CN104129817B - A kind of solvent displacement prepares the method for waterless cobaltous chloride - Google Patents
A kind of solvent displacement prepares the method for waterless cobaltous chloride Download PDFInfo
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- CN104129817B CN104129817B CN201410294456.3A CN201410294456A CN104129817B CN 104129817 B CN104129817 B CN 104129817B CN 201410294456 A CN201410294456 A CN 201410294456A CN 104129817 B CN104129817 B CN 104129817B
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- cobaltous chloride
- waterless cobaltous
- chloride
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Abstract
The method that solvent displacement prepares waterless cobaltous chloride relates to an a kind of preparation method of inorganic salt, and its key step is as follows: (1) carries out CoCl under middle low temperature
26H
2the preliminary hydro-extraction of O, this step can be taken off the crystal water of 4 molecules thus be obtained CoCl
22H
2o; (2) by CoCl
22H
2add organic solvent in O, utilize organic solvent to be replaced by water molecules; (3) carry out azeotropic distillation dehydration, obtain solvation waterless cobaltous chloride; (4) under nitrogen atmosphere, the waterless cobaltous chloride of solvation is carried out drying in tube furnace, steams solvent, obtain waterless cobaltous chloride.The purity of prepared cobalt chloride is greater than 99%, and the rate of recovery is more than 99%.Present invention process is simple, and easy to operate, processing parameter easily controls, and to equipment without particular requirement, is easy to suitability for industrialized production.
Description
Technical field
The present invention relates to inorganic chemicals industry field.
Background technology
Waterless cobaltous chloride is a kind of important fine chemical material, and the application of cobalt chloride is mainly included in instrument manufacturing and is used as to produce weather gauge, specific gravity hydrometer, dry wet indicator etc.Ceramic industry is used as tinting material.Coatings industry is for the manufacture of paint drier.For configuring mixed feed in livestock industry.Brewery industry is used as Beer Foam Stabilizers.National defense industry is for the manufacture of poison gas cover.Catalyzer is used as in chemical reaction.Divide for spot analysis zinc in folding chemistry, haploid breeding, in addition, also for the manufacture of sympathetic ink, paper of cobalt chloride,test, discolour silica gel etc.Also be used as the absorption agent of ammonia.Domesticly at present do not produce on a large scale, the PRODUCTION TRAITS of industrialization waterless cobaltous chloride is subject to the attention of China's chemical engineering industry always.
Cobalt chloride crystal is at room temperature stablized, and loses crystal water and becomes blue, in malaria, then become redness again again after being heated.Therefore the preparation of waterless cobaltous chloride seems more complicated.The production method of prior art is that cobalt chloride hexahydrate is directly carried out thermal dehydration, this method length consuming time, and energy consumption is large, and in heat-processed, cobalt chloride hydrolysis can occur and then generates cobalt oxide black solid simultaneously.Patent CN102357308A report adopts and is heated by air, spray-drying chamber is entered and cobalt chloride solution carries out heat exchange to prepare waterless cobaltous chloride with rotating state, number of devices required for this method is many, and complicated, needs higher temperature (230-280 DEG C) simultaneously.The burn high-temperature gas that produces and cobalt chloride of CN101041473A report hydrogen and chlorine carries out heat exchange, and need electromagnetic catalysis, this method complicated operation, require high to equipment performance, operational danger is large, chlorine gas leakage can pollute surrounding enviroment, higher to the requirement of equipment.
Summary of the invention
For the deficiency that prior art exists, the object of the present invention is to provide a kind of operating process equipment simple, the solvent exchange that safety and environmental protection, energy consumption are low prepares the method for waterless cobaltous chloride.
The present invention adopts following technical scheme for this reason:
Solvent displacement prepares a method for waterless cobaltous chloride,
1, the water molecules in low hydrated cobalt chloride is carried out displacement and obtain solvation waterless cobaltous chloride, then it is carried out in nitrogen atmosphere drying and obtain waterless cobaltous chloride, avoid the hydrolysis of the cobalt chloride caused when water exists.Key step comprises the following steps:
CoCl is carried out at step 1:50-150 DEG C
26H
2the preliminary hydro-extraction of O, this step can be taken off the crystal water of 4 molecules thus be obtained CoCl
22H
2o;
Step 2: by CoCl
22H
2o to adding ethanol, Virahol, n-propyl alcohol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, sec-butyl alcohol, amylalcohol, primary isoamyl alcohol, low-carbon alcohol and the acetonitriles such as 3-amylalcohol, in the organic solvents such as propionitrile, mechanical stirring mixes fully, is replaced by water with organic solvent;
Step 3: carry out azeotropic distillation dehydration, obtains solvation waterless cobaltous chloride;
Step 4: under nitrogen protection, carries out drying by the waterless cobaltous chloride of solvation, steams solvent, obtain waterless cobaltous chloride in tube furnace;
2, in step 1, Heating temperature is 120 DEG C, heat-up time 120min;
3, described in step 2 organic solvent be ethanol, Virahol, n-propyl alcohol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, sec-butyl alcohol, amylalcohol, primary isoamyl alcohol, 3-amylalcohol etc. and low-carbon alcohol and acetonitrile, the organic solvents such as propionitrile, the low hydrated cobalt chloride obtained in the first step is added in organic solvent, is uniformly mixed fully, organic solvent is replaced fully to water;
4, carry out the dehydration of normal pressure azeotropic distillation altogether in step 3, carry out azeotropic distillation dehydration with organic solvent as entrainer, the amount of organic solvent used is 1-5 times of low hydrated cobalt chloride quality, and rectifying reflux ratio is 5:1-10:1;
5, in step 4 in drying process, need to protect with nitrogen, the Heating temperature of tube furnace is 100 DEG C, and time of drying is 120min, and the flow velocity of nitrogen is 50mL/min.
The technical program technique is simple, and easy to operate, without the need to high-temperature operation, processing parameter easily controls, and to equipment without particular requirement, safety non-pollution, is easy to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is process flow sheet prepared by waterless cobaltous chloride.
Embodiment
Example one: (1) takes 500g cobalt chloride hexahydrate CoCl
26H
2o, puts into 120 DEG C, baking oven heating 120min, obtains two hydrated cobalt chloride CoCl
22H
2o;
(2) two hydrated cobalt chlorides the first step obtained join in dehydrated alcohol, stir fully, are cemented out by the water molecules in low hydrated cobalt chloride with ethanol, and the consumption of ethanol is 1 times of two hydrated cobalt chloride quality;
(3) material obtained in second step is carried out azeotropic distillation, Heating temperature is 150 DEG C, and reflux ratio is that 10:1 carries out extraction liquid of top of the tower, until when tower top temperature reaches 78.5 DEG C, stop extraction, azeotropic distillation terminates, then unnecessary ethanol is steamed recovery, obtain solvation waterless cobaltous chloride;
(4) the solvation waterless cobaltous chloride obtained in the 3rd step is put into tube furnace, in nitrogen atmosphere, carry out 100 DEG C of heating 120min steamed by ethanol, obtain waterless cobaltous chloride, weigh m=270g, and the purity of cobalt chloride is 99.1%.
Example two: (1) takes 500g cobalt chloride hexahydrate, puts into 120 DEG C, baking oven heating 120min, obtains two hydrated cobalt chlorides;
(2) two hydrated cobalt chlorides the first step obtained join in anhydrous n-propyl alcohol, stir fully, are cemented out by the water molecules in low hydrated cobalt chloride with n-propyl alcohol, and the consumption of n-propyl alcohol is 3 times of two hydrated cobalt chloride quality;
(3) material obtained in second step is carried out azeotropic distillation, Heating temperature is 150 DEG C, and reflux ratio is that 8:1 carries out extraction liquid of top of the tower, until when tower top temperature reaches 97.2 DEG C, stop extraction, azeotropic distillation terminates, then unnecessary n-propyl alcohol is steamed recovery, obtain solvation waterless cobaltous chloride;
(4) the solvation waterless cobaltous chloride obtained in the 3rd step is put into tube furnace, in nitrogen atmosphere, n-propyl alcohol steams by 100 DEG C of heating 120min, and obtain waterless cobaltous chloride, weigh m=270.5g, and the purity of cobalt chloride is 99.5%.
Example three: (1) takes 500g cobalt chloride hexahydrate, puts into 120 DEG C, baking oven heating 120min, obtains two hydrated cobalt chlorides;
(2) two hydrated cobalt chlorides the first step obtained join in anhydrous isopropyl alcohol, stir fully, are cemented out by the water molecules in low hydrated cobalt chloride with Virahol, and the consumption of Virahol is 4 times of two hydrated cobalt chloride quality;
(3) material obtained in second step is carried out azeotropic distillation, Heating temperature is 150 DEG C, and reflux ratio is that 6:1 carries out extraction liquid of top of the tower, until when tower top temperature reaches 82.4 DEG C, stop extraction, azeotropic distillation terminates, then unnecessary Virahol is steamed recovery, obtain solvation waterless cobaltous chloride;
(4) the solvation waterless cobaltous chloride obtained in the 3rd step is put into tube furnace, in nitrogen atmosphere, Virahol steams by 100 DEG C of heating 120min, and obtain waterless cobaltous chloride, weigh m=270.0g, and the purity of cobalt chloride is 99.6%.
Example four: (1) takes 500g cobalt chloride hexahydrate, puts into 120 DEG C, baking oven heating 120min, obtains two hydrated cobalt chlorides;
(2) two hydrated cobalt chlorides the first step obtained join in acetonitrile, stir fully, are cemented out by the water molecules in low hydrated cobalt chloride with acetonitrile, and the consumption of acetonitrile is 5 times of two hydrated cobalt chloride quality;
(3) material obtained in second step is carried out azeotropic distillation, Heating temperature is 150 DEG C, and reflux ratio is that 5:1 carries out extraction liquid of top of the tower, until when tower top temperature reaches 76 DEG C, stop extraction, azeotropic distillation terminates, then unnecessary acetonitrile is steamed recovery, obtain solvation waterless cobaltous chloride;
(4) the solvation waterless cobaltous chloride obtained in the 3rd step is put into tube furnace, in nitrogen atmosphere, carry out 100 DEG C of heating 120min steamed by acetonitrile, obtain waterless cobaltous chloride, weigh m=271.1g, and the purity of cobalt chloride is 99.4%.
Claims (7)
1. solvent displacement prepares a method for waterless cobaltous chloride, it is characterized in that: carry out as follows:
Step 1: carry out CoCl
26H
2the preliminary hydro-extraction of O, this step can be taken off the crystal water of 4 molecules thus be obtained CoCl
22H
2o;
Step 2: by CoCl
22H
2o joins in low-carbon alcohol or acetonitrile, propionitrile organic solvent, stirs fully, carries out the displacement of water; Described low-carbon alcohol is ethanol, Virahol, n-propyl alcohol, propyl carbinol, isopropylcarbinol, the trimethyl carbinol, sec-butyl alcohol, amylalcohol, primary isoamyl alcohol, in 3-amylalcohol any one; The quality of described organic solvent is CoCl
22H
2the 1-5 of O quality doubly;
Step 3: carry out azeotropic distillation dehydration to the cobalt chloride after solvent exchange, obtains solvation waterless cobaltous chloride; During described azeotropic distillation dehydration, control of reflux ratio is 1:1-10:1, and tower top temperature is 50-150 DEG C, and the Heating temperature of tower reactor is 100-200 DEG C;
Step 4: under nitrogen protection, carries out drying by the waterless cobaltous chloride of solvation, steams solvent, obtain waterless cobaltous chloride in tube furnace.
2. a kind of solvent displacement according to claim 1 prepares the method for waterless cobaltous chloride, it is characterized in that: in step 1, preliminary hydro-extraction temperature is 60 DEG C-150 DEG C, and dewatering time is 60min-240min.
3. a kind of solvent displacement according to claims 1 or 2 prepares the method for waterless cobaltous chloride, it is characterized in that: drying mode used in step 1 is electric heating forced air drying method or boulton process.
4. a kind of solvent displacement according to claim 1 prepares the method for waterless cobaltous chloride, it is characterized in that: alr mode used in step 2 is magnetic agitation or mechanical stirring, and the time of stirring is 30-90min.
5. a kind of solvent displacement according to claim 1 prepares the method for waterless cobaltous chloride, it is characterized in that: the rectifying mode adopted in step 3 is atmospheric distillation, and the height of rectifying column is 1-2m.
6. a kind of solvent displacement according to claim 1 prepares the method for waterless cobaltous chloride, it is characterized in that: when adopting tube furnace to carry out drying in step 4, and heating and temperature control is at 50-200 DEG C, and the time is 30-150min, and protection gas is nitrogen or argon gas.
7. a kind of solvent displacement according to claim 1 or 6 prepares the method for waterless cobaltous chloride, it is characterized in that: when adopting tube furnace to carry out drying in step 4, and the flow velocity of nitrogen is 10-60mL/min.
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| CN101254942A (en) * | 2008-04-07 | 2008-09-03 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
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| CN101254942A (en) * | 2008-04-07 | 2008-09-03 | 昆明理工大学 | Method for preparing high-purity anhydrous indium trichloride |
Non-Patent Citations (2)
| Title |
|---|
| 6H2O的脱水步骤及有关的动力学.《山西大学学报》.1987,(第3期),第73-78页. * |
| 李国顺等.CoC12• * |
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