CN110054203B - Method for recycling industrial waste salt - Google Patents
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- CN110054203B CN110054203B CN201910297362.4A CN201910297362A CN110054203B CN 110054203 B CN110054203 B CN 110054203B CN 201910297362 A CN201910297362 A CN 201910297362A CN 110054203 B CN110054203 B CN 110054203B
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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
- C01D3/08—Preparation by working up natural or industrial salt mixtures or siliceous minerals
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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
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- 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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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/82—Compositional purity water content
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Abstract
The invention belongs to the field of treatment and disposal of industrial solid waste, and particularly discloses a recycling method of industrial waste salt taking sodium sulfate or sodium chloride as a main component, which comprises the following steps: dissolving a certain amount of industrial waste salt in water, and fully dissolving under the combined action of ultrasound and stirring to obtain a nearly saturated salt solution A; carrying out two-stage filtration and purification on the salt solution A to remove insoluble impurities in the salt solution A to obtain a salt solution B; and (3) feeding the salt solution B into a spray combustion furnace, pyrolyzing and oxidizing soluble organic matters in the salt solution B at a temperature lower than the melting point of the salt, and then discharging the dissolved organic matters together with water vapor to finally obtain a dried sodium salt product. The method of the invention not only can efficiently remove organic matters in the waste salt and realize the harmlessness of the hazardous waste of the industrial waste salt, but also can prepare the sodium salt byproduct meeting the quality requirement of industrial products, thereby realizing the harmlessness and the recycling of the industrial waste salt.
Description
Technical Field
The invention belongs to the field of treatment and disposal of industrial solid waste, and particularly relates to a resource method of industrial waste salt taking sodium sulfate or sodium chloride as a main component.
Background
In recent years, cases of illegal treatment and disposal of hazardous wastes frequently occur, and the cases attract extensive attention of all social circles. Many of the cases relate to the treatment and disposal of hazardous wastes, especially waste slag and salt, in the chemical industry. The waste has the characteristics of wide sources, various types, complex components, high content of toxic and harmful substances and the like, is large in environmental hazard, and is faced with increasingly strict treatment and disposal requirements and environmental management policies, and the treatment and disposal requirements and the cost are continuously improved, so that the treatment difficulty is very high, and the waste becomes one of the main problems to be solved urgently in the current environmental protection industry. On the other hand, the salt is also an important chemical raw material, if the waste salt in the chemical industry can be subjected to harmless and recycling treatment and reused as an industrial raw material or other purposes in the form of byproducts, the harm to the environment can be eliminated, the waste salt resource can be fully utilized, and the waste recycling and recycling economy of the chemical industry can be realized.
At present, the harmless treatment and resource utilization of waste salt in the chemical industry mainly have the following technical approaches:
1) a melting purification technology;
namely, under the condition of high temperature, the waste salt is melted, organic matters in the waste salt are volatilized from the melt due to low boiling point, then the waste gas is treated by gas purification technology such as incineration, and finally organic toxic and harmful substances in the waste salt are removed, so that the purified inorganic salt is obtained. The technology is the most common technology which is effective and feasible for treating dangerous waste salt, and is reported in the invention patents of the publication No. CN104310434A 'a device and a process for treating waste salt', CN106152109A 'a device for thermally separating substances of a gas-fuel-oil molten salt integrated boiler', and the utility model patents of the publication No. CN203928459U 'a molten salt cooling and recycling system', CN205659976U 'equipment for treating waste sodium chloride in a melting process'. Although the technology can remove toxic and harmful organic matters in the waste salt, the technology has some defects, such as influence of factors such as waste salt components, forms and granularity, uneven heating and low energy efficiency, and organic matters can also be carbonized and coked to influence the quality of the salt; the waste salt has serious fusion and adhesion phenomena, is easy to corrode the surface of equipment, and can cause equipment damage in serious cases; only toxic and harmful organic matters in the waste salt are removed, the content of impurities in the treated hazardous waste salt is high, the hazardous waste salt is still difficult to be recycled, and only landfill treatment can be carried out, so that not only is the resource waste caused, but also the landfill cost is high.
2) Pyrolysis technology
Namely, under the condition of high temperature and lower than the melting temperature of the waste salt, the organic matters in the waste salt are volatilized, and the volatilized organic matters are removed by technologies such as oxidation or combustion, and the detoxification and harmless treatment of the waste salt are realized. The technology is reported in patent publications such as CN106424112A, a multistage thermal desorption process and equipment for waste salt refining, CN106824980A, a harmless treatment method of coal chemical industry crystallization waste salt, CN107185948A, an industrial waste salt system and method, CN107062836A, a radiation type rotary drying device for waste salt treatment, CN108408744A, a system and method for treating organic matters in industrial waste salt by thermal fluid fractional stripping and the like. The technology has good detoxification effect on the waste salt, achieves harmless treatment, does not consider inorganic and other impurities which are not easy to volatilize at high temperature in the waste salt, and limits the resource utilization of the waste salt.
However, the technology has some problems in operation, such as uneven heating and low energy efficiency, due to the influence of waste salt components, forms, particle sizes and other factors; the waste salt has serious fusion and adhesion phenomena, is easy to corrode the surface of equipment, and can cause equipment damage in serious cases; only toxic and harmful organic matters in the waste salt are removed, the content of impurities in the treated hazardous waste salt is high, the hazardous waste salt is still difficult to be recycled, and only landfill treatment can be carried out, so that not only is the resource waste caused, but also the landfill cost is high.
3) Water-soluble and salt-solution purifying and resource-recovering technology
The technique is to dissolve the waste salt with water to become liquid, then to separate and purify the salt from the liquid phase by means of waste water treatment, such as chemical impurity removal or membrane solid-liquid separation, to obtain a relatively pure salt solution, and then to further prepare the salt. For example, the invention patent of publication No. CN103693658A "industrial waste salt comprehensive treatment device based on three-stage incinerator and its using method" is to dissolve industrial waste salt mainly containing sodium chloride, remove inorganic impurities through chemical treatment, then dry and pyrolyze to dehydrate, in the process, organic matter volatilizes and enters into gas phase, then the waste gas meets the emission requirement through incineration treatment, and the waste salt is purified to meet the requirement of salt for chlor-alkali industry. The invention patent with publication No. CN105883859A 'a waste salt treatment method' comprises roasting waste salt at 600 deg.C for 0.5-4 hr at 300-. The utility model with the authorization number of CN207933534U 'a purification device of waste salt' adds water to dissolve NaCl waste salt slag obtained in pesticide synthesis; filtering the salt water obtained in the salt dissolving tank by using a nanofiltration membrane connected to the salt dissolving tank; the cationic impurity removing device is connected to the permeation side of the nanofiltration membrane and is used for removing cationic impurities from the permeation liquid obtained by the nanofiltration membrane; the chelating resin column is connected with the cationic impurity removing device and is used for desalting the produced water obtained by the cationic impurity removing device by resin; and the ionic membrane electrolytic cell is connected to the chelate resin column and is used for carrying out electrolytic treatment on the produced water of the chelate resin column to finally obtain caustic soda and chlorine.
The technology can be used for obtaining purer salt, and even can be used for deep processing the obtained salt into other chemical raw materials, so that the method is an ideal method for recycling waste salt, but the currently reported technical process is complex and high in treatment cost, and particularly for waste salt with high sodium chloride content, resin poisoning is caused by containing a large amount of chloride ions in a salt solution formed by dissolving the waste salt in water, so that the effect of adsorbing organic matters is poor, and even the adsorption effect is lost, so that the industrial popularization and application of the technology for adsorbing and removing the organic matters in the water through the resin are limited.
In conclusion, a harmless and recycling treatment technology for waste salt, which has the advantages of simple process, strong operability and low treatment cost, is urgently needed to be developed.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the technical problem of providing a method for recycling industrial waste salt, which can not only efficiently remove organic matters in the waste salt and realize the harmlessness of hazardous waste, namely the industrial waste salt, but also can prepare sodium salt byproducts meeting the quality requirements of industrial products, thereby realizing the harmlessness and recycling of the industrial waste salt.
The invention content is as follows: in order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a resource method of industrial waste salt, wherein the industrial waste salt takes sodium chloride or sodium sulfate as a main component; the industrial waste salt is subjected to resource treatment by the following method, specifically:
step 1, dissolving a certain amount of industrial waste salt in water, and fully dissolving under the combined action of ultrasound and stirring to obtain a nearly saturated salt solution A;
step 2, carrying out two-stage filtration and purification on the salt solution A to remove insoluble impurities in the salt solution A to obtain a salt solution B;
and 3, feeding the salt solution B into a spray combustion furnace, pyrolyzing and oxidizing soluble organic matters in the salt solution B at a temperature lower than the melting point of the salt, and then discharging the organic matters together with water vapor to finally obtain a dried sodium salt product.
In the step 1, the ultrasonic working frequency is 15-60 kHz when the salt is dissolved.
In the step 1, the mass concentration of sodium sulfate in the waste salt solution obtained by fully dissolving the waste salt with sodium sulfate as a main component is 15-28%.
In the step 1, the mass concentration of sodium chloride in the waste salt solution obtained by fully dissolving the waste salt with sodium chloride as a main component is 20-25%.
In the step 2, in the two-stage filtration, the first stage filtration is ordinary filtration, the second stage filtration is precise filtration, and the precise filtration adopts microporous filtration.
Wherein, in the step 3, the heating temperature of the spray combustion furnace is 500-850 ℃.
The method adopts an ultrasonic combined stirring and dissolving technology, and can fully dissolve the waste salt containing organic matters and impurities and having high viscosity by virtue of the cavitation effect of ultrasonic waves; the cavitation effect is that under the action of ultrasonic wave, a large amount of micro bubbles are continuously generated in the liquid, the small bubbles grow and grow gradually along with the ultrasonic vibration and then break suddenly, and the broken bubbles continue to grow and break. When the small bubbles are broken rapidly, high temperature and high pressure are generated in the bubbles, and strong local fluctuation is generated in the liquid near the bubbles due to the fact that the liquid around the bubbles is rushed into the bubbles at high speed, and local high temperature and high pressure are also formed, so that ultrasonic crushing and emulsification are generated, and the dissolving efficiency of soluble substances in waste salt is accelerated and improved; meanwhile, the invention sprays the strong brine to form tiny liquid drops, in the spray combustion furnace, at the high temperature lower than the melting point of the salt, the soluble organic matters in the salt solution are continuously heated and decomposed, and are oxidized by air and discharged out of the combustion furnace along with the steam, the water in the salt solution is discharged out of the spray combustion furnace in the form of steam, and the dried salt particles are settled to the bottom of the tower.
Has the advantages that: the treatment method has simple process, on one hand, utilizes the ultrasonic combined stirring technology to promote the dissolution of the salt and improve the dissolution efficiency, and simultaneously utilizes the spray combustion technology to remove organic matters dissolved in the salt solution and simultaneously realize dehydration, thereby finally obtaining the sodium salt meeting the product quality requirement.
Detailed Description
The invention will be better understood from the following examples. However, those skilled in the art will readily appreciate that the description of the embodiments is only for illustrating the present invention and should not be taken as limiting the invention as detailed in the claims.
The method comprises the steps of firstly, fully dissolving soluble components in the waste salt by utilizing an ultrasonic technology to realize high salt recovery rate, then, fully removing insoluble impurities by two-stage filtration, feeding the obtained concentrated brine into a spray combustion furnace, and combusting and decomposing soluble organic matters in the concentrated brine at high temperature to obtain dry sodium salt at the same time.
Example 1
A certain pesticide production enterprise contains high-concentration salt-containing wastewater, and evaporation salt precipitation residues are formed after triple effect evaporation and are light yellow and are treated as hazardous wastes. According to detection, 850-895 g of sodium chloride, 46-95 g of water, 4-12 g of organic matters and other impurities are contained in every 1kg of waste salt slag; the waste salt is treated according to the following steps:
step 1, adding water into a dissolving tank, setting the ultrasonic frequency to be 20kHz, starting an ultrasonic driving power supply, continuously adding waste salt into the water, wherein the adding amount is close to the saturated adding amount of sodium chloride, and fully dissolving the waste salt in the dissolving tank under ultrasonic stirring to obtain crude concentrated salt water;
step 2, performing two-stage filtration on the crude concentrated brine obtained in the step 1, wherein the first stage is common filtration, and removing insoluble substances in the concentrated brine; the second stage is precise filtration, the precise filtration adopts microporous filtration, and fine particles which cannot be removed by common filtration in the brine are sufficiently removed by virtue of the interception effect of a microfiltration membrane to obtain clean strong brine; the detection shows that the mass concentration of sodium chloride in the brine is 22 percent, and the TOC (total organic carbon) is 820 mg/L;
step 3, feeding clean strong brine into an electrically heated spray combustion furnace through a feed liquid atomizer, setting the furnace temperature to be about 750 ℃, feeding hot air into the furnace to keep the oxidation atmosphere in a hearth, continuously heating and decomposing organic matters in drops of the strong brine at the temperature as well as steam, simultaneously continuously oxidizing the organic matters in the oxidation atmosphere, and finally discharging the organic matters out of a furnace body; and the dried liquid drops form salt particles which continuously settle to the bottom of the combustion furnace to obtain a dried sodium chloride product.
Through detection, the obtained product comprises the following components: 99.2 percent of sodium chloride, 0.2 percent of sulfate radical, 0.32 percent of calcium and magnesium, 0.2 percent of water and 0.08 percent of insoluble substances, which meet the quality standard requirements of first-grade industrial dry salt in the Industrial salt (GB/T5462-2015).
Example 2
The waste salt of a chemical industry enterprise is mainly sodium chloride, is light gray, is solidified into a block shape and slightly sticky, and comprises the following components by sampling analysis: 90.1% of sodium chloride, 7.6% of water, 1.05% of organic matters and other impurities; the waste salt is treated according to the following steps:
step 1, adding water into a dissolving tank, setting the ultrasonic frequency to be 30kHz, starting an ultrasonic driving power supply, continuously adding waste salt into the water, wherein the adding amount is close to the saturated adding amount of sodium chloride, and fully dissolving the waste salt in the dissolving tank under ultrasonic stirring to obtain crude concentrated salt water;
step 2, performing two-stage filtration on the crude concentrated brine obtained in the step 1, wherein the first stage is common filtration, and removing insoluble substances in the concentrated brine; the second stage is precise filtration, the precise filtration adopts microporous filtration, and fine particles which cannot be removed by common filtration in the brine are sufficiently removed by virtue of the interception effect of a microfiltration membrane to obtain clean strong brine; through detection, the mass concentration of sodium chloride in the brine is 24 percent, and TOC (total organic carbon) is 6190 mg/L;
step 3, feeding clean strong brine into an electrically heated spray combustion furnace through a feed liquid atomizer, setting the furnace temperature to be about 750 ℃, feeding hot air into the furnace to keep the oxidation atmosphere in a hearth, continuously heating and decomposing organic matters in drops of the strong brine at the temperature as well as steam, simultaneously continuously oxidizing the organic matters in the oxidation atmosphere, and finally discharging the organic matters out of a furnace body; and the dried liquid drops form salt particles which continuously settle to the bottom of the combustion furnace to obtain a dried sodium chloride product.
Through detection, the obtained product comprises the following components: 98.9 percent of sodium chloride, 0.45 percent of sulfate radical, 0.25 percent of calcium and magnesium, 0.34 percent of water and 0.06 percent of insoluble substances, which meet the quality standard requirements of first-grade industrial dry salt in the Industrial salt (GB/T5462-2015).
Example 3
The salt waste of the salting-out and filtering section of a certain fine chemical industry enterprise is mainly sodium sulfate and is offwhite, and the salt waste is sampled and analyzed, and comprises the following components: 86.8% of sodium sulfate, 12.1% of water, 0.86% of organic matters and other impurities; the waste salt is treated according to the following steps:
step 1, adding water into a dissolving tank, setting the ultrasonic frequency to be 30kHz, starting an ultrasonic driving power supply, continuously adding waste salt into the water, wherein the adding amount is close to the saturated adding amount of sodium sulfate, and fully dissolving the waste salt in the dissolving tank under ultrasonic stirring to obtain crude concentrated salt water;
step 2, performing two-stage filtration on the crude concentrated brine obtained in the step 1, wherein the first stage is common filtration, and removing insoluble substances in the concentrated brine; the second stage is precise filtration, the precise filtration adopts microporous filtration, fine particles which cannot be removed by common filtration in the brine are sufficiently removed by means of the interception effect of a microfiltration membrane, and clean strong brine is obtained after two-stage filtration; the detection shows that the mass concentration of sodium sulfate in the brine is 19 percent, and the TOC (total organic carbon) is 2200 mg/L;
step 3, feeding clean strong brine into an electrically heated spray combustion furnace through a feed liquid atomizer, setting the furnace temperature to be about 850 ℃, feeding hot air into the furnace to keep the oxidation atmosphere in a hearth, continuously heating and decomposing organic matters in drops of the strong brine at the temperature as well as steam, simultaneously continuously oxidizing the organic matters in the oxidation atmosphere, and finally discharging the organic matters out of a furnace body; and the dried liquid drops form salt particles which continuously settle to the bottom of the combustion furnace to obtain a dried anhydrous sodium sulfate product.
Through detection, the prepared anhydrous sodium sulfate product comprises the following components: 99.3 percent of sodium sulfate, 0.2 percent of chloride, 0.15 percent of calcium and magnesium, 0.15 percent of water and 0.03 percent of insoluble substances, and the whiteness is 85 percent, thereby meeting the quality standard requirement of class I first-class products in the industrial anhydrous sodium sulfate (GB/T6009-2014).
Compared with the traditional waste salt mechanical stirring and dissolving, the ultrasonic-assisted stirring and dissolving technology is adopted, so that the waste salt can be fully dissolved in water, particularly, the dissolution efficiency of the waste salt containing many organic matters and impurities and high in viscosity is higher, and a crude salt solution close to saturation can be prepared.
Spray burning is carried out to strong brine under the temperature that is less than the salt melting point, can not only make the organic matter pyrolysis and the oxidation of strong brine, the organic matter in the salt brine is got rid of to the high efficiency, still can effectively avoid the waste salt melt bonding phenomenon more than the melting point temperature, has not only improved the sodium salt quality that finally obtains, but also has reduced equipment surface corrosion, leads to the emergence of more serious problems such as equipment damage even.
The product quality of the sodium sulfate and the sodium chloride recovered by the method respectively meets the quality standard requirements of 'industrial anhydrous sodium sulfate' (GB/T6009-2014) and 'industrial salt' (GB/T5462-2015). The method not only can realize the harmless treatment of hazardous wastes such as industrial waste salt taking sodium sulfate or sodium chloride as a main component, but also can prepare anhydrous sodium sulfate or sodium chloride byproducts meeting the product quality standard requirements, effectively solves the problem of treatment of the waste industrial waste salt, and has simple process flow, strong operability, obvious environmental benefit, economic benefit and practical value.
Claims (5)
1. A method for recycling industrial waste salt is characterized in that: the industrial waste salt takes sodium chloride or sodium sulfate as a main component; the industrial waste salt is subjected to resource treatment by the following method, specifically:
step 1, dissolving a certain amount of industrial waste salt in water, and fully dissolving under the combined action of ultrasound and stirring to obtain a nearly saturated salt solution A;
step 2, carrying out two-stage filtration and purification on the salt solution A to remove insoluble impurities in the salt solution A to obtain a salt solution B;
step 3, feeding the salt solution B into a spray combustion furnace, pyrolyzing and oxidizing soluble organic matters in the salt solution B at a temperature lower than the melting point of the salt, and then discharging the organic matters together with water vapor to finally obtain a dried sodium salt product; and (3) carrying out spray incineration on the strong brine at the temperature lower than the melting point of the salt, wherein the heating temperature of a spray combustion furnace is 500-850 ℃.
2. The method for recycling industrial waste salt as claimed in claim 1, wherein: in the step 1, the ultrasonic working frequency is 15-60 kHz when the salt is dissolved.
3. The method for recycling industrial waste salt as claimed in claim 1, wherein: in the step 1, the mass concentration of sodium sulfate in a waste salt solution obtained by fully dissolving waste salt with sodium sulfate as a main component is 15-28%.
4. The method for recycling industrial waste salt as claimed in claim 1, wherein: in the step 1, the mass concentration of sodium chloride in the waste salt solution obtained by fully dissolving the waste salt with sodium chloride as a main component is 20-25%.
5. The method for recycling industrial waste salt as claimed in claim 1, wherein: in the step 2, in the two-stage filtration, the first stage filtration is common filtration, the second stage filtration is precise filtration, and the precise filtration adopts microporous filtration.
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| CN110695059B (en) * | 2019-10-23 | 2022-04-05 | 绍兴市上虞众联环保有限公司 | Industrial organic waste salt treatment process |
| CN110711764A (en) * | 2019-10-29 | 2020-01-21 | 江苏盛勤环境工程有限公司 | Solid waste salt recycling process technology |
| CN110937611B (en) * | 2019-11-01 | 2023-05-23 | 临涣焦化股份有限公司 | System and method for improving purity of secondary salt of desulfurization waste liquid |
| CN111994915A (en) * | 2020-08-28 | 2020-11-27 | 山西华康绿色建材有限公司 | Method and device for producing sodium silicate and sulfuric acid from high-sulfur-content salt |
| CN114660184A (en) * | 2020-12-22 | 2022-06-24 | 沈阳沈化院测试技术有限公司 | Method for evaluating risks of harmlessness and recycling of pesticide waste salt |
| CN114408946B (en) * | 2022-01-20 | 2023-08-15 | 陕西聚泰新材料科技有限公司 | Useless sodium sulfate treatment purification system |
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| CN105712555A (en) * | 2014-12-02 | 2016-06-29 | 中国科学院大连化学物理研究所 | Resource utilization method of high-salinity organic wastewater formed in light stabilizer 944 production |
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