CN114314615A - Resource treatment method of industrial waste salt containing organic matters - Google Patents
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Abstract
The invention discloses a recycling treatment method of industrial waste salt containing organic matters, which specifically comprises the following steps: 1) putting industrial salt into an organic solvent, and removing partial organic matters in waste salt; 2) heating industrial waste salt in an aerobic environment by a heating device to remove organic matters carried by the industrial waste salt; 3) dissolving the industrial salt subjected to high-temperature treatment in water, and performing water washing treatment; 4) filtering the water washing liquid to remove water-insoluble impurities, and evaporating and crystallizing to obtain pure industrial salt. The method has the advantages of reasonable process route, simple operation and high efficiency, can realize the resource recycling of industrial salt, and saves a large amount of resources.
Description
(I) technical field
The invention relates to a resource treatment method of industrial waste salt, in particular to a treatment method of high-temperature incineration after purification, which can remove organic matters in the waste salt and is suitable for resource recycling of waste salt in the production of chemical industry, pesticides and the like.
(II) background of the invention
The organic matter-containing industrial waste salt is solid waste generated in the production processes of petrochemical industry, fine chemical industry, medical chemical industry and the like at present, and the organic matter contained in the waste salt is complex in composition and high in concentration and cannot be biologically treated due to different raw materials and production processes used in the production processes. Industrial salt as an important national resource cannot be well recycled at present, so that it is necessary to develop and design a method for recycling chemical waste salt.
The treatment methods adopted at present mainly comprise landfill, organic matter oxidation, incineration and other treatment modes. The landfill is mainly divided into rigid landfill and flexible landfill, wherein the rigid landfill is to carry out sanitary landfill treatment by curing waste salt through concrete and the like and then sending the waste salt into a rigid landfill according to landfill technical specifications, but the rigid landfill has higher cost and larger floor area, and the flexible landfill is selected according to hazardous waste landfill pollution control standard GB18598-2019, the total amount of water-soluble salt required by the flexible landfill is less than 10%, so the direct flexible landfill is limited by policy. The organic matter oxidation method is a method for dissolving waste salt in water and decomposing organic matter by a deep oxidation technology, but because the organic matter contained in industrial waste salt is complex, multiple technologies are often needed for common treatment, the operation is complex and the cost is high. The carbonization decomposition is a method for carbonizing organic matters in the waste salt to convert the organic matters into solid organic carbon under the melting condition lower than that of inorganic salt, organic matters can be removed, the purity of the inorganic salt is improved, and the obtained product can be blackened or grayed, so that the quality of the product is influenced. Different treatment technologies of waste salt have different advantages, and compared with the three methods, carbonization treatment is an accepted method at present, so the research and development of organic matter carbonization process equipment and the application of a combined process are the mainstream directions of the treatment of the waste salt containing organic matters.
In order to improve the removal efficiency of organic matters in the waste salt, save the treatment cost and realize the resource recycling of industrial salt. The invention provides a method for recycling industrial salt, which obviously improves the removal efficiency of organic matters in the salt, and simultaneously improves the purity of the salt by adding a washing purification process after carbonization.
The combined treatment process of organic solvent pretreatment, high-temperature carbonization and water purification has higher organic matter removal and salt recovery efficiency than the single technology, the organic matter content in salt can be effectively reduced by using the organic solvent washing pretreatment, the residual organic matter is further removed by high-temperature carbonization, and finally insoluble substances such as carbon and the like generated by the organic matter in the carbonization process are removed by washing and filtering, so that the quality of the salt is improved, and the problems encountered in the carbonization treatment are effectively solved.
Disclosure of the invention
The invention aims to provide a resource treatment method of industrial salt containing organic matters, which solves the problems that the organic matters are not completely removed in the traditional treatment process and the industrial salt meeting the national standard cannot be obtained after treatment. The invention carries out high-temperature roasting under proper conditions after the industrial waste salt is dissolved and pretreated by an organic solvent, burns and degrades the contained complex organic matters, and then carries out the processes of dissolving, washing, filtering, recrystallizing and the like on the roasted product to realize the recycling of the industrial salt.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a resource treatment method of industrial waste salt containing organic matters, which comprises the following steps:
(1) adding an organic solvent into industrial waste salt containing organic matters, oscillating and mixing for 10min-40min (preferably 30min) to fully dissolve the organic matters in the organic solvent, centrifuging (4000r/min for 10min), drying the obtained precipitate (removing residual organic solvent) at 90-110 ℃ (preferably 105 ℃) to obtain pretreated industrial waste salt; the organic solvent is ethanol or benzene (preferably ethanol); the volume of the organic solvent is 1-2 mL/g (preferably 1mL/g) based on the mass of the industrial waste salt containing the organic matters;
the organic solvent centrifuged in the step (1) can be recycled and can be used as subsequent high-temperature incineration energy after being used for multiple times.
(2) Roasting the pretreated industrial waste salt in the step (1) in an oxygen-containing atmosphere (preferably an air atmosphere) at 550-650 ℃ for 1.5-3.5h (preferably 600 ℃ for 2h) to obtain organic substance decomposed industrial salt;
during the heating process, an oxygen-containing atmosphere (preferably an air atmosphere) is adopted to ensure that sufficient oxygen is available for the combustion of the organic matters, so that the organic matters are thoroughly degraded. After the combustion furnace is cooled to room temperature, the industrial salt in the crucible is taken out, and the industrial salt is blackened due to carbon generated by decomposition of organic matters in the process.
(3) And (3) dissolving the industrial salt decomposed by the organic matters in the step (2) in water, filtering, and recrystallizing the filtrate to obtain the salt subjected to resource treatment.
In the dissolving process, substances such as carbon and the like generated by high-temperature combustion of organic matters are insoluble in water, suspended in the water and filtered by filter paper to obtain a treated solution, namely, a decomposition product of the organic matters is removed. At the moment, organic matters in the salt are basically removed, and the industrial salt recrystallized after washing and filtering can be reused for chemical industry and pesticide production, and other subsequent treatments are needed when the industrial salt is used in other industries such as cement, dyeing and the like.
Further, the organic matter-containing industrial waste salt in the step (1) is one or a mixture of more than two of chemical production waste salt, pesticide production waste salt, petrochemical production, fine chemical production waste salt and medical chemical production waste salt, and the main component is Na2SO4。
Preferably, the industrial waste salt containing organic matters in the step (1) is obtained by removing the solvent from the filtrate in salting out and reducing acid precipitation in the production process for preparing DSD acid from p-nitrotoluene-o-sulfonic acid; the organic-containing industrial waste salt in the step (1) can also be obtained by washing the reaction solution with saturated sodium sulfate water in the production process of preparing dimethomorph from acetyl morpholine and then removing the solvent from the layered water phase.
Preferably, the mass ratio of the industrial salt decomposed by the organic matter in the step (3) to the water is 1:80-110 (further preferably 1: 100).
Preferably, the temperature of the recrystallization in step (3) is 105 ℃.
Compared with the prior art, the invention has the following beneficial effects: because in the traditional treatment process of industrial salt containing organic matters, the chemical treatment operation is complex, various composite processes need to be established for the organic matters in the salt for treatment, the universality is poor, the removal efficiency is low, the high-temperature melting treatment always needs to set the temperature at 800 ℃, and the energy consumption is increased, and the treatment cost is increased. In addition, the organic solvent pretreatment can remove part of organic matters in salt, improve the removal efficiency of the organic matters, reduce the temperature required in the high-temperature incineration process, and can incinerate the organic solvents after the organic solvents are recycled to provide energy for the subsequent roasting process, so that the energy consumption in the treatment process can be reduced, the waste organic solvents can be harmlessly treated, the problem that the industrial salt is blackened and the salt quality is reduced in the incineration process can be effectively solved by adopting a water purification process, the cost is saved, and the trouble of the subsequent treatment is also reduced.
(IV) description of the drawings
FIG. 1 is a process flow diagram of the present invention.
(V) specific embodiment
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto:
example 1:
the waste salt treatment process comprises the following steps of: sulfonation: p-nitrotoluene and oleum react to generate p-nitrotoluene-o-sulfonic acid. Oxidation and condensation: adding 0.15 wt% of aqueous solution of manganese sulfate in formaldehyde into p-nitrotoluene-o-sulfonic acid for catalysis, and adding Na2SO4Salting out to obtain intermediate 4,4 '-dinitrostilbene-2, 2' -disulfonic acid precipitate, and performing suction filtration to obtain intermediate 4,4 '-dinitrostilbene-2, 2' -disulfonic acid solid and salt-containing filtrate. ③ reduction acidification: adding sulfuric acid and sodium hydroxide into the intermediate product generated in the step (II) for reaction, performing acid precipitation by using sulfuric acid to obtain a DSD acid solid precipitate, and filtering and drying to obtain a DSD acid finished product. The industrial waste salt in the embodiment is the filtrate obtained in the salting-out and acidification processes in the production processes II and III, and the waste salt is obtained after evaporation treatment of the filtrate. The waste salt after sampling analysis contains Na as main component2SO492.29% of waste salt, 3931mg/kg of COD and 5.84% of water, 5g of dried waste salt is dissolved in 50g of water, the pH value of the solution is 5.79, and organic matters in the DSD acid are easily dissolved in ethanol.
1) Respectively taking four parts of 50g of the industrial waste salt, wherein one part is not processed, respectively adding 50g of benzene, ethanol and a benzene/ethanol (25 g of benzene and ethanol respectively) solvent with the mass ratio of 1:1 into the remaining three parts, washing, shaking, uniformly mixing for 30min, centrifuging, pouring out supernatant, and drying the salt at 105 ℃ to remove residual organic solvent in the salt. The organic solvent can be repeatedly used. The waste organic solvent can provide combustion energy for the subsequent roasting treatment process.
2) Respectively taking 10g of pretreated waste salt containing organic matters, uniformly spreading the waste salt on the bottom of a crucible, placing the crucible in a muffle furnace, setting the temperature of the muffle furnace to be 600 ℃, and starting to heat, wherein the actual temperature is between 585-. And when the temperature of the muffle furnace reaches 600 ℃, timing is started, the experiment verifies the experiment effect that the residence time is 1, 1.5, 2, 2.5 and 3 hours respectively, when the residence time is reached, the muffle furnace is set to 25 ℃, and the muffle furnace is taken out after being cooled to the room temperature.
3) Respectively taking 5g of the industrial salt after incineration treatment, dissolving the industrial salt in 500g of water, oscillating and uniformly mixing in a shaking table to ensure that the industrial salt is fully dissolved, and filtering by using filter paper. COD detection was performed on the filtered solution, and the detection results are shown in Table 1.
Evaporating the filtered solution at 105 ℃ to recover the salt in the solution into a crystal state again, thereby completing the recycling of the industrial salt, wherein the COD removal effect of the industrial salt washed by ethanol is the best, and the recrystallized color is white.
TABLE 1 COD content (mg/kg) in Industrial waste salt
TABLE 2 COD removal in Industrial waste salt
Comparative example 1
The other points are the same as example 1 except that 50g of waste salt is pretreated by adding 25g, 50g and 100g of ethanol solvent, respectively, and then calcined at 600 ℃ for 2 hours. After COD detection, the comparison result is as follows:
through comparative analysis, when the mass ratio of the industrial salt is 1:1, namely the using amount of the ethanol is 50g, the treatment effect is good, and the treatment effect is almost the same as that when the using amount of the ethanol is 100 g.
Example 2
The treated salt is brown salt mud formed by evaporating and concentrating waste liquid generated in the production process of dimethomorph in a pesticide production workshop, and the preparation process comprises the following steps: preparing acetyl morpholine: dripping morpholine into dimethylbenzene and acetic anhydride at normal temperature, heating to 110 ℃ after dripping is finished, and rectifying to obtain the acetyl morpholine. Preparing dimethomorph: adding dimethylbenzene, E-benzophenone and sodium amide into a reaction kettle, dropwise adding acetylmorpholine, carrying out catalytic reaction by using concentrated sulfuric acid, washing by using saturated sodium sulfate salt water, layering obtained reaction liquid, carrying out liquid separation to obtain dimethomorph, and carrying out subsequent treatment on lower-layer waste liquid. The waste salt used in this example is salt slurry obtained by evaporating and dehydrating the waste liquid remaining after liquid separation in the step (II). After sampling and analysis, the main component is Na2SO4The content was 94.12%, COD was 6671mg/kg, the water content was 5.84%, the pH of the solution was 6.23 when 5g of salt was dissolved in 50g of water, and the solution was dark yellow when waste salt was dissolved in water.
1) Taking 20g of the waste salt, adding 20g of ethanol solvent into the waste salt, shaking and uniformly mixing for 30min to fully dissolve organic matters in the salt, centrifuging at the rotating speed of 4000r/min for 10min, then removing supernatant, and drying the treated salt. The organic solvent can be repeatedly used.
2) Taking 10g of pretreated waste salt containing organic matters, uniformly spreading the waste salt on the bottom of a crucible, placing the crucible in a muffle furnace, setting the temperature of the muffle furnace to be 600 ℃, starting to heat, keeping the actual temperature between 585-. When the residence time was reached, the muffle was set to 25 ℃, cooled to room temperature and taken out.
3) Dissolving 5g of incinerated industrial salt in 500g of water, shaking and uniformly mixing in a shaking table to fully dissolve the industrial salt, and filtering by using filter paper. Evaporating the filtered solution at 105 deg.C to recover the salt to crystal state, detecting organic content to be 208mg/kg, and recrystallizing to obtain pure white salt.
Comparative example 2
The other example is the same as example 2 except that the sample was directly calcined without pretreatment at a temperature of 600 ℃ for 2 hours.
Comparative example 3
The other point is the same as example 2, except that the sample is washed with benzene during pretreatment, the calcination temperature is 600 ℃ and the treatment time is 2 hours.
Comparative example 4
The other point is that the sample is pretreated by washing with a mixed solution of benzene and ethanol (10 g of benzene and ethanol, respectively) at a mass ratio of 1:1, the calcination temperature is 600 ℃ and the treatment time is 2 hours.
The samples recrystallized from comparative examples 2, 3 and 4 were subjected to COD detection and compared with example 2, and the results are shown in the following table:
TABLE 3 comparison of the removal efficiency of different cases
The comparison shows that the treatment effect of the example 2 is best under the same other treatment conditions, namely the organic matter in the waste salt is best removed when the roasting is carried out after the washing pretreatment by using the ethanol organic solvent.
Comparative example 5
The other points are the same as example 1 except that 20g of waste salt is pretreated by adding 10g, 20g and 40g of absolute ethanol solvent, respectively. After COD detection, the comparison result is as follows:
through comparative analysis, when the mass ratio of the industrial salt is 1:1, namely the using amount of the ethanol is 20g, the treatment effect is good, and the treatment effect is almost the same as that when the using amount of the ethanol is 40 g.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A resource treatment method of industrial waste salt containing organic matters is characterized by comprising the following steps:
(1) adding an organic solvent into industrial waste salt containing organic matters, oscillating and mixing for 10-40 min, centrifuging, and drying the obtained precipitate at 90-110 ℃ to obtain pretreated industrial waste salt; the organic solvent is ethanol or benzene; the volume of the organic solvent is 1-2 mL/g based on the mass of the industrial waste salt containing the organic matters; the organic matter-containing industrial waste salt is one or a mixture of more than two of chemical production waste salt, pesticide production waste salt, petrochemical production, fine chemical production waste salt and medical chemical production waste salt, and the main component is Na2SO4；
(2) Roasting the pretreated industrial waste salt in the step (1) for 1.5-3.5h at the temperature of 550-650 ℃ in an oxygen-containing atmosphere to obtain industrial salt for decomposing organic matters;
(3) and (3) dissolving the industrial salt decomposed by the organic matters in the step (2) in water, filtering, and recrystallizing the filtrate to obtain the salt subjected to resource treatment.
2. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the drying temperature in the step (1) is 105 ℃. .
3. The method for recycling industrial waste salt containing organic matter according to claim 1 or 2, wherein: the industrial waste salt containing organic matters in the step (1) is obtained by removing the solvent from the filtrate in salting out and reducing acid precipitation in the production process of preparing DSD acid from p-nitrotoluene-o-sulfonic acid.
4. The method for recycling industrial waste salt containing organic matter according to claim 1 or 2, wherein: the organic-containing industrial waste salt in the step (1) is obtained by washing reaction liquid with saturated sodium sulfate water in a production process for preparing dimethomorph from acetyl morpholine and then removing a solvent from a layered water phase.
5. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the organic solvent in the step (1) is ethanol.
6. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the volume of the organic solvent in the step (1) is 1mL/g based on the mass of the industrial waste salt containing the organic matters.
7. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the roasting temperature in the step (2) is 600 ℃.
8. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: and (3) the oxygen-containing atmosphere in the step (2) is an air atmosphere.
9. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the mass ratio of the industrial salt decomposed by the organic matters to the water in the step (3) is 1: 80-110.
10. The method for recycling industrial waste salts containing organic substances according to claim 1, wherein: the temperature of the recrystallization in the step (3) was 105 ℃.
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| CN115072786A (en) * | 2022-07-15 | 2022-09-20 | 盐城市国投环境技术股份有限公司 | Method for preparing manganese chloride by utilizing by-product manganese carbonate salt generated in prochloraz production |
| CN116495753A (en) * | 2023-04-26 | 2023-07-28 | 中国科学院生态环境研究中心 | Method for recycling industrial waste salt through recrystallization and purification |
Citations (10)
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| CN116495753A (en) * | 2023-04-26 | 2023-07-28 | 中国科学院生态环境研究中心 | Method for recycling industrial waste salt through recrystallization and purification |
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