CN115583632A - Method for producing electronic-grade sulfuric acid by absorption method - Google Patents
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- CN115583632A CN115583632A CN202211332214.XA CN202211332214A CN115583632A CN 115583632 A CN115583632 A CN 115583632A CN 202211332214 A CN202211332214 A CN 202211332214A CN 115583632 A CN115583632 A CN 115583632A
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
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Abstract
The invention discloses a process method for producing electronic-grade sulfuric acid by an absorption method. The pure sulfur trioxide raw material is obtained by utilizing a multi-stage condensation impurity removal mode to prepare the electronic grade sulfuric acid. The method improves the purification mode of the raw materials for producing the electronic-grade sulfuric acid and the system operation index, has low energy consumption, little environmental pollution, low production cost and efficient and convenient production process, and can completely realize that the product reaches the G5-grade quality level.
Description
Technical Field
The invention relates to the production industry of electronic-grade chemicals, in particular to a method for producing electronic-grade sulfuric acid by using an absorption method.
Background
At present, electronic-grade sulfuric acid is a key basic chemical reagent widely applied to the field of microelectronic technology development of large-scale Integrated Circuits (ICs), semiconductors and the like. With the rapid development of the microelectronic industry in China, the demand of electronic-grade sulfuric acid is increasing day by day, and the method has a good application prospect.
The current general production methods of electronic grade sulfuric acid are divided into absorption method and distillation method, and the distillation method is not used as a preferential production method due to complex production process, high process energy consumption and slightly poor product cleanliness. The invention mainly introduces a process for producing electronic-grade sulfuric acid by an absorption method, and overcomes the defect that the quality of products is unstable due to unstable production process of the electronic-grade sulfuric acid.
When the absorption method is used for preparing electronic-grade sulfuric acid, fuming sulfuric acid gas sulfur trioxide is generally used as a raw material in the industry, so that the purification of sulfur trioxide becomes the key of reaching the standard of a product when the electronic-grade sulfuric acid is prepared. In the method and the system for producing the G1-G5 electronic-grade sulfuric acid, which are provided by CN114804036A, sulfur trioxide is purified by using a rectification and impurity removal mode of a rectification tower. The core of the rectifying tower is to achieve the purpose of purification by continuously gasifying and condensing the materials for many times. However, the rectifying tower has a relatively complex structural design, a large number of pipelines need to be laid, the process control difficulty is high, the operation requirement is high, the problem of unstable product quality caused by unstable process parameters is easily caused, and meanwhile, more energy is consumed in the purification process. The physical and chemical properties of sulfur trioxide are relatively unstable, and serious environmental accidents can be caused by pipeline leakage; the temperature required for the sulfur trioxide to maintain the liquid phase or the gas phase also needs to be considered in the purification and preparation processes, especially in winter, the heat tracing of equipment and pipelines needs to consume a large amount of heat, and the energy consumption is not negligible.
Meanwhile, the applicant is a professional sulfuric acid production enterprise, the product line is rich, a large amount of hot flue gas and steam are generated in the daily production process, a large amount of heat energy is needed just in the process of producing electronic-grade sulfuric acid, the heat generated in the daily production process can be considered to be utilized, and the energy consumption is saved.
Disclosure of Invention
The invention aims to produce sulfur trioxide by evaporating fuming sulfuric acid by using conversion flue gas, purify the sulfur trioxide by a two-stage condensation gas-liquid separation mode, and reasonably utilize hot flue gas and steam generated in industrial production to reduce energy consumption. By purifying the raw materials, the purity of the final product is improved, and the electronic-grade sulfuric acid meeting the requirements of the semiconductor chip industry is produced.
The technical scheme adopted for realizing the purpose of the invention is as follows:
the invention provides a method for producing electronic-grade sulfuric acid by an absorption method, and provides a way for effectively purifying production raw material sulfur trioxide, so that pure sulfur trioxide reacts with sulfuric acid with a certain concentration in an absorption tower, and the required electronic-grade sulfuric acid is obtained by cooling, degassing, filtering and other steps.
The high-concentration oleum firstly exchanges heat with the 140-DEG C22-percent oleum evaporated by the evaporator through an oleum preheater in the conveying process, the oleum is heated to 110 ℃ and then enters the evaporator, and the 22-percent oleum returns to an oleum system after the cooling temperature of the 22-percent oleum is reduced to 60 ℃ through an oleum heat exchanger. In a oleum system, the sulfur trioxide in the converted flue gas is continuously absorbed by an oleum absorption tower, the concentration of 22% oleum returned from an oleum evaporator is increased to 30% -35%, and then the 22% oleum is conveyed to the oleum evaporator again. The temperature of oleum from an oleum system is 60-80 ℃, preferably 70 ℃, the concentration of free sulfur trioxide of the oleum is not less than 30%, preferably 30-35% in order to ensure the quality of the evaporated sulfur trioxide flue gas, and the oleum is stably conveyed to an oleum evaporator.
The fuming sulfuric acid evaporator is heated by using conversion flue gas, a large amount of gas is generated after combustion when the conversion flue gas comes from liquid sulfur to prepare industrial sulfuric acid, heat release is accompanied, the heat release temperature can reach about 1000 ℃, and the gas components are as follows: 10% of sulfur dioxide, 80% of nitrogen, 10% of oxygen and other gases, because the reaction temperature of a catalyst in the converter is 400 ℃, the temperature of the gases is required to be reduced from 1000 ℃ to 400 ℃ by means of boiler cooling water circulation before entering the converter, the gases enter the converter and are converted into sulfur trioxide gas, namely conversion flue gas, 10% of the sulfur dioxide gas is converted into the sulfur trioxide gas through the catalyst, the conversion flue gas is cooled to 150 ℃, and then the sulfur trioxide gas enters a fuming sulfuric acid absorption tower to be absorbed.
The fuming sulfuric acid evaporator in the process utilizes the heat released when the temperature of the conversion flue gas is reduced from 400 ℃ to 150 ℃, the temperature is preferably 300 ℃, the stability of the evaporation process is ensured, and the temperature of the sulfur trioxide gas evaporated by the fuming sulfuric acid evaporator is 120-180 ℃, and the temperature is preferably 150 ℃. The sulfur trioxide gas evaporated from the oleum evaporator first passes through a gas-liquid separator at the bottom of the evaporator and then enters a sulfur trioxide cooler. The temperature of a sulfur trioxide cooler is kept between 45 and 50 ℃, the preferable temperature is 45 ℃, most impurities are condensed into liquid after being purified by a precise gas-liquid separator, and the liquid is discharged to a collecting tank from the bottom of the cooler; the method comprises the following steps of enabling gas sulfur trioxide to enter a sulfur trioxide condenser, keeping the temperature of the sulfur trioxide condenser at 35 ℃, obtaining pure sulfur trioxide liquid, enabling the pure sulfur trioxide liquid to flow into a sulfur trioxide storage tank, obtaining liquid sulfur trioxide with the purity not less than 99.9976%, meeting international high-class product standards, and conveying the liquid sulfur trioxide meeting the standards to an evaporator through a pump.
Heating in an evaporator with hot water at 60-100 deg.C, preferably 95 deg.C; the temperature of the sulfur trioxide gas evaporated is 70-80 ℃, preferably 75 ℃; and the sulfur trioxide gas enters a gas-liquid separator to obtain pure sulfur trioxide gas.
The pure sulfur trioxide gas enters a sulfuric acid absorption tower, sulfuric acid with the concentration of 96.5% is used for absorbing sulfur trioxide in the sulfuric acid absorption tower, the outlet temperature of the mixed absorption tower in a mixing tank is 60-95 ℃, the preferred temperature is 88 ℃, and a proper amount of ultrapure water is added for adjusting the concentration. A circulating cooler is arranged in the absorption tower, and the water flow of the cooler is 25-50m 3 H, preferably 45m 3 The reaction heat is continuously removed through cooling water circulation, so that the normal reaction is ensured; the outlet temperature of the sulfuric acid cooler is 60-80 ℃, and the preferred temperature is 75 ℃. The absorption tower continuously absorbs sulfur trioxide and simultaneously continuously leads out a certain amount of sulfuric acid as a product, and partial sulfuric acid led out from the absorption tower passes through the secondary regulator and is regulated in concentration again through ultrapure water, so that the concentration of the sulfuric acid is ensured. The temperature of the sulfuric acid after the secondary adjustment is 100-150 ℃, the preferred temperature is 130 ℃, the obtained sulfuric acid enters a degassing tower, and dry air is introduced into the degassing tower to remove SO in the sulfuric acid 2 To ensure the production of SO in sulfuric acid 2 The content is less than 1ppm. The outer ends of the absorption tower and the degassing tower are connected with a tail gas recovery device, and a pure hydrogen peroxide reagent is added to recover SO 2 Oxidation to SO 3 The absorption of sulfuric acid is convenient, and the absorption liquid adopts 25-27% dilute sulfuric acid to absorb SO in the waste gas 2 Is converted into dilute sulfuric acid, and the part of the dilute sulfuric acid is recycled to an analytically pure sulfuric acid reaction tower. After the particles are removed by the filter element in the tank after being cooled by the cooler, the 0.01um particles are ensured to be 5pcs/ml, and finally, the filling and the shipment are carried out.
Compared with the prior art, the invention has the beneficial effects that:
1. gaseous sulfur trioxide of the fuming sulfuric acid evaporator is subjected to two-stage gasification-condensation, pure sulfur trioxide is prepared through gas-liquid separation, and the raw material is purified to produce the electronic-grade sulfuric acid with the G5 specification, so that the purification process is simpler and more efficient.
2. The fuming sulfuric acid evaporation heat source selects the heat released when the gas generated in the industrial sulfuric acid production process is converted into the converted flue gas, does not need to additionally consume other fuels to provide heat, and can improve the process safety. Different from the common process using steam as a heat source at present, the chemical reaction heat of the converted flue gas and fuming sulfuric acid is extremely low, the problem that fuming sulfuric acid and steam react to generate a large amount of heat and even explode due to the fact that fuming sulfuric acid evaporator tubes are leaked can be avoided, and production personnel and environment safety are guaranteed.
3. Compared with the traditional method, the method can save 281400 kilocalories of heat by evaporating one ton of sulfur trioxide.
4. The concentration regulator is configured behind the absorption tower, the concentration regulation error of the sulfuric acid is 0.05 percent, the stability of the product concentration is ensured, meanwhile, the temperature of the sulfuric acid is increased through the reaction heat generated by the ultrapure water and the sulfuric acid, and then the sulfuric acid enters the degassing tower, so that the degassing efficiency of the degassing tower is improved.
5. The tail gas absorption devices are arranged outside the absorption tower and the exhaust tower, so that the sulfur pollution is reduced, the sulfur element can be recycled, the sulfur element is used for producing analytically pure sulfuric acid, and the materials are saved to a greater extent.
Drawings
FIG. 1 is a schematic flow diagram of the production of electronic grade sulfuric acid from high concentration oleum as a feedstock.
The method comprises the following steps of 1-fuming sulfuric acid evaporator, 2-sulfur trioxide gas cooling tower, 3-condensate collecting tank, 4-sulfur trioxide condenser, 5-sulfur trioxide storage tank, 6-evaporator, 7-gas-liquid separator, 8-absorption tower, 9-mixing tank and 10-degassing tower.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
Example 1
According to the attached drawing, in the conveying process, 30% oleum firstly passes through an oleum preheater to exchange heat with 140% oleum evaporated by an evaporator, the oleum is heated to 110 ℃ and then enters the evaporator, and the 22% oleum returns to an oleum system after the cooling temperature of the oleum is reduced to 60 ℃ through an oleum heat exchanger. High-concentration oleum enters the evaporator 1 after being preheated, the preheater and the oleum evaporator 1 utilize the heat of the large-flow conversion flue gas of a sulfuric acid device to evaporate the oleum, and the temperature of the conversion flue gas is 300 ℃. And after the converted flue gas is cooled to 150 ℃, the converted flue gas enters an absorption tower in a fuming sulfuric acid system, the concentration of 22% fuming sulfuric acid returned from the fuming sulfuric acid evaporator is increased to 30% -35% by absorbing sulfur trioxide in the converted flue gas in the absorption tower, and then the converted flue gas is conveyed to the fuming sulfuric acid evaporator again.
The temperature of sulfur trioxide gas evaporated by the fuming sulfuric acid evaporator 1 is 150 ℃, the gas enters a sulfur trioxide cooler 2, the temperature of the cooler is 45 ℃, most impurities are condensed into liquid, the liquid passes through a gas-liquid separator and then is discharged from the bottom of the cooler to a condensate collecting tank 3 to be discharged, and the liquid discharge amount is 200-325kg/h. The gaseous sulfur trioxide is conveyed to a sulfur trioxide condenser 4, the condensing temperature of the condenser 4 is kept at 35 ℃, and the gaseous sulfur trioxide is condensed into pure sulfur trioxide liquid, and the purity of the sulfur trioxide reaches 99.9976 percent. Pure liquid sulfur trioxide is delivered from a sulfur trioxide storage tank 5 to an evaporator 6 through a pump to be gasified. The sulfur trioxide evaporator is heated by hot water, the temperature of the hot water is 95 ℃, the hot water is heated and evaporated, the hot water is introduced into a gas-liquid separator 7 for purification, and the temperature of the sulfur trioxide gas is 75 ℃ when the pure sulfur trioxide gas is obtained from the separator 7. The purpose of purifying sulfur trioxide is achieved through two-stage gasification-condensation, and the purification process is more efficient and convenient.
In the purification process, the fuming sulfuric acid evaporator adopts a mode of heating conversion flue gas, and a large part of energy consumption can be saved by the mode. Therefore, the following results are obtained through theoretical calculation and calculation of the energy consumption of self system for generating heat energy and converting flue gas:
the heat capacity of 30 percent fuming sulfuric acid is 1.3416 kJ/(kg.K),
1kg of 30% oleum, Q1=1 × 1.3416 × 40=53.66kJ, converted to 12.9 kcal,
evaporating 1kg of 30% oleum to obtain SO with nicotinic acid concentration of 25% 3 The amount is: 0.07kg.
SO at 100 ℃ according to the handbook of sulfuric acid Process design P45 3 The latent heat is 406kJ/kg, namely 97.44 kilocalories/kg;
evaporate 0.07kg SO 3 The latent heat of vaporization required is:
q2=0.07 × 97.44 kcal/kg =6.82 kcal,
heating 1kg of 30% oleum from 90 deg.C to 120 deg.C while evaporating 0.07kg of SO 3 The total heat required is: q1+ Q2=12.9+6.82=19.7 kcal,
production of 1kg SO 3 The total heat required is: 19.7/0.07=281 kcal,
total heat required for production of 2 t/h:
281.4 kcal 2000=562800 kcal,
the enthalpy value of 0.5MPa saturated steam is 660 kcal/kg, and the steam quantity required per hour is as follows: 852.7kg
Steam consumption per day: 852.7 × 24= 20465kg/day.
It can be concluded that the steam consumption is completely saved by using the conversion waste heat to heat the fuming sulfuric acid evaporator.
The evaporated sulfur trioxide gas enters an absorption tower 8 and is mixed with sulfuric acid with the concentration of 96.5 percent in a mixing tank 9, cooling water is circulated in the absorption tower 8 to remove redundant reaction heat, the outlet temperature of the absorption tower 8 is 88 ℃, and part of the sulfuric acid is led out to be used as a product after being fully mixed with the sulfuric acid in the mixing tank.
Part of the sulfuric acid product which is subsequently withdrawn is fed toAnd (4) feeding the mixture into a secondary concentration regulator, and regulating the concentration by adding ultrapure water, wherein the flow of the ultrapure water is 200L/min. The sulfuric acid with the required concentration after the secondary adjustment enters a degassing tower 10, and dry air is introduced into the degassing tower 10 at a rate of 260L/min to remove SO 2 To obtain SO in sulfuric acid 2 The content is less than 1ppm.
The outer ends of the absorption tower 8 and the degassing tower 10 are connected with a tail gas recovery device, and pure hydrogen peroxide solution reagent is added to recover SO 2 Oxidation to SO 3 The absorption of sulfuric acid is convenient, and the absorption liquid adopts 25-27% dilute sulfuric acid to absorb SO in the waste gas 2 The part of dilute sulfuric acid is recycled to the analytically pure sulfuric acid reaction tower, and the material energy is saved to the maximum extent.
And finally, introducing filter element filter particles into the prepared electronic acid product to ensure that the particles of 0.01um are 5pcs/ml, and after the particles of the sulfuric acid in the tank are removed by the filter element, determining that the sulfuric acid meets the G5-level standard, and filling and delivering.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A method for producing electronic-grade sulfuric acid by an absorption method is characterized in that sulfur trioxide gas is sent into a sulfuric acid absorption tower to react with sulfuric acid with certain concentration to prepare sulfuric acid with required concentration, and the electronic-grade sulfuric acid is obtained after degassing, cooling and filtering, and is characterized in that: the method also comprises the processes of multi-stage gasification and condensation impurity removal purification of the raw material sulfur trioxide, and comprises the following steps: (1) Heating high-concentration oleum in an oleum evaporator to evaporate gaseous sulfur trioxide; (2) Condensing gaseous sulfur trioxide through a sulfur trioxide gas cooler to discharge condensed liquid impurities; (3) The collected gas sulfur trioxide enters a sulfur trioxide condenser for condensation; (4) introducing sulfur trioxide liquid into an evaporator for evaporation; (5) And separating the obtained gas sulfur trioxide by a gas-liquid separator to obtain high-purity gas sulfur trioxide, and allowing the high-purity gas sulfur trioxide to enter the absorption tower for reaction.
2. A process for producing electronic grade oleum according to claim 1, wherein: the temperature of the high-concentration oleum entering the oleum evaporator in the step (1) is 60-80 ℃, the concentration of free sulfur trioxide of the oleum is not less than 30%, and the temperature of sulfur trioxide gas evaporated by the oleum evaporator is 120-180 ℃; in the step (2), the temperature of the cooler is kept at 45-50 ℃, and most of impurities are condensed into liquid and discharged from the bottom of the cooler to a collecting tank; the condensation temperature of the sulfur trioxide condenser in the step (3) is kept at 35 ℃; in the step (4), the sulfur trioxide evaporator is heated by hot water, and the temperature of the hot water is 60-100 ℃.
3. A process for producing electronic grade oleum according to claim 2, wherein: the fuming sulfuric acid evaporator is heated by conversion flue gas.
4. The process for producing electronic grade sulfuric acid by the absorption process according to claim 1, wherein: high concentration oleum before getting into oleum evaporimeter, still set up the preheating step, oleum heaies up through the high temperature oleum heat transfer after oleum preheater and the evaporimeter evaporation, gets into the evaporimeter, and oleum after the evaporimeter evaporation returns the oleum system through the oleum heat exchanger cooling back, and the oleum system continuously provides required high concentration oleum.
5. A process for producing electronic grade oleum according to claim 1, wherein: and the sulfuric acid product from the absorption tower enters a secondary concentration regulator, and the concentration is regulated by ultrapure water.
6. The method for producing electronic grade oleum according to claim 1, wherein gas recovery devices are arranged at the top of the degassing tower and the top of the absorption tower for recovering sulfur dioxide gas for preparing analytically pure sulfuric acid.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116281876A (en) * | 2023-03-09 | 2023-06-23 | 山东鲁东化学研究院有限公司 | Preparation method and production system of electronic grade sulfuric acid |
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