CN112679021A - Method for preparing salt from seawater - Google Patents
Method for preparing salt from seawater Download PDFInfo
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- CN112679021A CN112679021A CN202011561318.9A CN202011561318A CN112679021A CN 112679021 A CN112679021 A CN 112679021A CN 202011561318 A CN202011561318 A CN 202011561318A CN 112679021 A CN112679021 A CN 112679021A
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention relates to a method for preparing salt from seawater, which comprises the steps of filtering seawater, adding sodium carbonate and a purifying agent under the heating condition, enabling the purifying agent to act in the seawater to generate a polymer, enabling the polymer to absorb nonionic soluble impurities in the seawater to form flocs, then filtering under the condition of carbon dioxide, adding a settling agent into filtrate to heat, introducing neutral gas to filter, reducing impurities, facilitating subsequent sodium chloride crystallization and seawater desalination, concentrating the seawater through a reverse osmosis membrane to obtain concentrated brine and fresh water, finally adding hydrochloric acid into the concentrated brine to acidify, rapidly cooling after heating and refluxing, enabling sodium chloride to be separated out, obtaining salt with less impurities and high purity, and then refining the salt without needing to be carried out. The salt production process has the advantages of simple operation and low cost, can desalt seawater while producing salt, improves the utilization rate of the seawater, has no pollution in the whole process, and can further utilize the precipitate and the wastewater generated in the salt production process.
Description
Technical Field
The invention relates to the field of salt preparation from seawater, in particular to a method for preparing salt from seawater.
Background
The production of sea salt by human has been a long history for thousands of years, the most extensive salt-making method is the traditional solarization method, and in the long-term sea salt production practice, people also find out various effective methods, such as hot-pressing salt-making technology, vacuum salt-making technology, reverse osmosis method, ion exchange membrane electrodialysis method concentration sea water salt-making technology, and the like. The electrodialysis method can remove most of salt in seawater, has no phase change in the desalting process, and is widely applied in the fields of seawater desalination and salt preparation. The reverse osmosis method can completely isolate impurities such as bacteria, viruses, heavy metals, micromolecular organic matters and the like mixed in water, and the quality of the outlet water reaches the physicochemical index and the sanitary standard specified for drinking, so that the outlet water is considered to be generally accepted high-quality drinking water at present. However, reverse osmosis has high requirements on the quality of inlet water, ordinary seawater, especially surface seawater, cannot be directly subjected to reverse osmosis treatment, and high energy consumption is also a great problem restricting the application of reverse osmosis technology.
At present, single technologies such as seawater cooling, seawater desalination, industrial salt production, seawater chemical extraction and the like are quite mature, and a plurality of independent project examples are provided. But the energy consumption of a single project is larger, the production cost is higher, and more impurity components in the discharged by-products cause adverse effects on the environment. And modern seawater pollutes seriously, and the impurity variety is numerous in the seawater, and the impurity is difficult to directly get rid of to current seawater salt manufacturing technique, leads to the salt manufacturing inefficiency, and the product salt quality is low.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing salt from seawater.
The method is realized according to the following steps:
s1, introducing the seawater into a filtering tank for filtering;
s2, heating the filtered seawater to 30-40 ℃, sequentially adding sodium carbonate and a purifying agent for continuous heating, introducing carbon dioxide after floccules are separated out, filtering to obtain filtrate, adding a settling agent into the filtrate under the conditions of heating and stirring, heating to 70-85 ℃, keeping the temperature for 30-60 min, introducing neutral gas, filtering to obtain filtrate, and passing the filtrate through a reverse osmosis membrane to obtain concentrated brine and fresh water;
s3, adding hydrochloric acid with the volume concentration of 70-80% into the concentrated brine, adjusting the pH value to 2-3, heating and refluxing, rapidly cooling, separating out crystals, and performing vacuum filtration to obtain the salt.
Furthermore, the filtering tank sequentially comprises a first layer, a second layer and a third layer from bottom to top, wherein the first layer is cobblestone, the second layer is ceramsite with the particle size of 2.0-3.0 mm, and the third layer is mesoporous activated carbon with the pore diameter of 10-40 nm.
Furthermore, a water outlet is arranged above the third layer in the filtering tank, and a filtering net is arranged at the water outlet.
Further, in step S2, the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin, and the ratio of the purifying agent to the purifying agent is 5-7: 1: 3 in a mass ratio of 3.
Further, in step S2, the mass ratio of the seawater, the sodium carbonate and the purifying agent is 20-30: 1: 2.
further, in step S2, the settling agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to a mass ratio of 0.6-1: 1.
Further, in step S2, the mass ratio of the filtrate to the settling agent is 6-10: 1.
Further, in the step S2, the concentration of the concentrated brine is 26-28 degrees Beˊ。
Further, in step S3, the temperature is rapidly decreased after heating and refluxing to 80-100 ℃ for reflux reaction for 20-60 min, and then the temperature is rapidly decreased to 0-10 ℃.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention relates to a method for preparing salt from seawater, which comprises the steps of filtering seawater, adding sodium carbonate and a purifying agent under the heating condition, enabling the purifying agent to act in the seawater to generate a polymer, enabling the polymer to absorb nonionic soluble impurities in the seawater to form flocs, then filtering under the condition of carbon dioxide, adding a settling agent into filtrate to heat, introducing neutral gas to filter, reducing impurities, facilitating subsequent sodium chloride crystallization and seawater desalination, concentrating the seawater through a reverse osmosis membrane to obtain concentrated brine and fresh water, finally adding hydrochloric acid into the concentrated brine to acidify, rapidly cooling after heating and refluxing, enabling sodium chloride to be separated out, obtaining salt with less impurities and high purity, and then refining the salt without needing to be carried out. The salt production process has the advantages of simple operation and low cost, can desalt seawater while producing salt, improves the utilization rate of the seawater, has no pollution in the whole process, and can further utilize the precipitate and the wastewater generated in the salt production process.
(2) The invention introduces seawater into a filter tank to remove insoluble substances under the multiple actions of cobblestones, ceramsite and active carbon, reduces impurities, removes nonionic soluble impurities through the purification of a purifying agent prepared from silicic acid, sodium carboxymethylcellulose and lignin, removes ionic soluble impurities from a settling agent prepared from sodium carbonate and absolute ethyl alcohol, and finally obtains fresh water and brine with higher concentration through the concentration of a reverse osmosis membrane.
Detailed Description
In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.
Example 1
A method for preparing salt from seawater comprises the following steps:
s1, introducing seawater into a filtering tank for filtering, wherein the filtering tank sequentially comprises a first layer, a second layer and a third layer from bottom to top, the first layer is cobblestone, the second layer is ceramsite with the particle size of 2.0-3.0 mm, the third layer is mesoporous activated carbon with the pore size of 10-40 nm, a water outlet is formed in the upper portion of the third layer, and a filter screen is arranged at the water outlet;
s2, heating the filtered seawater to 38 ℃, sequentially adding sodium carbonate and a purifying agent for continuous heating, wherein the mass ratio of the seawater, the sodium carbonate and the purifying agent is (26: 1): 2, after the floccule is separated out, introducing carbon dioxide, filtering to obtain filtrate, adding a settling agent into the filtrate under the condition of heating and stirring, wherein the mass ratio of the filtrate to the settling agent is 8:1, heating to 85 ℃, keeping the temperature for 30min, introducing nitrogen gas, filtering to obtain filtrate, and passing the filtrate through a composite reverse osmosis membrane to obtain a product with the concentration of 26-28 DEG BeˊThe concentrated brine and the fresh water; wherein the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin, and the weight ratio of the purifying agent to the purifying agent is 6:1: 3 in a mass ratio; the settling agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to the mass ratio of 0.8: 1;
s3, adding hydrochloric acid with volume concentration of 76% into the concentrated brine, adjusting the pH to 2, heating to 95 ℃, carrying out reflux reaction for 30min, rapidly cooling to 5 ℃, precipitating crystals, and carrying out vacuum filtration to obtain the salt.
Example 2
A method for preparing salt from seawater comprises the following steps:
s1, introducing seawater into a filter tank for filtering, paving quartz sand with the particle size of 2.0-3.0 mm in the filter tank, arranging a water outlet above the quartz sand layer, and arranging a filter screen at the water outlet;
s2, heating the filtered seawater to 30 ℃, sequentially adding sodium carbonate and a purifying agent for continuous heating, wherein the mass ratio of the seawater, the sodium carbonate and the purifying agent is 30: 1:2, after the floccule is separated out, introducing carbon dioxide, filtering to obtain filtrate, introducing carbon dioxide, adding a settling agent into the filtrate under the condition of heating and stirring, wherein the mass ratio of the filtrate to the settling agent is 10:1, heating to 80 ℃, keeping the temperature for 40min, introducing oxygen gas, filtering to obtain filtrate, and passing the filtrate through a composite reverse osmosis membrane to obtain a product with the concentration of 26-28 DEG BeˊThe concentrated brine and the fresh water; wherein the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin, and the weight ratio of the purifying agent to the raw materials is 5: 1: 3 in a mass ratio; the settling agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to the mass ratio of 0.6: 1;
s3, adding hydrochloric acid with volume concentration of 76% into the concentrated brine, adjusting the pH to 2, heating to 100 ℃, carrying out reflux reaction for 20min, rapidly cooling to 10 ℃, precipitating crystals, and carrying out vacuum filtration to obtain the salt.
Example 3
Example 3 differs from example 1 in that:
in step S2, the mass ratio of seawater, sodium carbonate and purifying agent is 18: 1: 2.
example 4
Example 4 differs from example 1 in that:
in step S2, the mass ratio of the filtrate to the settling agent is 5: 1.
Example 5
Example 5 differs from example 1 in that:
in step S2, the purifying agent is prepared by mixing polysilicate iron and polysilicate zinc according to the mass ratio of 1: 1.
Example 6
Example 6 differs from example 1 in that:
in step S2, the settling agent is obtained by mixing lime milk and sodium carbonate according to the mass ratio of 2: 1.
Comparative example 1
A conventional seawater salt making method comprises the following steps:
s1, filtering and decoloring the seawater;
s2, heating the seawater, and evaporating and crystallizing to obtain crude salt;
s3, dissolving the crude salt in a barium chloride solution, filtering after precipitating a precipitate, adding sodium hydroxide, filtering after precipitating a precipitate, adding sodium carbonate into a filtrate, filtering after precipitating a precipitate, adding hydrochloric acid with the volume concentration of 76%, adjusting the pH value to 5, heating, evaporating, crystallizing, and carrying out vacuum filtration to obtain the salt.
Comparative example 2
Comparative example 2 differs from example 1 in that:
step S2, heating filtered seawater to 38 ℃, adding sodium carbonate for heating, wherein the mass ratio of seawater to sodium carbonate is 23:1, precipitating, introducing carbon dioxide, filtering to obtain filtrate, adding a settling agent into the filtrate under the condition of heating and stirring, wherein the mass ratio of the filtrate to the settling agent is 8:1, heating to 85 ℃, keeping the temperature for 30min, introducing nitrogen, filtering to obtain filtrate, and passing the filtrate through a reverse osmosis membrane to obtain concentrated brine and fresh water with the concentration of 26-28 degrees Be'; wherein the settling agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to the mass ratio of 0.6: 1.
Comparative example 3
Comparative example 3 differs from example 1 in that:
step S2, heating the filtered seawater to 38 ℃, sequentially adding sodium carbonate and a purifying agent for continuous heating, wherein the mass ratio of the seawater, the sodium carbonate and the purifying agent is (26: 1): 2, precipitating floccules, filtering to obtain filtrate, adding a settling agent into the filtrate under the condition of heating and stirring, wherein the mass ratio of the filtrate to the settling agent is 8:1, heating to 85 ℃, keeping the temperature for 30min, introducing nitrogen, filtering to obtain filtrate, and passing the filtrate through a reverse osmosis membrane to obtain concentrated brine and fresh water with the concentration of 26-28 DEG Be'; wherein the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin, and the weight ratio of the purifying agent to the purifying agent is 6:1: 3 in a mass ratio; the settling agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to the mass ratio of 0.8: 1.
Comparative example 4
Comparative example 4 differs from example 1 in that:
step S2 is heating filtered seawater to 38 deg.C, sequentially adding sodium carbonate and purifying agent, and heating to obtain sea waterThe mass ratio of water to sodium carbonate is 26:1:2, after flocculating constituent is separated out, carbon dioxide is introduced, and filtrate is obtained by filtration，Enabling the filtrate to pass through a composite reverse osmosis membrane to obtain concentrated brine and fresh water with the concentration of 26-28 degrees Be'; wherein the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin, and the weight ratio of the purifying agent to the purifying agent is 6:1: 3 in a mass ratio of 3.
Comparative example 5
Comparative example 5 differs from example 1 in that:
and step S3, adding hydrochloric acid with volume concentration of 76% into concentrated brine, adjusting pH to 2, heating to 95 ℃, refluxing and reacting for 6 hours, separating out crystals, and performing vacuum filtration to obtain salt.
Test examples
The salt prepared in the embodiment and the salt prepared in the comparative example are respectively detected, the physical and chemical indexes of the industrial salt are shown in the table 1, and the detection results are shown in the table 2;
TABLE 1 physical and chemical indexes of industrial salt
And (3) moisture determination: reference is made to GB/T13025.3-2012 determination of moisture in general test methods in the salt industry;
determination of water-insoluble matter: reference is made to GBT13025.4-2012 "determination of water insoluble matter in general test methods in the salt industry";
and (3) measuring the total amount of calcium and magnesium ions: reference is made to GB/T13025.6-2012, determination of calcium and magnesium by general test methods in the salt industry;
sulfate radical content determination: reference is made to GB/T13025.8-2012 "determination of sulfate in general test method for salt industry";
and (3) measuring the content of sodium chloride: reference is made to GB T5462-2015 Industrial salt.
TABLE 2 test results
The experimental data show that the salt prepared by the salt preparation process has high quality, high sodium chloride content and low water, water insoluble substances, total calcium and magnesium ions and sulfate radical content. Wherein, the embodiment 1 is the best scheme of the salt preparation process; example 2 the filtering tank is only provided with a layer of quartz sand, the filtering effect is poor, and the water content and the water-insoluble substances in the salt are more than those in example 1; in example 3, the sodium carbonate and the purifying agent are used in large amount, the purifying agent does not completely react with seawater, and impurities are increased due to the difficulty in removal during filtration; in the embodiment 4, the dosage of the settling agent is large, and the settling effect is over-saturated, so that the residual settling agent is dissolved in the brine to increase the content of ionic impurities; example 5 without using the purifying agent of the present invention, the purifying effect was poor, the sodium chloride content in the salt was low, and the impurities were more than those in example 1; the settling agent of example 6, which does not use absolute ethanol, has a poor settling effect.
Comparative example 1 salt prepared by the conventional salt preparation method has low sodium chloride content and more impurities, and needs to be further refined; comparative example 2 salt obtained by treating seawater without purifying agent has low sodium chloride content, and salt is prepared directly from unpurified brine, and impurities in the salt are more; comparative example 3 no carbon dioxide was introduced, the flocs were not filtered completely, and water-insoluble impurities were abundant; comparative example 4 salts obtained without the addition of a settling agent, which have low sodium chloride content and many impurities; comparative example 5 no cooling after heating reflux, not only the time consumed is long, but also the sodium chloride content of the prepared salt is low, the moisture content is more, and the impurities are more.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A method for preparing salt from seawater is characterized by comprising the following steps:
s1, introducing the seawater into a filtering tank for filtering;
s2, heating the filtered seawater to 30-40 ℃, sequentially adding sodium carbonate and a purifying agent for continuous heating, introducing carbon dioxide after floccules are separated out, filtering to obtain filtrate, adding a settling agent into the filtrate under the conditions of heating and stirring, heating to 70-85 ℃, keeping the temperature for 30-60 min, introducing neutral gas, filtering to obtain filtrate, and passing the filtrate through a reverse osmosis membrane to obtain concentrated brine and fresh water;
s3, adding hydrochloric acid with the volume concentration of 70-80% into the concentrated brine, adjusting the pH value to 2-3, heating and refluxing, rapidly cooling, separating out crystals, and performing vacuum filtration to obtain the salt.
2. The method for preparing salt from seawater as claimed in claim 1, wherein the filtering tank comprises a first layer, a second layer and a third layer from bottom to top in sequence, the first layer is cobblestone, the second layer is ceramsite with the particle size of 2.0-3.0 mm, and the third layer is mesoporous activated carbon with the pore size of 10-40 nm.
3. The method for preparing salt from seawater as claimed in claim 1, wherein in step S2, the purifying agent is silicic acid, sodium carboxymethyl cellulose and lignin in a ratio of 5-7: 1: 3 in a mass ratio of 3.
4. The method for preparing salt from seawater as claimed in claim 1, wherein in step S2, the mass ratio of seawater, sodium carbonate and purifying agent is 20-30: 1: 2.
5. the method for preparing salt from seawater as claimed in claim 1, wherein in step S2, the sedimentation agent is obtained by mixing sodium carbonate and absolute ethyl alcohol according to a mass ratio of 0.6-1: 1.
6. The method for preparing salt from seawater as claimed in claim 1, wherein in step S2, the mass ratio of the filtrate to the settling agent is 6-10: 1.
7. The method of claim 1, wherein in step S2, the neutral gas is one of hydrogen, nitrogen and oxygen.
8. The method for producing salt from seawater according to claim 1, wherein in step S2, the concentrated brine has a concentration of 26 to 28 ° Be'.
9. The method of claim 1, wherein in step S3, the temperature is rapidly decreased after the heating and refluxing step, namely, after the heating to 80-100 ℃ and the refluxing reaction for 20-60 min, the temperature is rapidly decreased to 0-10 ℃.
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Cited By (2)
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| CN113979451A (en) * | 2021-11-05 | 2022-01-28 | 山东岱岳制盐有限公司 | Preparation method of ecological well mineral salt |
| CN114314612A (en) * | 2021-12-16 | 2022-04-12 | 唐山市银海食盐有限公司 | Production process for regulating and controlling sea salt crystal morphology |
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| CN114314612A (en) * | 2021-12-16 | 2022-04-12 | 唐山市银海食盐有限公司 | Production process for regulating and controlling sea salt crystal morphology |
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