CN116281876A - Preparation method and production system of electronic grade sulfuric acid - Google Patents
Preparation method and production system of electronic grade sulfuric acid Download PDFInfo
- Publication number
- CN116281876A CN116281876A CN202310220873.2A CN202310220873A CN116281876A CN 116281876 A CN116281876 A CN 116281876A CN 202310220873 A CN202310220873 A CN 202310220873A CN 116281876 A CN116281876 A CN 116281876A
- Authority
- CN
- China
- Prior art keywords
- sulfuric acid
- tank
- electronic grade
- sulfur trioxide
- absorption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 title claims abstract description 197
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Chemical compound O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 claims abstract description 138
- 238000010521 absorption reaction Methods 0.000 claims abstract description 53
- 238000001816 cooling Methods 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 44
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 42
- 239000012498 ultrapure water Substances 0.000 claims abstract description 42
- 238000007664 blowing Methods 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 22
- 238000003860 storage Methods 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- 238000001914 filtration Methods 0.000 claims abstract description 15
- 238000007599 discharging Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000012544 monitoring process Methods 0.000 claims abstract description 5
- 238000005070 sampling Methods 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 239000012528 membrane Substances 0.000 claims description 12
- 238000000108 ultra-filtration Methods 0.000 claims description 12
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 238000002309 gasification Methods 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract 1
- 230000001276 controlling effect Effects 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 150000001450 anions Chemical class 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/74—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
A preparation method and a production system of electronic grade sulfuric acid comprise the following steps: step one: the sulfur trioxide is sent into a heating tank to be heated to generate gaseous sulfur trioxide, and the gaseous sulfur trioxide is sent into an absorption tank to be absorbed with electronic grade ultrapure water to generate sulfuric acid through filtration and rectification; step two: monitoring the concentration of sulfuric acid in the absorption tank, and discharging the sulfuric acid into a cooling kettle for cooling when the concentration reaches 97-98%; step three: after cooling, feeding the mixture into a blowing tower for impurity removal; step four: filtering after blowing to obtain the finished product electronic grade sulfuric acid, and sending the finished product electronic grade sulfuric acid into a finished product storage tank for storage. The method for finally obtaining the electronic grade sulfuric acid by adopting the reaction of the sulfur trioxide gasification and the ultrapure water has low energy consumption, performs safety protection on a large amount of gas and heat generated by the reaction of the sulfur trioxide gasification and the ultrapure water, and simultaneously can effectively recycle a large amount of heat generated by the reaction of the gasified sulfur trioxide and the ultrapure water, thereby fully utilizing energy.
Description
Technical Field
The invention belongs to the field of electronic grade sulfuric acid production, and particularly relates to a preparation method and a production system of electronic grade sulfuric acid.
Background
Electronic grade sulfuric acid is a common reagent applied to the electronic industry, and along with the continuous development of the electronic industry, the demand of the electronic grade sulfuric acid is also continuously increased, but the most adopted method in the current production is to heat and rectify industrial grade concentrated sulfuric acid to obtain the electronic grade sulfuric acid, but the sulfuric acid has high boiling point and can be evaporated only at the temperature of more than 340 ℃ generally, so that the energy consumption is high, the sulfuric acid has strong corrosiveness, and the high-temperature heating can cause the sulfuric acid to dissolve a part of substances in equipment so as to introduce unknown impurities.
Disclosure of Invention
The invention provides a preparation method and a production system of electronic grade sulfuric acid, which are used for solving the defects in the prior art.
The invention is realized by the following technical scheme:
the preparation method of the electronic grade sulfuric acid comprises the following steps:
step one: the sulfur trioxide is sent into a heating tank to be heated at the temperature of 70-90 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is sent into an absorption tank to be absorbed with electronic grade ultrapure water to generate sulfuric acid through filtration and rectification, the temperature in the absorption tower is controlled at 90-110 ℃, and a safety protection device is additionally arranged on the heating tank and the absorption tank;
step two: monitoring the concentration of sulfuric acid in the absorption tank, controlling the reaction by controlling the flow of gaseous sulfur trioxide and ultrapure water, discharging sulfuric acid into a cooling kettle for cooling when the concentration reaches 97-98%, and cooling to 35-55 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into an air blowing tower for impurity removal, wherein compressed air enters the air blowing tower from the lower part of the air blowing tower to remove impurities from the sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 2-4bar;
step four: filtering after blowing to obtain the finished product electronic grade sulfuric acid, and sending the finished product electronic grade sulfuric acid into a finished product storage tank for storage.
According to the preparation method of the electronic grade sulfuric acid, the ultrafiltration membrane is adopted for filtration in the first step and the fourth step, and the ultrafiltration membrane is made of tetrafluoroethylene.
According to the preparation method of the electronic grade sulfuric acid, heat exchanged in the absorption tank and the cooling kettle can be used for gasifying and heating sulfur trioxide.
The utility model provides a production system of electronic grade sulfuric acid, includes the heating jar, heating jar top intercommunication sulfur trioxide inlet pipe and sulfur trioxide discharging pipe, the first filter of sulfur trioxide discharging pipe connection, pipeline intercommunication is passed through with the bottom of rectifying column to first filter, pipeline and absorption jar lower part intercommunication are passed through at the top of rectifying column, the absorption jar top advances the pipe intercommunication with ultrapure water, the ultrapure water advances the pipe and is being connected the water spray orifice board with one end in the absorption jar, the absorption jar bottom passes through pipeline and cooling kettle upper portion intercommunication, set up first acid pump on the communicating pipe of absorption jar and cooling kettle, the cooling kettle bottom passes through pipeline and the top intercommunication of blowing tower, set up the second acid pump on the pipeline between cooling kettle and the blowing tower, the blowing tower bottom passes through pipeline and finished product storage tank top intercommunication, set up third acid pump and second filter on the pipeline between blowing tower and the finished product storage tank.
The theoretical plate number of the rectifying tower is 20-30, the operating temperature is 50-80 ℃, the operating pressure is 0.4-0.5MPa, and the reflux ratio is 40-60.
According to the electronic grade sulfuric acid production system, the top ends of the heating tank and the absorbing tank are communicated with one end of the safety valve, and the other end of the safety valve is communicated with the buffer tank.
According to the production system of the electronic grade sulfuric acid, the lower parts of the heating tank, the absorbing tank and the cooling kettle are hollow cavities, one side of the cavity of the heating tank is communicated with one side of the cavity of the absorbing tank through a pipeline, the other side of the cavity of the absorbing tank is communicated with one side of the cavity of the cooling kettle through a pipeline, the other side of the cavity of the cooling kettle is communicated with the other side of the cavity of the heating tank through a pipeline, and a heat pump is arranged between the other side of the cavity of the cooling kettle and the communicated pipeline of the other side of the cavity of the heating tank.
According to the production system of the electronic grade sulfuric acid, the one-way valve is arranged on the sulfur trioxide feeding pipe.
According to the electronic grade sulfuric acid production system, the sulfur trioxide control valve is arranged on the pipeline, communicated with the absorption tank, of the rectifying tower, and the ultrapure water inlet pipe is provided with the ultrapure water control valve.
According to the electronic grade sulfuric acid production system, the sampling pipe is arranged at the lower part of the absorption tower, and the sampling valve is arranged on the sampling pipe.
The invention has the advantages that: the method for finally obtaining the electronic grade sulfuric acid by adopting the reaction of the sulfur trioxide gasification and the ultrapure water has low energy consumption, performs safety protection on a large amount of gas and heat generated by the reaction of the sulfur trioxide gasification and the ultrapure water, and simultaneously can effectively recycle a large amount of heat generated by the reaction of the gasified sulfur trioxide and the ultrapure water, thereby fully utilizing energy.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments or the description of the prior art will be briefly described below, it will be obvious that the drawings in the following description are some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort to a person skilled in the art.
FIG. 1 is a schematic diagram of the structure of the present invention; .
Reference numerals: 1. a heating tank; 2. a sulfur trioxide feed tube; 3. a sulfur trioxide discharge tube; 4. a first filter; 5. a rectifying tower; 6. an absorption tank; 7. ultrapure water enters a pipe; 8. a water spraying pore plate; 9. cooling the kettle; 10. a first acid pump; 11. a blowing tower; 12. a second acid pump; 13. a finished product storage tank; 14. a third acid pump; 15. a second filter; 16. a safety valve; 17. a buffer tank; 18. a heat pump; 19. a one-way valve; 20. a sulfur trioxide control valve; 21. an ultrapure water control valve; 22. a sampling tube; 23. and a sampling valve.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The preparation method of the electronic grade sulfuric acid comprises the following steps:
step one: the sulfur trioxide is sent into a heating tank to be heated at the temperature of 70-90 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is sent into an absorption tank to be absorbed with electronic grade ultrapure water to generate sulfuric acid through filtration and rectification, the temperature in the absorption tower is controlled at 90-110 ℃, and a safety protection device is additionally arranged on the heating tank and the absorption tank;
step two: monitoring the concentration of sulfuric acid in the absorption tank, controlling the reaction by controlling the flow of gaseous sulfur trioxide and ultrapure water, discharging sulfuric acid into a cooling kettle for cooling when the concentration reaches 97-98%, and cooling to 35-55 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into an air blowing tower for impurity removal, wherein compressed air enters the air blowing tower from the lower part of the air blowing tower to remove impurities from the sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 2-4bar;
step four: filtering after blowing to obtain the finished product electronic grade sulfuric acid, and sending the finished product electronic grade sulfuric acid into a finished product storage tank for storage.
Preferably, the filtering in the first step and the fourth step adopts ultrafiltration membranes, and the ultrafiltration membranes are made of tetrafluoroethylene. Tetrafluoroethylene is resistant to high temperature and organic solvent corrosion, and smooth completion of filtration can be ensured.
Preferably, the heat exchanged in the absorption tank and the cooling kettle can be used for gasifying and heating sulfur trioxide. The gasified sulfur trioxide reacts with the ultrapure water to generate a large amount of heat energy, so that the gasified sulfur trioxide is used for heating the sulfur trioxide and realizing the full utilization of energy in other fields such as hot water heating in a bathroom, heating in a central heating system or other heat utilization fields.
The utility model provides a production system of electronic grade sulfuric acid, includes heating jar 1, heating jar 1 top intercommunication sulfur trioxide inlet pipe 2 and sulfur trioxide discharging pipe 3, first filter 4 is connected to sulfur trioxide discharging pipe 3, pipeline intercommunication is passed through with the bottom of rectifying column 5 to first filter 4, pipeline and absorption jar 6 lower part intercommunication are passed through at the top of rectifying column 5, absorption jar 6 top and ultrapure water advance pipe 7 intercommunication, ultrapure water advance pipe 7 is for being connected water spray orifice 8 with absorption jar 6 inner end, absorption jar 6 bottom passes through pipeline and cooling kettle 9 upper portion intercommunication, the communicating pipe on of absorption jar 6 and cooling kettle 9 sets up first acid pump 10, cooling kettle 9 bottom passes through pipeline and the top intercommunication of blowing column 11, set up second acid pump 12 on the pipeline between cooling kettle 9 and the blowing column 11, pipeline and the top intercommunication of finished product storage jar 13 are passed through to the bottom of rectifying column 11, set up third acid pump 14 and second filter 15 on the pipeline between blowing column 11 and the finished product storage jar 13. The gaseous sulfur trioxide is purified by the first filter 4 and the rectifying tower 5 to obtain pure sulfur trioxide gas, the purity of sulfuric acid obtained by the reaction of the pure sulfur trioxide gas and the ultrapure water can be ensured, meanwhile, the reaction efficiency of the ultrapure water and the sulfur trioxide can be accelerated by the reaction of the ultrapure water and the sulfur trioxide in the absorption tower 6 in a spraying mode, and the sulfuric acid obtained by the absorption tower 6 is subjected to gas removal and most of impurities removal through the blowing tower 11 and further micro impurities removal through the second filter 15, so that the purity of the obtained electronic grade sulfuric acid is ensured.
Preferably, the theoretical plate number of the rectifying tower 5 is 20-30, the operating temperature is 50-80 ℃, the operating pressure is 0.4-0.5MPa, and the reflux ratio is 40-60.
Preferably, the top ends of the heating tank 1 and the absorbing tank 6 are communicated with one end of a safety valve 16, and the other end of the safety valve 16 is communicated with a buffer tank 17. When the pressure in the heating tank 1 or the absorbing tank 6 is concentrated and raised due to sudden and violent release of gas or heat through the safety valve 16, the pressure can be quickly released, and raw material waste can be avoided while the pollution to the external environment is avoided through the buffer tank 17.
Preferably, the lower parts of the heating tank 1, the absorbing tank 6 and the cooling kettle 8 are hollow cavities, one side of the cavity of the heating tank 1 is communicated with one side of the cavity of the absorbing tank 6 through a pipeline, the other side of the cavity of the absorbing tank 6 is communicated with one side of the cavity of the cooling kettle 9 through a pipeline, the other side of the cavity of the cooling kettle 9 is communicated with the other side of the cavity of the heating tank 1 through a pipeline, and a heat pump 18 is arranged between the other side of the cavity of the cooling kettle 9 and the communication pipeline of the other side of the cavity of the heating tank 1. The heating tank 1, the absorption tank 6 and the cooling kettle 8 form a closed loop, so that heat exchange is realized conveniently by flowing a heat medium among the three through the heat pump 18, and meanwhile, waste heat can be connected into other heat utilization units, so that energy sources are fully utilized.
Preferably, the sulfur trioxide feeding pipe 2 is provided with a one-way valve 19. The check valve 19 can avoid gaseous sulfur trioxide from flowing out of the sulfur trioxide feeding pipe 2, and ensures that the reaction is carried out normally.
Preferably, a sulfur trioxide control valve 20 is arranged on a pipeline of the rectifying tower 5 communicated with the absorption tank 6, and an ultrapure water control valve 21 is arranged on the ultrapure water inlet pipe 7. The degree of the reaction between the sulfur trioxide control valve 20 and the ultrapure water control valve 21 can be controlled, so that the normal and safe reaction is ensured.
Preferably, a sampling tube 22 is disposed at the lower part of the absorption tower 6, and a sampling valve 23 is disposed on the sampling tube 22. The sampling tube 22 and the sampling valve 23 can conveniently obtain a sulfuric acid sample for purity detection, the next operation is carried out after the sulfuric acid sample is qualified, and the reaction proportion of the sulfur trioxide and the ultrapure water is regulated through detection, so that the normal reaction is ensured.
Example 1
Step one: the sulfur trioxide is sent into a heating tank 1 to be heated at 73+/-2 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is filtered by a tetrafluoroethylene ultrafiltration membrane in a first filter 4, the theoretical plate number is 20, the operating temperature is 50 ℃, the operating pressure is 0.4MPa, a rectifying tower 5 with the reflux ratio of 40 is sent into an absorption tank 6 to be absorbed with electronic grade ultrapure water to generate sulfuric acid, and the temperature in the absorption tower is controlled to be 90-110 ℃;
step two: the sampling tube 22 and the sampling valve 23 control the flow of gaseous sulfur trioxide and ultrapure water through the sulfur trioxide control valve 20 and the ultrapure water control valve 21 to control the reaction, when the concentration of the sulfuric acid reaches 97%, the sulfuric acid is discharged and sent into the cooling kettle 9 to be cooled, and the temperature is cooled to 37 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into a blowing tower 11 for impurity removal, wherein compressed air enters from the lower part of the blowing tower 11 for impurity removal of sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 2bar;
step four: and filtering the blown product by using a tetrafluoroethylene ultrafiltration membrane in the second filter 15 to obtain finished product electronic grade sulfuric acid, and conveying the finished product electronic grade sulfuric acid into a finished product storage tank 13 for storage.
The content of the obtained electronic grade sulfuric acid is 97.3%, the chromaticity is 6, the metal impurity is 50ppt, the anion impurity is 80ppb, and the dust particle is 3/ml, which accords with the production standard of the electronic grade sulfuric acid.
Example 2
Step one: the sulfur trioxide is sent into a heating tank 1 to be heated at the temperature of 80+/-2 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is filtered by a tetrafluoroethylene ultrafiltration membrane in a first filter 4, the theoretical plate number is 25, the operating temperature is 65 ℃, the operating pressure is 0.45MPa, the reflux ratio is 50, the rectifying tower 5 is sent into an absorption tank 6 to be absorbed with electronic grade ultrapure water to generate sulfuric acid, and the temperature in the absorption tower is controlled to be 90-110 ℃;
step two: the sampling tube 22 and the sampling valve 23 control the flow of gaseous sulfur trioxide and ultrapure water through the sulfur trioxide control valve 20 and the ultrapure water control valve 21 to control the reaction, when the concentration of the sulfuric acid reaches 97.5%, the sulfuric acid is discharged and sent into the cooling kettle 9 to be cooled, and the temperature is cooled to 40 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into a blowing tower 11 for impurity removal, wherein compressed air enters from the lower part of the blowing tower 11 for impurity removal of sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 3bar;
step four: and filtering the blown product by using a tetrafluoroethylene ultrafiltration membrane in the second filter 15 to obtain finished product electronic grade sulfuric acid, and conveying the finished product electronic grade sulfuric acid into a finished product storage tank 13 for storage.
The content of the obtained electronic grade sulfuric acid is 97.6%, the chromaticity is 7, the metal impurity is 45ppt, the anion impurity is 70ppb, and the dust particle is 2/ml, so that the electronic grade sulfuric acid meets the production standard of the electronic grade sulfuric acid.
Example 3
Step one: the sulfur trioxide is sent into a heating tank 1 to be heated at 86+/-2 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is filtered by a tetrafluoroethylene ultrafiltration membrane in a first filter 4, the theoretical plate number is 30, the operating temperature is 80 ℃, the operating pressure is 0.5MPa, the reflux ratio is 60, the rectifying tower 5 is sent into an absorption tank 6 to be absorbed with electronic grade ultrapure water to generate sulfuric acid, and the temperature in the absorption tower is controlled to be 90-110 ℃;
step two: the sampling tube 22 and the sampling valve 23 control the reaction by monitoring the sulfuric acid concentration in the absorption tank and controlling the flow of gaseous sulfur trioxide and ultrapure water through the sulfur trioxide control valve 20 and the ultrapure water control valve 21, when the sulfuric acid concentration reaches 97.8%, the sulfuric acid is discharged and sent into the cooling kettle 9 for cooling, and the temperature is cooled to 50 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into a blowing tower 11 for impurity removal, wherein compressed air enters from the lower part of the blowing tower 11 for impurity removal of sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 4bar;
step four: and filtering the blown product by using a tetrafluoroethylene ultrafiltration membrane in the second filter 15 to obtain finished product electronic grade sulfuric acid, and conveying the finished product electronic grade sulfuric acid into a finished product storage tank 13 for storage.
The content of the obtained electronic grade sulfuric acid is 97.7%, the chromaticity is 5, the metal impurity is 40ppt, the anion impurity is 50ppb, and the dust particle is 1 per ml, so that the electronic grade sulfuric acid meets the production standard of the electronic grade sulfuric acid.
According to the embodiment 1-3, the electronic grade sulfuric acid prepared by the method meets the standard, the energy consumption of the preparation method is low, the whole process is monitored completely, the operation is convenient and safe, and therefore, the high-quality electronic grade sulfuric acid can be produced in a low-cost and safe environment.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. A preparation method of electronic grade sulfuric acid is characterized in that: the method comprises the following steps:
step one: the sulfur trioxide is sent into a heating tank to be heated at the temperature of 70-90 ℃ to generate gaseous sulfur trioxide, the gaseous sulfur trioxide is sent into an absorption tank to be absorbed with electronic grade ultrapure water to generate sulfuric acid through filtration and rectification, the temperature in the absorption tower is controlled at 90-110 ℃, and a safety protection device is additionally arranged on the heating tank and the absorption tank;
step two: monitoring the concentration of sulfuric acid in the absorption tank, controlling the reaction by controlling the flow of gaseous sulfur trioxide and ultrapure water, discharging sulfuric acid into a cooling kettle for cooling when the concentration reaches 97-98%, and cooling to 35-55 ℃;
step three: after cooling, feeding the cooled sulfuric acid liquid into an air blowing tower for impurity removal, wherein compressed air enters the air blowing tower from the lower part of the air blowing tower to remove impurities from the sulfuric acid liquid falling from the upper part, and the pressure of the compressed air is 2-4bar;
step four: filtering after blowing to obtain the finished product electronic grade sulfuric acid, and sending the finished product electronic grade sulfuric acid into a finished product storage tank for storage.
2. The method for preparing electronic grade sulfuric acid according to claim 1, characterized in that: the filtering in the first step and the fourth step adopts ultrafiltration membranes, and the ultrafiltration membranes are made of tetrafluoroethylene.
3. The method for preparing electronic grade sulfuric acid according to claim 1, characterized in that: the heat exchanged in the absorption tank and the cooling kettle can be used for gasifying and heating sulfur trioxide.
4. A production system of electronic grade sulfuric acid, which is characterized in that: including heating jar (1), heating jar (1) top intercommunication sulfur trioxide inlet pipe (2) and sulfur trioxide discharging pipe (3), first filter (4) are connected in sulfur trioxide discharging pipe (3), pipeline intercommunication is passed through with the bottom of rectifying column (5) in first filter (4), pipeline and absorption jar (6) lower part intercommunication are passed through at the top of rectifying column (5), absorption jar (6) top and ultrapure water advance pipe (7) intercommunication, ultrapure water advance pipe (7) be with absorption jar (6) in one end connect water spray orifice plate (8), absorption jar (6) bottom passes through pipeline and cooling kettle (9) upper portion intercommunication, the communicating pipeline of absorption jar (6) and cooling kettle (9) sets up first acid pump (10), cooling kettle (9) bottom passes through pipeline and blowing acid tower (11) top intercommunication, set up second acid pump (12) on the pipeline between cooling kettle (9) and blowing tower (11), blowing tower (11) bottom passes through pipeline and storage tank (13), blowing tower (13) bottom and third storage tank (13) are connected.
5. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the theoretical plate number of the rectifying tower (5) is 20-30, the operating temperature is 50-80 ℃, the operating pressure is 0.4-0.5MPa, and the reflux ratio is 40-60.
6. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the top ends of the heating tank (1) and the absorbing tank (6) are communicated with one end of a safety valve (16), and the other end of the safety valve (16) is communicated with a buffer tank (17).
7. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the utility model discloses a heating tank, absorption tank, cooling kettle, heating tank, absorption tank, cooling tank, wherein the lower part of heating tank (1), absorption tank (6) and cooling tank (8) be the cavity, cavity one side of heating tank (1) is passed through cavity one side of pipeline intercommunication absorption tank (6), the cavity opposite side of absorption tank (6) is passed through cavity one side of pipeline intercommunication cooling tank (9), the cavity opposite side of cooling tank (9) is passed through the cavity opposite side of pipeline intercommunication heating tank (1), the cavity opposite side of cooling tank (9) sets up heat pump (18) with the intercommunication pipeline merchant of the cavity opposite side of heating tank (1).
8. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the sulfur trioxide feeding pipe (2) is provided with a one-way valve (19).
9. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the utility model is characterized in that a sulfur trioxide control valve (20) is arranged on a pipeline which is communicated with the rectifying tower (5) and the absorbing tank (6), and an ultrapure water control valve (21) is arranged on the ultrapure water inlet pipe (7).
10. The system for producing electronic grade sulfuric acid according to claim 4, wherein: the lower part of the absorption tower (6) is provided with a sampling tube (22), and the sampling tube (22) is provided with a sampling valve (23).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310220873.2A CN116281876A (en) | 2023-03-09 | 2023-03-09 | Preparation method and production system of electronic grade sulfuric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310220873.2A CN116281876A (en) | 2023-03-09 | 2023-03-09 | Preparation method and production system of electronic grade sulfuric acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116281876A true CN116281876A (en) | 2023-06-23 |
Family
ID=86780960
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310220873.2A Pending CN116281876A (en) | 2023-03-09 | 2023-03-09 | Preparation method and production system of electronic grade sulfuric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116281876A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117886279A (en) * | 2024-01-22 | 2024-04-16 | 江苏捷创新材料有限责任公司 | Electronic grade sulfuric acid production facility |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110318260A1 (en) * | 2010-06-29 | 2011-12-29 | Shanghai Huayi Microelectric Material Co., Ltd. | Manufacture method of ultra-pure sulfuric acid |
| KR101541908B1 (en) * | 2014-05-07 | 2015-08-19 | (주) 맥코이교역 | Apparatus of manufacturing for ultra pure electronics grade sulphuric acid |
| CN106477532A (en) * | 2015-08-27 | 2017-03-08 | 诚胜工程股份有限公司 | The technique that a kind of acid pickle recycles |
| 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 |
| 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 |
| CN114804036A (en) * | 2022-04-12 | 2022-07-29 | 南京佳华工程技术有限公司 | Method and system for producing G1-G5 electronic-grade sulfuric acid |
| CN217418195U (en) * | 2022-05-07 | 2022-09-13 | 南京正源化学工程科技有限公司 | Electronic-grade sulfuric acid production device |
| 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 |
-
2023
- 2023-03-09 CN CN202310220873.2A patent/CN116281876A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110318260A1 (en) * | 2010-06-29 | 2011-12-29 | Shanghai Huayi Microelectric Material Co., Ltd. | Manufacture method of ultra-pure sulfuric acid |
| KR101541908B1 (en) * | 2014-05-07 | 2015-08-19 | (주) 맥코이교역 | Apparatus of manufacturing for ultra pure electronics grade sulphuric acid |
| CN106477532A (en) * | 2015-08-27 | 2017-03-08 | 诚胜工程股份有限公司 | The technique that a kind of acid pickle recycles |
| 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 |
| 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 |
| CN114804036A (en) * | 2022-04-12 | 2022-07-29 | 南京佳华工程技术有限公司 | Method and system for producing G1-G5 electronic-grade sulfuric acid |
| CN217418195U (en) * | 2022-05-07 | 2022-09-13 | 南京正源化学工程科技有限公司 | Electronic-grade sulfuric acid production device |
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 纪罗军等: "超纯硫酸的生产与应用现状", 硫酸工业, no. 02, pages 13 - 17 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117886279A (en) * | 2024-01-22 | 2024-04-16 | 江苏捷创新材料有限责任公司 | Electronic grade sulfuric acid production facility |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111704109A (en) | Method and system for preparing electronic-grade hydrofluoric acid by continuous method | |
| CN109264674B (en) | Process and system for preparing sulfuric acid by using smelting flue gas | |
| CN116281876A (en) | Preparation method and production system of electronic grade sulfuric acid | |
| CN104829494A (en) | Energy-saving urea production system and production process thereof | |
| CN114307368A (en) | Method and device for producing high-purity electronic grade ethanol | |
| CN111533091A (en) | Production device and production process of EL-grade sulfuric acid | |
| CN105084359B (en) | A kind of method that formic acid dehydration industry prepares high-purity CO | |
| CN111661828B (en) | Preparation method of high-purity reagent nitric acid | |
| CN103332751B (en) | Ferrous sulfate method of comprehensive utilization | |
| CN103072962B (en) | Preparation method of electronic grade nitric acid | |
| CN114436293B (en) | Method for directly producing sodium bromide from low-concentration brine | |
| CN114573493B (en) | Purification method of methyl pyrrolidone waste liquid | |
| CN113233434B (en) | Production process and production device of electronic-grade nitric acid | |
| CN109852434A (en) | A kind of method of coke-oven-gas desulfurization and decyanation concentration relieving haperacidity | |
| CN111715028B (en) | Product diversified helium high-yield separation and purification coupling process | |
| CN218665415U (en) | Equipment for preparing hydrobromic acid by distillation with finished liquid as raw material | |
| CN104498983A (en) | Method for preparation of high purity oxygen by water electrolysis | |
| CN102277205B (en) | Method for extracting salt from coke oven gas by desulfuration and decyanation | |
| CN210796289U (en) | High-efficient low energy consumption sodium methoxide purification equipment | |
| CN211733857U (en) | Oxidation tower for preparing hydrogen peroxide by anthraquinone process | |
| CN211896042U (en) | Oxidation tower for preparing hydrogen peroxide by anthraquinone process | |
| CN108530316B (en) | Fixed bed heat recovery type ammoximation reaction system | |
| CN208265798U (en) | Taurine wastewater zero discharge processing unit | |
| CN112279225A (en) | Production system and process for co-production of industrial-grade nitric acid and electronic-grade nitric acid | |
| CN212403469U (en) | Production device of EL-grade sulfuric acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20230802 Address after: 265200 No. 79 Changjiang Road, Laiyang Economic Development Zone, Yantai City, Shandong Province Applicant after: Yantai Far East Fine Chemical Co.,Ltd. Address before: 265200 No.79 Changjiang Road, Laiyang economic and Technological Development Zone, Yantai City, Shandong Province Applicant before: Shandong Ludong Chemical Research Institute Co.,Ltd. |
|
| TA01 | Transfer of patent application right |