CN114477237A - Method for treating and recycling organic waste salt - Google Patents

Method for treating and recycling organic waste salt Download PDF

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Publication number
CN114477237A
CN114477237A CN202210116706.9A CN202210116706A CN114477237A CN 114477237 A CN114477237 A CN 114477237A CN 202210116706 A CN202210116706 A CN 202210116706A CN 114477237 A CN114477237 A CN 114477237A
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heat treatment
salt
waste salt
temperature
organic waste
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CN202210116706.9A
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汤亚飞
王顺
王劲松
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Wuhan Institute of Technology
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Wuhan Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/14Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values

Abstract

The invention provides a method for treating and recycling organic waste salt, which comprises the following steps: placing organic waste salt to be treated in a first-stage heat treatment device for first heat treatment to obtain first-stage treated waste salt; adding the primary treatment waste salt into a secondary heat treatment device for secondary heat treatment to obtain secondary treatment waste salt, wherein the temperature of the secondary heat treatment is higher than that of the primary heat treatment; dissolving the two-stage treatment waste salt in water to obtain a salt residue mixture, and filtering to obtain a salt solution and filter residues; and recrystallizing the filter residue to obtain the industrial salt. According to the invention, the organic waste salt is firstly dried at a lower temperature and then is subjected to heat treatment, so that the purpose of preparing industrial salt from the organic waste salt is achieved, and the generation of hydrogen chloride is reduced in the treatment process, thereby reducing the corrosion rate of the furnace body.

Description

Method for treating and recycling organic waste salt
Technical Field
The invention relates to the technical field of solid waste recycling, in particular to a method for treating and recycling organic waste salt.
Background
With the rapid development of economy in China, the amount of waste salt generated in the wastewater treatment process of industries such as electric power petrochemical industry, coal chemical industry and the like at home and abroad also shows a continuously increasing trend, and the annual output of the waste salt exceeds 2000 million tons at present, and the waste salt is already qualified as dangerous waste. The waste salt which cannot be treated has the characteristic of being easy to be leached and dissolved, can directly influence the pollution of surface water and underground water, destroys the surrounding ecological environment, causes the salinization of soil and harms the health of human bodies. Therefore, whether the waste salt can be properly treated and utilized becomes a key part in the wastewater zero discharge link.
At present, a heat treatment method is mostly adopted to treat waste salt with more organic impurities, and the organic impurities in salt slag are decomposed into volatile gas and carbon slag at high temperature by utilizing the characteristic that the organic impurities are easy to decompose and volatilize at high temperature, so that the aim of removing the organic impurities is fulfilled. The method has the advantages of obvious reduction effect on waste salt and obvious organic matter removal effect, is considered to be the most effective and feasible method for harmless treatment of hazardous solid waste containing salt as a byproduct, is widely applied to treatment of various waste salts such as waste salt in coal chemical industry, industrial waste salt, pesticide waste salt and the like, and has some defects, such as corrosion of a furnace body in a high-temperature treatment process.
Some researchers have proposed some solutions to the corrosion problem of the furnace body, such as: the aluminum coating is brushed or the furnace main body is made of nickel-based alloy materials to resist corrosion and abrasion, or compounds containing Si and Al are added in the burning process to achieve the effect of capturing alkali metal chlorides, and the components of the chlorides in the deposited salt are reduced. However, the above methods have problems of complicated process, high cost, etc.
Disclosure of Invention
In view of the above, the invention provides a method for treating and recycling organic waste salt, so as to solve the problem of high corrosion rate of a furnace body in the existing organic waste salt treatment process.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
a method for treating and recycling organic waste salt comprises the following steps:
s1, placing the organic waste salt to be treated in a first-stage heat treatment device for first heat treatment to obtain first-stage treated waste salt;
s2, adding the primary treatment waste salt into a secondary heat treatment device for secondary heat treatment to obtain secondary treatment waste salt, wherein the temperature of the secondary heat treatment is higher than that of the primary heat treatment;
s3, dissolving the two-stage treatment waste salt in water to obtain a salt residue mixture, and filtering to obtain a salt solution and filter residues;
s4, recrystallizing the filter residue to obtain the industrial salt.
In the above technical solution, the difference between the temperature of the second heat treatment and the temperature of the first heat treatment is within a range of 400 ℃ to 600 ℃.
In the above technical scheme, the temperature of the first heat treatment is in the range of 150 ℃ to 200 ℃, and the time of the first heat treatment is in the range of 30min to 90 min.
In the above technical solution, the temperature of the second heat treatment is within a range of 600 ℃ to 750 ℃, and the time of the second heat treatment is within a range of 60min to 120 min.
In the above technical scheme, the atmosphere of the first heat treatment and the atmosphere of the second heat treatment are air, oxygen or nitrogen.
In the technical scheme, the reaction gas generated by the first-stage heat treatment device and the second-stage heat treatment device is introduced into the alkali solution to be absorbed.
In the above technical scheme, the alkali solution is a sodium hydroxide solution.
In the above technical scheme, the organic pollutants in the organic waste salt to be treated include at least one of ammonium chloride, ammonium acetate and 3-pyridinecarboxaldehyde.
Compared with the prior art, the invention has the following advantages:
according to the invention, the organic waste salt is treated at the lower temperature section and then sent to the high temperature section for heat treatment, so that not only can the organic matter energy be effectively removed, and a better industrial salt production effect be realized, but also the generation of hydrogen chloride in the heat treatment process is reduced, the corrosion rate of the furnace body in the heat treatment process is reduced, and the method has better application and popularization prospects.
Drawings
In order to more clearly illustrate the technical solutions of the present invention or the prior art, some brief descriptions will be given below to the drawings used in the description of the embodiments or the prior art, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a flow chart of a method for treating and recycling organic waste salt according to an embodiment of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below.
It should be noted that in the description of the embodiments herein, the description of the term "some embodiments" means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Throughout this specification, the schematic representations of the terms used above do not necessarily refer to the same implementation or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The term "in.. range" as used herein includes both ends, such as "in the range of 1 to 100" including both ends of 1 and 100.
In the prior art, the technologies for improving the corrosion of the furnace body in the high-temperature treatment process have the problems of complex process, high cost and the like, the analysis and the practical application research on the relevant mechanism influencing the condition of generating hydrogen chloride by the reaction of alkali metal chloride under the heat treatment condition are less, and a large amount of work such as the establishment of a reaction system, the optimization of the reaction condition and the like is not completed.
Based on the above problems, with reference to fig. 1, an embodiment of the present invention provides a method for treating and recycling organic waste salt, including the following steps:
s1, placing the organic waste salt to be treated in a first-stage heat treatment device for first heat treatment to obtain first-stage treated waste salt;
s2, adding the primary treatment waste salt into a secondary heat treatment device for secondary heat treatment to obtain secondary treatment waste salt, wherein the temperature of the secondary heat treatment is higher than that of the primary heat treatment;
s3, dissolving the secondary treatment waste salt in water to obtain a salt residue mixture, and filtering to obtain a salt solution and filter residues;
s4, recrystallizing the filter residue to obtain the industrial salt.
According to the embodiment of the invention, the organic waste salt is dried at a lower temperature and then is subjected to heat treatment at a proper reaction temperature, so that the aim of preparing industrial salt from the organic waste salt is fulfilled, and the generation of hydrogen chloride is reduced in the treatment process, thereby reducing the corrosion rate of the furnace body.
Further, the difference between the temperature of the second heat treatment and the temperature of the first heat treatment is in the range of 400 ℃ to 600 ℃. According to reaction 2NaCl + H2O=Na2And the reaction is easier to be carried out in the positive direction under the condition of high temperature and water, and more hydrogen chloride is generated.
Preferably, the temperature of the first heat treatment is in the range of 150 ℃ to 200 ℃ and the time of the first heat treatment is in the range of 30min to 90 min. By adopting low-temperature drying, free moisture and most of crystal water in the waste salt are removed, and the reaction is kept in a relatively dry environment as much as possible.
The temperature of the second heat treatment is in the range of 600 ℃ to 750 ℃, and the time of the second heat treatment is in the range of 60min to 120 min. After low-temperature drying, high-temperature heat treatment is adopted, so that organic matters in the waste salt are incinerated into carbon dioxide or pyrolyzed into coke, and the aim of separating the coke from the salt is further fulfilled.
Wherein, the atmosphere of the first heat treatment and the second heat treatment is air, oxygen or nitrogen. In the embodiment of the present invention, the heat treatment apparatus is a tube furnace, but may be other apparatuses that can be used for heat treatment, and is not particularly limited herein.
Reaction gas generated by the first-stage heat treatment device and the second-stage heat treatment device is introduced into the alkali solution to be absorbed. Preferably, the alkali solution is a sodium hydroxide solution. By absorbing the reaction gas, the influence on the environment can be effectively reduced.
In an embodiment of the present invention, the organic contaminants in the organic waste salt to be treated include at least one of ammonium chloride, ammonium acetate and 3-pyridinecarboxaldehyde.
The method provided by the embodiment of the invention can realize a better industrial salt production effect, reduces the generation of hydrogen chloride in the heat treatment process, reduces the corrosion rate of the furnace body in the heat treatment process, and reduces the maintenance cost of equipment such as an incinerator and the like.
On the basis of the above embodiments, the present invention is further illustrated by the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The following examples are examples of experimental procedures not specified under specific conditions, generally according to the conditions recommended by the manufacturer. Unless otherwise indicated, percentages and parts are by mass.
The organic waste salt treated in this example is sourced from pharmaceutical and technology limited of magnolia denudata, Hubei (main product of pyraclonil), abbreviated as magnolia denudata waste salt, and the waste salt is organic matter-containing waste salt. Through detection, the main indexes of the waste salt of the golden magnolia are as follows: the waste salt is in the form of colored powder particles and has pungent smell, the water content is about 2%, the whiteness is 19.23, and the TOC is 355632 mg/kg.
Example 1
The embodiment provides a method for treating and recycling organic waste salt, which comprises the following steps:
1) weighing 10g of waste salt of the golden magnolia, pouring the waste salt into a burning boat and uniformly distributing the waste salt, introducing air into a tubular furnace by using a small air pump to keep the atmosphere in a quartz tube, sending the burning boat into the furnace and carrying out heat treatment for 2 hours when the temperature in the furnace rises to 600 ℃, and introducing reaction tail gas into 200ml of NaOH solution for absorption in the heat treatment process;
2) when the temperature in the furnace is reduced to room temperature, the air pump is closed, the burning boat is taken out, the waste salt after heat treatment is dissolved by distilled water, and 200ml of salt solution and filter residue are obtained by suction filtration;
3) and putting the salt solution on a universal electronic furnace for recrystallization to obtain precipitated crystal salt F1+600 ℃.
The embodiment provides a method for treating and recycling organic waste salt, which comprises the following steps:
1) weighing 10g of waste salt of the golden magnolia, pouring the waste salt into a burning boat and uniformly distributing the waste salt, introducing air into a tube furnace by using a small air pump to keep the atmosphere in a quartz tube, sending the burning boat into the furnace and carrying out heat treatment for 2 hours when the temperature in the furnace rises to 600 ℃, and introducing reaction tail gas into 200ml of NaOH solution for absorption in the heat treatment process.
2) Cooling the furnace to room temperature, closing the air pump, taking out the burning boat, dissolving the heat-treated waste salt with distilled water, and filtering to obtain 200ml salt solution and filter residue
3) The salt solution is placed on a universal electronic furnace for recrystallization, and the crystalline salt F1+600 ℃ is obtained.
Example 2
The embodiment provides a method for treating and recycling organic waste salt, which comprises the following steps:
1) weighing 10g of waste salt of magnolia denudata, pouring the waste salt into a burning boat, uniformly distributing the waste salt, introducing air into a tubular furnace by using a small air pump to keep the atmosphere in a quartz tube, and sending the burning boat into the furnace and carrying out heat treatment for 1 hour when the temperature in the furnace is raised to 200 ℃; dragging the burning boat to the opening of the quartz tube, and when the temperature in the furnace rises to 600 ℃, sending the burning boat into the furnace and carrying out heat treatment for 2 hours to obtain secondary treatment waste salt; in the heat treatment process, introducing reaction tail gas into 200ml of NaOH solution for absorption;
2) when the temperature in the furnace is reduced to room temperature, the air pump is closed, the burning boat is taken out, the two-stage treatment waste salt is dissolved by distilled water, and 200ml of salt solution and filter residue are obtained by suction filtration;
3) and putting the salt solution on a universal electronic furnace for recrystallization to obtain precipitated crystal salt F2+600 ℃.
Example 3
The present embodiment is a method for treating and recycling organic waste salt, which is different from embodiment 1 in that:
in the step 1), keeping a nitrogen atmosphere in a quartz tube;
the remaining steps and parameters were the same as in example 1, giving the crystalline salt N1+600 ℃.
Example 4
The present embodiment is a method for treating and recycling organic waste salt, which is different from embodiment 2 in that:
in the step 1), keeping a nitrogen atmosphere in a quartz tube;
the remaining steps and parameters were the same as in example 1, giving the crystalline salt N2+600 ℃.
The chlorine ion concentration of the absorption solution of the crystal salt obtained in examples 1 to 4, and the whiteness and TOC content of the crystal salt were measured, respectively, to obtain tables 1 and 2.
TABLE 1 influence of different treatment modes on the chloride ion concentration of the absorption solution
Treatment method F1+600℃ F2+600℃ N1+600℃ N2+600℃
Chloride ion concentration (mg/L) 52.71 6.47 8.58 4.57
As can be seen from Table 1, under the same heat treatment conditions, the two-stage heat treatment can effectively reduce the generation amount of hydrogen chloride, reduce the generation amount of 87.25% of hydrogen chloride under the air incineration condition and reduce the generation amount of 46.74% of hydrogen chloride under the nitrogen pyrolysis condition, which shows that the method for treating and recycling the organic waste salt provided by the invention is beneficial to reducing the corrosion rate in the furnace and reducing the maintenance cost of equipment such as an incinerator and the like.
TABLE 2 Effect of different treatments on whiteness and TOC of crystalline salts
Treatment method F1+600℃ F2+600℃ N1+600℃ N2+600℃
Whiteness degree 85.76 86.82 78.55 80.61
TOC(mg/L) / 26.80 / 32.04
As can be seen from Table 2, under the same heat treatment conditions, the whiteness of the crystal salt after the two-stage heat treatment is slightly higher than that of the one-stage heat treatment; the whiteness of the crystal salt treated by the two-stage thermal method can reach more than 80 of the industrial salt standard, and the TOC content under the incineration condition can reach less than 30mg/kg of the industrial salt standard. The method selects proper treatment conditions, and the organic waste salt can reach the industrial salt standard after the method for treating and recycling the organic waste salt provided by the invention is used.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Various changes and modifications may be effected therein by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present disclosure, and these changes and modifications are intended to be within the scope of the present disclosure.

Claims (8)

1. A method for treating and recycling organic waste salt is characterized by comprising the following steps:
s1, placing the organic waste salt to be treated in a first-stage heat treatment device for first heat treatment to obtain first-stage treated waste salt;
s2, adding the primary treatment waste salt into a secondary heat treatment device for secondary heat treatment to obtain secondary treatment waste salt, wherein the temperature of the secondary heat treatment is higher than that of the primary heat treatment;
s3, dissolving the two-stage treatment waste salt in water to obtain a salt residue mixture, and filtering to obtain a salt solution and filter residues;
s4, recrystallizing the filter residue to obtain the industrial salt.
2. The method according to claim 1, wherein the difference between the temperature of the second heat treatment and the temperature of the first heat treatment is in the range of 400 ℃ to 600 ℃.
3. The method for preparing a ceramic material according to claim 2, wherein the temperature of the first heat treatment is in the range of 150 ℃ to 200 ℃ and the time of the first heat treatment is in the range of 30min to 90 min.
4. The method of claim 3, wherein the temperature of the second heat treatment is in the range of 600 ℃ to 750 ℃ and the time of the second heat treatment is in the range of 60min to 120 min.
5. The method according to claim 1, wherein the atmosphere for the first heat treatment and the atmosphere for the second heat treatment are air, oxygen, or nitrogen.
6. The preparation method according to any one of claims 1 to 5, wherein reaction tail gas generated by the primary heat treatment device and the secondary heat treatment device is introduced into the alkali solution for absorption.
7. The method according to claim 6, wherein the alkali solution is a sodium hydroxide solution.
8. The method according to claim 1, wherein the organic contaminants in the organic waste salt to be treated comprise at least one of ammonium chloride, ammonium acetate and 3-pyridinecarboxaldehyde.
CN202210116706.9A 2022-02-07 2022-02-07 Method for treating and recycling organic waste salt Pending CN114477237A (en)

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CN112879922A (en) * 2021-01-06 2021-06-01 浙江工业大学 Method and device for treating industrial waste salt by plasma torch

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