CN109384250A - A method of mixing sodium salt direct utilization - Google Patents
A method of mixing sodium salt direct utilization Download PDFInfo
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- CN109384250A CN109384250A CN201811382651.6A CN201811382651A CN109384250A CN 109384250 A CN109384250 A CN 109384250A CN 201811382651 A CN201811382651 A CN 201811382651A CN 109384250 A CN109384250 A CN 109384250A
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- sodium
- sodium salt
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/16—Preparation from compounds of sodium or potassium with amines and carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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Abstract
The present invention provides a kind of methods for mixing sodium salt direct utilization, comprising the following steps: A) mixing sodium salt is added in ammonium hydroxide, obtain ammonial brine；The mass concentration of the ammonium hydroxide is 6~8%；The mass ratio of sodium sulphate and sodium chloride is 1:(0.5~2 in the mixing sodium salt)；B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer precipitated；C) crystallization of the precipitation is calcined, obtains resource product.The present invention passes through the ratio of control sodium sulphate and sodium chloride first, then in a certain temperature conditions, it is configured to certain density ammonial brine, then carbonization recycling is carried out to the mixing sodium salt in ammonial brine under alkaline condition using carbon dioxide gas, the sodium carbonate product that the mixing sodium salt of no utility value is converted to high added value, is recycled.
Description
Technical field
The invention belongs to reclamation of solid wastes technical field more particularly to a kind of mixing sodium salt direct utilizations
Method.
Background technique
The mixing sodium salt of sodium sulphate and sodium chloride largely results from industrial production, as solid waste especially in coal
In chemical field and wastewater zero discharge processing, the mixing sodium salt generated every year in the two industries according to statistics about 500~
6000000 tons；Simultaneously according to the continuous increase of current environmental protection pressure, the continuous harshness of total salt norm controlling, will can be produced in waste water
The inorganic abraum salt of raw greater amount.
The main disposal options of mixing sodium salt solid waste are largely to stack, or pass through cold crystallization, thermal crystalline, film point at present
From etc. means, carry out the separation of two kinds of inorganic sodiums, reach the standard of sodium sulphate and sodium chloride technical grade salt.
There is following deficiencies for sodium sulfate salt and sodium chloride salt isolation technics and technique: first technically, industrially
Two kinds of sodium salts can not be temporarily completely separated by the separating technology of sodium sulfate salt and sodium chloride salt, can only be carried out single component and be returned
Receive or can generate a large amount of mother liquor with high salt；The operating cost of followed by current separation means is excessively high, so that the work of separating treatment
Skill is uneconomical；Finally, the sodium sulphate and sodium chloride economic value that separation generates are low, application market is small.
Summary of the invention
The purpose of the present invention is to provide it is a kind of mix sodium salt direct utilization method, the present invention in method without
The separation of sodium chloride and sodium sulphate need to be passed through, the utilization of resources directly is carried out to mixing sodium salt, at low cost, economic value is high.
The present invention provides a kind of method for mixing sodium salt direct utilization, comprising the following steps:
A) mixing sodium salt is added in ammonium hydroxide, obtains ammonial brine；
The mass concentration of the ammonium hydroxide is 6~8%；
The mass ratio of sodium sulphate and sodium chloride is 1:(0.5~2 in the mixing sodium salt)；
B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer precipitated；
C) crystallization of the precipitation is calcined, obtains resource product.
Preferably, the step A) in, mixing sodium salt is added in ammonium hydroxide at 40~45 DEG C.
Preferably, the mass concentration that sodium salt is mixed in the ammonial brine is 15~17%.
Preferably, the step B) in gas liquid reaction temperature be 35~45 DEG C.
Preferably, the step B) in be precipitated crystallization using saturated sodium bicarbonate solution washing, then calcined again.
Preferably, the temperature of the calcining is 260~300 DEG C；
The time of the calcining is 1~2 hour.
Preferably, the resource product is sodium carbonate.
The present invention provides a kind of methods for mixing sodium salt direct utilization, comprising the following steps: A) by mixed sodium
Salt is added in ammonium hydroxide, obtains ammonial brine；The mass concentration of the ammonium hydroxide is 6~8%；Sodium sulphate and chlorination in the mixing sodium salt
The mass ratio of sodium is 1:(0.5~2)；B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer
It is precipitated；C) crystallization of the precipitation is calcined, obtains resource product.The present invention passes through control sodium sulphate and chlorination first
Then in a certain temperature conditions the ratio of sodium is configured to certain density ammonial brine, then existed using carbon dioxide gas
Carbonization recycling is carried out to the mixing sodium salt in ammonial brine under alkaline condition, the mixing sodium salt of no utility value is converted to high attached
Value added sodium carbonate product, is recycled.This technology may be implemented to mixing sodium salt direct utilization, need not move through sodium chloride and
The separation of sodium sulphate provides a kind of completely new technology for the resource utilization of a large amount of mixing sodium salts industrially generated.
Novelty and value of the invention is mainly reflected in:
1) the preparation of low concentration ammonia salt water solves the problems, such as that sodium sulphate is spent low dissolve in ammonia water, and can satisfy
The preparation of later period carbonization resource product；
2) chemical principle of the present invention is simple, and influence factor is few, it is ensured that the stability of technology；
3) can be reduced directly to the sodium sulphate and sodium chloride progress resource utilization in mixing sodium salt by this technology
Sodium chloride and sodium sulphate separation bring technology and economic headache；
4) present invention process route is short, and operation difficulty is low, and reproducibility is strong, can be widely used for the recycling benefit of mixing sodium salt
With；
5) on the basis of disposition mixes sodium salt, CO_2 Resource is fully utilized.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis
The attached drawing of offer obtains other attached drawings.
Fig. 1 is the method flow diagram in the present invention.
Specific embodiment
The present invention provides a kind of methods for mixing sodium salt direct utilization, comprising the following steps:
A) mixing sodium salt is added in ammonium hydroxide, obtains ammonial brine；
The mass concentration of the ammonium hydroxide is 6~8%；
The mass ratio of sodium sulphate and sodium chloride is 1:(0.5~2 in the mixing sodium salt)；
B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer precipitated；
C) crystallization of the precipitation is calcined, obtains resource product.
In the present invention, the main component of the mixing sodium salt is sodium sulphate and sodium chloride, the sodium sulphate and sodium chloride
Mass ratio be preferably 1:(0.5~2), more preferably 1:1.In view of the ratio of industrial mixed salt is unstable, sulfuric acid can be used
Sodium and sodium chloride are proportionally adjusted, or are configured using the industrial salt of variety classes content, specifically, at this
In the embodiment of invention, steam power plant's mixed salt can be used and configured with agrochemical salt, e.g., chlorine in steam power plant's mixed salt that the present invention uses
Change sodium accounting 37.92%, sodium sulphate accounting 54.36%, sodium chloride accounting 89.53% in agrochemical salt, sodium sulphate accounting 3.17%,
Steam power plant's mixed salt is matched with agrochemical salt according to the mass ratio of 5.1:1, sodium sulphate, which can be obtained, with sodium chloride mass ratio is
The mixing sodium salt of 1:1.
It is 25~28% pure ammonium hydroxide of analysis that the present invention, which preferably takes concentration, and deionized water is added, is configured to low concentration ammonium hydroxide,
The mass concentration of the low concentration ammonium hydroxide is preferably 6~8%, specifically, in an embodiment of the present invention, can be 6%, 7%
Or 8%.
Then, preferably in 40~45 DEG C of water bath with thermostatic control, mixing sodium salt is added in ammonium hydroxide, is completely dissolved, obtains ammonia
Salt water, in the present invention, the mass concentration that sodium salt is mixed in the ammonial brine is preferably 15~17%, specifically, in the present invention
Embodiment in, can be 16.11%, 16.67% or 17.53%.40~45 DEG C at a temperature of prepare ammonial brine, can make
Sodium sulphate in ammonial brine exists with the state of no crystal water, improves the yield and purity of final sodium carbonate product.
After obtaining ammonial brine, the present invention is passed through carbon dioxide in ammonial brine, carries out gas liquid reaction, has in reaction process
Mass crystallization is precipitated, until crystallization no longer evolution reaction stops.
After being passed through carbon dioxide, reaction designed by the present invention is as follows:
CO2+NH3+H2O=NH4HCO3……(a)
NaCl+NH4HCO3=NaHCO3↓+NH4Cl……(b)
Na2SO4+2NH4HCO3=2NaHCO3↓+(NH4)2SO4……(c)
Acid-base neutralization reaction (a) generation NH occurs for carbon dioxide and ammonium hydroxide first4HCO3, then NH4HCO3With sodium chloride and
Sodium sulphate carries out metathesis reaction (b) and (c), generates the lower sodium bicarbonate of solubility, after filtering carries out salt water separation, solid carbon
Sour hydrogen sodium heating, which is decomposed, reacts (d), obtains sodium carbonate product.
The CO generated by above-mentioned reaction2, the raw material that can be used as above-mentioned reaction is passed through in ammonial brine again, circulation benefit
With, sufficiently realization resource utilization.
In the present invention, the temperature of the gas liquid reaction is preferably 35~45 DEG C, and more preferably 38~43 DEG C, specifically,
In an embodiment of the present invention, 40 DEG C, 43 DEG C or 38 DEG C be can be.
After the gas liquid reaction stops, reaction product is filtered, obtains solid crystal, the solid crystal is carbonic acid
The solubility of hydrogen sodium crystal, sodium bicarbonate is lower relative to sodium sulphate and sodium chloride.
Then the crystallization of precipitation is washed using saturated sodium bicarbonate solution, the sodium bicarbonate knot after being washed
It is brilliant.
Sodium bicarbonate crystal after washing is placed in Muffle furnace, is calcined, sodium carbonate product is obtained, the calcining
Temperature is preferably 260~300 DEG C, specifically, in an embodiment of the present invention, can be 260 DEG C, 280 DEG C or 300 DEG C；It is described
The time of calcining is preferably 1~2 hour, specifically, in an embodiment of the present invention, it is small to can be 1 hour, 1.5 hours or 2
When.
It as configuring low concentration ammonium hydroxide used in above-mentioned ammonial brine is prepared by high concentration ammonium hydroxide in the present invention,
Washing lotion saturated sodium bicarbonate after washing can be used to deploy ammonia concn, also, since sodium bicarbonate is consistent with final products,
Therefore, it is enough economized on resources using used cleaning solution preparation low concentration ammonia water energy and does not introduce new impurity.
The present invention provides a kind of methods for mixing sodium salt direct utilization, comprising the following steps: A) by mixed sodium
Salt is added in ammonium hydroxide, obtains ammonial brine；The mass concentration of the ammonium hydroxide is 6~8%；Sodium sulphate and chlorination in the mixing sodium salt
The mass ratio of sodium is 1:(0.5~2)；B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer
It is precipitated；C) crystallization of the precipitation is calcined, obtains resource product.The present invention passes through control sodium sulphate and chlorination first
Then in a certain temperature conditions the ratio of sodium is configured to certain density ammonial brine, then existed using carbon dioxide gas
Carbonization recycling is carried out to the mixing sodium salt in ammonial brine under alkaline condition, the mixing sodium salt of no utility value is converted to high attached
Value added sodium carbonate product, is recycled.This technology may be implemented to mixing sodium salt direct utilization, need not move through sodium chloride and
The separation of sodium sulphate provides a kind of completely new technology for the resource utilization of a large amount of mixing sodium salts industrially generated.
In order to further illustrate the present invention, with reference to embodiments to a kind of direct resource of mixing sodium salt provided by the invention
Change the method utilized to be described in detail, but limiting the scope of the present invention cannot be understood as.
Embodiment 1
Analysis pure sodium chloride, each 48g of sodium sulphate are weighed, after being sufficiently mixed uniformly, is configured to the mixed sodium that mass ratio is 1:1
Salt；
Weigh concentration be 28% the pure ammonium hydroxide 143g of analysis, be added deionized water 357g, be configured to concentration be 8% it is low dense
Ammonium hydroxide is spent, under 45 DEG C of water bath with thermostatic control, mixing sodium salt is dissolved in 8% low concentration ammonium hydroxide, salinity is configured to and exists
16.11% ammonial brine；
By prepared ammonial brine, under 40 DEG C of water bath with thermostatic control, carbonization recycling is carried out using carbon dioxide and is reacted, is made
Under alkaline condition, successively with ammonium hydroxide, sodium chloride, sodium sulphate reaction gradually generates a large amount of bicarbonate in system to carbon dioxide
Sodium sediment, forming salt water mixed system；
Saline mixture is filtered, after the washing of saturated sodium bicarbonate cleaning solution, recycling sodium bicarbonate crystallization, so
Afterwards using Muffle furnace under the conditions of 300 DEG C, calcining 1h or so obtains sodium carbonate product, is computed, the rate of recovery 56%, purity
99.05%.
Embodiment 2
Certain steam power plant mixed salt 200g, certain agrochemical salt 100g are taken, wherein sodium chloride accounting 37.92% in thermoelectricity salt, sodium sulphate
Accounting 54.36%, sodium chloride accounting 89.53% in agrochemical salt, sodium sulphate accounting 3.17%.Take thermoelectricity salt 100.32g, agrochemical salt
19.68g is sufficiently mixed the mixed salt for being uniformly configured to that mass ratio is 1:1.
Analytically pure 25% ammonium hydroxide 144g is taken, deionized water 456g is added, is configured to the low concentration ammonia that concentration is 6%
Mixing sodium salt is dissolved in 6% low concentration ammonium hydroxide under 40 DEG C of water bath with thermostatic control, is configured to salinity 16.67% by water
Ammonial brine；
By prepared ammonial brine, under 38 DEG C of water bath with thermostatic control, carbonization recycling is carried out using carbon dioxide and is reacted, is made
Under alkaline condition, successively with ammonium hydroxide, sodium chloride, sodium sulphate reaction gradually generates a large amount of sodium bicarbonate precipitating to carbon dioxide
Object, forming salt water mixed system；
Saline mixture is filtered, after the washing of saturated sodium bicarbonate cleaning solution, recycling sodium bicarbonate crystallization, so
Afterwards using Muffle furnace under the conditions of 260 DEG C, calcining 2h or so obtains sodium carbonate product, is computed, the rate of recovery 54%, purity
99.76%.
Embodiment 3
Analysis pure sodium chloride, each 85g of sodium sulphate are taken, the mixing sodium salt for being uniformly configured to that mass ratio is 1:1 is sufficiently mixed；
Analytically pure 28% ammonium hydroxide 200g is taken, deionized water 600g is added, is configured to the low concentration ammonia that concentration is 7%
Mixing sodium salt is dissolved in 7% low concentration ammonium hydroxide under 42 DEG C of water bath with thermostatic control, is configured to salinity 17.53% by water
Ammonial brine；
By prepared ammonial brine, under 43 DEG C of water bath with thermostatic control, carbonization recycling is carried out using carbon dioxide and is reacted, is made
Under alkaline condition, successively with ammonium hydroxide, sodium chloride, sodium sulphate reaction gradually generates a large amount of sodium bicarbonate precipitating to carbon dioxide
Object, forming salt water mixed system；
Saline mixture is filtered, after the washing of saturated sodium bicarbonate cleaning solution, recycling sodium bicarbonate crystallization, so
Afterwards using Muffle furnace under the conditions of 280 DEG C, calcining 1.5h or so obtains sodium carbonate product, is computed, the rate of recovery 54% is pure
Degree 99.73%.
Comparative example 1
The direct utilization of mixing ammonia salt is carried out according to the method in embodiment 2, unlike, it is low in this comparative example
The concentration of concentration ammonium hydroxide is 5%.
Obtained sodium carbonate product recovery rate is 41%, purity 98.74%.
Comparative example 2
The direct utilization of mixing ammonia salt is carried out according to the method in embodiment 2, unlike, it is mixed in this comparative example
Closing the temperature of sodium salt dissolve in ammonia water is 30 DEG C.
Obtained sodium carbonate product recovery rate is 39%, purity 98.55%.
The performance detection of resource product in 1 embodiment of the present invention of table and comparative example
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method for mixing sodium salt direct utilization, comprising the following steps:
A) mixing sodium salt is added in ammonium hydroxide, obtains ammonial brine；
The mass concentration of the ammonium hydroxide is 6~8%；
The mass ratio of sodium sulphate and sodium chloride is 1:(0.5~2 in the mixing sodium salt)；
B it) is passed through carbon dioxide in the ammonial brine, carries out gas liquid reaction, until crystallization is no longer precipitated；
C) crystallization of the precipitation is calcined, obtains resource product.
2. the method according to claim 1, wherein the step A) in, sodium salt will be mixed at 40~45 DEG C
It is added in ammonium hydroxide.
3. the method according to claim 1, wherein in the ammonial brine mix sodium salt mass concentration be 15~
17%.
4. the method according to claim 1, wherein the step B) in the temperature of gas liquid reaction be 35~45
℃。
5. the method according to claim 1, wherein the step B) in the crystallization that is precipitated use unsaturated carbonate hydrogen
Sodium solution washing, is then calcined again.
6. the method according to claim 1, wherein the temperature of the calcining is 260~300 DEG C；
The time of the calcining is 1~2 hour.
7. the method according to claim 1, wherein the resource product is sodium carbonate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811382651.6A CN109384250A (en) | 2018-11-20 | 2018-11-20 | A method of mixing sodium salt direct utilization |
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| CN201811382651.6A CN109384250A (en) | 2018-11-20 | 2018-11-20 | A method of mixing sodium salt direct utilization |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116040657A (en) * | 2022-12-08 | 2023-05-02 | 中国恩菲工程技术有限公司 | System and method for preparing sodium carbonate from sodium sulfate |
| WO2023103770A1 (en) * | 2021-12-09 | 2023-06-15 | 中国科学院过程工程研究所 | Method for preparing sodium carbonate and co-producing ammonium sulfate and ammonium chloride from mixed waste salt |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153113A (en) * | 2011-03-01 | 2011-08-17 | 中国中轻国际工程有限公司 | Process for producing mirabilite type bittern, sodium carbonate, sodium chloride, sodium sulfate and ammonium chloride |
| CN105712382A (en) * | 2016-04-14 | 2016-06-29 | 中国中轻国际工程有限公司 | Technology for producing sodium bicarbonate from mirabilite |
| CN106082281A (en) * | 2016-06-14 | 2016-11-09 | 史永军 | Process with sodium sulfate preparing soda |
| CN108529652A (en) * | 2018-04-16 | 2018-09-14 | 黄河三角洲京博化工研究院有限公司 | A kind of industrial chlorinations sodium resource utilization process |
-
2018
- 2018-11-20 CN CN201811382651.6A patent/CN109384250A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153113A (en) * | 2011-03-01 | 2011-08-17 | 中国中轻国际工程有限公司 | Process for producing mirabilite type bittern, sodium carbonate, sodium chloride, sodium sulfate and ammonium chloride |
| CN105712382A (en) * | 2016-04-14 | 2016-06-29 | 中国中轻国际工程有限公司 | Technology for producing sodium bicarbonate from mirabilite |
| CN106082281A (en) * | 2016-06-14 | 2016-11-09 | 史永军 | Process with sodium sulfate preparing soda |
| CN108529652A (en) * | 2018-04-16 | 2018-09-14 | 黄河三角洲京博化工研究院有限公司 | A kind of industrial chlorinations sodium resource utilization process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023103770A1 (en) * | 2021-12-09 | 2023-06-15 | 中国科学院过程工程研究所 | Method for preparing sodium carbonate and co-producing ammonium sulfate and ammonium chloride from mixed waste salt |
| CN116040657A (en) * | 2022-12-08 | 2023-05-02 | 中国恩菲工程技术有限公司 | System and method for preparing sodium carbonate from sodium sulfate |
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Application publication date: 20190226 |