CN103407972B - Production method of electronic-grade sulphuric acid - Google Patents
Production method of electronic-grade sulphuric acid Download PDFInfo
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- CN103407972B CN103407972B CN201310340782.9A CN201310340782A CN103407972B CN 103407972 B CN103407972 B CN 103407972B CN 201310340782 A CN201310340782 A CN 201310340782A CN 103407972 B CN103407972 B CN 103407972B
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Abstract
The invention discloses a production method of electronic-grade sulphuric acid. The production method comprises the following steps in sequence: industrial-grade sulfur trioxide raw materials are provided and placed into a raw material storage tank; the sulfur trioxide raw materials are conveyed into an evaporator tank; the evaporator tank is heated; sulfur trioxide steam generated by heating enters into an absorption tower through a filter; the sulfur trioxide steam is absorbed by electronic-grade ultrapure water in the absorption tower, the concentration of absorption liquid is controlled, and the absorbed solution enters into a degassing tower after cooled by a cooler; air stripping is performed on a sulfuric acid solution by the degassing tower through compressed air; the sulfuric acid solution enters into a finished product storage tank after cooled; finally, the final electronic-grade sulphuric acid applied to the integrated circuit industry is obtained after ultrafiltration to remove particles. The operating temperature of the technology, compared with a conventional technology, is lower than 120 DEG C. Therefore, the technology is safer than a high-temperature distillation technology which takes industrial-grade sulfuric acid as raw material, and in addition, compared with adopting equipment made of quartz glass, non-pollution to electronic-grade sulphuric acid products is guaranteed from equipment material.
Description
Technical field
The present invention relates to a kind of sulfuric acid manufacture method, particularly relate to the Production method of electronic-grade sulphuric acid required for the production of a kind of large-scale integrated circuit.
Background technology
Sulfuric acid, chemical formula is H
2sO
4, relative molecular mass is 98.08, is a kind of colorless and odorless oily liquids, is the strong acid of a kind of high boiling point difficulty volatilization, soluble in water, can with arbitrarily than miscible with water.Sulfuric acid is one of staple product in basic chemical industry.It not only as the raw material of many Chemicals, but also is widely used in other sector of the national economy.
Electronic-grade sulfuric acid is widely used in ic manufacturing process at present, and peel off as resist, the concentration of the most frequently used sulfuric acid is about 96%.The organic pollutant remained on substrate and relevant device can to normally exerting an adverse impact, and the hydrogen peroxide that sulfuric acid combined or ozone can remove the organic pollutant on substrate surface before metal refining.
The preparation technology of electronic-grade sulfuric acid mainly contains rectification method etc.What current Application comparison was many is the electronic-grade sulfuric acid product adopting the technical grade vitriol oil of concentration 98% to obtain about 98% after high temperature rectifying.Because the boiling point of sulfuric acid is very high, the sulfuric acid boiling point at ambient pressure of 98% is 338 DEG C, therefore electrical heating wire must be used in quartz container, to add thermal distillation to sulphuric acid soln, operate at such high temperatures, not only energy consumption is high, also brings certain security risk, in addition, due to the severe corrosive of the vitriol oil, the sulfuric acid that pyrogenic distillation goes out can dissolve the part impurity in glass equipment, and the sulfuric acid caused with this method is produced is difficult to reach the electronic-grade standard really meeting unicircuit and require.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of Production method of electronic-grade sulphuric acid, and process safety is reliable, and product mass-energy reaches the electronic-grade standard of unicircuit requirement, and can realize continuous print scale operation.
In order to solve the problems of the technologies described above, technical scheme of the present invention there is provided a kind of Production method of electronic-grade sulphuric acid, it is characterized in that, step is:
Step 1, provide the incoming stock storage tank of sulphur trioxide raw material of technical grade;
Step 2, the sulphur trioxide raw material being positioned at raw material storage tank are transported into evaporator tank again;
Step 3, to the sulphur trioxide heating raw materials in evaporator tank, heating after produce sulfur trioxide vapor after strainer, enter absorption tower;
Step 4, absorb sulfur trioxide vapor with electronic grade ultrapure water in adsorption tower, control the concentration of absorption liquid, the sulphuric acid soln after absorption is admitted in the first water cooler by the first transmission pump and cools, and cooled sulphuric acid soln enters in degassing tower;
Step 5, in degassing tower, adopt pressurized air to carry out stripping to sulphuric acid soln, then enter the second water cooler cooling again, cooled sulphuric acid soln enters finished product storage tank and stores;
Sulphuric acid soln in step 6, finished product storage tank is removed after particle through ultrafiltration and is obtained the final electronic-grade sulfuric acid being applied to integrated circuit industry.
Preferably, described raw material storage tank is stainless steel.
Preferably, in described step 2, the mode of movement of sulphur trioxide raw material is pump transmission or uses nitrogen binder; The material of described evaporating pot is stainless steel.
Preferably, in described step 3, the mode of heating is the one in hot water heating, steam heating or electrically heated, and the temperature of heating controls at 45-60 DEG C.
Preferably, the filter core of the first strainer in described step 3 adopts tetrafluoroethylene material filter core, and its filter housing is stainless steel or carbon steel inner liner polytetrafluoroethylene material.
Preferably, when the electronic grade ultrapure water in described step 4 is 25 DEG C, resistivity can reach 18M Ω cm.
Preferably, described absorption tower and described first water cooler are stainless steel or the included tetrafluoroethylene material of carbon steel; The filler of the two-layer tetrafluoroethylene arranged up and down is housed in described absorption tower, and described electronic grade ultrapure water enters absorption tower by between two-layer filler, and described sulfur trioxide vapor enters absorption tower by the below of the filler being positioned at lower floor; The temperature on described absorption tower controls at 80-120 DEG C; The temperature out of described first water cooler controls at 40-80 DEG C.
Preferably, described degassing tower is the included tetrafluoroethylene material of stainless steel or carbon steel, the filler of tetrafluoroethylene is housed in this degassing tower, and described cooled sulphuric acid soln enters degassing tower by the top of filler, and described pressurized air enters degassing tower by the below of filler.
Preferably, the pressurized air clean without oil of to be pressure the be 1bar-3bar of the pressurized air in described step 5.
Preferably, described finished product storage tank adopts stainless steel or carbon steel liner fluorine material.
Preferably, in described step 6, sulphuric acid soln in finished product storage tank enters in the second strainer via the second transmission pump and carries out ultrafiltration, and the filter core of the second strainer is submicron order tetrafluoroethylene material, and its filter housing is stainless steel or carbon steel inner liner polytetrafluoroethylene material.
The present invention contrasts prior art following beneficial effect: Production method of electronic-grade sulphuric acid provided by the invention, adopts that the sulphur trioxide of technical grade absorbs through pervaporation, ultrapure water, cooling, degassed, cooling, obtained after ultrafiltration.Compare with existing technique, the service temperature of present invention process is lower than 120 DEG C, therefore more safer as raw material pyrogenic distillation technique than technical grade sulfuric acid, in addition, the device that present invention process adopts is substantially all stainless steel or carbon steel inner liner polytetrafluoroethylene material, tetrafluoroethylene is a kind of synthetic macromolecular material employing fluorine and replace all hydrogen atoms in polyethylene, this material has antiacid alkali resistant, the feature of anti-various organic solvent, be dissolved in all soda acids hardly, simultaneously, tetrafluoroethylene has resistant to elevated temperatures feature, therefore contrast adopts in quartz glass apparatus slave unit material and ensure that and can not bring pollution to electronic-grade sulfuric acid product.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the system that the present invention adopts.
Embodiment
For making the present invention become apparent, hereby with preferred embodiment, and accompanying drawing is coordinated to be described in detail below.
Composition graphs 1, Production method of electronic-grade sulphuric acid provided by the invention, comprises the steps:
S1: the incoming stock storage tank of sulphur trioxide raw material that technical grade is provided;
S2: above-mentioned sulphur trioxide feedstock transportation is entered in evaporator tank, sulphur trioxide mode of movement includes but not limited to pump transmission and uses nitrogen binder;
S3: adopt hot water, steam or electrically heated to the sulphur trioxide heating raw materials in evaporator tank, add thermogenetic sulfur trioxide vapor and enter absorption tower 2 after the first strainer 1;
S4: with electronic grade ultrapure water, sulfur trioxide vapor is absorbed in absorption tower 2, be 97% ± 0.5% by controlling the concentration of the flow of sulfur trioxide vapor and the Flow-rate adjustment absorbent solution of ultrapure water, the solution after absorption is sent into after the first water cooler 4 cools via the first transmission pump 3 and is entered degassing tower 7;
S5: degassing tower 7 adopts pressurized air to carry out stripping to sulphuric acid soln, then after the second water cooler 5 cools, enter finished product storage tank 6 again, compressed-air actuated pressure is 1bar-3bar;
S6: sulfuric acid finished product is sent in the second strainer 8 by the second transmission pump 9 again, obtains final qualified product after the filter element filtering of the second strainer 8 tetrafluoroethylene material.
The sulfuric acid product technical indicator obtained sees the following form:
| Technical indicator | Product |
| Content (H 2SO 4) | 96-98％ |
| Colourity (APHA) | ＜10 |
| Various metallic impurity | ≤100ppt |
| Various anionic impurity content | ≤100ppb |
| Dust granules (>=0.5um) | ≤ 5/ml |
As seen from the above table, present invention process produces single metal ion content < 100ppt in the sulfuric acid obtained, and single anion-content < 100ppb is greater than the particle < 5/milliliter of 0.5um.
Embodiment 1
See Fig. 1, the implementation step of embodiment 1 is as follows:
1): the incoming stock storage tank of sulphur trioxide raw material that technical grade is provided;
2): above-mentioned sulphur trioxide raw material impeller pump is delivered in evaporator tank;
3): adopt hot water to heat evaporator tank, heating and temperature control, at 60 DEG C, adds thermogenetic sulfur trioxide vapor and enter absorption tower 2 after the first strainer 1;
4): with electronic grade ultrapure water, sulfur trioxide vapor is absorbed in adsorption tower 2, be 97% ± 0.5% by controlling the concentration of the flow of sulfur trioxide vapor and the Flow-rate adjustment absorbent solution of ultrapure water, the temperature on absorption tower 2 controls at 100 DEG C, solution after absorption enters degassing tower 7 after the first water cooler 4 cools, and the temperature out of the first water cooler 4 controls at 50 DEG C;
5): degassing tower 7 adopts pressurized air to carry out stripping to sulphuric acid soln, then again through overcooling laggard enter finished product storage tank, compressed-air actuated pressure is 2bar;
6): sulfuric acid finished product obtains final qualified product again after the filter element filtering of tetrafluoroethylene material.
The sulfuric acid product technical indicator obtained sees the following form:
| Technical indicator | Product |
| Content (H 2SO 4) | 96-98％ |
| Colourity (APHA) | 5 |
| Various metallic impurity | ≤90ppt |
| Various anionic impurity content | ≤80ppb |
| Dust granules (>=0.5um) | 3/ml |
Embodiment 2
See Fig. 1, the implementation step of embodiment 2 is as follows:
1): the incoming stock storage tank of sulphur trioxide raw material that technical grade is provided;
2): by above-mentioned sulphur trioxide raw material nitrogen press-in evaporator tank;
3): adopt steam to heat evaporator tank, heating and temperature control, at 70 DEG C, adds thermogenetic sulfur trioxide vapor and enter absorption tower 2 after the first strainer 1;
4): with electronic grade ultrapure water, sulfur trioxide vapor is absorbed in adsorption tower 2, be 97% ± 0.5% by controlling the concentration of the flow of sulfur trioxide vapor and the Flow-rate adjustment absorbent solution of ultrapure water, the temperature on absorption tower 2 controls at 95 DEG C, solution after absorption enters degassing tower 7 after the first water cooler 4 cools, and the temperature out of the first water cooler 4 controls at 45 DEG C;
5): degassing tower 7 adopts pressurized air to carry out stripping to sulphuric acid soln, then again through overcooling laggard enter finished product storage tank 6, compressed-air actuated pressure is 3bar;
6): sulfuric acid finished product obtains final qualified product again after the filter element filtering of tetrafluoroethylene material.
The sulfuric acid product technical indicator obtained sees the following form:
| Technical indicator | Product |
| Content (H 2SO 4) | 96-98％ |
| Colourity (APHA) | 10 |
| Various metallic impurity | ≤80ppt |
| Various anionic impurity content | ≤100ppb |
| Dust granules (>=0.5um) | 5/ml |
Embodiment 3
See Fig. 1, the implementation step of embodiment 3 is as follows:
1): the incoming stock storage tank of sulphur trioxide raw material that technical grade is provided;
2): above-mentioned sulphur trioxide raw material impeller pump is delivered in evaporator tank;
3): adopt electrical heating wire to heat evaporator tank, heating and temperature control, at 50 DEG C, adds thermogenetic sulfur trioxide vapor and enter absorption tower 2 after the first strainer 1;
4): with electronic grade ultrapure water, sulfur trioxide vapor is absorbed in adsorption tower 2, be 97% ± 0.5% by controlling the concentration of the flow of sulfur trioxide vapor and the Flow-rate adjustment absorbent solution of ultrapure water, the temperature on absorption tower 2 controls at 85 DEG C, solution after absorption enters degassing tower 7 after the first water cooler 4 cools, and the temperature out of the first water cooler 4 controls at 45 DEG C;
5): degassing tower 7 adopts pressurized air to carry out stripping to sulphuric acid soln, then again through overcooling laggard enter finished product storage tank 6, compressed-air actuated pressure is 1bar;
6): sulfuric acid finished product obtains final qualified product again after the filter element filtering of tetrafluoroethylene material.
The sulfuric acid product technical indicator obtained sees the following form:
| Technical indicator | Product |
| Content (H 2SO 4) | 96-98％ |
| Colourity (APHA) | 5 |
| Various metallic impurity | ≤100ppt |
| Various anionic impurity content | ≤100ppb |
| Dust granules (>=0.5um) | 3/ml |
As can be seen here, Production method of electronic-grade sulphuric acid process safety provided by the invention is reliable, and product purity is high, and impurity ion content is low, can be applied to the production of large-scale integrated circuit.Sulfuric acid boiling point due to 98% is very high at about 338 DEG C, the present invention is by carrying out production electronic-grade sulfuric acid by the method that ultrapure water absorbs after evaporation sulphur trioxide, and do not need the technique of high temperature rectifying, in addition, the device adopted is substantially all stainless steel lined tetrafluoroethylene material, and contrast adopts in quartz glass apparatus slave unit material and ensure that and can not bring pollution to electronic-grade sulfuric acid product.
Although the present invention discloses as above with preferred embodiment; so itself and be not used to limit the present invention, any those skilled in the art, without departing from the spirit and scope of the present invention; when doing a little amendment and perfect, therefore protection scope of the present invention is when being as the criterion of defining with claims.
Claims (11)
1. a Production method of electronic-grade sulphuric acid, is characterized in that, step is:
Step 1, provide the incoming stock storage tank of sulphur trioxide raw material of technical grade;
Step 2, the sulphur trioxide raw material being positioned at raw material storage tank are transported into evaporator tank again;
Step 3, to the sulphur trioxide heating raw materials in evaporator tank, the sulfur trioxide vapor produced after heating enters absorption tower (2) after strainer (1), and the filter core of strainer (1) adopts tetrafluoroethylene material filter core;
Step 4, with electronic grade ultrapure water, sulfur trioxide vapor to be absorbed in absorption tower (2), control the concentration of absorption liquid, sulphuric acid soln after absorption is admitted to cooling in the first water cooler (4) by the first transmission pump (3), and cooled sulphuric acid soln enters in degassing tower (7);
Absorption tower (2) is stainless steel or the included tetrafluoroethylene material of carbon steel; The filler of the two-layer tetrafluoroethylene arranged up and down is housed in absorption tower (2), electronic grade ultrapure water is by entering absorption tower (2) between two-layer filler, sulfur trioxide vapor enters absorption tower (2) by the below of the filler being positioned at lower floor, and the cooled sulphuric acid soln going out the first water cooler (4) is back to (2) top, absorption tower and the packing layer top position being positioned at upper strata sprays;
Step 5, in degassing tower (7) adopt pressurized air stripping is carried out to sulphuric acid soln, then enter again the second water cooler (5) cooling, cooled sulphuric acid soln enter finished product storage tank (6) store;
Sulphuric acid soln in step 6, finished product storage tank (6) is removed after particle through ultrafiltration and is obtained the final electronic-grade sulfuric acid being applied to integrated circuit industry.
2. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, described raw material storage tank is stainless steel.
3. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, in described step 2, the mode of movement of sulphur trioxide raw material is pump transmission or uses nitrogen binder; The material of described evaporator tank is stainless steel.
4. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, in described step 3, the mode of heating is the one in hot water heating, steam heating or electrically heated, and the temperature of heating controls at 45-60 DEG C.
5. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, described strainer (1) filter housing is stainless steel or carbon steel inner liner polytetrafluoroethylene material.
6. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, when the electronic grade ultrapure water in described step 4 is 25 DEG C, resistivity can reach 18M Ω cm.
7. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, described absorption tower (2) and described first water cooler (4) are stainless steel or the included tetrafluoroethylene material of carbon steel; The filler of the two-layer tetrafluoroethylene arranged up and down is housed in described absorption tower (2), and described electronic grade ultrapure water is by entering absorption tower (2) between two-layer filler, described sulfur trioxide vapor enters absorption tower (2) by the below of the filler being positioned at lower floor; The temperature on described absorption tower (2) controls at 80-120 DEG C; The temperature out of described first water cooler (4) controls at 40-80 DEG C.
8. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, it is characterized in that, described degassing tower (7) is stainless steel or the included tetrafluoroethylene material of carbon steel, the filler of tetrafluoroethylene is housed in this degassing tower (7), described cooled sulphuric acid soln enters degassing tower (7) by the top of filler, and described pressurized air enters degassing tower (7) by the below of filler.
9. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, the pressurized air clean without oil of to be pressure the be 1bar-3bar of the pressurized air in described step 5.
10. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, is characterized in that, described finished product storage tank (6) adopts stainless steel or carbon steel liner fluorine material.
11. a kind of Production method of electronic-grade sulphuric acid as claimed in claim 1, it is characterized in that, in described step 6, sulphuric acid soln in finished product storage tank (6) enters in the second strainer (8) via the second transmission pump (9) and carries out ultrafiltration, the filter core of the second strainer (8) is submicron order tetrafluoroethylene material, and its filter housing is stainless steel or carbon steel inner liner polytetrafluoroethylene material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621374A (en) * | 2016-02-16 | 2016-06-01 | 江苏达诺尔科技股份有限公司 | Preparation method of ultra-pure sulfuric acid |
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| CN104925759B (en) * | 2015-04-29 | 2017-04-19 | 苏州晶瑞化学股份有限公司 | Continuous production method of sulfuric acid with ultrahigh purity |
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| CN110255506A (en) * | 2019-07-15 | 2019-09-20 | 湖北兴福电子材料有限公司 | A kind of apparatus and method of electronic-grade sulfuric acid production |
| CN110980657B (en) * | 2019-12-02 | 2022-03-18 | 湖北兴福电子材料有限公司 | Sulfuric acid production device and method for reducing electronic-grade sulfuric acid oxidizable substances |
| CN111994879A (en) * | 2020-08-27 | 2020-11-27 | 福建天甫电子材料有限公司 | Preparation process of electronic-grade sulfuric acid |
| CN111908432A (en) * | 2020-09-09 | 2020-11-10 | 江苏庆峰工程集团有限公司 | Production method and production device for refining 98% sulfuric acid for electronic industry |
| CN112320768B (en) * | 2021-01-04 | 2021-03-30 | 联仕(昆山)化学材料有限公司 | Production method of electronic-grade sulfuric acid |
| CN114212759A (en) * | 2021-11-26 | 2022-03-22 | 安徽金禾实业股份有限公司 | Production process of high-purity liquid sulfur trioxide |
| CN114348972B (en) * | 2021-12-10 | 2023-05-05 | 湖北兴福电子材料股份有限公司 | Intelligent vaporization and energy recycling method and device for electronic grade sulfuric acid production |
| CN115448259A (en) * | 2022-07-22 | 2022-12-09 | 江化微(镇江)电子材料有限公司 | Production method of electronic-grade sulfuric acid |
| CN116374967B (en) * | 2023-04-17 | 2024-07-23 | 四川金象赛瑞化工股份有限公司 | Preparation process of high-purity nitric acid |
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| DE19963509A1 (en) * | 1999-12-28 | 2001-07-05 | Merck Patent Gmbh | Process for the production of high-purity sulfuric acid |
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| CN105621374A (en) * | 2016-02-16 | 2016-06-01 | 江苏达诺尔科技股份有限公司 | Preparation method of ultra-pure sulfuric acid |
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Address after: 201108 Minhang District Spring Road, No. 56, Shanghai Patentee after: SHANGHAI ZHENGFAN TECHNOLOGY CO., LTD. Patentee after: Hefei Zhengfan Electronic Material Co., Ltd. Address before: 201108 Minhang District Spring Road, No. 56, Shanghai Patentee before: Shanghai Zhengfan Technology Co., Ltd. Patentee before: Hefei Zhengfan Electronic Material Co., Ltd. |