CN107653492A - A kind of method for preparing alkali magnesium sulfate crystal whisker from bittern using solar energy - Google Patents

A kind of method for preparing alkali magnesium sulfate crystal whisker from bittern using solar energy Download PDF

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Publication number
CN107653492A
CN107653492A CN201710443955.8A CN201710443955A CN107653492A CN 107653492 A CN107653492 A CN 107653492A CN 201710443955 A CN201710443955 A CN 201710443955A CN 107653492 A CN107653492 A CN 107653492A
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bittern
magnesium sulfate
crystal whisker
sulfate crystal
exposed
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吴健松
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Lingnan Normal University
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Lingnan Normal University
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    • 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
    • C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a kind of method for preparing alkali magnesium sulfate crystal 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 to 50~60 DEG C；S3. Na is added into the bittern after being exposed to the sun2SO4With NaOH mixed solutions, continue to be exposed to the sun under sunshine, filter bittern, obtain alkali magnesium sulfate crystal whisker presoma；S4. alkali magnesium sulfate crystal whisker presoma is put into water, is warming up to 80~100 DEG C, and grow 25~35h at this temperature, you can obtain alkali magnesium sulfate crystal whisker.The present invention prepares alkali magnesium sulfate crystal 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

A kind of method for preparing alkali magnesium sulfate crystal whisker from bittern using solar energy
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 sulfate crystal whisker.
Background technology
Alkali magnesium sulfate crystal 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.
Because under certain preparation condition, alkali formula shepardite whisker has " self-cleaning "（Whisker tool " self-cleaning " 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 free of（Or seldom contain）It is defective；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 magnesium sulfate crystal 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 The method that sun can prepare alkali magnesium sulfate crystal 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 magnesium sulfate crystal 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 to 50~60 DEG C；
S3. Na is added into the bittern after being exposed to the sun2SO4With NaOH mixed solutions, it is exposed to the sun under sunshine 2~4 days, filtering is bitter Halogen, obtain alkali magnesium sulfate crystal whisker presoma；
S4. alkali magnesium sulfate crystal whisker presoma is put into water, is warming up to 80~100 DEG C, and at this temperature growth 25~ 35h, you can obtain alkali magnesium sulfate crystal whisker；
Na described in step S32SO4With Na in NaOH mixed solutions2SO4Final concentration of 0.5~2mol/L, NaOH final concentration of 0.2 ~1mol/L；
Na described in step S32SO4It is 0.5~1 with the volume ratio of NaOH mixed solutions and bittern：1.
The present invention by two kinds it is different be exposed to the sun mode to prepare alkali magnesium sulfate crystal whisker, when salt lake or the bittern of seawater In magnesium chloride when reaching saturation, in wind or shine upon lower while add a certain amount of Na2SO4, you can generation is corresponding Alkali magnesium sulfate crystal whisker, its reaction equation are as follows：
After alkali magnesium sulfate crystal whisker is separated by filtration, collection can obtain alkali magnesium sulfate crystal whisker.It is mainly water, sodium chloride in filtrate With the material such as 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 chlorination Magnesium is without precipitation, therefore the concentration of magnesium chloride inevitably enlarges that (it is certain that the growth of alkali magnesium sulfate crystal whisker requires that magnesium chloride has Concentration).Now, if the circulation of a new round can be entered by injecting alkali into system again.But meanwhile this circulation is also limited Degree 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 steamed Go out, but also necessarily there is the fraction component (such as iron, aluminium plasma) to be still staying in system, and with cycle-index Increase, this concentration of component accumulation is increasing, as a result causes whisker sample to receive contamination, whisker purity is lowered so that not Meet national standard.
Preferably, when the magnesium ion concentration in the bittern after step S3 is exposed to the sun is 2.1~3.1mol/L, can add Na2SO4With NaOH mixed solutions, circulated next time.
Preferably, the time is exposed to the sun described in step S3 for 3 days.
Preferably, step S4 is obtained into alkali magnesium sulfate crystal whisker and 20~30h is dried at 77~83 DEG C, produce alkali formula sulfuric acid Magnesium crystal whisker products.
Preferably, methods described is that the bittern after filtering is introduced into salt pan, is exposed to the sun under sunshine to 55~60 DEG C；To 0.5~1mol/L Na are added in bittern after being exposed to the sun2SO4With 0.2~0.5mol/L NaOH mixed solutions, under sunshine after It is continuous to be exposed to the sun, refilter bittern, you can obtain alkali magnesium sulfate crystal whisker presoma.
It is highly preferred that described be exposed to the sun to be exposed to the sun to 60 DEG C；The Na2SO4With Na in NaOH mixed solutions2SO4It is final concentration of The final concentration of 0.3mol/L of 0.7mol/L, NaOH.
Preferably, the bittern after filtering is is introduced in transparent vessel by methods described, be exposed to the sun under sunshine to 50~ 55℃；1~2mol/L Na are added into the bittern after being exposed to the sun2SO4With 0.5~1mol/LNaOH mixed solutions, under sunshine Continue to be exposed to the sun, refilter bittern, you can obtain alkali magnesium sulfate crystal whisker presoma.
It is highly preferred that described be exposed to the sun to be exposed to the sun to 55 DEG C；The Na2SO4With Na in NaOH mixed solutions2SO4Final concentration For 1.5mol/L, the final concentration of 0.7mol/L of 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 magnesium sulfate crystal whisker comes from salt lake or sea Water can prepare mass height, the high alkali magnesium sulfate crystal whisker of purity.Therefore, it is above-mentioned that alkali is prepared from bittern using solar energy The method of formula magnesium sulfate crystal 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：
It is simple to operate the invention provides a kind of method for preparing alkali magnesium sulfate crystal whisker using solar energy and whisker self-cleaning, 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, obtains Whisker yield is high, best in quality, prepares magnesium salt whisker on a large scale suitable for actual production, has larger application prospect.
Brief description of the drawings
Fig. 1 is the process chart that the present invention prepares alkali magnesium sulfate crystal 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 magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, specifically comprised the following steps：
（1）By bittern in salt lake（Bittern is taken at Qinghai Chaerhan salt lakes）Filtered, discard insoluble matter；
（2）In the salt field that area is 0.1 mu, 2m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 60 DEG C；
（3）Prepare final concentration of 0.7mol/L Na2SO4With 0.3mol/L NaOH mixed solutions；
（4）By step（3）Mixed solution introduces above-mentioned salt pan for 1 ︰ 1 by volume with bittern solution；Then proceed in sunshine Under be exposed to the sun three days（After the daily sun sets, salt pan can be covered with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post again Shine）, then the filtered through gauze bittern with densification, you can what is obtained is alkali magnesium sulfate crystal whisker, then scrubbed, drying product；
（5）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration is 2.600 ± 0.5 Mol/L, then add Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（6）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 15 or so, amorphous whiskerses matter is few, and whisker yield is 95%, good dispersion.
Embodiment 2
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, specifically comprised the following steps：
（1）By bittern in salt lake（Bittern is taken at Guangdong Xuwen saltern）Filtered, discard insoluble matter；
（2）In the salt field that area is 0.1 mu, 2m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 58 DEG C；
（3）Prepare final concentration of 1mol/L Na2SO4With 0.2mol/L NaOH mixed solutions；
（4）By step（3）Mixed solution introduces above-mentioned salt pan for 0.5 ︰ 1 by volume with bittern solution；Then proceed in the sun It is exposed to the sun under light three days（After the daily sun sets, salt pan can be covered with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post again Shine）, then the filtered through gauze bittern with densification, you can what is obtained is alkali magnesium sulfate crystal whisker, then scrubbed, drying product；
（5）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration is 2.600 ± 0.5 Mol/L, then add Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（6）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 16 or so, amorphous whiskerses matter is less, and whisker yield is 80%, and dispersiveness is preferably.
Embodiment 3
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, specifically comprised the following steps：
（1）By bittern in salt lake（Bittern is taken at Guangdong Leizhou saltern）Filtered, discard insoluble matter；
（2）In the salt field that area is 0.1 mu, 2m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 55 DEG C；
（3）Prepare final concentration of 0.5mol/L Na2SO4With 0.2mol/L NaOH mixed solutions；
（4）By step（3）Mixed solution introduces above-mentioned salt pan for 1 ︰ 1 by volume with bittern solution；Then proceed in sunshine Under be exposed to the sun three days（After the daily sun sets, salt pan can be covered with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post again Shine）, then the filtered through gauze bittern with densification, you can what is obtained is alkali magnesium sulfate crystal whisker, then scrubbed, drying product；
（5）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration is 2.600 ± 0.5 Mol/L, then add Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（6）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 18 or so, amorphous whiskerses matter is less, and whisker yield is 85%, and dispersiveness is preferably.
Embodiment 4
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, specifically comprised the following steps：
（1）By bittern in salt lake（Bittern is taken at Qinghai Chaerhan salt lakes）Filtered, discard insoluble matter；
（2）In the salt field that area is 0.1 mu, 2m is introduced3Bittern after filtering, and be exposed to the sun under sunshine to 50 DEG C；
（3）Prepare final concentration of 2mol/L Na2SO4With 1mol/L NaOH mixed solutions；
（4）By step（3）Mixed solution introduces above-mentioned salt pan for 0.8 ︰ 1 by volume with bittern solution.Then proceed in the sun It is exposed to the sun under light three days（After the daily sun sets, salt pan can be covered with canvas or other plastic clothes, when the second light is come out of retirement and taken up an official post again Shine）, then the filtered through gauze bittern with densification, you can what is obtained is alkali magnesium sulfate crystal whisker, then scrubbed, drying product；
（5）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration is 2.600 ± 0.5 Mol/L, then add Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（6）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 14 or so, amorphous whiskerses matter is less, and whisker yield is 76%, and dispersiveness is preferably.
Embodiment 5
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, specifically comprised the following steps：
（1）Take 50L bitterns（Bittern is taken at Qinghai Chaerhan salt lakes）, filter and discard insoluble matter；
（2）Prepare final concentration of 1.5mol/L Na2SO4And 0.7mol/L NaOH mixed solutions.
（3）By step（1）Bittern after filtering pours into the circular uncovered that radius is 60cm, depth is 30cm and transparent glass In glass water vat, and it is placed under sunshine and is exposed to the sun to 55 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, by step（2）Mixed liquor is poured at a slow speed step under agitation（3） Have warmed up into 55 DEG C of bittern, then proceed to be placed under sunshine and be exposed to the sun three days（, can be by reaction system after the daily sun sets Cover, shone again when the second light is come out of retirement and taken up an official post）；Filtering, that is, the alkali magnesium sulfate crystal whisker presoma with whisker blank is made.
（5）The alkali magnesium sulfate crystal whisker presoma of generation is put into water, is continuously heating to 90 DEG C, makes it at this temperature Continued growth 30h, you can obtain alkali magnesium sulfate crystal whisker；Sample is placed in 80 DEG C of baking 24h in baking oven, produces alkali magnesium sulfate crystalline substance Must product.
（6）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ± 0.5 mol/L, then adds Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（7）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 15 or so, amorphous whiskerses matter is few, and whisker yield is 94%, good dispersion.
Embodiment 6
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, specifically comprised the following steps：
（1）Take 50L bitterns（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
（2）Prepare final concentration of 1mol/L Na2SO4And 1mol/L NaOH mixed solutions.
（3）By step（1）Bittern after filtering pours into the circular uncovered that radius is 60cm, depth is 30cm and transparent glass In glass water vat, and it is placed under sunshine and is exposed to the sun to 53 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, by step（2）Mixed liquor is poured at a slow speed step under agitation （3）Have warmed up into 53 DEG C of bittern, then proceed to be placed under sunshine and be exposed to the sun three days（After the daily sun sets, it will can react System covers, and is shone again when the second light is come out of retirement and taken up an official post）；Filtering, that is, the alkali magnesium sulfate crystal whisker presoma with whisker blank is made.
（5）The alkali magnesium sulfate crystal whisker presoma of generation is put into water, is continuously heating to 80 DEG C, makes it at this temperature Continued growth 35h, you can obtain alkali magnesium sulfate crystal whisker；Sample is placed in 75 DEG C of baking 30h in baking oven, produces alkali magnesium sulfate crystalline substance Must product.
（6）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ± 0.5 mol/L, then adds Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（7）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 17 or so, amorphous whiskerses matter is less, and whisker yield is 82%, and dispersiveness is preferably.
Embodiment 7
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, specifically comprised the following steps：
（1）Take 50L bitterns（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
（2）Prepare final concentration of 2mol/L Na2SO4And 0.5mol/L NaOH mixed solutions；
（3）By step（1）Bittern after filtering pours into the circular uncovered that radius is 60cm, depth is 30cm and transparent bath of glass In cylinder, and it is placed under sunshine and is exposed to the sun to 50 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added and mended Fill, or a transparent glass cover is capped on water vat；
（4）It is 1 by mixed liquor and bittern volume ratio：1, by step（2）Mixed liquor is poured at a slow speed step under agitation（3）Rise Temperature is then proceeded to be placed under sunshine and is exposed to the sun three days into 50 DEG C of bittern（, can be by reaction system lid after the daily sun sets On, shone again when the second light is come out of retirement and taken up an official post）；Filtering, that is, the alkali magnesium sulfate crystal whisker presoma with whisker blank is made.
（5）The alkali magnesium sulfate crystal whisker presoma of generation is put into water, is continuously heating to 100 DEG C, makes it in this temperature Lower continued growth 20h, you can obtain alkali magnesium sulfate crystal whisker；Sample is placed in 85 DEG C of baking 20h in baking oven, produces alkali magnesium sulfate Crystal whisker products.
（6）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ± 0.5 mol/L, then adds Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（7）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, 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 magnesium sulfate crystal whisker is prepared from bittern using solar energy, specifically comprised the following steps：
（1）Take 50L bitterns（Bittern is taken at Guangdong Xuwen saltern）, filter and discard insoluble matter；
（2）Prepare final concentration of 0.5mol/L Na2SO4And 0.2mol/L NaOH mixed solutions；
（3）By step（1）Bittern after filtering pours into the circular uncovered that radius is 60cm, depth is 30cm and transparent bath of glass In cylinder, and it is placed under sunshine and is exposed to the sun to 60 DEG C；If moisture evaporation is too fast when being exposed to the sun, synthermal water can be added and mended Fill, or a transparent glass cover is capped on water vat；
（4）It is 0.5 by mixed liquor and bittern volume ratio:1, by step（2）Mixed liquor is poured at a slow speed step under agitation（3） It is warming up in 60 DEG C of bittern, then proceedes to be placed under sunshine and be exposed to the sun three days（, can be by reaction system lid after the daily sun sets On, shone again when the second light is come out of retirement and taken up an official post）；Filtering, that is, the alkali magnesium sulfate crystal whisker presoma with whisker blank is made.
（5）The alkali magnesium sulfate crystal whisker presoma of generation is put into water, is continuously heating to 90 DEG C, makes it at this temperature Continued growth 30h, you can obtain alkali magnesium sulfate crystal whisker；Sample is placed in 80 DEG C of baking 24h in baking oven, produces alkali magnesium sulfate crystalline substance Must product.
（6）By step（4）The filtrate of gained is placed in sunshine and is exposed to the sun, by water evaporation, until magnesium ion concentration be 2.600 ± 0.5 mol/L, then adds Na2SO4With NaOH mixed solutions, enter circulation next time by above-mentioned steps；
（7）When iron, the aluminium plasma accumulated in bittern solution can be infected with whisker, stop circulation.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate；The SEM of sample Test result shows that sample has good crystal whisker-shaped, and diameter of whiskers is isometric, and uniformly surface is smooth, and straight brilliant rate is good, and size distribution is equal Even, for draw ratio about 16 or so, amorphous whiskerses matter is less, and whisker yield is 77%, and dispersiveness is preferably.
Comparative example 1
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, concrete operation method is substantially the same manner as Example 1, only One difference is bittern being 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 magnesium sulfate, but sample knot Brilliant degree 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 Only 32%.
Comparative example 2
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, concrete operation method is substantially the same manner as Example 1, only One difference is step（3）Na2SO4Be Na in NaOH mixed solutions2SO4Final concentration 2.5mol/L, NaOH is final concentration of 0.1mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 Only 36%.
Comparative example 3
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, concrete operation method is substantially the same manner as Example 1, only One difference is step（3）Na2SO4Be Na in NaOH mixed solutions2SO4Final concentration 0.3mol/L, NaOH is final concentration of 1.2mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 26%.
Comparative example 4
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, concrete operation method is substantially the same manner as Example 1, only One difference is step（2）In temperature of being exposed to the sun for 46 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 Only 62%.
Comparative example 5
1st, alkali magnesium sulfate crystal whisker is prepared from bittern in salt lake using salt pan, concrete operation method is substantially the same manner as Example 1, only One difference is step（2）In temperature of being exposed to the sun for 63 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 Only 55%.
Comparative example 6
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（2）Middle Na2SO4Be Na in NaOH mixed solutions2SO4Final concentration 2.3mol/L, NaOH is final concentration of 0.1mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 Only 39%.
Comparative example 7
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（2）Na2SO4Be Na in NaOH mixed solutions2SO4Final concentration 0.2mol/L, NaOH is final concentration of 1.5mol/L。
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 36%.
Comparative example 8
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（3）In temperature of being exposed to the sun for 45 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 Only 53%.
Comparative example 9
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（3）In temperature of being exposed to the sun for 62 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 For 65%.
Comparative example 10
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（5）In hydrothermal temperature be 70 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 For 50%.
Comparative example 11
1st, alkali magnesium sulfate crystal whisker is prepared from bittern using solar energy, concrete operation method is substantially the same manner as Example 5, uniquely Difference is step（5）In hydrothermal temperature be 60 DEG C.
2nd, result
Sample XRD test results show that it coincide substantially with standard diffraction, it was confirmed that sample is alkali magnesium sulfate, but sample knot Brilliant degree 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 For 44%.

Claims (10)

  1. A kind of 1. method for preparing alkali magnesium sulfate crystal 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 50~60 DEG C；
    S3. Na is added into the bittern after being exposed to the sun2SO4With NaOH mixed solutions, it is exposed to the sun under sunshine 2~4 days, filters bittern, Obtain alkali magnesium sulfate crystal whisker presoma；
    S4. alkali magnesium sulfate crystal whisker presoma is put into water, is warming up to 80~100 DEG C, and at this temperature growth 25~ 35h, you can obtain alkali magnesium sulfate crystal whisker；
    Na described in step S32SO4With Na in NaOH mixed solutions2SO4Final concentration of 0.5~2mol/L, NaOH final concentration of 0.2~ 1mol/L；
    Na described in step S32SO4It is 0.5~1 with the volume ratio of NaOH mixed solutions and bittern：1.
  2. 2. the method according to claim 1 for being prepared alkali magnesium sulfate crystal 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, Na can be added2SO4Mixed with NaOH Solution, circulated next time.
  3. 3. the method according to claim 1 for being prepared alkali magnesium sulfate crystal 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. 4. the method according to claim 1 for being prepared alkali magnesium sulfate crystal whisker from bittern using solar energy, its feature are existed In, by step S4 obtain alkali magnesium sulfate crystal whisker at 77~83 DEG C dry 20~30h, produce alkali magnesium sulfate crystal whisker product.
  5. 5. the method according to claim 1 for being prepared alkali magnesium sulfate crystal 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 55~60 DEG C；0.5 is added into the bittern after being exposed to the sun ~1mol/L Na2SO4With 0.2~0.5mol/L NaOH mixed solutions, continue to be exposed to the sun under sunshine, refilter bittern, you can Obtain alkali magnesium sulfate crystal whisker presoma.
  6. 6. the method according to claim 5 for being prepared alkali magnesium sulfate crystal 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 60 DEG C；The Na2SO4With Na in NaOH mixed solutions2SO4Final concentration of 0.7mol/L, NaOH Final concentration of 0.3mol/L.
  7. 7. the method according to claim 1 for being prepared alkali magnesium sulfate crystal 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 50~55 DEG C；Add into the bittern after being exposed to the sun Enter 1~2mol/L Na2SO4With 0.5~1mol/LNaOH mixed solutions, continue to be exposed to the sun under sunshine, refilter bittern, you can Obtain alkali magnesium sulfate crystal whisker presoma.
  8. 8. the method according to claim 7 for being prepared alkali magnesium sulfate crystal 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 55 DEG C；The Na2SO4With Na in NaOH mixed solutions2SO4Final concentration of 1.5mol/L, NaOH Final concentration of 0.7mol/L.
  9. 9. the method according to claim 1 for being prepared alkali magnesium sulfate crystal whisker from bittern using solar energy, its feature are existed In the transparent vessel is clear glass water vat.
  10. 10. any one of claim 1~9 is described to prepare the method for alkali magnesium sulfate crystal whisker in salt lake using solar energy from bittern Or application on alkali formula magnesium salt whisker is prepared in seawater.
CN201710443955.8A 2017-06-13 2017-06-13 A kind of method for preparing alkali magnesium sulfate crystal whisker from bittern using solar energy Withdrawn CN107653492A (en)

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CN115573026A (en) * 2022-09-09 2023-01-06 中国科学院青海盐湖研究所 Monodisperse 51n type basic magnesium sulfate whisker and preparation method thereof

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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
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CN115573026A (en) * 2022-09-09 2023-01-06 中国科学院青海盐湖研究所 Monodisperse 51n type basic magnesium sulfate whisker and preparation method thereof
CN115573026B (en) * 2022-09-09 2024-04-19 中国科学院青海盐湖研究所 Monodisperse 51 n-type basic magnesium sulfate whisker and preparation method thereof

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Application publication date: 20180202