CN107687020A - A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy - Google Patents
A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy Download PDFInfo
- Publication number
- CN107687020A CN107687020A CN201710443026.7A CN201710443026A CN107687020A CN 107687020 A CN107687020 A CN 107687020A CN 201710443026 A CN201710443026 A CN 201710443026A CN 107687020 A CN107687020 A CN 107687020A
- Authority
- CN
- China
- Prior art keywords
- bittern
- whisker
- exposed
- sun
- alkali formula
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy.Comprise the following steps：S1. the insoluble matter in bittern is filtered；S2. the bittern after filtering is introduced in salt pan or transparent vessel, be exposed to the sun under sunshine；S3. NaI and NaOH mixed solutions are added into the bittern after being exposed to the sun, is exposed to the sun under sunshine 2~4 days, refilters bittern, you can obtain alkali formula magnesium iodide whisker.The present invention prepares alkali formula magnesium iodide whisker using solar energy and whisker self-cleaning from bittern, it is simple to operate, without complicated equipment, not only energy consumption is low and does not produce pollutant and public hazards, cleanable to utilize salt lake resources environmentally friendlyly, obtained whisker yield is high, best in quality, prepare magnesium salt whisker on a large scale suitable for actual production, there is larger application prospect.
Description
Technical field
The invention belongs to technical field of salt chemical industry.Alkali formula is prepared from bittern using solar energy more particularly, to one kind
The method of magnesium iodide whisker.
Background technology
Alkali formula magnesium iodide whisker is prepared from bittern in salt lake, seawater bittern, presently mainly utilizes electric energy or gas-fired
The heat energy of releasing.Solar energy is approximately equivalent to 130,000,000,000,000 as a kind of new energy, the annual solar radiant energy reached on earth surface
Ton coal, the maximum energy that its total amount category can be developed in the world now.It has three big features compared with conventional energy resource such as electric energy：
First：It is the utilizable most abundant energy of the mankind.It is estimated that in past very long 1,100,000,000 years, the sun consumes it
The 2% of itself energy.It is enough to supply the earth mankind from now on, is inexhaustible using tens years.Second：Ground
On ball, anywhere there is solar energy, can develop on the spot, especially to traffic and underdeveloped Qinghai Salt Lake, island etc.
Remote districts have more significance.3rd：Solar energy is a kind of clean energy.Utilize when, will not produce waste residue, waste water,
Waste gas, there is no noise yet, do not interfere with the ecological balance more.It can never pollute and public hazards.This and low energy consumption, clean environment firendly
Ground using salt lake resources be it is highly consistent, to both can low cost, develop to high level salt lake resources, protect salt lake life again
State environment has important scientific meaning.
Magnesium salt whisker is directly produced without purification ＆ isolation, the characteristic mainly in itself using whisker with " self-cleaning ", it
It is not easy to be infected with, is not easy absorption, entrainment impurity, this is the very big difference of whisker and other amorphous sediments, and amorphous sediment is such as
Flocculence magnesium hydroxide is very easy absorption, entrainment impurity.
Due under certain preparation condition, alkali formula shepardite whisker has " self-cleaning ", and (" self-cleaning " of whisker tool be
Refer to whisker atomic arrangement high-sequential, intact filling or seldom lack filling, difficult adsorbing contaminant, the difficult characteristic being infected with by impurity), therefore,
Complicated removal of impurities is not present in preparation process, as long as whisker samples with water is washed.
The scientific basis of whisker self-cleaning is：First, as described above, whisker is defective without (or seldom containing)；Second,
The whisker surface field of force is distributed in high degree of symmetry and specific surface area is small, thus is not easy adsorbing contaminant.Theoretical, the surface according to surface chemistry
The field of force is more symmetrical, specific surface area is smaller, to the adsorption capacity of impurity with regard to smaller, it is difficult to which chemisorbed occurs.3rd, whisker
Require that growth unit there must be specific stabilization energy in growth course, otherwise can not enter lattice.But, the physics of whisker
Absorption is on the contrary certainly existing, but this weak physical absorption need to only be washed with water and can remove the impurity of absorption.It is but brilliant
Must grow straight play its self-cleaning be conditional, be not in no instance can adsorbing contaminant, be infected with by impurity.
What this condition referred to is exactly the suitable Chemical Physics condition of whisker growth system, such as concentration and the addition of alkali, system pH, anti-
Answer temperature, reaction time etc..Therefore, how alkali formula magnesium iodide whisker is prepared from bittern using solar energy and whisker self-cleaning is
The problem of current in the urgent need to address.
The content of the invention
The technical problems to be solved by the invention are the defects of overcoming above-mentioned prior art and deficiency, there is provided one kind is using too
Sun can prepare the method for alkali formula magnesium iodide whisker from bittern.
The above-mentioned purpose of the present invention is to give realization by the following technical programs：
A kind of method for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, is comprised the following steps：
S1. the insoluble matter in bittern is filtered；
S2. the bittern after filtering is introduced in salt pan or transparent vessel, be exposed to the sun under sunshine 30~40 DEG C；
S3. NaI and NaOH mixed solutions are added into the bittern after being exposed to the sun, is exposed to the sun 2~4 days, refilters under sunshine
Bittern, you can obtain alkali formula magnesium iodide whisker；
Final concentration of 2~the 4mol/L of NaI in NaI and NaOH mixed solutions described in step S3, NaOH final concentration of 0.1~
1mol/L；
The volume ratio of NaI and NaOH mixed solutions and bittern described in step S3 is 0.5~1：1.
The present invention different is exposed to the sun mode to prepare alkali formula magnesium iodide whisker, when in the bittern of salt lake or seawater by two kinds
Magnesium chloride when reaching saturation, in wind or shine upon lower while add a certain amount of NaI and NaOH, you can generation is accordingly
Alkali formula magnesium iodide whisker, its reaction equation are as follows：
After alkali formula magnesium iodide whisker is separated by filtration, collection can obtain alkali formula magnesium iodide whisker.It is mainly water, chlorination in filtrate
The material such as sodium and other soluble-salts, now, magnesium ion concentration necessarily reduces in filtrate systems.If filtrate is continued to allow the sun
Be exposed to the sun, water is distilled out of, and sodium chloride (and the less salt of some solubility) also due to the reduction of aqueous solvent and separate out, but magnesium chloride
Inevitably enlarge that (it is certain dense that the growth of alkali formula magnesium iodide whisker requires that magnesium chloride has without the concentration of precipitation, therefore magnesium chloride
Degree).Now, if the circulation of a new round can be entered by injecting alkali into system again.But meanwhile this circulation is also limited
And the circulation that can not have no limits down.Because：Sodium chloride, potassium chloride and some other salt can be precipitated, and water can be distilled out of, but
It is that also necessarily to have fraction component (such as iron, aluminium plasma) be still to stay in system, and increasing with cycle-index, this
Kind concentration of component accumulation is increasing, as a result causes whisker sample to receive contamination, whisker purity, which is lowered so that, does not meet country
Standard.
Preferably, when the magnesium ion concentration in the bittern after step S3 is exposed to the sun is 2.1~3.1mol/L, NaI can be added
With NaOH mixed solutions, circulated next time.
Preferably, the time is exposed to the sun described in step S3 for 3 days.
Preferably, methods described is that the bittern after filtering is introduced into salt pan, is exposed to the sun under sunshine to 35~40 DEG C；
2~3mol/L NaI and 0.1~0.5mol/L NaOH mixed solutions are added into the bittern after being exposed to the sun, are continued under sunshine
It is exposed to the sun, refilters bittern, you can obtains alkali formula magnesium iodide whisker.
It is highly preferred that described be exposed to the sun to be exposed to the sun to 35 DEG C；NaI is final concentration of in NaI the and NaOH mixed solutions
The final concentration of 0.2mol/L of 2.6mol/L, NaOH.
Preferably, the bittern after filtering is is introduced in transparent vessel by methods described, be exposed to the sun under sunshine to 30~
35℃；Into the bittern after being exposed to the sun add 3~4mol/L NaI and 0.6~1mol/L NaOH mixed solutions, under sunshine after
It is continuous to be exposed to the sun, refilter bittern, you can obtain alkali formula magnesium iodide whisker.
It is highly preferred that described be exposed to the sun to be exposed to the sun to 30 DEG C；The final concentration of 3mol/ of NaI in NaI the and NaOH mixed solutions
The final concentration of 0.8mol/L of L, NaOH.
Preferably, the transparent vessel is that can receive the uniform irradiation of sunshine, the container for being heated evenly bittern, such as
Clear glass water vat.
No matter the above-mentioned bittern prepared using solar energy needed for the method for alkali formula magnesium iodide whisker comes from salt lake or sea
Water can prepare mass height, the high alkali formula magnesium iodide whisker of purity.Therefore, it is above-mentioned that alkali is prepared from bittern using solar energy
The method of formula magnesium iodide whisker prepares application on alkali formula magnesium salt whisker also in the scope of the present invention in salt lake or seawater.
The invention has the advantages that：
The invention provides a kind of method that alkali formula magnesium iodide whisker is prepared using solar energy and whisker self-cleaning, operation letter
Single, without the equipment of complexity, not only energy consumption is low and does not produce pollutant and public hazards, cleanable to utilize salt lake resources environmentally friendlyly, obtains
The whisker yield arrived is high, best in quality, prepares magnesium salt whisker on a large scale suitable for actual production, before having larger application
Scape.
Brief description of the drawings
Fig. 1 is the process chart that the present invention prepares alkali formula magnesium iodide whisker using solar energy from bittern.
Embodiment
The present invention is further illustrated below in conjunction with Figure of description and specific embodiment, but embodiment is not to the present invention
Limit in any form.Unless stated otherwise, the reagent of the invention used, method and apparatus routinely try for the art
Agent, method and apparatus.
Unless stated otherwise, following examples agents useful for same and material are purchased in market.
Embodiment 1
1st, alkali formula magnesium iodide whisker is prepared from bittern in salt lake using salt pan, is specifically comprised the following steps：
(1) bittern in salt lake (bittern is taken at Qinghai Chaerhan salt lakes) is filtered, discards insoluble matter；
(2) in the salt field that area is 0.1 mu, 1m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 35 DEG C；
(3) final concentration of 2.60mol/L NaI and 0.2mol/L NaOH mixed solutions are prepared；
(4) step (3) mixed solution and bittern solution are introduced into above-mentioned salt pan for 1 ︰ 1 by volume；Then proceed to too
Being exposed to the sun under sunlight three days (after the daily sun sets, can be covered salt pan with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post
Shine again), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker, then scrubbed, drying production
Product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 18 or so, amorphous whiskerses matter is few, and whisker yield is 94%, good dispersion.
Embodiment 2
1st, alkali formula magnesium iodide whisker is prepared from bittern in salt lake using salt pan, is specifically comprised the following steps：
(1) bittern in salt lake (bittern is taken at Guangdong Xuwen saltern) is filtered, discards insoluble matter；
(2) in the salt field that area is 0.1 mu, 1m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 37 DEG C；
(3) final concentration of 2.0mol/L NaI and 0.5mol/L NaOH mixed solutions are prepared；
(4) step (3) mixed solution and bittern solution are introduced into above-mentioned salt pan for 0.5 ︰ 1 by volume；Then proceed to
Being exposed to the sun under sunshine three days (after the daily sun sets, can be covered salt pan with canvas or other plastic clothes, treat that the second light is come out of retirement and taken up an official post
When shine again), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker, then scrubbed, drying production
Product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 17 or so, amorphous whiskerses matter is less, and whisker yield is 83%, and dispersiveness is preferably.
Embodiment 3
1st, alkali formula magnesium iodide whisker is prepared from bittern in salt lake using salt pan, is specifically comprised the following steps：
(1) bittern in salt lake (bittern is taken at Guangdong Leizhou saltern) is filtered, discards insoluble matter；
(2) in the salt field that area is 0.1 mu, 1m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 40 DEG C；
(3) final concentration of 3.0mol/L NaI and 0.1mol/L NaOH mixed solutions are prepared；
(4) step (3) mixed solution and bittern solution are introduced into above-mentioned salt pan for 1 ︰ 1 by volume；Then proceed to too
Being exposed to the sun under sunlight three days (after the daily sun sets, can be covered salt pan with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post
Shine again), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker, then scrubbed, drying production
Product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 19 or so, amorphous whiskerses matter is less, and whisker yield is 82%, and dispersiveness is preferably.
Embodiment 4
1st, alkali formula magnesium iodide whisker is prepared from bittern in salt lake using salt pan, is specifically comprised the following steps：
(1) bittern in salt lake (bittern is taken at Qinghai Chaerhan salt lakes) is filtered, discards insoluble matter；
(2) in the salt field that area is 0.1 mu, 1m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 30 DEG C；
(3) final concentration of 4.0mol/L NaI and 1mol/L NaOH mixed solutions are prepared；
(4) step (3) mixed solution and bittern solution are introduced into above-mentioned salt pan for 0.8 ︰ 1 by volume.Then proceed to
Being exposed to the sun under sunshine three days (after the daily sun sets, can be covered salt pan with canvas or other plastic clothes, treat that the second light is come out of retirement and taken up an official post
When shine again), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker, then scrubbed, drying production
Product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 15 or so, amorphous whiskerses matter is less, and whisker yield is 86%, and dispersiveness is preferably.
Embodiment 5
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, is specifically comprised the following steps：
(1) 50L bitterns (bittern is taken at Qinghai Chaerhan salt lakes) are taken, filters and discards insoluble matter；
(2) final concentration of 3mol/L NaI and 0.8mol/L NaOH mixed solutions are prepared.
(3) bittern after step (1) is filtered pours into the circular uncovered and transparent glass that radius is 60cm, depth is 30cm
In glass water vat, and it is placed under sunshine and is exposed to the sun to 30 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added
Supplement, or a transparent glass cover is capped on water vat.
(4) it is 1 by mixed liquor and bittern volume ratio:1, step (2) mixed liquor is poured at a slow speed step (3) under agitation
Have warmed up into 30 DEG C of bittern, then proceed to be placed under sunshine be exposed to the sun three days (after the daily sun sets, can be by reaction system
Cover, shone again when the second light is come out of retirement and taken up an official post), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker,
Scrubbed again, drying product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 18 or so, amorphous whiskerses matter is few, and whisker yield is 92%, good dispersion.
Embodiment 6
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, is specifically comprised the following steps：
(1) 50L bitterns (bittern is taken at Guangdong Xuwen saltern) are taken, filters and discards insoluble matter；
(2) final concentration of 3.5mol/L NaI and 0.6mol/L NaOH mixed solutions are prepared.
(3) bittern after step (1) is filtered pours into the circular uncovered and transparent glass that radius is 60cm, depth is 30cm
In glass water vat, and it is placed under sunshine and is exposed to the sun to 35 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added
Supplement, or a transparent glass cover is capped on water vat.
(4) it is 0.8 by mixed liquor and bittern volume ratio：1, step (2) mixed liquor is poured at a slow speed step under agitation
(3) have warmed up into 35 DEG C of bittern, then proceeding to be placed under sunshine to be exposed to the sun three days (after the daily sun sets, will can react
System covers, and is shone again when the second light is come out of retirement and taken up an official post), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide
Whisker, then scrubbed, drying product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 18 or so, amorphous whiskerses matter is less, and whisker yield is 83%, and dispersiveness is preferably.
Embodiment 7
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, is specifically comprised the following steps：
(1) 50L bitterns (bittern is taken at Guangdong Xuwen saltern) are taken, filters and discards insoluble matter；
(2) final concentration of 4mol/L NaI and 1mol/L NaOH mixed solutions are prepared；
(3) bittern after step (1) is filtered pours into the circular uncovered and transparent glass that radius is 60cm, depth is 30cm
In glass water vat, and it is placed under sunshine and is exposed to the sun to 30 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added
Supplement, or a transparent glass cover is capped on water vat；
(4) it is 0.5 by mixed liquor and bittern volume ratio:1, step (2) mixed liquor is poured at a slow speed step under agitation
(3) have warmed up into 30 DEG C of bittern, then proceeding to be placed under sunshine to be exposed to the sun three days (after the daily sun sets, will can react
System covers, and is shone again when the second light is come out of retirement and taken up an official post), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide
Whisker, then scrubbed, drying product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 19 or so, amorphous whiskerses matter is less, and whisker yield is 84%, and dispersiveness is preferably.
Embodiment 8
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, is specifically comprised the following steps：
(1) 50L bitterns (bittern is taken at Guangdong Xuwen saltern) are taken, filters and discards insoluble matter；
(2) final concentration of 2mol/L NaI and 0.1mol/L NaOH mixed solutions are prepared；
(3) bittern after step (1) is filtered pours into the circular uncovered and transparent glass that radius is 60cm, depth is 30cm
In glass water vat, and it is placed under sunshine and is exposed to the sun to 40 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added
Supplement, or a transparent glass cover is capped on water vat；
(4) it is 1 by mixed liquor and bittern volume ratio：1, step (2) mixed liquor is poured at a slow speed step (3) under agitation
Have warmed up into 40 DEG C of bittern, then proceed to be placed under sunshine be exposed to the sun three days (after the daily sun sets, can be by reaction system
Cover, shone again when the second light is come out of retirement and taken up an official post), then the filtered through gauze bittern with densification, you can what is obtained is alkali formula magnesium iodide whisker,
Scrubbed again, drying product；
(5) filtrate obtained by step (4) is placed in into sunshine to be exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ±
0.5mol/L, NaI and NaOH mixed solutions are then added, by the circulation of above-mentioned steps entrance next time；
(6) when iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, circulation is stopped.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide；Sample
SEM test results show that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, size distribution
Uniformly, for draw ratio about 16 or so, amorphous whiskerses matter is less, and whisker yield is 78%, and dispersiveness is preferably.
Comparative example 1
1st, alkali formula magnesium iodide whisker, concrete operation method and 1 basic phase of embodiment are prepared from bittern in salt lake using salt pan
Together, only difference is that bittern is introduced directly into salt pan without filtering.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 30%.
Comparative example 2
1st, alkali formula magnesium iodide whisker, concrete operation method and 1 basic phase of embodiment are prepared from bittern in salt lake using salt pan
Together, only difference is that the final concentration of 1.5mol/L of NaI, NaOH are final concentration of in NaI the and NaOH mixed solutions of step (3)
1.2mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 35%.
Comparative example 3
1st, alkali formula magnesium iodide whisker, concrete operation method and 1 basic phase of embodiment are prepared from bittern in salt lake using salt pan
Together, only difference is that the final concentration of 4.2mol/L of NaI, NaOH are final concentration of in NaI the and NaOH mixed solutions of step (3)
0.05mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is very low, and purity is also very low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is a lot,
Whisker yield is only 20%.
Comparative example 4
1st, alkali formula magnesium iodide whisker, concrete operation method and 1 basic phase of embodiment are prepared from bittern in salt lake using salt pan
Together, only difference is that the temperature of being exposed to the sun in step (2) is 25 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 60%.
Comparative example 5
1st, alkali formula magnesium iodide whisker, concrete operation method and 1 basic phase of embodiment are prepared from bittern in salt lake using salt pan
Together, only difference is that the temperature of being exposed to the sun in step (2) is 45 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 58%.
Comparative example 6
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5,
Only difference is that the final concentration of 1.7mol/L of NaI, NaOH are final concentration of in NaI the and NaOH mixed solutions of step (2)
1.4mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 39%.
Comparative example 7
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5,
Only difference is that the final concentration of 4.5mol/L of NaI, NaOH are final concentration of in NaI the and NaOH mixed solutions of step (2)
0.08mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is very low, and purity is also very low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is a lot,
Whisker yield is only 34%.
Comparative example 8
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5,
Only difference is that the temperature of being exposed to the sun in step (3) is 22 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is only 53%.
Comparative example 9
1st, alkali formula magnesium iodide whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5,
Only difference is that the temperature of being exposed to the sun in step (3) is 43 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali formula magnesium iodide, but sample
Product crystallinity is not high, and purity is low；SEM test results show that sample only possesses basic crystal whisker-shaped, and non-whisker material is more, whisker
Yield is 65%.
Claims (9)
- A kind of 1. method for preparing alkali formula magnesium iodide whisker from bittern using solar energy, it is characterised in that comprise the following steps：S1. the insoluble matter in bittern is filtered；S2. the bittern after filtering is introduced in salt pan or transparent vessel, be exposed to the sun under sunshine to 30~40 DEG C；S3. NaI and NaOH mixed solutions are added into the bittern after being exposed to the sun, is exposed to the sun under sunshine 2~4 days, refilters bittern, It can obtain alkali formula magnesium iodide whisker；Final concentration of 2~4 mol/L of NaI in NaI and NaOH mixed solutions described in step S3, the final concentration of 0.1~1mol/ of NaOH L；The volume ratio of NaI and NaOH mixed solutions and bittern described in step S3 is 0.5~1：1.
- 2. the method according to claim 1 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In, when the magnesium ion concentration in the bittern after step S3 is exposed to the sun is 2.1~3.1mol/L, can add NaI mixed with NaOH it is molten Liquid, circulated next time.
- 3. the method according to claim 1 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In the time of being exposed to the sun described in step S3 is 3 day.
- 4. the method according to claim 1 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In the bittern after filtering is introduced into salt pan, is exposed to the sun under sunshine to 35~40 DEG C；2~3 are added into the bittern after being exposed to the sun Mol/L NaI and 0.1~0.5mol/L NaOH mixed solutions, continue to be exposed to the sun, refilter bittern, you can obtain under sunshine Alkali formula magnesium iodide whisker.
- 5. the method according to claim 4 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In described to be exposed to the sun to be exposed to the sun to 35 DEG C；Final concentration of 2.6 mol/L of NaI, NaOH are dense eventually in NaI the and NaOH mixed solutions Spend for 0.2 mol/L.
- 6. the method according to claim 1 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In the bittern after filtering is introduced in transparent vessel, is exposed to the sun under sunshine to 30~35 DEG C；Add into the bittern after being exposed to the sun Enter 3~4 mol/L NaI and 0.6~1mol/L NaOH mixed solutions, continue to be exposed to the sun under sunshine, refilter bittern, you can Obtain alkali formula magnesium iodide whisker.
- 7. the method according to claim 6 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In described to be exposed to the sun to be exposed to the sun to 30 DEG C；Final concentration of 3 mol/L of NaI, NaOH final concentrations in NaI the and NaOH mixed solutions For 0.8 mol/L.
- 8. the method according to claim 1 for being prepared alkali formula magnesium iodide whisker from bittern using solar energy, its feature are existed In the transparent vessel is clear glass water vat.
- 9. any one of claim 1~8 is described to prepare the method for alkali formula magnesium iodide whisker in salt lake using solar energy from bittern Or application on alkali formula magnesium salt whisker is prepared in seawater.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710443026.7A CN107687020A (en) | 2017-06-13 | 2017-06-13 | A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710443026.7A CN107687020A (en) | 2017-06-13 | 2017-06-13 | A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107687020A true CN107687020A (en) | 2018-02-13 |
Family
ID=61152627
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710443026.7A Withdrawn CN107687020A (en) | 2017-06-13 | 2017-06-13 | A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107687020A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353815A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Method for preparing basic magnesium chloride whisker from dolomite and bittern |
| CN101956234A (en) * | 2010-10-09 | 2011-01-26 | 中国科学院青海盐湖研究所 | Method for preparing basic magnesium sulfate whiskers by recycling mother liquor |
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
-
2017
- 2017-06-13 CN CN201710443026.7A patent/CN107687020A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101353815A (en) * | 2008-08-19 | 2009-01-28 | 浙江大学 | Method for preparing basic magnesium chloride whisker from dolomite and bittern |
| CN101956234A (en) * | 2010-10-09 | 2011-01-26 | 中国科学院青海盐湖研究所 | Method for preparing basic magnesium sulfate whiskers by recycling mother liquor |
| CN102002751A (en) * | 2010-10-11 | 2011-04-06 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
| CN102002751B (en) * | 2010-10-11 | 2012-04-11 | 国家海洋局天津海水淡化与综合利用研究所 | Method for directly synthesizing basic magnesium sulfate whiskers by brine |
Non-Patent Citations (1)
| Title |
|---|
| 吴健松等: "徐闻盐场苦卤制备碱式氯化镁晶须", 《中山大学学报(自然科学版)》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104131352B (en) | The preparation method of large scale perovskite structure methylamine bustamentite crystal | |
| CN102602966B (en) | Method for separating magnesium and lithium in salt lake brine and preparing lithium carbonate | |
| WO2013053165A1 (en) | Method for production of lithium carbonate by applying multi-bittern-adding method, and using carbonate type bittern and sulfate type bittern as raw material | |
| CN105776257B (en) | Salt lake bittern separating magnesium and lithium and the method for producing magnesium hydroxide and high-purity magnesium oxide | |
| CN103570048A (en) | Method for refining lithium from salt lake brine with high magnesium-lithium ratio | |
| CN103723875A (en) | Seawater full recycling process | |
| CN107119200B (en) | A kind of method of waste and old mischmetal fluorescent powder high efficiente callback rare earth element | |
| CN104150499A (en) | Preparation method of high-purity boric acid and nuclear grade high-purity boric acid | |
| CN1212271C (en) | Method for integrated production of magnesium sulfate, magnesium carbonate and magnesium hydroxide from magnesite | |
| CN102826556A (en) | Method for separating and extracting diatom shells from diatom | |
| CN102774860B (en) | Method for preparing lithium carbonate by brine | |
| CN107653492A (en) | A kind of method for preparing alkali magnesium sulfate crystal whisker from bittern using solar energy | |
| CN107675246A (en) | A kind of method for preparing magnesia crystal whisker from bittern using solar energy | |
| CN107675252A (en) | A kind of method for preparing magnesium hydroxide crystal whisker from bittern using solar energy | |
| CN107687020A (en) | A kind of method for preparing alkali formula magnesium iodide whisker from bittern using solar energy | |
| CN107675253A (en) | A kind of method for preparing Basic magnesium bromide whisker from bittern using solar energy | |
| CN107675254A (en) | A kind of method for preparing basic magnesium chloride whisker from bittern using solar energy | |
| CN107675259A (en) | A kind of method for preparing basic magnesium carbonate whisker from bittern using solar energy | |
| CN107675245A (en) | A kind of method for preparing alkali formula magnesium borate crystal whisker from bittern using solar energy | |
| CN109847716B (en) | Natural mineral-based uranium extraction adsorbent from seawater and preparation method thereof | |
| CN102491406B (en) | Method for preparing gallium sulfate | |
| CN107687019A (en) | A kind of method for preparing hollow tubular basic magnesium carbonate whisker from bittern using solar energy | |
| CN114835233B (en) | Method for rapidly removing chloride ions in wastewater by bismuth-based metal organic framework material | |
| CN103993179A (en) | Method for recovering germanium from germanium-silicon alloy | |
| CN108070907A (en) | A kind of method that bittern of dried-up lake prepares basic magnesium chloride whisker |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180213 |