CN111870862A - Harmless treatment method for waste salt in production of alkylxanthate beneficiation reagent - Google Patents
Harmless treatment method for waste salt in production of alkylxanthate beneficiation reagent Download PDFInfo
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- CN111870862A CN111870862A CN202010743704.3A CN202010743704A CN111870862A CN 111870862 A CN111870862 A CN 111870862A CN 202010743704 A CN202010743704 A CN 202010743704A CN 111870862 A CN111870862 A CN 111870862A
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- A—HUMAN NECESSITIES
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- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/38—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by oxidation; by combustion
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- C07C329/12—Dithiocarbonic acids; Derivatives thereof
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- C07C329/16—Esters of dithiocarbonic acids having sulfur atoms of dithiocarbonic groups bound to acyclic carbon atoms
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
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- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
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Abstract
The invention belongs to the technical field of industrial waste salt treatment methods, and particularly relates to a harmless treatment method for waste salt produced by an alkyl xanthate beneficiation reagent. The method has the advantages of simple and easy operation process, mild reaction conditions and low treatment cost, the treated salt can be used as a production raw material of the ionic membrane caustic soda and the soda ash, certain economic benefit is realized, the generated wastewater can be reused for dissolving the oxidant, and no new wastewater is generated.
Description
Technical Field
The invention belongs to the technical field of industrial waste salt treatment methods, and particularly relates to a harmless treatment method for waste salt produced by an alkyl xanthate beneficiation reagent.
Background
Along with the stricter environmental protection policy in China, mine enterprises put forward higher requirements on the product performances of the beneficiation reagent, such as green, low toxicity, low residue and the like. The alkyl xanthate is a novel ester environment-friendly beneficiation reagent, is mainly used for flotation separation of nonferrous metal sulfide ores, particularly has outstanding selection indexes in the flotation application of copper-molybdenum sulfide ores, and has the outstanding advantages of high selectivity, low toxicity, low residue, low pollution and the like.
But the high-salinity wastewater generated in the synthesis of the chemical agent is difficult to carry out harmless treatment. The waste water contains a small amount of pungent odor by-products and alkyl xanthate, and the pungent odor by-products and the alkyl xanthate remain in solid salt removed after the waste water is distilled by a triple-effect evaporator, so that the salt becomes dangerous waste. Brings great problems for subsequent environmental protection treatment: firstly, strong pungent smell exists in the salt; secondly, a small amount of alkyl xanthate exists in the salt.
Disclosure of Invention
In order to solve the technical problems, the invention provides a harmless treatment method for waste salt in the production of an alkyl xanthate beneficiation reagent.
The invention is realized in such a way, and provides a harmless treatment method for waste salt produced by an alkyl xanthate beneficiation reagent, which is used for oxidizing and refining the waste salt produced by the alkyl xanthate beneficiation reagent, namely:
under the heating condition, dissolving the waste salt produced by the alkylxanthate beneficiation reagent in an aqueous solution of an oxidant, adding an oxidation auxiliary agent, oxidizing the waste salt produced by the alkylxanthate beneficiation reagent by the oxidant and the oxidation auxiliary agent, adding diatomite to form a membrane, filtering, passing through an automatic filter, adsorbing the filtrate by active carbon, concentrating, cooling, crystallizing and centrifuging to obtain refined salt.
Preferably, the method specifically comprises the following steps:
1) preparing an oxidant aqueous solution;
2) adding waste salt produced by alkyl xanthate beneficiation reagent into the oxidant aqueous solution in the step 1), heating to 40-120 ℃, and stirring until the waste salt is completely dissolved to prepare saturated brine;
3) adding an oxidation auxiliary agent into the saturated saline water obtained in the step 2), and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a heat-insulating mixing kettle, and adding a certain mass of diatomite into the liquid under a stirring state for mixing;
5) introducing the mixed material obtained in the step 4) into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a triple-effect evaporator for concentration;
7) introducing the concentrated solution into a crystallization kettle for cooling crystallization;
8) introducing the crystallized mixed solution into a centrifugal machine under a stirring state for centrifugal separation to obtain refined salt;
9) standing the liquid obtained after centrifugal separation, recovering xanthate and carbon disulfide, and reusing the remaining liquid in the preparation of the aqueous oxidant solution in the step 1) without water treatment.
More preferably, in step 1), the concentration of the aqueous oxidizing agent solution is 1 to 5%.
Preferably, in step 1), the oxidizing agent is a strong oxidizing agent, and is one of chlorine dioxide, potassium permanganate, potassium hypochlorite, sodium hypochlorite and hydrogen peroxide.
More preferably, in step 3), the oxidation assistant is one of hydrochloric acid, phosphoric acid and sulfuric acid.
More preferably, the concentrations of hydrochloric acid, phosphoric acid and sulfuric acid are all 10-15%.
More preferably, the addition amount of the oxidation assistant is 1 to 3% by mol based on the oxidant.
Further preferably, in the step 4), the mass of the diatomite is 20-100 kg, and the particle size is 100-300 meshes.
Further preferably, in the step 8), the obtained refined salt is used as a production raw material of the ionic membrane caustic soda and the sodium carbonate.
Compared with the prior art, the invention has the advantages that:
the method has the advantages that the waste salt produced by the alkyl xanthate beneficiation reagent is subjected to environment-friendly treatment, the process flow is simple and easy to operate, the reaction conditions are mild, the treatment cost is low, the treated salt can be used as a production raw material of ionic membrane caustic soda and soda ash, certain economic benefits are realized, the generated wastewater can be reused for dissolving an oxidant, and no new wastewater is generated.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Referring to fig. 1, in order to perform harmless treatment on waste salt produced by an alkylxanthate beneficiation reagent, the invention provides a treatment method, wherein under a heating condition, the waste salt produced by the alkylxanthate beneficiation reagent is dissolved in an aqueous solution of an oxidant, an oxidation assistant is added, the waste salt produced by the alkylxanthate beneficiation reagent is oxidized by the oxidant and the oxidation assistant, then diatomite is added for film formation and filtration, and then an automatic filter is used, filtrate is subjected to active carbon adsorption, concentration, cooling, crystallization and centrifugation to obtain refined salt, and the method is characterized in that:
1. the invention relates to a harmless treatment process of waste salt in the production of an alkyl xanthate beneficiation reagent, which is characterized in that a strong oxidant is applied for oxidation;
2. the key point of the invention is that the oxidation auxiliary agent is used for catalytic reaction;
3. the key point of the invention is that diatomite is used for auxiliary filtration;
4. the obtained refined salt can be compatible with the ionic membrane salt and used as a raw material of the ionic membrane caustic soda, and magnesium and calcium are not introduced in the whole production process, so that magnesium and calcium are not required to be removed.
Examples 1,
1) Preparing 1800 kilograms of 1 percent chlorine dioxide aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 15% hydrochloric acid of an oxidation assistant into the step 2) under the stirring state, wherein the adding amount is about 1-3% of the molar mass of the chlorine dioxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recovering the upper organic phase obtained in the step 9), and then merging the recovered upper organic phase into a xanthate product, wherein the recovered lower organic phase can be used for reproducing alkyl xanthate, and the water phase in the middle layer is used for preparing a chlorine dioxide aqueous solution;
11) the salt obtained after centrifugal separation is used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 2,
1) Preparing 1800 kilograms of 2 percent hydrogen peroxide solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 14% hydrochloric acid of an oxidation auxiliary agent into the step 2) in a stirring state, wherein the adding amount is 1-3% of the molar mass of the hydrogen peroxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recovering the upper organic phase obtained in the step 9), and then merging the recovered upper organic phase into a xanthate product, wherein the recovered lower organic phase can be used for reproducing alkyl xanthate, and the water phase in the middle layer is used for preparing a hydrogen peroxide solution;
11) the salt obtained after centrifugal separation is used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 3,
1) Preparing 1800 kilograms of 3 percent sodium hypochlorite aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 13% hydrochloric acid serving as an oxidation auxiliary agent into the step 2) in a stirring state, wherein the addition amount is 1-3% of the molar mass of the sodium hypochlorite, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recovering the upper organic phase obtained in the step 9), and then merging the recovered upper organic phase into a xanthate product, recovering the lower organic phase, and then recycling the lower organic phase to produce alkyl xanthate, wherein the water phase in the middle layer is used for preparing a sodium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 4,
1) 1800 kilograms of 4 percent potassium hypochlorite aqueous solution is prepared in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 12% hydrochloric acid of an oxidation assistant into the step 2) under stirring, wherein the adding amount is about 1-3% of the molar mass of the potassium hypochlorite, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing a potassium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 5,
1) Preparing 1800 kilograms of 5 percent potassium permanganate aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 11% hydrochloric acid serving as an oxidation assistant into the step 2) in a stirring state, wherein the addition amount is about 1-3% of the molar mass of the potassium permanganate, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) and (3) recovering the upper organic phase obtained in the step (9) and then merging the recovered upper organic phase into a xanthate product, and recovering the lower organic phase to be used for reproducing alkyl xanthates. The water phase of the middle layer is used for preparing a potassium permanganate aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 6,
1) Preparing 1800 kilograms of 5 percent chlorine dioxide aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 10% of phosphoric acid which is used as an oxidation auxiliary agent into the step 2) in a stirring state, wherein the adding amount is about 1-3% of the molar mass of the chlorine dioxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase in the middle layer is used for preparing chlorine dioxide water solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Example 7,
1) Preparing 1800 kilograms of 1 percent hydrogen peroxide solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 15% of phosphoric acid serving as an oxidation auxiliary agent into the step 2) in a stirring state, wherein the adding amount is about 1-3% of the molar mass of the hydrogen peroxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing hydrogen peroxide solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Example 8,
1) Preparing 1800 kilograms of 2 percent sodium hypochlorite aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 14% of phosphoric acid serving as an oxidation assistant into the step 2) in a stirring state, wherein the addition amount is about 1-3% of the molar mass of the sodium hypochlorite, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing sodium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 9,
1) 1800 kilograms of 3 percent potassium hypochlorite aqueous solution is prepared in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 13 percent of phosphoric acid as an oxidation assistant into the mixture 2) under the stirring state, wherein the adding amount is about 1 to 3 percent of the molar mass of the potassium hypochlorite, and stirring for 30 to 150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) and (3) recovering the upper organic phase obtained in the step (9) and then merging the recovered upper organic phase into a xanthate product, and recovering the lower organic phase to be used for reproducing alkyl xanthates. The water phase of the middle layer is used for preparing a potassium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 10,
1) Preparing 1800 kilograms of 4 percent potassium permanganate aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 12 percent of phosphoric acid as an oxidation assistant into the step 2) under the stirring state, wherein the adding amount is about 1 to 3 percent of the molar mass of the potassium permanganate, and stirring for 30 to 150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing a potassium permanganate aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 11,
1) Preparing 1800 kilograms of 5 percent chlorine dioxide aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 11% sulfuric acid as an oxidation assistant into the step 2) in a stirring state, wherein the addition amount is about 1-3% of the molar mass of the chlorine dioxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase in the middle layer is used for preparing chlorine dioxide water solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 12,
1) Preparing 1800 kilograms of 1 percent hydrogen peroxide solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 10% sulfuric acid of an oxidation auxiliary agent into the step 2) under the stirring state, wherein the adding amount is about 1-3% of the molar mass of the hydrogen peroxide, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing hydrogen peroxide solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 13,
1) Preparing 1800 kilograms of 1 percent sodium hypochlorite aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 40-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 15% sulfuric acid as an oxidation assistant into the step 2) in a stirring state, wherein the addition amount is about 1-3% of the molar mass of the sodium hypochlorite, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing sodium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 14,
1) 1800 kilograms of 2 percent potassium hypochlorite aqueous solution is prepared in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the mixture obtained in the step 1), heating the mixture to 50-90 ℃, and stirring the mixture until the mixture is completely dissolved to prepare saturated brine;
3) slowly dripping 14% sulfuric acid as an oxidation assistant into the mixture in the step 2) under stirring, wherein the addition amount of the sulfuric acid is about 1-3% of the molar mass of the potassium hypochlorite, and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing a potassium hypochlorite aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
Examples 15,
1) Preparing 1800 kilograms of 3 percent potassium permanganate aqueous solution in a reaction kettle;
2) adding 700Kg of waste alkyl xanthate salt into the step 1), heating to 50-90 ℃, and stirring until the waste alkyl xanthate salt is completely dissolved to prepare saturated brine;
3) slowly dripping 13 percent sulfuric acid serving as an oxidation auxiliary agent into the step 2) in a stirring state, wherein the addition amount is about 1 to 3 percent of the molar mass of the potassium permanganate, and stirring for 30 to 150 minutes;
4) pumping the liquid obtained in the step 3) into a mixing kettle with a jacket for heat preservation, and adding 20-100 kg of 100-mesh and 300-mesh diatomite into the liquid for mixing under a stirring state;
5) introducing the mixed materials into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a three-effect evaporator for concentration;
7) cooling the concentrated solution to below 20 ℃ for cooling crystallization;
8) introducing the mixed solution after crystallization into a centrifuge for centrifugal separation under a stirring state;
9) standing the liquid obtained after centrifugal separation for more than three days, and separating out an upper organic phase and a lower organic phase;
10) recycling the upper organic phase obtained in the step 9) and then merging the organic phase into a xanthate product, and recycling the lower organic phase and then using the organic phase for reproducing alkylxanthates. The water phase of the middle layer is used for preparing a potassium permanganate aqueous solution;
11) the salt obtained after centrifugal separation can be used as a production raw material of ion membrane caustic soda and soda ash;
12) repeating the steps 1) to 9), reducing the amount of the waste salt added in the step 2) to 350 kg, and circulating.
The results of the examination of the alkyl xanthate waste salts before and after the treatment of examples 1 to 5 show in the following tables, and it can be seen from the results that no xanthate leaching or sodium xanthate leaching was detected in the treated salts by the method of the present invention, and the appearance changed from orange before the treatment, pungent odor to white, tasteless, demonstrating the effectiveness of the method provided by the present invention.
Claims (9)
1. The harmless treatment method of the waste salt produced by the alkyl xanthate beneficiation reagent is characterized in that the waste salt produced by the alkyl xanthate beneficiation reagent is oxidized and refined, namely:
under the heating condition, dissolving the waste salt produced by the alkylxanthate beneficiation reagent in an aqueous solution of an oxidant, adding an oxidation auxiliary agent, oxidizing the waste salt produced by the alkylxanthate beneficiation reagent by the oxidant and the oxidation auxiliary agent, adding diatomite to form a membrane, filtering, passing through an automatic filter, adsorbing the filtrate by active carbon, concentrating, cooling, crystallizing and centrifuging to obtain refined salt.
2. The method for the innocent treatment of the waste salt in the production of the alkylxanthates beneficiation reagent according to claim 1, which is characterized by comprising the following steps:
1) preparing an oxidant aqueous solution;
2) adding waste salt produced by alkyl xanthate beneficiation reagent into the oxidant aqueous solution in the step 1), heating to 40-120 ℃, and stirring until the waste salt is completely dissolved to prepare saturated brine;
3) adding an oxidation auxiliary agent into the saturated saline water obtained in the step 2), and stirring for 30-150 minutes;
4) pumping the liquid obtained in the step 3) into a heat-insulating mixing kettle, and adding a certain mass of diatomite into the liquid under a stirring state for mixing;
5) introducing the mixed material obtained in the step 4) into an automatic filter for filtering;
6) adsorbing the filtered filtrate by active carbon, and pumping into a triple-effect evaporator for concentration;
7) introducing the concentrated solution into a crystallization kettle for cooling crystallization;
8) introducing the crystallized mixed solution into a centrifugal machine under a stirring state for centrifugal separation to obtain refined salt;
9) standing the liquid obtained after centrifugal separation, recovering xanthate and carbon disulfide, and reusing the remaining liquid in the preparation of the aqueous oxidant solution in the step 1) without water treatment.
3. The method for harmlessly treating the waste salt generated in the production of the alkylxanthate beneficiation reagent according to claim 2, wherein in the step 1), the concentration of the aqueous oxidant solution is 1 to 5%.
4. The method for harmlessly treating the waste salt generated in the production of the alkylxanthate beneficiation reagent according to claim 2, wherein in the step 1), the oxidizing agent is a strong oxidizing agent selected from chlorine dioxide, potassium permanganate, potassium hypochlorite, sodium hypochlorite and hydrogen peroxide.
5. The method for harmlessly treating the waste salt generated in the production of the alkylxanthate beneficiation reagent according to claim 2, wherein in the step 3), the oxidation auxiliary agent is one of hydrochloric acid, phosphoric acid and sulfuric acid.
6. The method for the innocent treatment of the waste salt generated in the production of the alkylxanthate beneficiation reagent according to claim 5, wherein the concentrations of the hydrochloric acid, the phosphoric acid and the sulfuric acid are all 10 to 15 percent.
7. The method for harmlessly treating the waste salt generated in the production of the alkylxanthate beneficiation reagent according to claim 2, wherein the addition amount of the oxidation auxiliary agent is 1 to 3% by mol based on the oxidant.
8. The method for the innocent treatment of the waste salt generated in the production of the alkylxanthate beneficiation reagent as claimed in claim 2, wherein in the step 4), the diatomite has a mass of 20-100 kg and a particle size of 100-300 meshes.
9. The method for harmless treatment of waste salt from alkylxanthate beneficiation reagent production according to claim 2, wherein in step 8), the obtained refined salt is used as a raw material for production of ionic membrane caustic soda and soda ash.
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