts for 1.5～3.5% of product total mass in the described high sodium metal lithium.

The quality of sodium accounts for about 2.5% of product total mass in the described high sodium metal lithium.

The manufacture method of product high sodium metal lithium:

A. batching is mixed technical hydrochloric acid by mass ratio with the technical grade Quilonum Retard at 3.5: 1, carries out stirring reaction at normal temperatures, in 1～10 hour reaction times, after reaction is finished, add the sodium salt of batch mixing total mass 5～15% again, get mixed solution, control its pH value, pH value is 7～8;

B. press filtration is carried out press filtration with pressure filter to mixed solution, gets clear liquid;

C. concentrate, clear liquid is heated concentrated, 150～350 ℃ of Heating temperatures, obtain the anhydrous crystal body at 4～20 hours heat-up times;

D. oven dry, further to anhydrous crystal body oven dry, 200～350 ℃ of temperature, time 1-8 hour obtain the anhydrous crystalline mixing salt of moisture content＜0.1% under the vacuum state;

E. electrolysis, the Repone K (moisture＜0.1%) of mixing salt and respective quality is carried out electrolysis in electrolyzer, strength of current 2800～3200A, bath voltage 6.8～8.2V, 460～580 ℃ of temperature, in time take out the metallic lithium that floats in the groove, and with white oil protection, replenish once electrolytic matter simultaneously, the ionogen magnitude of recruitment be the lithium amount 6-7 doubly;

F, founding packing, the lithium piece is taken out in electrolysis put into white oil founding pot, heat 183～250 ℃, remove by filter ionogen and oxide compound, again metallic lithium is injected the mould demoulding to be solidified, put into the white oil bucket, after draining white oil, in the drying room of relative humidity≤5%, pack pressure≤5Pa with Vacuum Packaging Machine.

The present invention accounts under the prerequisite more than 96.5% of product total mass in the quality that guarantees metallic lithium, its sodium content accounts for 1.5～3.5% of product total mass, the sodium content height, the activity of sodium is stronger, at first participates in reaction, cause the metallic lithium reaction, play katalysis, shortened the reaction times, increased production capacity, save energy consumption, increased benefit.

Embodiment

A kind of manufacture method of high sodium metal lithium:

A. batching, 875 kilograms of technical hydrochloric acids with 31% mix for 250 kilograms with 99% technical grade Quilonum Retard, carry out stirring reaction at normal temperatures, reacts 3 hours, add 125 kilograms sodium-chlor, must mixed solution, control pH value, make its pH value in 7～8 scopes;

B. press filtration is carried out press filtration with pressure filter to mixed solution, and pressure is 0.3MPa, and filter cloth is 300 orders, gets clear liquid;

C. concentrate, clear liquid is heated concentrated, 260 ℃ of Heating temperatures, 8 hours heat-up times, the anhydrous crystal body;

D. oven dry, further to the oven dry of anhydrous crystal body, 280 ℃ of bake out temperatures, make xln institute water content less than 0.1% at 3 hours time under vacuum state;

E. electrolysis, with anhydrous crystal body (moisture content＜0.1%) and etc. the Repone K (moisture content＜0.1%) of quality in electrolyzer, carry out electrolysis, strength of current 3000A, bath voltage 7.2V, 520 ℃ of temperature were taken out the metallic lithium that floats in the groove, metallic lithium are protected with white oil in per 2～3 hours, and electrolyte supplement simultaneously, magnitude of recruitment is 6 times of lithium amount;

F founding packing, with the metallic lithium that takes out after the electrolysis, put into white oil founding pot, be heated to 200 ℃ for each 3～4 kilograms, after removing by filter ionogen and oxide compound, metallic lithium is injected mould, solidify the demoulding after, put into the white oil bucket, after draining white oil, in the drying room of relative humidity≤5%, be packaged as finished product with Vacuum Packaging Machine, pressure is less than 5Pa.

High sodium metal lithium of the present invention, its sodium content height, activity is stronger, when playing katalysis, shortens and knows clearly the reaction times, saves energy consumption, has increased benefit.

Claims (3)

1, high sodium metal lithium comprises metallic lithium and trace element, and the quality of metallic lithium accounts for more than 96.5% of product total mass, it is characterized in that: the quality of sodium accounts for 1.5～3.5% of product total mass in the described high sodium metal lithium.

2, high sodium metal lithium according to claim 1 is characterized in that: the quality of described sodium accounts for about 2.5% of product total mass.

3, the manufacture method of product high sodium metal lithium:

A. batching is mixed technical hydrochloric acid by mass ratio with the technical grade Quilonum Retard at 3.5: 1, carries out stirring reaction at normal temperatures, in 1～10 hour reaction times, after reaction is finished, add the sodium salt of batch mixing total mass 5～15% again, get mixed solution, control its pH value, pH value is 7～8;

B. press filtration is carried out press filtration with pressure filter to mixed solution, gets clear liquid;

C. concentrate, clear liquid is heated concentrated, 150～350 ℃ of Heating temperatures, obtain the anhydrous crystal body at 4～20 hours heat-up times;

D. oven dry, further to anhydrous crystal body oven dry, 200～350 ℃ of temperature, time 1-8 hour obtain the anhydrous crystalline mixing salt of moisture content＜0.1% under the vacuum state;

E. electrolysis, the Repone K (moisture＜0.1%) of mixing salt and respective quality is carried out electrolysis in electrolyzer, strength of current 2800～3200A, bath voltage 6.8～8.2V, 460～580 ℃ of temperature, in time take out the metallic lithium that floats in the groove, and with white oil protection, replenish once electrolytic matter simultaneously, the ionogen magnitude of recruitment be the lithium amount 6-7 doubly;

F, founding packing, the lithium piece is taken out in electrolysis put into white oil founding pot, heat 183～250 ℃, remove by filter ionogen and oxide compound, again metallic lithium is injected the mould demoulding to be solidified, put into the white oil bucket, after draining white oil, in the drying room of relative humidity≤5%, pack pressure≤5Pa with Vacuum Packaging Machine.