CN217418195U - Electronic-grade sulfuric acid production device - Google Patents
Electronic-grade sulfuric acid production device Download PDFInfo
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- CN217418195U CN217418195U CN202221083942.7U CN202221083942U CN217418195U CN 217418195 U CN217418195 U CN 217418195U CN 202221083942 U CN202221083942 U CN 202221083942U CN 217418195 U CN217418195 U CN 217418195U
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Abstract
The utility model belongs to the technical field of chemical reagent apparatus for producing technique and specifically relates to an electronic grade sulphuric acid apparatus for producing, including consecutive nicotinic acid absorption tower, one-level rectifying column, second grade rectifying column, absorption tower, first desorption tower, second degassing tower, tail gas washing tower and electric demister. This device adopts the sulfur trioxide-containing gas that the acid making device sent to absorb and resolve out sulfur trioxide and produce electronic level sulphuric acid through fuming sulphuric acid, and is supporting with the acid making device, low cost. The device adopts a continuous rectification process, light component impurities and heavy component impurities are removed respectively in different rectification towers, the rectification steps can be repeated for multiple times, sulfur trioxide with very high purity can be prepared, the product quality can be flexibly changed according to requirements, and the product grade can reach and exceed the SEMI-C12 grade.
Description
Technical Field
The utility model relates to a chemical reagent apparatus for producing technical field, the concrete field is an electronic grade sulphuric acid apparatus for producing.
Background
The electronic grade sulfuric acid is also called high-purity sulfuric acid and ultrapure sulfuric acid, belongs to an ultra-clean high-purity reagent, and is an indispensable key basic chemical reagent in the microelectronic technology development process. At present, the core technology of electronic grade sulfuric acid is monopolized by Germany, Japan, America and other countries, and the domestic and foreign literature reports of the key technology are few. There are only a few companies that can produce electronic-grade sulfuric acid internationally, such as e.merck company in germany, Ashland company, Arch company and mallinkradt Baker company in the united states, Wako, Sumitomo synthesis, delavay and mitsubishi in japan, etc., taiwan region mainly includes companies such as Merck, vinpock, changsheng chemistry, tainit share and companionship, and korea mainly includes companies such as Dongwoo (Dongwoo Fine Chem), dongkin (Donjin semiconductor) and samyong Fine Chem.
Ultra-clean high-purity reagents for 0.09 to 0.2 μm and more have been produced in large scale in the United states, Germany, Japan, Korea and Taiwan China, and high-specification electronic grade sulfuric acid is not in demand as an upstream industry for raw material supply in the integrated circuit manufacturing industry, the package testing industry and the whole machine assembly industry.
Electronic grade sulfuric acid is one of eight common chemical reagents in semiconductor industry, is widely used in the assembly and processing processes of semiconductors and very large scale integrated circuits, is mainly used for cleaning and etching silicon wafers, and can effectively remove impurity particles, inorganic residues and carbon deposits on the wafers. Electronic grade sulfuric acid has been used for cleaning silicon wafers for over 40 years. Are indispensable key basic chemical reagents in the semiconductor industry, and the purity of the reagents directly affects the yield of integrated circuits.
At present, the production of Chinese electronic grade sulfuric acid generally adopts an industrial grade concentrated sulfuric acid atmospheric distillation method to produce, the atmospheric distillation temperature is up to 330 ℃, the equipment material is quartz glass, and a heater is electrically heated. The method for producing the electronic-grade sulfuric acid has the advantages of large energy consumption, high cost, difficult removal of impurities, ineffective treatment of generated waste gas, large environmental protection pressure, small size of glass equipment, small yield and unsuitability for large-scale production.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide an electronic grade sulphuric acid apparatus for producing.
In order to achieve the above object, the utility model provides a following technical scheme:
an electronic-grade sulfuric acid production device comprises a nicotinic acid absorption tower, a primary rectifying tower, a secondary rectifying tower, an absorption tower, a first desorption tower, a second degassing tower, a tail gas washing tower and an electric demister which are connected in sequence.
A nicotinic acid circulating tank is arranged below the nicotinic acid absorption tower, a nicotinic acid circulating pump is arranged in the nicotinic acid circulating tank, an outlet of the nicotinic acid circulating pump is respectively connected with an upper inlet of the nicotinic acid absorption tower and an upper inlet of a nicotinic acid evaporator, and a lower outlet of the nicotinic acid evaporator is communicated with the nicotinic acid circulating tank;
the top outlet of the nicotinic acid evaporator is communicated with the middle inlet of the first-stage rectifying tower, the top of the first-stage rectifying tower is provided with a tower top condenser, the tower top condenser is connected with the inlet of the tail gas washing tower through a pipeline, and the bottom of the first-stage rectifying tower is provided with a first reboiler;
the bottom outlet of the first-stage rectifying tower is respectively communicated with the inlet of the first reboiler and the inlet of the second-stage rectifying tower, the top of the second-stage rectifying tower is provided with a condenser, one outlet of the condenser is connected with the inlet of the tail gas washing tower, the bottom of the second-stage rectifying tower is provided with a second reboiler,
the other outlet of the condenser is respectively communicated with the upper inlet of the secondary rectifying tower and the water bath evaporator; the water bath evaporator is communicated with an inlet of an absorption tower, an outlet at the lower part of the absorption tower is communicated with an inlet of an absorption acid pump, an outlet of the absorption acid pump is respectively communicated with an inlet of a sulfuric acid cooler and an inlet of a first desorption tower, and an outlet of the sulfuric acid cooler is communicated with an inlet at the upper part of the absorption tower;
the lower outlet of the first desorption tower is communicated with the inlet of a circulating pump of the first desorption tower, the outlet of the circulating pump of the first desorption tower is respectively communicated with the inlet of a first cooler and the inlet of a second degassing tower, and the outlet of the first cooler is communicated with the upper inlet of the first desorption tower;
an outlet at the lower part of the second degassing tower is communicated with a circulating pump, and an outlet of the circulating pump is respectively communicated with an inlet at the upper part of the second degassing tower and a conveying pipeline;
the top outlet of the absorption tower, the top outlet of the first desorption tower and the top outlet of the second degassing tower are connected with the inlet of the tail gas washing tower; an outlet at the lower part of the tail gas washing tower is connected with an inlet of a tower bottom circulating pump, an outlet of the tower bottom circulating pump is respectively communicated with an inlet of a second cooler and a bypass pipeline, and an outlet of the second cooler is communicated with an inlet at the upper part of the tail gas washing tower;
and a top outlet of the tail gas washing tower is communicated with a lower inlet of the electric demister, and a top outlet of the electric demister is used for discharging waste gas B.
Wherein, the lower part entry of nicotinic acid absorption tower is used for letting in the gas that contains sulfur trioxide, the top export of nicotinic acid absorption tower is used for discharging the residual gas.
Wherein, the inlet of the nicotinic acid circulating tank is used for introducing 98 percent of sulfuric acid.
Wherein, the top outlet of the primary rectifying tower is communicated with the inlet of the tower top condenser, and one outlet of the tower top condenser is communicated with the upper inlet of the primary rectifying tower; and an outlet of the first reboiler is communicated with a lower inlet of the first-stage rectifying tower.
Wherein, the top outlet of the secondary rectifying tower is communicated with the inlet of a condenser, and one outlet of the condenser is communicated with the upper inlet of the secondary rectifying tower; and the bottom outlet of the secondary rectifying tower is communicated with the inlet of a second reboiler, and one outlet of the second reboiler is communicated with the lower inlet of the secondary rectifying tower.
Wherein, the bypass pipeline is connected with a sulfur acid-making device.
Wherein, an inlet at the lower part of the absorption tower is used for introducing ultrapure water, and an inlet at the lower part of the first desorption tower is used for introducing first ultra-clean compressed air.
And an inlet at the lower part of the second degassing tower is used for introducing second ultra-clean compressed air and electronic-grade hydrogen peroxide.
Compared with the prior art, the beneficial effects of the utility model are that:
(1) this device adopts the sulfur trioxide-containing gas that the acid making device sent to absorb and resolve out sulfur trioxide and produce electronic level sulphuric acid through fuming sulphuric acid, and is supporting with the acid making device, low cost. The existing common process adopts nicotinic acid as a raw material to prepare sulfur trioxide by analysis, so that the transportation cost is high, the amount of concentrated sulfuric acid after analysis is large, and the sulfuric acid serving as a byproduct is difficult to sell.
(2) The device adopts a continuous rectification process, light component impurity removal and heavy component impurity removal are respectively completed in different rectification towers, and the rectification steps can be repeated for a plurality of times, so that the method can prepare sulfur trioxide with very high purity, the product quality can be flexibly changed according to the requirements, and the product grade can reach and exceed the SEMI-C12 grade.
(3) The device adopts 98% electronic-grade sulfuric acid to absorb high-purity sulfur trioxide to generate ultrapure sulfuric acid, adjusts the concentration of the electronic-grade sulfuric acid to keep constant by using the ultrapure water, and has high absorption rate and less loss of sulfur trioxide discharged by tail gas.
(4) The device adopts secondary high-purity air to blow off sulfur dioxide, and adds electronic grade hydrogen peroxide in a secondary degassing tower to further increase the content of sulfur dioxide in electronic acid. The process is reliable, the product quality is stable, and the residual quantity of sulfur dioxide can be better than the requirements of SEMI-C12 grade.
(5) The core equipment and the pipeline of the device are made of polytetrafluoroethylene lining, so that impurities can be prevented from being dissolved in electronic-grade sulfuric acid, and the stable quality is ensured.
(6) The tail gas of the device is treated by hydrogen peroxide washing and electric defogging, so that the waste gas can reach the standard and is discharged without waste liquid.
Drawings
Fig. 1 is a schematic diagram of the electronic-grade sulfuric acid production device of the present invention.
Wherein, 1-sulfur trioxide-containing gas, 2-98 percent sulfuric acid, 3-nicotinic acid absorption tower, 4-nicotinic acid circulating tank, 5-nicotinic acid circulating pump, 7-residual gas, 8-fuming sulfuric acid, 9-nicotinic acid evaporator, 11-first-stage rectifying tower, 12-first reboiler, 13-tower top condenser, 14-pipeline, 15-liquid SO 3 16-second-stage rectifying tower, 17-second reboiler, 18-condenser, 19-non-condensable gas, 20-water bath evaporator and 21-high-purity gas SO 3 22-absorption tower, 23-ultrapure water, 24-absorption acid pump, 25-sulfuric acid cooler, 26-first desorption tower, 27-first desorption tower circulating pump, 28-first cooler, 29-absorption tower tail gas, 30-desorption tower tail gas A, 31-tail gas washing tower, 32-tower bottom circulating pump, 33-second cooler, 34-waste gas A, 35-bypass pipeline, 36-electric demister, 37-waste gas B, 38-conveying pipeline, 39-first ultra-clean compressed air, 40-second degassing tower; 41-circulating pump, 42-second ultra-clean compressed air, 43-degassing tower tail gas B, 44-electronic grade hydrogen peroxide.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1, an electronic-grade sulfuric acid production device comprises a nicotinic acid absorption tower 3, a primary rectifying tower 11, a secondary rectifying tower 16, an absorption tower 22, a first desorption tower 26, a second degassing tower 40, a tail gas washing tower 31 and an electric demister 36 which are connected in sequence.
A nicotinic acid circulating tank 4 is arranged below the nicotinic acid absorption tower 3, a nicotinic acid circulating pump 5 is arranged in the nicotinic acid circulating tank 4, an outlet of the nicotinic acid circulating pump 5 is respectively connected with an upper inlet of the nicotinic acid absorption tower 3 and an upper inlet of a nicotinic acid evaporator 9, and a lower outlet of the nicotinic acid evaporator 9 is communicated with the nicotinic acid circulating tank 4; the inlet of the nicotinic acid circulation tank 4 is used for introducing 98% sulfuric acid 2. The lower inlet of the nicotinic acid absorption tower 3 is used for introducing the gas 1 containing sulfur trioxide, and the top outlet of the nicotinic acid absorption tower 3 is used for discharging the residual gas 7.
The top outlet of the nicotinic acid evaporator 9 is communicated with the middle inlet of a first-stage rectifying tower 11, the top of the first-stage rectifying tower 11 is provided with a tower top condenser 13, the tower top condenser 13 is connected with the inlet of a tail gas washing tower 31 through a pipeline 14, and the bottom of the first-stage rectifying tower 11 is provided with a first reboiler 12;
the bottom outlet of the first-stage rectifying tower 11 is respectively communicated with the inlet of the first reboiler 12 and the inlet of the second-stage rectifying tower 16, the top of the second-stage rectifying tower 16 is provided with a condenser 18, one outlet of the condenser 18 is connected with the inlet of a tail gas washing tower 31, the bottom of the second-stage rectifying tower 16 is provided with a second reboiler 17,
an outlet at the top of the primary rectifying tower 11 is communicated with an inlet of a tower top condenser 13, and an outlet of the tower top condenser 13 is communicated with an inlet at the upper part of the primary rectifying tower 11; an outlet of the first reboiler 12 communicates with a lower inlet of the first-stage rectification column 11.
The top outlet of the secondary rectifying tower 16 is communicated with the inlet of a condenser 18, and one outlet of the condenser 18 is communicated with the upper inlet of the secondary rectifying tower 16; the bottom outlet of the secondary rectification column 16 is communicated with the inlet of a second reboiler 17, and one outlet of the second reboiler 17 is communicated with the lower inlet of the secondary rectification column 16.
The other outlet of the condenser 18 is respectively communicated with the upper inlet of the secondary rectifying tower 16 and the water bath evaporator 20; the water bath evaporator 20 is communicated with an inlet of an absorption tower 22, an outlet at the lower part of the absorption tower 22 is communicated with an inlet of an absorption acid pump 24, an outlet of the absorption acid pump 24 is respectively communicated with an inlet of a sulfuric acid cooler 25 and an inlet of a first desorption tower 26, and an outlet of the sulfuric acid cooler 25 is communicated with an inlet at the upper part of the absorption tower 22;
the lower outlet of the first desorption tower 26 is communicated with the inlet of a first desorption tower circulating pump 27, the outlet of the first desorption tower circulating pump 27 is respectively communicated with the inlet of a first cooler 28 and the inlet of a second degassing tower 40, and the outlet of the first cooler 28 is communicated with the upper inlet of the first desorption tower 26;
the lower outlet of the second degassing tower 40 is communicated with a circulating pump 41, and the outlet of the circulating pump 41 is respectively communicated with the upper inlet of the second degassing tower 40 and the conveying pipeline 38;
an inlet at the lower part of the absorption tower 22 is used for introducing ultrapure water 23, and an inlet at the lower part of the first desorption tower 26 is used for introducing first ultra-clean compressed air 39. The ultrapure water is 18.M omega ultrapure water. The ultra-clean compressed air is subjected to oil removal, water removal and precise filtration.
The top outlet of the absorption tower 22, the top outlet of the first desorption tower 26 and the top outlet of the second degassing tower 40 are connected with the inlet of the tail gas washing tower 31; an outlet at the lower part of the tail gas washing tower 31 is connected with an inlet of a tower bottom circulating pump 32, an outlet of the tower bottom circulating pump 32 is respectively communicated with an inlet of a second cooler 33 and a bypass pipeline 35, and an outlet of the second cooler 33 is communicated with an inlet at the upper part of the tail gas washing tower 31; the bypass pipe 35 is connected with a sulfur acid-making device.
The top outlet of the tail gas washing tower 31 is communicated with the lower inlet of the electric demister 36, and the top outlet of the electric demister 36 is used for discharging the waste gas B37;
the lower inlet of the second degassing tower 40 is used for introducing second ultra-clean compressed air 42 and electronic-grade hydrogen peroxide 44.
The device is used for producing electronic-grade sulfuric acid, and the specific process flow is as follows:
(1) the gas 1 containing sulfur trioxide at 170-180 ℃ which is transferred from the sulfur acid-making device is filtered by a filter to remove dust impurities, enters a nicotinic acid absorption tower 3,
(2) the sulfur trioxide in the gas is in countercurrent contact with nicotinic acid which is conveyed by a nicotinic acid circulating pump 5 and cooled to 50-60 ℃ by a nicotinic acid cooler, most of the sulfur trioxide in the gas is sprayed and absorbed by the circulating fuming sulfuric acid in a nicotinic acid tower, and the residual gas 7 returns to an absorption tower inlet of a sulfur acid-making device. The concentration of the nicotinic acid in the nicotinic acid circulating tank 4 is adjusted by adding 98 percent of sulfuric acid 2 and is always maintained in the range of 104.5 to 106 percent.
(3) A part of fuming sulfuric acid produced by the nicotinic acid absorption tower 3 is sent to a nicotinic acid evaporator 9 through a nicotinic acid circulating pump 5, gaseous sulfur trioxide is analyzed through heating, and the temperature of the fuming sulfuric acid condensed into liquid sulfur trioxide through a condenser is about 30-40 ℃, and then the liquid sulfur trioxide enters a storage tank for temporary storage. The nicotinic acid after evaporation returns to the nicotinic acid absorption tower to continuously absorb sulfur trioxide.
(4) The liquid sulfur trioxide in the storage tank is pumped to the middle upper part of the first-stage rectifying tower 11 and is heated and gasified with the first reboiler 12 to form SO 3 The gas contacts with the surface of the filler from bottom to top to carry out mass transfer and heat transfer, rectification and purification, wherein heavy components and part of unvaporized liquid flow back to the bottom of the tower and are continuously heated and gasified in the first reboiler 12; SO after gasification 3 The gas continuously rises to the rectifying section, and continuously carries out mass transfer and heat transfer with the reflux liquid from top to bottom, and further purification is carried out, wherein heavy components are refluxed to the stripping section, and the purified SO 3 Condensing and liquefying the gas to 30-40 ℃ by a tower top condenser 13, and completely refluxing the gas to a primary rectifying tower 11, wherein the uncondensed gas SO 3 And other non-condensable gases are discharged from the line 14 to the tail gas scrubber 31 for absorption treatment.
(5) Liquid SO extracted from the bottom of the first-stage rectifying tower 11 3 15 entering the middle lower part of a second-stage rectifying tower 16, rectifying and purifying through the second-stage rectifying tower 16, discharging residual liquid from a tower kettle, and removing SO 3 The heavy component impurities such as sulfuric acid, metal ions and the like. And condensing and liquefying the sulfur trioxide at the tower top to 30-40 ℃ through a condenser 18, partially refluxing the condensate to a secondary rectifying tower 16, and extracting the other part of the condensate as high-purity liquid sulfur trioxide to a storage tank for temporary storage. The sulfur trioxide content is not less than 99.999 percent, the sulfur dioxide content is less than 1.8ppm, and the total impurity content is controlled within 2.0 mu g/kg. The non-condensable gas 19 at the top of the secondary rectifying tower 16 is sent to a tail gas washing tower 31 for absorption treatment.
(6) The high purity sulfur trioxide in the storage tank is pumped into the water bath evaporator 20. Heating and gasifying 40-50 ℃ high-purity SO gas demisted by a demister with the diameter of 1 mu m 3 21 enter the bottom of an absorption tower 22And flows from bottom to top.
(7) The sulfur trioxide gas and 98.0 percent high-purity sulfuric acid which flows down from the upper part of the absorption tower 22 are in countercurrent contact with each other in the packing layer to generate electronic-grade sulfuric acid, and acid mist particles generated in the absorption process are removed by the tower top fiber demister. And the electronic-grade sulfuric acid generated by absorption is conveyed to a sulfuric acid cooler 25 by an absorption acid pump 24 to be cooled to 40-60 ℃, and then returns to the absorption tower 22 for circulating absorption. The concentration of the circulating acid was adjusted to be stabilized at about 98% by adding ultrapure water to the absorption tower 22. The high-purity sulfuric acid generated in the absorption tower 22 overflows into the SO through a pipeline 2 In the first stripping column 26.
The high purity part is conveyed to a second degassing tower 40 by a first desorption tower circulating pump 27, the other part is cooled by a first cooler 28 and then is conveyed to a first desorption tower 26 for circulation, the high purity part is contacted with clean first ultra-clean compressed air 39 entering from the bottom of the first desorption tower 26 from top to bottom on the surface of a filler, and a small amount of SO dissolved in sulfuric acid 2 The gas is blown out. The temperature of 98% of the electronic acid throughout the degassing is regulated by the first cooler 28.
(8) The electronic-grade sulfuric acid entering the second degassing tower 40 is conveyed to the second degassing tower 40 for circulation through a circulating pump 41, and contacts with clean second ultra-clean compressed air 42 entering from the bottom of the second degassing tower 40 from top to bottom on the surface of the filler to dissolve a small amount of SO in the sulfuric acid 2 The gas is further blown out, and meanwhile, electronic-grade hydrogen peroxide 44 is added to react with sulfur dioxide, so that the content of the sulfur dioxide is effectively controlled to be below 1 ppm. The degassed electronic grade sulfuric acid is conveyed by a pump through a conveying pipeline 38 to enter a finished product storage tank for storage, and is further filtered by a precision filter to obtain SEMI-C12 grade electronic grade sulfuric acid.
(9) The tail gas 29 of the absorption tower 22, the tail gas A30 of the desorption tower of the first desorption tower 26 and the tail gas B43 of the degassing tower of the second degassing tower 40, which are discharged from the top condenser 13 and the condenser 18, enter the bottom of the tail gas washing tower 31, flow from bottom to top, and are in countercurrent contact with the absorption liquid which is conveyed by the bottom circulating pump 32 and flows downwards from the upper part on the surface of a packing, hydrogen peroxide in the absorption liquid reacts with sulfur dioxide to generate sulfuric acid, and the temperature of the absorption liquid is regulated by the second cooler 33. The generated 20-30% dilute sulfuric acid is conveyed to a sulfur acid making device through a bypass pipeline 35 at the outlet of a tower bottom circulating pump 32 and is recycled as absorption tower liquid supplement.
(10) And the waste gas A34 at the top outlet of the tail gas washing tower 31 enters an electric demister 36 to remove acid mist, and the waste gas B37 is discharged from a chimney at high altitude up to the standard.
Wherein, the steps (1) to (3) can be replaced by adopting finished product nicotinic acid or pure sulfur trioxide as raw materials.
The nicotinic acid after evaporation in the step (3) can enter a preheater and be used as a heat source to heat fuming sulfuric acid sent for evaporation, so that the energy consumption is saved.
The steps (4) and (5) can be repeatedly arranged for a plurality of times according to different requirements on the quality of the electronic-grade sulfuric acid product, and the quality of the electronic-grade sulfuric acid product can reach a higher level.
In the step (6), the heat source of the water bath evaporator is preferably heated by hot water, and other heating media such as steam, heat-conducting oil and the like can also be adopted. The sulfur trioxide gasified by the water bath evaporator adopts a PFA demister, liquid foam can be removed, and the purity of the sulfur trioxide is ensured.
In the step (7), the absorption tower and the absorption tower circulating tank can be made into an integral device which is connected together, or can be made into two independent devices separately.
In the step (8), the ultra-clean compressed air can be replaced by other inert gases such as high-purity nitrogen and the like.
Core equipment such as a rectifying tower, an absorption tower, a degassing tower, an electronic-grade sulfuric acid storage tank and the like adopt fluoroplastic linings to prevent impurities from being dissolved into a product.
The electronic-grade sulfuric acid detection report prepared by the device is shown in table 1.
TABLE 1 electronic-grade sulfuric acid test report
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. An electronic-grade sulfuric acid production device is characterized in that: comprises a nicotinic acid absorption tower (3), a first-stage rectifying tower (11), a second-stage rectifying tower (16), an absorption tower (22), a first desorption tower (26), a second degassing tower (40), a tail gas washing tower (31) and an electric demister (36) which are connected in sequence.
2. The electronic grade sulfuric acid production plant of claim 1, characterized in that: a nicotinic acid circulating tank (4) is arranged below the nicotinic acid absorption tower (3), a nicotinic acid circulating pump (5) is arranged in the nicotinic acid circulating tank (4), an outlet of the nicotinic acid circulating pump (5) is respectively connected with an upper inlet of the nicotinic acid absorption tower (3) and an upper inlet of a nicotinic acid evaporator (9), and a lower outlet of the nicotinic acid evaporator (9) is communicated with the nicotinic acid circulating tank (4);
the top outlet of the nicotinic acid evaporator (9) is communicated with the middle inlet of a first-stage rectifying tower (11), the top of the first-stage rectifying tower (11) is provided with an overhead condenser (13), the overhead condenser (13) is connected with the inlet of a tail gas washing tower (31) through a pipeline (14), and the bottom of the first-stage rectifying tower (11) is provided with a first reboiler (12);
the bottom outlet of the first-stage rectifying tower (11) is respectively communicated with the inlet of the first reboiler (12) and the inlet of the second-stage rectifying tower (16), the top of the second-stage rectifying tower (16) is provided with a condenser (18), one outlet of the condenser (18) is connected with the inlet of the tail gas washing tower (31), and the bottom of the second-stage rectifying tower (16) is provided with a second reboiler (17);
the other outlet of the condenser (18) is respectively communicated with the upper inlet of the secondary rectifying tower (16) and the water bath evaporator (20); the water bath evaporator (20) is communicated with an inlet of an absorption tower (22), an outlet at the lower part of the absorption tower (22) is communicated with an inlet of an absorption acid pump (24), an outlet of the absorption acid pump (24) is respectively communicated with an inlet of a sulfuric acid cooler (25) and an inlet of a first desorption tower (26), and an outlet of the sulfuric acid cooler (25) is communicated with an inlet at the upper part of the absorption tower (22);
the lower outlet of the first desorption tower (26) is communicated with the inlet of a first desorption tower circulating pump (27), the outlet of the first desorption tower circulating pump (27) is respectively communicated with the inlet of a first cooler (28) and the inlet of a second desorption tower (40), and the outlet of the first cooler (28) is communicated with the upper inlet of the first desorption tower (26);
the lower outlet of the second degassing tower (40) is communicated with a circulating pump (41), and the outlet of the circulating pump (41) is respectively communicated with the upper inlet of the second degassing tower (40) and the conveying pipeline (38);
the top outlet of the absorption tower (22), the top outlet of the first desorption tower (26) and the top outlet of the second degassing tower (40) are connected with the inlet of a tail gas washing tower (31); an outlet at the lower part of the tail gas washing tower (31) is connected with an inlet of a tower bottom circulating pump (32), an outlet of the tower bottom circulating pump (32) is respectively communicated with an inlet of a second cooler (33) and a bypass pipeline (35), and an outlet of the second cooler (33) is communicated with an inlet at the upper part of the tail gas washing tower (31);
and a top outlet of the tail gas washing tower (31) is communicated with a lower inlet of an electric demister (36), and a top outlet of the electric demister (36) is used for discharging waste gas B (37).
3. The electronic grade sulfuric acid production plant of claim 2, characterized in that: the lower inlet of the nicotinic acid absorption tower (3) is used for introducing gas (1) containing sulfur trioxide, and the top outlet of the nicotinic acid absorption tower (3) is used for discharging residual gas (7).
4. The electronic grade sulfuric acid production plant of claim 3, characterized in that: the inlet of the nicotinic acid circulating tank (4) is used for introducing 98 percent of sulfuric acid (2).
5. The electronic grade sulfuric acid production plant of claim 4, characterized in that: an outlet at the top of the primary rectifying tower (11) is communicated with an inlet of a tower top condenser (13), and an outlet of the tower top condenser (13) is communicated with an inlet at the upper part of the primary rectifying tower (11); an outlet of the first reboiler (12) is communicated with a lower inlet of the first-stage rectifying tower (11).
6. The electronic grade sulfuric acid production plant of claim 5, characterized in that: the top outlet of the secondary rectifying tower (16) is communicated with the inlet of a condenser (18), and one outlet of the condenser (18) is communicated with the upper inlet of the secondary rectifying tower (16); the bottom outlet of the secondary rectifying tower (16) is communicated with the inlet of a second reboiler (17), and one outlet of the second reboiler (17) is communicated with the lower inlet of the secondary rectifying tower (16).
7. The electronic grade sulfuric acid production plant of claim 6, characterized in that: the bypass pipeline (35) is connected with a sulfur acid-making device.
8. The electronic grade sulfuric acid production plant of claim 7, characterized in that: an inlet at the lower part of the absorption tower (22) is used for introducing ultrapure water (23), and an inlet at the lower part of the first desorption tower (26) is used for introducing first ultra-clean compressed air (39).
9. The electronic grade sulfuric acid production plant of claim 8, characterized in that: and an inlet at the lower part of the second degassing tower (40) is used for introducing second ultra-clean compressed air (42) and electronic-grade hydrogen peroxide (44).
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115583632A (en) * | 2022-10-28 | 2023-01-10 | 天津环渤新材料有限公司 | Method for producing electronic-grade sulfuric acid by absorption method |
| 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 |
| CN117205856A (en) * | 2023-09-21 | 2023-12-12 | 福建天甫电子材料有限公司 | Automatic control system for electronic grade sulfuric acid production and method for producing electronic grade sulfuric acid |
| CN117427362A (en) * | 2023-12-21 | 2024-01-23 | 联仕新材料(苏州)股份有限公司 | Method and system for producing electronic grade sulfuric acid |
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2022
- 2022-05-07 CN CN202221083942.7U patent/CN217418195U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115583632A (en) * | 2022-10-28 | 2023-01-10 | 天津环渤新材料有限公司 | Method for producing electronic-grade sulfuric acid by absorption method |
| 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 |
| CN117205856A (en) * | 2023-09-21 | 2023-12-12 | 福建天甫电子材料有限公司 | Automatic control system for electronic grade sulfuric acid production and method for producing electronic grade sulfuric acid |
| CN117427362A (en) * | 2023-12-21 | 2024-01-23 | 联仕新材料(苏州)股份有限公司 | Method and system for producing electronic grade sulfuric acid |
| CN117427362B (en) * | 2023-12-21 | 2024-03-08 | 联仕(江西)新材料有限公司 | Method and system for producing electronic grade sulfuric acid |
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