CN110975613A - Regeneration method of sodium-alkali desulfurizing agent - Google Patents
Regeneration method of sodium-alkali desulfurizing agent Download PDFInfo
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/96—Regeneration, reactivation or recycling of reactants
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D—SEPARATION
- B01D2251/00—Reactants
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- B01D2251/304—Alkali metal compounds of sodium
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract
The invention relates to a regeneration method of a sodium-alkali method desulfurizer, which solves the problems that desulfurization residues cannot be recycled and are difficult to treat after domestic sodium-alkali method desulfurization, and can remove Na from the desulfurization residues in sodium-alkali method desulfurization wastewater2SO4The NaOH is converted into NaOH and is reused in a desulfurization system, so that the operation efficiency of the system is improved; the whole system is subjected to acid-base reaction process and Na2SO4Realizing Na-alkali desulphurization slag Na in conversion process and alkali making process2SO4Converting the calcium sulfate into NaOH, wherein the NaOH with the mass concentration of 3.4% can be finally obtained and can be returned to a desulfurization system for desulfurization, and the calcium sulfate with higher purity discharged from the system can be prepared into gypsum products with higher quality to be sold in the market; the invention has the advantages that the industrial waste salt can be recycled, the operation efficiency of enterprises is improved, secondary waste which is difficult to treat is not generated in the regeneration process, a series of problems caused by adopting a landfill mode to treat inorganic salt at the present stage are fundamentally solved, and a new way for treating and disposing the inorganic salt is developed.
Description
Technical Field
The invention relates to a regeneration method of a sodium-alkali desulfurizing agent, which can regenerate desulfurizing slag of the sodium-alkali desulfurizing agent into a desulfurizing agent NaOH and recycle the desulfurizing agent NaOH into a desulfurizing system, improves the desulfurizing efficiency, effectively and reasonably utilizes inorganic salt resources, and belongs to the technical field of environmental protection.
Technical Field
In modern desulfurization processes, SO2Reacts with alkaline substances in the slurry to generate sulfite, and then is converted into sulfate through an oxidation process. Most of the conventional wet desulphurization methods adopt lime (limestone) slurry as an absorbent, and because the solubility of calcium sulfite and calcium sulfate generated in the lime desulphurization process is very low, the calcium sulfite and the calcium sulfate are easy to oversaturate and crystallize out, new crystal nuclei are attached to the wall of the device to promote the growth of crystals, and finally a thick scale layer is formed on the wall of the device, so that the pipeline is blocked seriously, and the normal operation of the device is influenced.
In order to avoid the phenomenon, a considerable part of domestic enterprises adopt sodium-alkali desulphurization, namely NaOH is used as a desulfurizer to carry out desulphurization, so that the scaling condition is avoided, and the sodium-alkali desulphurization method has the advantage of high absorption efficiency. However, the medicament for desulfurization by the sodium-alkali method has high cost, and the desulfurization product is 60-70% of Na2SO4And Na2SO4The direct economic value of the method is lower, the desulfurization products of a considerable part of domestic small and medium boilers are not recycled, but the desulfurization cost can be reduced if the desulfurization products are recycled. The main component of the desulfurization slag of a certain enterprise in Hubei after desulfurization by a sodium-alkali method is Na2SO4And a small amount of Na2SO3The inorganic salt is always stored in a park, cannot be digested internally and can only be transported and buried externally, the inorganic salt burying mode at the present stage has great problems, and the disposal mode of burying is adopted, so that the potential risks of land resource waste and environment are caused, and meanwhile, the burying cost is largeThe economic burden of enterprises is increased, and the waste of sodium salt resources is caused. Therefore, it is of great significance to develop a treatment technology capable of regenerating sodium sulfate generated after sodium-alkali desulfurization into a desulfurizing agent sodium hydroxide.
Disclosure of Invention
The invention provides Na capable of removing sulfur residue by sodium-alkali method, which has simple process, strong operability and stable process2SO4A processing system and a method for regenerating NaOH.
The invention relates to a regeneration method of a sodium-alkali desulfurizer, which has the technical key points that: the whole method comprises three chemical reaction processes: acid-base reaction Process, Na2SO4A conversion process and an alkali making process;
the first process is as follows: the acid-base reaction process is to add 0.1408 mol CaSO into prepared 100ml dilute sulfuric acid solution3The reaction process is fully stirred in an air-isolated state, when the pH value is approximately equal to 2.3-2.5, the reaction time is set to be 5 min-30 min, and a reaction product Ca (HSO) is obtained3)2With CaSO4The excessive high acid concentration at the beginning of the reaction causes the Ca (HSO) as the target product3)2Further reaction with sulfuric acid produces SO2SO to be generated2Trapped and reused in the system and CaSO not participating in the reaction3Further reaction; the reaction process needs to be air-insulated to avoid oxidation.
And a second process: said Na2SO4During the conversion, 0.06617 mol of Na2SO4Adding Ca (HSO) generated by the above process3)2Fully stirring the solution at normal temperature for 10-30 min to obtain the sodium bisulfite yield, wherein NaHSO is generated3The process of (2) is carried out in an air-isolated state; the process is used to generate CaSO4A discharge system with a content of 0.066 mol; the reaction process needs to be air-insulated to avoid oxidation.
The third process: the alkali making process is NaHSO generated in the process3Adding an equimolar amount of Ca (OH)2Stirring at room temperature, wherein the reaction temperature is room temperatureWherein the investigation time range is 0.5-24 h, the temperature range is 20-80 ℃, and NaOH is generated at the moment; the process is used to generate CaSO3And collecting and reusing the obtained product in the first process as raw material supplement, and finally returning NaOH with the mass concentration of 3.4 percent as a desulfurizing agent to a desulfurization system for desulfurization, namely finishing the regeneration process.
The mechanism is as follows: the first process is as follows: in the acid-base reaction process, dilute sulfuric acid with a certain concentration and analytically pure calcium sulfite powder are prepared to react to generate a target product Ca (HSO)3)2. The process is an acid-base reaction process, two reactants can be quantitatively added, and the addition amount of the two reactants can be judged and regulated by monitoring the PH. Due to the dilute sulfuric acid and CaSO3In the reaction process, the target product Ca (HSO) caused by too high concentration of the initial acid solution of the reaction exists3)2Further reaction with sulfuric acid produces SO2And CaSO4This results in part of the reactant CaSO3Does not participate in the reaction, and can lead the by-product SO2Collect and recycle the CaSO with the rest in the system3The reaction continues to improve system efficiency. Finally, the CaSO generated by the process4The precipitate is discharged and recovered as
The reaction equation is: 2CaSO3+H2SO4→Ca(HSO3)2+ CaSO4
The side reaction equation is: ca (HSO)3)2+H2SO4→CaSO4+ 2SO2+2H2O
And a second process: HSO3 -The exchange reaction process is to the sodium-alkali desulphurization slag Na2SO4The sodium-alkali desulfurization waste residue Na is obtained2SO4Ca (HSO) as a target product of Process one3)2Mixing and reacting, wherein the reaction is a precipitation reaction, and the CaSO generated is4Filtering and discharging, wherein the target product is NaHSO3The reaction equation is:
Ca(HSO3)2+ Na2SO4→2NaHSO3+CaSO4↓
said HSO3 -The exchange reaction of (A) is to Ca (HSO) produced in the first process3)2Sodium-alkali method for adding Na into solution to remove sulfur residue Na2SO4Ca in the solution after the two are fully mixed2+With SO4 2-The ion concentration product of (A) exceeds CaSO4The reaction is promoted by the precipitation generated by the solubility product of the reaction, thereby obtaining the target product NaHSO3And measuring the reaction conversion rate, and introducing the filtered solution into a device of the third process to carry out the sodium hydroxide regeneration process.
The third process: preparing alkali, and preparing target product NaHSO3Adding an equimolar amount of Ca (OH)2The reaction is a precipitation reaction which can generate NaOH and CaSO3Precipitating, filtering the precipitate to obtain a sodium hydroxide solution, namely completing the regeneration process. In which CaSO is generated3The precipitate is recycled to the first process as a raw material supplement, and the reaction equation is as follows:
NaHSO3+ Ca(OH)2→NaOH+CaSO3↓+H2O
the alkali-making reaction is NaHSO obtained in the second step3Adding powdered calcium hydroxide into the solution, and fully mixing the calcium hydroxide and the sodium bisulfite under the condition of isolating oxygen to generate CaSO (calcium sulfite)3The precipitation promotes the chemical reaction to generate the sodium hydroxide, and the alkali preparation process, namely the process of regenerating the sodium hydroxide, is completed.
The invention is further illustrated by the following examples and figures.
Drawings
FIG. 1 is a process flow diagram of a regeneration method of a sodium-alkali desulfurizer of the present invention;
FIG. 2 is a block diagram of the process flow for carrying out laboratory pilot experiments in accordance with the present invention, with the consumption and production of important substances.
Detailed Description
A regeneration system of sodium-alkali desulfurizing agent includes three chemical reaction processes, i.e. acid-alkali reaction process and HSO3 -By exchange reaction ofAnd alkali preparation process.
According to the regeneration method of the sodium-alkali desulfurizer, the acid-base reaction process is that the dilute sulfuric acid solution prepared in a laboratory and the analytically pure calcium sulfite powder are used for carrying out chemical reaction, but the industrial waste acid and the waste residue calcium sulfite generated after desulfurization are not excluded from mutual reaction, and the same result can be obtained, so that the operation cost of the system can be obviously reduced.
The acid-base reaction process comprises the steps of preparing sulfuric acid to a certain concentration or pH value at normal temperature, adding powdered calcium sulfite into the sulfuric acid, adjusting the pH value to be 2.3-2.5, and reacting for 10min to obtain a target product Ca (HSO)3)2The content reaches a maximum value, whereby the next reaction stage is carried out. This process prolongs the reaction time for Ca (HSO)3)2The yield is not beneficial. The reaction process needs to be air-insulated to avoid oxidation.
Said Na2SO4The conversion process is to desulfurize the waste residue Na by a sodium-alkali method2SO4Reaction with acid and alkali to obtain Ca (HSO) as target product3)2Replacement of bisulfite proceeds, and Ca (HSO) can be converted to3)2The bisulfite in (1) is replaced into sodium sulfate to generate NaHSO3。
Said Na2SO4In the conversion process, the reaction can be carried out at normal temperature, the conversion rate can be optimal after the reaction is carried out for 10-30 min, and the reaction time is prolonged to be useless for increasing the conversion rate. Due to HSO3 -The oxidation rate is higher in the air, and the reaction needs to be isolated from oxygen so as to avoid the negative influence of the oxidation on the experimental result.
The process for preparing the alkali, which is referred to as the process for preparing NaOH, is characterized in that the process II, Na is performed at normal temperature2SO4Adding Ca (OH) into the sodium bisulfite solution of the target product of the conversion process2Powder, when reacting for 6 h, the yield of NaOH reaches a better level, and if the reaction time is continued to be prolonged, the yield of NaOH does not increase significantly.
The alkali preparation process can be used for preparing CaSO generated in the process3Is collected and recycledAnd in the first process, the generated NaOH solution is used as a desulfurizer to supplement the original desulfurization system for desulfurization, so that the operation efficiency of the original desulfurization system is improved.
Example (b):
1. the acid-base reaction process is that a certain amount of calcium sulfite solid powder is added into dilute sulfuric acid, and when the pH value is approximately equal to 2.3-2.5, the target product Ca (HSO)3)2The content reaches a maximum at which the reaction product Ca (HSO) is obtained3)2With CaSO4The reaction process is an acid-base reaction process, and the process is implemented as follows:
0.1408 mol of CaSO is added into prepared 100mL of dilute sulfuric acid solution3The reaction process is fully stirred under the condition of air isolation, and the target product Ca (HSO) is caused due to the over-high acid liquid concentration at the beginning of the reaction3)2Further reaction with sulfuric acid produces SO2SO to be generated2Trapped and reused in the system and CaSO not participating in the reaction3And (4) further reacting.
Different reaction times of 5 min, 10min, 20min and 30 min are examined for the target product Ca (HSO)3)2The influence of yield finally determines that the target product Ca (HSO) is generated when the reaction time is 10min3)2With maximum yield, Ca (HSO) is produced3)20.06617 mol in total, yield 94.0%, CaSO produced by this process40.0746 mol in total, some Ca (HSO) still remained3)2Is oxidized.
In the invention, SO2Collected and reused in the system to react with the CaSO not participating in the reaction3Reabsorption is performed to increase Ca (HSO)3)2The generation rate of the system is improved, and the operation efficiency of the whole system is improved. The product solid CaSO4Discharge system, Ca (HSO)3)2The solution enters the next process for reaction. The reaction is rapid and stable in the process, Ca (HSO)3)2The yield is stable.
2. Said HSO3 -The exchange reaction process is to remove Na from the desulfurization waste residue produced by enterprises2SO4Introduced into the system, and the above processProduct Ca (HSO)3)2The solution is reacted, the process being carried out as follows:
0.06617 mol of Na2SO4Adding Ca (HSO) generated by the above process3)2Fully stirring the solution at normal temperature, carrying out the process in an air-isolated state, investigating the influence of different reaction time on the yield of the sodium bisulfite, and finally determining that the yield of the sodium bisulfite reaches the maximum when the reaction is carried out for 20min, wherein NaHSO is generated at the moment3The total amount was 0.132 mol, and the yield was 99.8%. The reaction time is prolonged, and the yield is not increased.
The process is used to generate CaSO4The content of the product was 0.066 mol.
3. The alkali making process is NaHSO generated in the process3Adding an equimolar amount of Ca (OH)2In the process, stirring is applied at normal temperature, and the influence of different reaction time and temperature on the yield of the sodium hydroxide is examined, wherein the examination time range is 0.5-24 h, and the temperature range is 20-80 ℃. Finally, the reaction temperature is determined to be room temperature, and in combination with economic factors, when the reaction time is 6 hours, the conversion rate is better, and 0.0853 mol is generated in total, and the yield is 64.6%. The reaction time is prolonged, and the yield of the sodium hydroxide is not increased obviously.
The process is used to generate CaSO3And collecting and reusing the mixture in the first process as raw material supplement, and returning NaOH as a desulfurizing agent to a desulfurization system for desulfurization again to finish the regeneration process. Through the verification of the small test process, the reaction effective conversion rates of the three processes respectively reach 94%, 99.8% and 64.6%, the finally obtained NaOH with the mass concentration of 3.4% can be returned to the desulfurization system for desulfurization, and the calcium sulfate with higher purity discharged from the system can be prepared into gypsum products with higher quality to be sold in the market.
The embodiments described above are intended to enable those skilled in the art to fully understand and effectively use the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-mentioned embodiments, and modifications made by those skilled in the art according to the teachings of the present invention without departing from the scope of the present invention should be within the protection scope of the present invention.
Claims (4)
1. A regeneration method of a sodium-alkali desulfurizer is characterized by comprising the following steps: the whole method comprises three chemical reaction processes: acid-base reaction Process, Na2SO4A conversion process and an alkali making process;
the first process is as follows: the acid-base reaction process is to add 0.1408 mol CaSO into prepared 100ml dilute sulfuric acid solution3The reaction process is fully stirred in an air-isolated state, when the pH value is approximately equal to 2.3-2.5, the reaction time is set to be 5 min-30 min, and a reaction product Ca (HSO) is obtained3)2With CaSO4The excessive high acid concentration at the beginning of the reaction causes the Ca (HSO) as the target product3)2Further reaction with sulfuric acid produces SO2SO to be generated2Trapped and reused in the system and CaSO not participating in the reaction3Further reaction; the reaction process needs to be isolated from air to avoid oxidation;
and a second process: said Na2SO4During the conversion, 0.06617 mol of Na2SO4Adding Ca (HSO) generated by the above process3)2Fully stirring the solution at normal temperature for 10-30 min to obtain the sodium bisulfite yield, wherein NaHSO is generated3The process of (2) is carried out in an air-isolated state; the process is used to generate CaSO4A discharge system with a content of 0.066 mol; the reaction process needs to be isolated from air to avoid oxidation;
the third process: the alkali making process is NaHSO generated in the process3Adding an equimolar amount of Ca (OH)2Stirring at room temperature in the process, wherein the reaction temperature is room temperature, the investigation time range is 0.5-24 h, the temperature range is 20-80 ℃, and NaOH is generated at the moment; the process is used to generate CaSO3Collecting and reusing the NaOH as a raw material supplement in the first process, and finally obtaining NaOH with the mass concentration of 3.4 percent as a desulfurizing agent to be returned to the desulfurizing system again for feedingAnd desulfurizing, namely completing the regeneration process.
2. The regeneration method of the sodium alkali method desulfurizing agent according to claim 1, characterized in that: setting the reaction time in the first process as 10min, and obtaining the target product Ca (HSO)3)2The content reaches a maximum.
3. The regeneration method of the sodium alkali method desulfurizing agent according to claim 1, characterized in that: when the reaction time in the second process is 20min, the yield of the sodium bisulfite reaches the maximum, and NaHSO is generated at the moment3The total amount was 0.132 mol, and the yield was 99.8%.
4. The regeneration method of the sodium alkali method desulfurizing agent according to claim 1, characterized in that: in the third process, when the reaction time is 6 h, the conversion rate is better, and the NaOH is generated to 0.0853 mol in total, and the yield is 64.6%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111701419A (en) * | 2020-06-16 | 2020-09-25 | 山西京耘环保科技有限公司 | Sodium-alkali dry-method desulfurized fly ash recycling method |
| CN112919503A (en) * | 2021-02-23 | 2021-06-08 | 攀枝花市蓝鼎环保科技有限公司 | Zero-discharge process for desulfurization wastewater and desulfurization slag |
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