CN112158860A - Refining method of chemical waste salt - Google Patents
Refining method of chemical waste salt Download PDFInfo
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- CN112158860A CN112158860A CN202011041367.XA CN202011041367A CN112158860A CN 112158860 A CN112158860 A CN 112158860A CN 202011041367 A CN202011041367 A CN 202011041367A CN 112158860 A CN112158860 A CN 112158860A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
- C01D3/16—Purification by precipitation or adsorption
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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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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- 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
- C01P2006/82—Compositional purity water content
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Abstract
Dissolving waste salt slag after pyrolysis and carbonization, adding precipitator into the dissolved solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further impurity removal, regulating the pH value of clear liquid to 7-7.5, adding Na into the clear liquid2And filtering the solution S to remove precipitates, and concentrating the filtrate through a nanofiltration membrane to obtain refined solution. The refining method can effectively remove impurity cations and heavy metal ions in the salt slag and can improve the removal rate of organic matters.
Description
Technical Field
The invention belongs to the technical field of environmental protection, and particularly relates to a refining method of chemical waste salt.
Background
The industrial waste salt is mainly generated in industrial production processes of pesticide intermediates, drug synthesis, printing and dyeing and the like, and processes of solid-liquid separation, solution concentration and crystallization, sewage treatment and the like, and has the characteristics of various types, complex components, numerous sources, high treatment cost, great environmental hazard and the like.
The existing tail end treatment technology of waste salt mainly comprises landfill, incineration and harmless comprehensive utilization. The landfill is to carry out sanitary landfill disposal by curing waste salt through concrete and the like and then sending the waste salt into a rigid landfill site according to landfill technical specifications. The incineration is that the waste salt is heated to 900 ℃, the inorganic salt is melted and flows into the furnace bottom, and the inorganic salt is recovered after cooling, and the organic matter is volatilized and decomposed at high temperature. Because the melting point interval of the waste salt has large fluctuation, adverse phenomena such as slag bonding, caking and the like are easy to occur in the incineration treatment process, and the process stability is influenced. Therefore, the harmless recycling comprehensive utilization of the waste salt becomes a necessary way for the waste salt, and the factors for restricting the large-scale recycling development of the waste salt are mainly the removal of organic matters and heavy metal ions in the waste salt.
At present, common treatment methods for reducing removal of organic matters in industrial waste salt comprise an incineration method, a high-temperature pyrolysis method, a landfill method and the like, and after the removal of the organic matters, heavy metal ions are further removed by a precipitation-filtration method, but the removal efficiency of the method is not high.
Disclosure of Invention
The invention aims to provide a refining method of chemical waste salt, which can effectively remove impurity cations and heavy metal ions in salt slag and can improve the removal rate of organic matters.
In order to achieve the above purpose, the solution of the invention is:
a method for refining chemical waste salt comprises dissolving pyrolytic carbonized waste salt residue, adding precipitant into the solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further removing impurities, adjusting pH of the clear solution to 7-7.5, adding Na2And filtering the solution S to remove precipitates, and concentrating the filtrate through a nanofiltration membrane to obtain refined solution.
The precipitant is selected from sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate.
The ion exchange resin is a cationic exchange resin.
Above Na2The concentration of the S solution is 8-12%.
Adding hydrogen peroxide into the waste salt residue solution before adding the precipitator into the waste salt residue solution, and then treating under an ultraviolet condition.
The pyrolysis carbonization process comprises the following steps: drying and dehydrating chemical waste salt, and then performing primary calcination and secondary calcination on the crude salt to obtain waste salt slag.
The drying and dehydrating conditions are 180-230 ℃ and 15-30 s.
The condition of the primary calcination is 500-520 ℃ and 2-4 min; the secondary calcination condition is 700-730 ℃ and 20-25 min.
After the scheme is adopted, the refining method adopted by the invention is that firstly the chemical waste salt after pyrolysis and carbonization is dissolved, and OH-containing chemical waste salt is adopted-And CO3 2-Removal of Ca as a precipitant2+、Mg2+Waiting for cation impurities, and then further removing impurity cations by using cation exchange resin; because the waste salt may contain trace heavy metals, Na is adopted after organic matters and cationic impurities are removed in the early stage2And finally, a nanofiltration membrane is used for concentrating the salt solution to perform more effective refining, so that the quality and the purity of the refined salt are improved. Because the method of pyrolysis and carbonization is adopted in the earlier stage to remove the organic matters carried by the chemical waste salt, the oxidation step of combining hydrogen peroxide and ultraviolet is added before the subsequent refining, so that the organic matters can be more effectively removed.
The crystal salt prepared by the method for refining the chemical waste salt can be dried to obtain refined industrial salt with more than two levels, and the refined industrial salt can be directly supplied to salt enterprises to be used as industrial raw material salt.
Detailed Description
The refining method adopted by the invention firstly needs to carry out pyrolysis carbonization treatment on the chemical waste salt, and then carries out subsequent refining.
The pyrolysis carbonization treatment is specifically as follows:
(1) and (3) drying: the method comprises the steps of utilizing high-temperature flue gas generated during calcination to pre-dry, oxidize and carbonize an original material, then separating salt particles from gas through a separator, enabling dry salt to enter a primary calciner, and enabling dry waste gas to enter a waste gas incinerator.
Specifically, the drying and dehydrating conditions are 180-230 ℃ and 15-30 s.
(2) Primary calcination: the 'primary calcining furnace' is adopted to lead the gas in the furnace to be in a continuous phase and lead the materials to be in a dispersed phase, thus greatly improving the oxidizing atmosphere in the furnace and leading the organic matters to be oxidized at high temperature, thereby obviously improving the calcining efficiency and the burnout degree of the organic matters in the slag salt and overcoming the problem of salt particle agglomeration and caking.
Specifically, the primary calcination is performed at 500-520 ℃ for 2-4 min.
(3) Secondary calcination: the slag salt can fully contact with oxygen through rolling and moving by utilizing the inclined and slow rotation action of the furnace body, and organic matters in the slag salt are combusted and decomposed into high-temperature flue gas and ash under the high-temperature combustion action.
Specifically, the secondary calcination is carried out at 700-730 ℃ for 20-25 min.
Thereafter, with OH groups-And CO3 2-Removal of Ca as a precipitant2+、Mg2+Waiting for cation impurities, and then further removing impurity cations by using cation exchange resin; because the waste salt may contain trace heavy metals, Na is adopted after organic matters and cationic impurities are removed in the early stage2And finally, a nanofiltration membrane is used for concentrating the salt solution to perform more effective refining, so that the quality and the purity of the refined salt are improved. Because the method of pyrolysis and carbonization is adopted in the earlier stage to remove the organic matters carried by the chemical waste salt, an oxidation step combining hydrogen peroxide and ultraviolet is added before the subsequent refining, so that the organic matters can be more effectively removed.
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
The detection shows that the content of sodium chloride in waste salt of a chemical industry enterprise is 90.8g/100g, the moisture content is 6.34g/100g, the organic matter content is 1.35g/100g, and the sodium sulfate and other impurities content is 1.22g/100 g.
Dissolving the waste salt dregs after pyrolysis and carbonization, adding precipitant into the solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further impurity removal, regulating the pH value of the clear solution to 7-7.5 by using 10% hydrochloric acid solution, adding Na2Filtering the S solution to remove precipitatePrecipitating, and concentrating the filtrate with nanofiltration membrane to obtain refined solution.
Wherein the precipitant is a mixture of sodium hydroxide and sodium carbonate to make Ca2+、Mg2+And the cationic impurities are completely converted into precipitates.
The ion exchange resin is cationic exchange resin, and the flow rate of the column loading liquid is 5 BV/h.
Added Na2The concentration of the S solution was 12%.
The pyrolysis carbonization is to dry and dehydrate chemical waste salt, and then to perform primary calcination and secondary calcination on the crude salt to obtain waste salt slag. Specifically, the method comprises the following steps: putting the waste salt into a flash evaporation dryer, drying for 30s at the temperature of 180 ℃, removing water in the waste salt and decomposing part of low molecular organic matters to obtain crude salt 1; the crude salt 1 enters a first-stage fluidized bed incinerator, and is carbonized or decomposed for 3min at the temperature of 500 ℃, and most organic matters are decomposed or carbonized to obtain crude salt 2; and (3) calcining the crude salt 2 in a secondary rotary kiln calcining furnace at 700 ℃ for 25min to obtain crude salt 3.
And (3) delivering the refined liquid obtained by the refining method into a multi-effect evaporation system, treating to obtain crystalline salt, and throwing the crystalline salt through a double-stage spiral centrifugal machine to remove moisture and then delivering the crystalline salt into a fluidized bed dryer to evaporate the moisture to obtain the industrial salt.
The detection shows that the obtained industrial salt sodium chloride has the content of 98.5g/100g, the moisture of 0.53g/100g, the water-insoluble substances of 0.11g/100g, the total amount of calcium and magnesium ions of 0.43g/100g and the sulfate radicals of 0.52g/100 g.
Example 2
The detection shows that the content of sodium chloride in waste salt of a chemical industry enterprise is 93.2g/100g, the moisture content is 3.74g/100g, the organic matter content is 1.52g/100g, and the sodium sulfate and other impurities content is 1.08g/100 g.
Dissolving the waste salt dregs after pyrolysis and carbonization, adding precipitant into the solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further impurity removal, adjusting the pH value of the clear liquid to 7-7.5 by 15% sodium hydroxide solution, adding Na2Filtering the S solution to remove precipitates, and performing nanofiltration on filtrateAnd (5) concentrating by using a membrane to obtain a refined solution.
Wherein the precipitant is a mixture of sodium hydroxide and sodium carbonate to make Ca2+、Mg2+And the cationic impurities are completely converted into precipitates.
The ion exchange resin is cationic exchange resin, and the flow rate of the column loading liquid is 4 BV/h.
Added Na2The concentration of the S solution was 12%.
The pyrolysis carbonization is to dry and dehydrate chemical waste salt, and then to perform primary calcination and secondary calcination on the crude salt to obtain waste salt slag. Specifically, the method comprises the following steps: putting the waste salt into a flash evaporation dryer, drying for 30s at the temperature of 180 ℃, removing water in the waste salt and decomposing part of low molecular organic matters to obtain crude salt 1; the crude salt 1 enters a first-stage fluidized bed incinerator, and is carbonized or decomposed for 3min at the temperature of 500 ℃, and most organic matters are decomposed or carbonized to obtain crude salt 2; and (3) calcining the crude salt 2 in a secondary rotary kiln calcining furnace at the temperature of 730 ℃ for 20min to obtain crude salt 3.
And (3) delivering the refined liquid obtained by the refining method into a multi-effect evaporation system, treating to obtain crystalline salt, and throwing the crystalline salt through a double-stage spiral centrifugal machine to remove moisture and then delivering the crystalline salt into a fluidized bed dryer to evaporate the moisture to obtain the industrial salt.
The detection shows that the obtained industrial salt sodium chloride has the content of 98.5g/100g, the moisture of 0.62g/100g, the water-insoluble substances are 0.14g/100g, the total amount of calcium and magnesium ions is 0.42g/100g, and the sulfate radical is 0.35g/100 g.
Example 3
The detection shows that the content of sodium chloride in waste salt of a chemical industry enterprise is 91.7g/100g, the moisture content is 4.66g/100g, the organic matter content is 1.98g/100g, and the content of sodium sulfate and other impurities is 0.95g/100 g.
Dissolving the waste salt dregs after pyrolysis and carbonization, adding precipitant into the solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further impurity removal, regulating the pH value of the clear liquid to 7-7.5 by using 10% hydrochloric acid solution, adding Na2And filtering the solution S to remove precipitates, and concentrating the filtrate through a nanofiltration membrane to obtain refined solution.
Wherein the precipitant is a mixture of sodium hydroxide and sodium carbonate to make Ca2+、Mg2+And the cationic impurities are completely converted into precipitates.
The ion exchange resin is cationic exchange resin, and the flow rate of the column loading liquid is 4 BV/h.
Added Na2The concentration of the S solution was 8%.
The pyrolysis carbonization is to dry and dehydrate chemical waste salt, and then to perform primary calcination and secondary calcination on the crude salt to obtain waste salt slag. Specifically, the method comprises the following steps: putting the waste salt into a flash evaporation dryer, drying for 30s at the temperature of 180 ℃, removing water in the waste salt and decomposing part of low molecular organic matters to obtain crude salt 1; the crude salt 1 enters a first-stage fluidized bed incinerator, and is carbonized or decomposed for 3min at the temperature of 500 ℃, and most organic matters are decomposed or carbonized to obtain crude salt 2; and (3) calcining the crude salt 2 in a secondary rotary kiln calcining furnace at 730 ℃ for 22min to obtain crude salt 3.
And (3) delivering the refined liquid obtained by the refining method into a multi-effect evaporation system, treating to obtain crystalline salt, and throwing the crystalline salt through a double-stage spiral centrifugal machine to remove moisture and then delivering the crystalline salt into a fluidized bed dryer to evaporate the moisture to obtain the industrial salt.
Through detection, the content of the obtained industrial salt sodium chloride is 98.8g/100g, the moisture is 0.37g/100g, the water-insoluble substances are 0.19g/100g, the total content of calcium and magnesium ions is 0.44g/100g, and the sulfate radicals are 0.28g/100 g.
Example 4
This example differs from example 2 in that: adding hydrogen peroxide into the waste salt residue solution before adding the precipitator into the waste salt residue solution, and then treating under an ultraviolet condition.
A process for refining chemical waste salt includes such steps as dissolving the dregs of waste salt after thermal decomposition and carbonization, adding hydrogen peroxide, treating under ultraviolet condition, adding precipitant to the treated liquid, filtering to remove precipitate, introducing the filtrate to ion exchange resin for further removing impurities, regulating pH value of supernatant to 7-7.5 with 15% sodium hydroxide solution, adding Na2Filtering the S solution to removeRemoving precipitate, and concentrating the filtrate with nanofiltration membrane to obtain refined solution.
Wherein the addition of hydrogen peroxide is 0.1% of the mass of the waste liquid, and the irradiation intensity of the ultraviolet lamp is 20mw/cm2。
The precipitant is mixture of sodium hydroxide and sodium carbonate to make Ca2+、Mg2+And the cationic impurities are completely converted into precipitates.
The ion exchange resin is cationic exchange resin, and the flow rate of the column loading liquid is 4 BV/h.
Added Na2The concentration of the S solution was 12%.
The pyrolysis carbonization is to dry and dehydrate chemical waste salt, and then to perform primary calcination and secondary calcination on the crude salt to obtain waste salt slag. Specifically, the method comprises the following steps: putting the waste salt into a flash evaporation dryer, drying for 30s at the temperature of 180 ℃, removing water in the waste salt and decomposing part of low molecular organic matters to obtain crude salt 1; the crude salt 1 enters a first-stage fluidized bed incinerator, and is carbonized or decomposed for 3min at the temperature of 500 ℃, and most organic matters are decomposed or carbonized to obtain crude salt 2; and (3) calcining the crude salt 2 in a secondary rotary kiln calcining furnace at the temperature of 730 ℃ for 20min to obtain crude salt 3.
And (3) delivering the refined liquid obtained by the refining method into a multi-effect evaporation system, treating to obtain crystalline salt, and throwing the crystalline salt through a double-stage spiral centrifugal machine to remove moisture and then delivering the crystalline salt into a fluidized bed dryer to evaporate the moisture to obtain the industrial salt.
Through detection, the content of the obtained industrial salt sodium chloride is 98.9g/100g, the moisture is 0.31g/100g, the water-insoluble substances are 0.12g/100g, the total content of calcium and magnesium ions is 0.31g/100g, and the sulfate radicals are 0.28g/100 g.
The above embodiments are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modifications made on the basis of the technical scheme according to the technical idea of the present invention fall within the protection scope of the present invention.
Claims (8)
1. A refining method of chemical waste salt is characterized in that: waste salt after pyrolysis and carbonizationDissolving the residue, adding precipitant into the solution, filtering to remove precipitate, introducing the filtrate into ion exchange resin for further removing impurities, adjusting pH of the clear solution to 7-7.5, adding Na2And filtering the solution S to remove precipitates, and concentrating the filtrate through a nanofiltration membrane to obtain refined solution.
2. The method for refining chemical waste salt as claimed in claim 1, wherein: the precipitant is sodium hydroxide, potassium hydroxide, sodium carbonate or potassium carbonate.
3. The method for refining chemical waste salt as claimed in claim 1, wherein: the ion exchange resin is a cationic exchange resin.
4. The method for refining chemical waste salt as claimed in claim 1, wherein: the Na is2The concentration of the S solution is 8-12%.
5. The method for refining chemical waste salt as claimed in claim 1, wherein: before the precipitant is added into the waste salt residue solution, hydrogen peroxide is added into the waste salt residue solution, and then the waste salt residue solution is treated under an ultraviolet condition.
6. The method for refining chemical waste salt as claimed in claim 1, wherein: the pyrolysis carbonization process comprises the following steps: drying and dehydrating chemical waste salt, and then performing primary calcination and secondary calcination on the crude salt to obtain waste salt slag.
7. The method for refining chemical waste salt as claimed in claim 6, wherein: the drying and dehydrating conditions are 180-230 ℃ and 15-30 s.
8. The method for refining chemical waste salt as claimed in claim 6, wherein: the condition of the primary calcination is 500-520 ℃ and 2-4 min; the secondary calcination condition is 700-730 ℃ and 20-25 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112978766A (en) * | 2021-01-28 | 2021-06-18 | 上海市机电设计研究院有限公司 | Advanced treatment method for industrial waste salt |
| CN113353957A (en) * | 2021-05-14 | 2021-09-07 | 江苏杰林环保科技有限公司 | Refining method of chemical waste salt |
| CN114408947A (en) * | 2022-01-20 | 2022-04-29 | 陕西聚泰新材料科技有限公司 | Waste sodium sulfate treatment and purification process |
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| CN109867296A (en) * | 2019-03-08 | 2019-06-11 | 浙江申联环保集团有限公司 | A kind of industrial chlorinations sodium waste salt dregs refining methd |
| CN109970232A (en) * | 2017-12-28 | 2019-07-05 | 江苏久吾高科技股份有限公司 | A kind of processing method and processing device of effluent brine |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109970232A (en) * | 2017-12-28 | 2019-07-05 | 江苏久吾高科技股份有限公司 | A kind of processing method and processing device of effluent brine |
| CN109867296A (en) * | 2019-03-08 | 2019-06-11 | 浙江申联环保集团有限公司 | A kind of industrial chlorinations sodium waste salt dregs refining methd |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112978766A (en) * | 2021-01-28 | 2021-06-18 | 上海市机电设计研究院有限公司 | Advanced treatment method for industrial waste salt |
| CN113353957A (en) * | 2021-05-14 | 2021-09-07 | 江苏杰林环保科技有限公司 | Refining method of chemical waste salt |
| CN114408947A (en) * | 2022-01-20 | 2022-04-29 | 陕西聚泰新材料科技有限公司 | Waste sodium sulfate treatment and purification process |
| CN114408947B (en) * | 2022-01-20 | 2023-08-15 | 陕西聚泰新材料科技有限公司 | Waste sodium sulfate treatment and purification process |
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