CN113979463A - Comprehensive utilization method of sodium bicarbonate desulfurization by-products and soda plant waste liquid - Google Patents
Comprehensive utilization method of sodium bicarbonate desulfurization by-products and soda plant waste liquid Download PDFInfo
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Abstract
The invention relates to the technical field of soda ash production, in particular to a comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda ash plant waste liquid, which comprises the following steps: (1) sequentially adding tap water and sulfuric acid into the reaction kettle for stirring and heating, adding a desulfurization byproduct, stirring and mixing, carrying out heat preservation reaction, filtering the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use; (2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use; (3) and (3) adding the filtrate reserved in the step (1) and the waste clear liquid collected in the step (2) into another reaction kettle, stirring and mixing, filtering the reacted feed liquid after the reaction of the feed liquid is finished, and respectively collecting a liquid phase and a solid phase. The method realizes the recycling of the sodium bicarbonate desulfurization by-products and the waste liquid of the soda plant, avoids resource waste and brings economic benefits.
Description
Technical Field
The invention relates to the technical field of soda ash production, in particular to a comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda ash plant waste liquid.
Background
The treatment of industrial flue gas mainly comprises two processes of wet desulphurization and dry desulphurization. The wet desulphurization process represented by calcium desulphurization is long in implementation time, and is mainly applied to the field with high sulfur content in tail gas such as thermoelectricity at present. In recent years, sodium-based dry desulphurization (SDS) using baking soda as an absorbent is distinguished from a plurality of dry desulphurization processes by virtue of unique advantages, and is increasingly widely applied to industries (such as glass, steel and the like) with relatively low tail gas sulfur content.
The SDS dry desulphurization technology is from Solvay company, is widely applied in developed areas of Europe, America and the like, has the advantages of mature technology, stable and reliable operation, simple operation and maintenance, full dry treatment, no waste water generation, small occupied area, high desulphurization efficiency (up to more than 95 percent), high flexibility and the like, can meet stricter emission indexes, is applied to steel, coking and glass enterprises at present in China, is popularized to the industries of cement, waste incineration and the like, and has wide application prospect. With the popularization of baking soda in the desulfurization industry, the byproduct yield of baking soda desulfurization is gradually increased. The main treatment modes of the desulfurization byproducts of the baking soda at present are as follows: some glass enterprises can recycle cleaner glass for producing colored glass; most of desulfurization byproducts (such as steel and iron and coking industries) are grey black and have high impurity content, and most of the desulfurization byproducts can be used for producing individual-grade cement and can be stored as solid wastes in a stockpiling mode, so that resources are wasted, and the occupied site is easy to cause secondary pollution.
At present, a large amount of waste liquid is generated in the process of producing the calcined soda by adopting an ammonia-soda process, the discharge amount of the waste liquid is influenced by the production process, and about 9m of the waste liquid is discharged every 1t of the calcined soda is basically produced3The disposal of waste liquid is always a worldwide problem and is also one of the bottlenecks limiting the development of ammonia-soda enterprises. Therefore, how to comprehensively utilize the desulfurization by-products and the waste liquid is the research focus of the invention.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: aiming at the defects of the prior art, the method for comprehensively utilizing the sodium bicarbonate desulfurization by-products and the soda plant waste liquid is provided, the sodium bicarbonate desulfurization by-products and the soda plant waste liquid are recycled by utilizing the method, the resource waste is avoided, and meanwhile, the economic benefit is brought.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) sequentially adding tap water and sulfuric acid into the reaction kettle for stirring and heating, adding a desulfurization byproduct, maintaining the same stirring speed, continuously stirring and mixing, carrying out heat preservation reaction, filtering the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate reserved in the step (1) into another reaction kettle, stirring and heating, adding the waste clear liquid collected in the step (2), keeping the same stirring speed, continuously stirring and mixing, carrying out heat preservation reaction, filtering the reacted feed liquid after the reaction of the feed liquid is finished, respectively collecting a liquid phase and a solid phase, washing and filtering the collected solid phase, and obtaining the solid, namely the dihydrate gypsum.
As an improved technical scheme, the molar ratio of the total alkali amount (calculated by sodium bicarbonate) in the sulfuric acid and the desulfurization by-products in the step (1) is 1: 1.9-2.1.
As an improved technical proposal, the adding amount of the desulphurization by-product in the step (1) is 2.5m per time3650kg of tap water was added.
As an improved technical scheme, the total alkalinity (calculated by sodium bicarbonate) of the desulphurization by-product in the step (1) is 0.8 wt% -52 wt%, and the content of sodium sulfate in the desulphurization by-product is 47 wt% -88.57 wt%.
As an improved technical scheme, the temperature for heat preservation reaction in the step (1) is 30-35 ℃, the time for stirring and mixing is 15-30min, and the stirring speed is 85-100 rpm.
As an improved technical scheme, the sulfuric acid in the step (1) is outsourced sulfuric acid or 75-85 wt% sulfuric acid recovered by a chlor-alkali plant.
As an improved technical proposal, Ca in the waste clear liquid in the step (2)2+And SO in the filtrate4 2+In a molar ratio of 0.8-1.5: 1.
As an improved technical scheme, the temperature for heat preservation reaction in the step (2) is 50-60 ℃, the time for stirring and mixing is 10-60min, and the stirring speed is 90-109 rpm.
As an improved technical scheme, the waste clear liquid in the step (2) is added into the reaction kettle within 10-30 min.
As an improved technical scheme, the liquid phase collected in the step (3) is used as salt dissolving water for producing the calcined soda.
After the technical scheme is adopted, the invention has the beneficial effects that:
by adopting the comprehensive utilization method, the desulphurization by-product, the soda plant waste liquid and the chlor-alkali plant waste sulfuric acid are comprehensively utilized, the pollution to the environment and the treatment cost of enterprises on the waste liquid, the desulphurization by-product and the waste sulfuric acid are reduced, the waste liquid and the desulphurization by-product are subjected to reaction and process optimization to obtain an ideal dihydrate gypsum product, and the economic benefit is increased for the enterprises. The liquid phase recycling can effectively reduce the consumption of the raw salt produced by the sodium carbonate, and the filtrate also contains lower content of calcium and magnesium ions, so that the use amount of lime milk and the sodium carbonate in the process of refining the salt water can be effectively reduced when the filtrate is used for producing the salt by the sodium carbonate, and the production cost of the sodium carbonate is reduced.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) 2.5m3Adding tap water and 3.37kg of sulfuric acid (80 wt% sulfuric acid recovered from chlor-alkali production) into a reaction kettle in sequence for stirring (the stirring speed is 85rpm) and heating (heating is carried out by using hot water at 60 ℃ in a jacket on the outer wall of the reaction kettle), adding 550kg of desulfurization by-products (the total alkalinity of the desulfurization by-products is 0.8 wt% in terms of sodium bicarbonate, the content of sodium sulfate in the desulfurization by-products is 88.57 wt%, and the molar ratio of the total alkali in the sulfuric acid and the desulfurization by-products is 1:1.9), keeping the same stirring speed, continuously stirring and mixing for 15min, and keeping the stirring speed to ensure that the total alkali in the sulfuric acid and the desulfurization by-products is 1:1.9Carrying out warm reaction (the temperature of the heat preservation reaction is controlled at 30 ℃) and filtering the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate obtained in step (1) into another reaction kettle, stirring (stirring speed is 90rpm), heating (heating with 60 deg.C hot water in jacket on outer wall of reaction kettle), and adding 6.3m3The waste clear liquid collected in the step (2) (the molar ratio of calcium ions in the waste clear liquid to sulfate ions in the filtrate is 1.5:1, and the addition is controlled to be completed in 10 min), the same stirring speed is maintained, the stirring and the mixing are continued for 10min, the heat preservation reaction (the temperature of the heat preservation reaction is 50 ℃) is carried out, after the reaction of the liquid material is finished, the liquid material after the reaction is filtered, the liquid phase and the solid phase are respectively collected, the collected solid phase is washed and filtered, and the obtained solid is the dihydrate gypsum; the collected liquid phase is used as salt dissolving water for producing the calcined soda.
Example 2
A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) 2.5m from the beginning3Adding 68.53kg of sulfuric acid (80 wt% sulfuric acid recovered from chlor-alkali production) into a reaction kettle in sequence for stirring (the stirring speed is 90rpm) and heating (heating is carried out by using 60 ℃ hot water in a jacket on the outer wall of the reaction kettle), adding 580kg of desulfurization by-products (the total alkalinity of the desulfurization by-products is 15.8 wt% calculated by sodium bicarbonate, the content of sodium sulfate in the desulfurization by-products is 77.8 wt%, the molar ratio of the total alkali in the sulfuric acid and the desulfurization by-products is 1:1.95), continuously stirring and mixing for 20min while maintaining the same stirring speed, carrying out heat preservation reaction (the temperature of the heat preservation reaction is controlled at 32 ℃) to filter the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate prepared in step (1) into another reaction kettle, stirring (stirring speed is 95rpm) and heating (60 deg.C hot water in jacket on outer wall of reaction kettleHeating) was performed, and 6.1m was further added3The waste clear liquid collected in the step (2) (the molar ratio of calcium ions in the waste clear liquid to sulfate ions in the filtrate is 1.35:1, the waste clear liquid is completely added within 15 min), the same stirring speed is maintained, stirring and mixing are continued for 20min, the temperature of the heat preservation reaction is 53 ℃, the reacted feed liquid is filtered after the reaction of the feed liquid is finished, the liquid phase and the solid phase are respectively collected, the collected solid phase is washed and filtered, and the obtained solid is the dihydrate gypsum; the collected liquid phase is used as salt dissolving water for producing the calcined soda.
Example 3 (best)
A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) 2.5m3Adding tap water and 99.75kg of sulfuric acid (80 wt% sulfuric acid recovered from chlor-alkali production) into a reaction kettle in sequence for stirring (the stirring speed is 95rpm) and heating (heating is carried out by using 60 ℃ hot water in a jacket on the outer wall of the reaction kettle), adding 600kg of desulfurization by-products (the total alkalinity of the desulfurization by-products is 28.8 wt% calculated by sodium bicarbonate, the content of sodium sulfate in the desulfurization by-products is 68.5 wt%, the molar ratio of the total alkalinity of the sulfuric acid to the desulfurization by-products is 1:2), continuously stirring and mixing for 25min by maintaining the same stirring speed, carrying out heat preservation reaction (the temperature of the heat preservation reaction is controlled at 33 ℃) to filter the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate obtained in step (1) into another reaction kettle, stirring (stirring speed is 98rpm), heating (heating with 60 deg.C hot water in jacket on outer wall of reaction kettle), and adding 5.39m3And (3) collecting waste clear liquid in the step (2) (the molar ratio of calcium ions in the waste clear liquid to sulfate ions in the filtrate is 1.2:1, the waste clear liquid is completely added in 20 min), maintaining the same stirring speed, continuously stirring and mixing for 30min, carrying out heat preservation reaction (the temperature of the heat preservation reaction is 55 ℃) to filter the reacted liquid after the reaction of the liquid is finished, respectively collecting a liquid phase and a solid phase, and washing and filtering the collected solid phase to obtain the productThe solid is dihydrate gypsum; the collected liquid phase is used as salt dissolving water for producing the calcined soda.
Example 4
A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) 2.5m3Adding tap water and 192.58kg of sulfuric acid (80 wt% sulfuric acid recovered from chlor-alkali production) into a reaction kettle in sequence for stirring (the stirring speed is 98rpm) and heating (heating is carried out by using hot water at 60 ℃ in a jacket on the outer wall of the reaction kettle), adding 630kg of desulfurization by-products (the total alkalinity of the desulfurization by-products is 43.6 wt% calculated by sodium bicarbonate, the content of sodium sulfate in the desulfurization by-products is 52.8 wt%, the molar ratio of the total alkali amount in the sulfuric acid and the desulfurization by-products is 1:2.08), continuously stirring and mixing for 15min while maintaining the same stirring speed, carrying out heat preservation reaction (the temperature of the heat preservation reaction is controlled at 35 ℃) to filter the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate obtained in step (1) into another reaction kettle, stirring (stirring speed of 102rpm) and heating (heating with 60 deg.C hot water in jacket on outer wall of reaction kettle), and adding 4.74m3The waste clear liquid collected in the step (2) (the molar ratio of calcium ions in the waste clear liquid to sulfate ions in the filtrate is 1:1, and the waste clear liquid is completely added in 25 min), the same stirring speed is maintained, stirring and mixing are continued for 40min, the reaction liquid is filtered after the reaction of the liquid is finished in a heat preservation reaction (the temperature of the heat preservation reaction is 58 ℃), the liquid phase and the solid phase are respectively collected, the collected solid phase is washed and filtered, and the obtained solid is the dihydrate gypsum; the collected liquid phase is used as salt dissolving water for producing the calcined soda.
Example 5
A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid comprises the following steps:
(1) 2.5m3Tap water and 234.7kg of sulfuric acid (80 wt% sulfuric acid recovered from chlor-alkali production) were sequentially added to the inside of the reaction vessel and stirred (stirring speed: 80 wt%)100rpm) and heating (heating by using 60 ℃ hot water in a jacket on the outer wall of the reaction kettle), adding 650kg of desulfurization byproducts (the total alkalinity of the desulfurization byproducts is 52 wt% calculated by sodium bicarbonate, the content of sodium sulfate in the desulfurization byproducts is 47 wt%, and the molar ratio of the total alkali in sulfuric acid to the desulfurization byproducts is 1:2.1), maintaining the same stirring speed, continuously stirring and mixing for 15min, carrying out heat preservation reaction (the temperature of the heat preservation reaction is controlled to be 35 ℃) to filter the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate obtained in step (1) into another reaction kettle, stirring (stirring speed of 109rpm) and heating (heating with 60 deg.C hot water in jacket on outer wall of reaction kettle), and adding 3.94m3The waste clear liquid collected in the step (2) (the molar ratio of calcium ions in the waste clear liquid to sulfate ions in the filtrate is 0.8:1, the waste clear liquid is completely added within 30 min), the same stirring speed is maintained, stirring and mixing are continued for 60min, the heat preservation reaction (the temperature of the heat preservation reaction is 60 ℃) is carried out, after the reaction of the liquid material is finished, the liquid material after the reaction is filtered, the liquid phase and the solid phase are respectively collected, wherein the collected solid phase is washed and filtered, and the obtained solid is the dihydrate gypsum; the collected liquid phase is used as salt dissolving water for producing the calcined soda.
The indexes of the dihydrate gypsum products obtained by the methods of example 1, example 2, example 3, example 4 and example 5 are shown in table 1.
TABLE 1
In order to better prove that the dihydrate gypsum product with better index can be obtained by the method under the process parameters of the example 3 of the invention, 4 comparative examples are given by taking the example 3 as a reference, and the specific results are detailed in the table 2.
Comparative example 1
The operation was the same as in example 3 except that the stirring speed in step (3) was 140 rpm.
Comparative example 2
The operation was the same as in example 3 except that the stirring speed in step (3) was 60 rpm.
Comparative example 3
Unlike example 3, the amount of desulfurization by-product added in step (1) was adjusted to 2.5m3500kg of tap water was added, and the rest was the same.
Comparative example 4
Unlike example 3, the amount of desulfurization by-product added in step (1) was adjusted to 2.5m3700kg of tap water was added, and the rest was the same.
TABLE 2
The data in table 2 show that the dihydrate gypsum product obtained by reducing the stirring speed or increasing the stirring speed is not ideal, the particle size of the dihydrate gypsum is reduced by increasing the consumption of the desulfurization product, and the reduction of the desulfurization product does not affect the product quality, but is not beneficial to the improvement of the equipment productivity.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. A comprehensive utilization method of sodium bicarbonate desulfurization byproducts and soda plant waste liquid is characterized by comprising the following steps:
(1) sequentially adding tap water and sulfuric acid into the reaction kettle for stirring and heating, adding a desulfurization byproduct, maintaining the same stirring speed, continuously stirring and mixing, carrying out heat preservation reaction, filtering the reacted feed liquid after the reaction of the feed liquid is finished, and collecting filtrate for later use;
(2) filtering waste liquid generated in the production of soda ash in a soda ash plant, and collecting waste clear liquid for later use;
(3) adding the filtrate reserved in the step (1) into another reaction kettle, stirring and heating, adding the waste clear liquid collected in the step (2), keeping the same stirring speed, continuously stirring and mixing, carrying out heat preservation reaction, filtering the reacted feed liquid after the reaction of the feed liquid is finished, washing and filtering the collected filter cake, and obtaining the solid, namely the dihydrate gypsum.
2. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: the addition amount of the desulfurization by-product in the step (1) is 2.5m per3650kg of tap water was added.
3. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: the molar ratio of the sulfuric acid to the desulfurization by-products in the step (1) is 1: 1.9-2.1.
4. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: in the step (1), the total alkalinity of the desulphurization by-product is 0.8-52 wt% calculated by sodium bicarbonate, and the content of sodium sulfate in the desulphurization by-product is 47-88.57 wt%.
5. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: the temperature of the heat preservation reaction in the step (1) is 30-35 ℃, the stirring and mixing time is 15-30min, and the stirring speed is 85-100 rpm.
6. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: the sulfuric acid in the step (1) is purchased sulfuric acid or 75-85 wt% sulfuric acid recovered from a chlor-alkali plant.
7. The method for comprehensively utilizing the desulfurization by-products of sodium bicarbonate and the waste liquid of soda ash plant according to claim 1, characterized in that: ca in the waste clear liquid in the step (2)2+And SO in the filtrate4 2+In a molar ratio of 0.8-1.5: 1.
8. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: the temperature of the heat preservation reaction in the step (2) is 50-60 ℃, the stirring and mixing time is 10-60min, and the stirring speed is 90-109 rpm.
9. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: and (3) adding the waste clear liquid in the step (2) into the reaction kettle within 10-30 min.
10. The method for comprehensively utilizing the desulfurization by-products of baking soda and the waste liquor of soda plants according to claim 1, which is characterized in that: and (4) taking the liquid phase collected in the step (3) as salt dissolving water for producing the calcined soda.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118005047A (en) * | 2024-04-09 | 2024-05-10 | 山东海天生物化工有限公司 | Novel production process for reducing total alkalinity of baking soda |
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| CN1297847A (en) * | 2000-12-06 | 2001-06-06 | 化学工业部连云港设计研究院 | Comprehensive utilization method of waste ammonia sode liquid and sodium sulfate containing waste liquid |
| CN102030353A (en) * | 2010-04-30 | 2011-04-27 | 汪晋强 | Method for preparing gypsum and simultaneously producing sodium sulfate and hydrochloric acid by distilled ammonia waste liquid of sodium carbonate |
| CN102351155A (en) * | 2011-07-12 | 2012-02-15 | 湖南恒光科技股份有限公司 | Alkali manufacturing technology for combined production of sulfuric acid and cement |
| CN110844987A (en) * | 2019-11-29 | 2020-02-28 | 江西富达盐化有限公司 | Method for treating sodium carbonate waste liquid by using lithium carbonate waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1297847A (en) * | 2000-12-06 | 2001-06-06 | 化学工业部连云港设计研究院 | Comprehensive utilization method of waste ammonia sode liquid and sodium sulfate containing waste liquid |
| CN102030353A (en) * | 2010-04-30 | 2011-04-27 | 汪晋强 | Method for preparing gypsum and simultaneously producing sodium sulfate and hydrochloric acid by distilled ammonia waste liquid of sodium carbonate |
| CN102351155A (en) * | 2011-07-12 | 2012-02-15 | 湖南恒光科技股份有限公司 | Alkali manufacturing technology for combined production of sulfuric acid and cement |
| CN110844987A (en) * | 2019-11-29 | 2020-02-28 | 江西富达盐化有限公司 | Method for treating sodium carbonate waste liquid by using lithium carbonate waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118005047A (en) * | 2024-04-09 | 2024-05-10 | 山东海天生物化工有限公司 | Novel production process for reducing total alkalinity of baking soda |
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