CN110255506A - A kind of apparatus and method of electronic-grade sulfuric acid production - Google Patents

A kind of apparatus and method of electronic-grade sulfuric acid production Download PDF

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Publication number
CN110255506A
CN110255506A CN201910636090.6A CN201910636090A CN110255506A CN 110255506 A CN110255506 A CN 110255506A CN 201910636090 A CN201910636090 A CN 201910636090A CN 110255506 A CN110255506 A CN 110255506A
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China
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sulfuric acid
vaporizer
tower
cooler
sulfur trioxide
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CN201910636090.6A
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Inventor
李少平
杜林�
郭岚峰
杨着
汪鹏
廖义
周建国
汪泳
岳兵
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Hubei Xingfa Chemicals Group Co Ltd
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Hubei Xingfa Chemicals Group Co Ltd
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Priority to CN201910636090.6A priority Critical patent/CN110255506A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/74Preparation
    • C01B17/76Preparation by contact processes
    • C01B17/775Liquid phase contacting processes or wet catalysis processes
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00Sulfur; Compounds thereof
    • C01B17/69Sulfur trioxide; Sulfuric acid
    • C01B17/74Preparation
    • C01B17/76Preparation by contact processes
    • C01B17/80Apparatus

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Gas Separation By Absorption (AREA)

Abstract

The invention discloses a kind of apparatus and method of electronic-grade sulfuric acid production.Sulfur trioxide raw material storage tank is pumped through raw material and is connected to vaporizer one, one top of vaporizer is connect with demister, at the top of demister with connected at the top of cooler one, one bottom of cooler is connect with surge tank one, and surge tank is connected once feed pump with vaporizer two, and vaporizer two is connect with absorption tower, absorb the bottom of the tower is connect with surge tank two, two bottom of surge tank is connect through cyclic acid pump with cooler two, and cooler two is connected to stripping tower, and stripping tower is connected to electronic-grade sulfuric acid storage tank.Sulfur trioxide is delivered to vaporizer one, sulfur trioxide after vaporization enters cooler one, enter surge tank one after being condensed into liquid, sulfur trioxide in surge tank one is delivered to vaporizer through feed pump, enter absorption tower after vaporizing again, cyclic absorption is carried out using ultrapure water in absorption tower, just goes out pipeline stabilization extraction in two finished product of cooler, after subsequent Air Exposure, sulfuric acid product quality reaches SEMI-C12 rank.

Description

A kind of apparatus and method of electronic-grade sulfuric acid production
Technical field
The invention belongs to electronic chemical product fields, and in particular to the apparatus and method of kind electronic-grade sulfuric acid production.
Background technique
Electronic-grade sulfuric acid is also known as ultra-pure sulfuric acid, belongs to ultra-clean and high pure chemical reagent.It is the maximum wet electron chemistry of industrial dosage, It is mainly used for the cleaning, photoetching, corrosion of silicon wafer, the corrosion and cleaning of printed circuit board can effectively remove magazine on chip Grain, inorganic residue and carbon deposits.History of the electronic-grade sulfuric acid for existing more than 40 years of the cleaning of silicon wafer.In semiconductor work Belong to indispensable key foundation chemical reagent in industry.Its purity directly affects ic yield.
Electronic-grade sulfuric acid main production process industrial sulphuric acid rectification method or the direct absorption process of sulfur trioxide gas;Rectification method can It is divided into atmospheric distillation and rectification under vacuum, the temperature of atmospheric distillation is generally up to 330 DEG C, and device material is more demanding, general to use Expensive quartz glass;The temperature of rectification under vacuum is generally 175~190 DEG C, and 1.33~2.67kPa of pressure, device can be adopted With more cheap Pyrex and fluoropolymer material.It is limited by equipment, the energy, rectification method is suitable for small-scale production.This Method is difficult to realize the electronic-grade sulfuric acid of large-scale production high-purity.
Some Domestic enterprise produces electronic-grade sulfuric acid using the direct absorption process of sulfur trioxide gas at present, but still faces original Material sulfur trioxide purity difference, impurity separating difficulty, liner equipment fragility easily calculate bad the problems such as in misoperation, cause at present Electronic-grade sulfuric acid product quality is difficult to further break through.The present invention is innovated from production equipment, production and control method, is solved Material purity difference and impurity separating difficulty problem, while protecting process units.
Summary of the invention
There is provided a kind of apparatus and method of electronic-grade sulfuric acid production when the purpose of the present invention, process, product quality is steady It is fixed, it can reach SEMI-C12 rank (metal concentration≤0.1 μ g/L).
The invention discloses a kind of devices of electronic-grade sulfuric acid production, including sulfur trioxide raw material storage tank, vaporizer one, remove Day with fog, cooler one, surge tank one, vaporizer two, absorption tower, surge tank two, cooler two, stripping tower, sulfur trioxide raw material Storage tank is pumped through raw material and is connected to vaporizer one, and one top of vaporizer is connect with demister, at the top of demister and at the top of cooler one Connection, one bottom of cooler are connect with surge tank one, and surge tank is connected once feed pump with vaporizer two, vaporizer two and absorption Tower connection, absorb the bottom of the tower are connect with surge tank two, and two bottom of surge tank is connect through cyclic acid pump with cooler two, cooler two It is connected to stripping tower, stripping tower is connected to electronic-grade sulfuric acid storage tank.
Cooler two connect with absorption tower and connect with the spray thrower in absorption tower, the absorption tower top be provided with to Few two-stage tower tray, tower tray have drip tray, display providing holes in drip tray.Array round hole in drip tray, such structure " wall stream " effect can be eliminated, avoiding absorption tower lower tray, high temperature damages due to lacking liquid;Add in the middle part of absorption tower equipped with ultrapure water Enter pipeline.
The absorption tower top is provided with ultrapure water and enters pipe;Air, which is provided with, on the stripping tower enters pipe.
In above scheme, sulfur trioxide raw material storage tank bottom is connected using pipeline with raw material pump, and is connected with vaporizer one; One bottom of surge tank is connected using pipeline with feed pump, and is connected with vaporizer two.
In above scheme, two-stage wire packing, material PP, PE or PTFE material silk screen are equipped in demister;
Two-stage wire packing, material PP, PE or PTFE material silk screen are equipped in the demister.
The vaporizer one, two material of vaporizer are the material stainless steel of 316L, 316 or 304, and vaporizer upper end is equipped with PFA or PTFE material silk screen.Its object is to intercept the micro droplet in sulfur trioxide gas.
In above scheme, drip tray is had equipped with recycle acid spray thrower, absorption tower upper end two-stage tower tray at the top of absorption tower, Array round hole in drip tray, such structure can eliminate " wall stream " effect, avoid absorption tower lower tray high because lacking liquid Temperature damage.
Ultrapure water is equipped in above scheme, in the middle part of absorption tower, and pipeline is added;The outlet of cooler two is equipped with finished product and produces pipeline; Gas tower bottom is equipped with high pure air and pipeline is added.
In above scheme, the absorption tower, cooler, stripping tower be PFA in 316L stainless steel or 304 stainless steels, Any one in PTFE, HDPE, metal ion amount of precipitation≤30w/10-12;Filler, filler are equipped in absorption tower and stripping tower For the Pall ring and Raschig ring filler of PFA material.
A kind of method of electronic-grade sulfuric acid production of the present invention, selects above-mentioned electronic-grade sulfuric acid process units, wraps Include following steps:
(1) three oxygen of the sulfur trioxide in sulfur trioxide raw material storage tank by raw material pump transport to vaporizer one, in vaporizer one Gas-liquid separator is carried out in demister after changing sulphur evaporation, the sulfur trioxide air lift for removing droplet impurity condenses in cooler one For liquid, into surge tank one;
(2) sulfur trioxide in surge tank one is delivered to absorption tower through feed pump after vaporizer two carries out gas-liquid separation, and It is passed through ultrapure water to be absorbed, absorbing liquid enters bottom surge tank two, and the sulfuric acid in surge tank two is delivered to by cyclic acid pump Cooler two, part of sulfuric acid after cooling return to absorption tower cyclic absorption, and part of sulfuric acid is produced to stripping tower;
(3) it is aerated into the sulfuric acid of stripping tower using high-purity compressed air, subsequently into sulfuric acid storage tank, SEMI- can be obtained The electronic-grade sulfuric acid (metal concentration≤0.1 μ g/L) of C12 rank.
In the above method, the temperature control of sulfur trioxide storage tank, surge tank one is at 32 DEG C~40 DEG C.
In the above method, vaporizer use coil pipe hot water or heat-conducting oil heating, one temperature of vaporizer control 50 DEG C~ 70 DEG C, two temperature of vaporizer is controlled at 40 DEG C~55 DEG C, and there are temperature differences for vaporizer one, vaporizer two, and its object is to vaporize The vaporization of one higher temperature of device, can be with the most liquid impurities of demisting, and two temperature of vaporizer is lower, and it is few to vaporize the droplet brought into, It can guarantee the quality for entering absorption tower sulfur trioxide by the way that silk screen does not intercept on vaporizer two.
In the above method, cooler one uses air as cooling medium, the control of sulfur trioxide drop temperature 32 DEG C~ 40 DEG C, the security risk after heat exchanger failure can be reduced;Sulfur trioxide drop temperature is controlled at 32 DEG C~40 DEG C, it is ensured that three oxidations Sulphur is liquid.
In the above method, sulfur trioxide air lift enters from absorb the bottom of the tower, and ultrapure water sprays under the tower tray of first piece of absorption tower Enter (from top to bottom);Temperature control is at 70 DEG C~110 DEG C in absorbing tower, the excessively high breaking-up equipment of temperature;Two sulfuric acid of cooler goes out Sour temperature control system is expected at 40 DEG C~70 DEG C, and temperature is too low to will affect subsequent aeration effect.
In the above method, ultrapure water is that resistivity is the >=ultrapure water of 18M Ω * cm at 25 DEG C.
In the above method, sulfuric acid enters from stripper-overhead, and high pure air enters from stripping tower lower part;Stripping tower aeration quantity Control is in 450 L/min~650L/min, by readily oxidizable substance concentration control in product within 2ppm;
A kind of working principle of the device of electronic-grade sulfuric acid production of the present invention is the sulfur trioxide of liquid in sulfur trioxide storage tank It is delivered to vaporizer one through sulfur trioxide raw material pump, and the vaporization that heats up in vaporizer one, gaseous sulfur trioxide is in demister Gas-liquid separation is carried out, sulfur trioxide gas enters cooler one and is cooled to liquid, and liquid sulphur trioxide is slow from cooler from flowing to Tank one is rushed, the liquid sulphur trioxide in surge tank one is delivered to vaporizer two by feed pump, and after vaporizing again, gaseous state three is aoxidized Sulphur enters absorption tower and reacts with ultrapure water, produces sulfuric acid, the sulfuric acid on absorption tower enters stripping tower after the cooling of cooler two, in gas Body tower is aerated using high pure air, is deviate from sulfur dioxide, is finally entered finished product storage tank.
Innovative point of the invention includes the following:
(1) the vaporizer top that the present invention uses is equipped with PFA silk screen, can remove liquid foam in the sulfur trioxide of vaporization, reach and remove Go the purpose of impurity in sulfur trioxide;
(2) present invention is vaporized by two-stage, and one temperature of vaporizer vaporizes compared with relative superiority or inferiority, then removes a large amount of impurity through demister, is vaporized Device two vaporizes at a lower temperature, brings less droplet into and is removed by vaporizer upper end silk screen, guarantees to enter sulfur trioxide The electronic-grade sulfuric acid of SEMI-C12 rank can be obtained in quality after absorption;
(3) sulfur trioxide cooler of the present invention does cooling medium using air, exchanges heat than condensed water safer;
(4) absorption tower upper end two-stage tower tray of the present invention has drip tray, array round hole in drip tray, and such structure can be with " wall stream " effect is eliminated, avoiding absorption tower lower tray, high temperature damages due to lacking liquid;
(5) equipment pipe that the present invention uses is all made of 316L stainless steel or 304 stainless steel inner lining polytetrafluoroethylplastic plastics, will Acid medium is thoroughly isolated with stainless steel, prevents polluted product quality due to equipment microcorrosion.
Detailed description of the invention
Fig. 1 is a kind of device figure of electronic-grade sulfuric acid production of the present invention.
Fig. 2 is the structural schematic diagram of spray thrower.
Wherein, 1. sulfur trioxide raw material storage tank, 2. raw materials pump, 3. vaporizers one, 4. demisters, 5. coolers one, 6. is slow Rush tank one, 7. feed pumps, 8. vaporizers two, 9. absorption towers, 10. spray throwers, 11. drip trays, 12. surge tanks two, 13. recycle acids Pump, 14. coolers two, 15. stripping towers, 16. tower trays, 17. holes.
Specific embodiment
Below with reference to embodiment, the invention will be further described, but should not be construed the above-mentioned subject area of the present invention only It is limited to following embodiments.Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and used With means, various replacements and change are made, should all include within the scope of the present invention.
Embodiment 1
A kind of device of electronic-grade sulfuric acid production, including sulfur trioxide raw material storage tank 1, vaporizer 1, demister 4, cooler one 5, surge tank 1, vaporizer 28, absorption tower 9, surge tank 2 12, cooler 2 14, stripping tower 15, sulfur trioxide raw material storage tank 1 is connected to through raw material pump 2 with vaporizer 1, and one 3 top of vaporizer is connect with demister 4, and 4 top of demister is pushed up with cooler 1 Portion's connection, one 5 bottom of cooler are connect with surge tank 1, and surge tank 1 is connected through feed pump 7 with vaporizer 28, vaporizer 28 connect with absorption tower 9, and 9 bottom of absorption tower is connect with surge tank 2 12, and 2 12 bottom of surge tank is through cyclic acid pump 13 and cooling Device 2 14 connects, and cooler 2 14 is connected to stripping tower 15, and stripping tower 15 is connected to electronic-grade sulfuric acid storage tank.
Cooler 2 14 connect with absorption tower 9 and connect with the spray thrower 10 in absorption tower 9,9 top of absorption tower It is provided at least two-stage tower tray 16, tower tray has drip tray 11, displays providing holes 17 in drip tray 11.
9 top of absorption tower is provided with ultrapure water and enters pipe;Air, which is provided with, on the stripping tower 15 enters pipe.
Originally bright to also disclose a kind of method of electronic-grade sulfuric acid production: technical grade sulfur trioxide discharging to raw material storage tank, warp Raw material pump is delivered to vaporizer one, and the sulfur trioxide after vaporization enters demister removal of impurities, and the sulfur trioxide after removal of impurities is in cooler One is condensed into liquid, and into surge tank one, the sulfur trioxide in surge tank one is delivered to vaporizer two through feed pump, vaporizes again Enter absorption tower afterwards, cyclic absorption carried out using ultrapure water in absorption tower, controls the concentration of absorbing liquid, and cooler two at Product just go out pipeline stabilization extraction, after subsequent Air Exposure, sulfuric acid product quality reach SEMI-C12 rank (metal concentration≤ 0.1 μ g/L).
Two-stage wire packing, material PP, PE or PTFE material silk screen are equipped in the demister;
The vaporizer one, two material of vaporizer are the material stainless steel of 316L, 316 or 304, and vaporizer upper end is equipped with PFA Or PTFE material silk screen.
Recycle acid spray thrower is equipped at the top of the absorption tower, absorption tower upper end two-stage tower tray has drip tray, drip tray Upper array round hole;
It is equipped with ultrapure water in the middle part of the absorption tower, pipeline is added;The outlet of cooler two is equipped with finished product and produces pipeline;Gas tower bottom Pipeline is added equipped with high pure air.
The absorption tower, cooler one, cooler two, stripping tower be PFA in 316L stainless steel or 304 stainless steels, Any one in PTFE, HDPE, metal ion amount of precipitation≤30w/10-12;Filler, filler are equipped in absorption tower and stripping tower For the Pall ring and Raschig ring filler of PFA material.
The cooler one uses air as cooling medium, and sulfur trioxide drop temperature is controlled at 32 DEG C~40 DEG C;Three Sulfur oxide drop temperature is controlled at 32 DEG C~40 DEG C;
The sulfur trioxide air lift enters from absorb the bottom of the tower, and ultrapure water is sprayed under the tower tray of first piece of absorption tower (from upper past Under);Temperature is controlled at 70 DEG C~110 DEG C in absorbing tower,;Two sulfuric acid of cooler discharges sour temperature control system at 40 DEG C~70 DEG C;
The ultrapure water is that resistivity is the >=ultrapure water of 18M Ω * cm at 25 DEG C.
The sulfuric acid enters from stripper-overhead, and high pure air enters from stripping tower lower part;Stripping tower aeration control exists 450 L/min~650L/min;
A kind of method of electronic-grade sulfuric acid production of the present embodiment, selects above-mentioned electronic-grade sulfuric acid process units, including following Step:
(1) by raw material pump transport to vaporizer one, liquid sulphur trioxide passes through the sulfur trioxide in raw material storage tank in vaporizer Bucket coil pipe hot water or heat-conducting oil heating vaporization, heating and temperature control is at 65 DEG C;Enter after sulfur trioxide evaporation in vaporizer Demister removal of impurities, the sulfur trioxide after removal of impurities enters cooler one, and is condensed into liquid in cooler one, into surge tank One, cooling medium is cooling water or air, and at 38 DEG C, one temperature of surge tank is controlled 38 the control of sulfur trioxide drop temperature ℃;
(2) sulfur trioxide in surge tank one is delivered to absorption tower by feed pump, and is passed through ultrapure water and is absorbed, absorbing liquid Into bottom surge tank two, the sulfuric acid in surge tank two is delivered to cooler two, part of sulfuric acid after cooling by cyclic acid pump Absorption tower cyclic absorption is returned to, part of sulfuric acid is produced to stripping tower;Wherein temperature is controlled at 95 DEG C in absorbing tower;Cooler two Sulfuric acid discharges sour temperature control system at 65 DEG C;
(3) it is aerated into the sulfuric acid of stripping tower using high-purity compressed air, the control of high pure air tolerance is exposed in 560L/min Product after gas enters finished product storage tank.
Through detecting, metal ion < 80ppt, anion concentration < 100ppb, readily oxidizable substance concentration in electronic-grade sulfuric acid < 2ppm, sulfuric acid concentration 96%~97%.
Embodiment 2
With reference to Fig. 1,2, the implementation steps of embodiment 2 are as follows:
(1) by raw material pump transport to vaporizer one, liquid sulphur trioxide passes through the sulfur trioxide in raw material storage tank in vaporizer Bucket coil pipe hot water heating vaporization, heating and temperature control is at 60 DEG C;Enter demister after sulfur trioxide evaporation in vaporizer to clean, Sulfur trioxide after removal of impurities enters cooler one, and is condensed into liquid in cooler one, and into surge tank one, cooling medium is Cooling water or air, at 38 DEG C, one temperature of surge tank is controlled at 36 DEG C the control of sulfur trioxide drop temperature;
(2) sulfur trioxide in surge tank one is delivered to absorption tower by feed pump, and is passed through ultrapure water and is absorbed, absorbing liquid Into bottom surge tank two, the sulfuric acid in surge tank two is delivered to cooler two, part of sulfuric acid after cooling by cyclic acid pump Absorption tower cyclic absorption is returned to, part of sulfuric acid is produced to stripping tower;Wherein temperature is controlled at 90 DEG C in absorbing tower;Cooler two Sulfuric acid discharges sour temperature control system at 60 DEG C;
(3) it is aerated into the sulfuric acid of stripping tower using high-purity compressed air, the control of high pure air tolerance is exposed in 520L/min Product after gas enters finished product storage tank.
Through detecting, metal ion < 70ppt, anion concentration < 100ppb, readily oxidizable substance concentration in electronic-grade sulfuric acid < 2ppm, sulfuric acid concentration 96%~97%.
Embodiment 3
With reference to Fig. 1,2, the implementation steps of embodiment 3 are as follows:
(1) by raw material pump transport to vaporizer one, liquid sulphur trioxide passes through the sulfur trioxide in raw material storage tank in vaporizer Bucket coil pipe hot water heating vaporization, heating and temperature control is at 55 DEG C;Enter demister after sulfur trioxide evaporation in vaporizer to clean, Sulfur trioxide after removal of impurities enters cooler one, and is condensed into liquid in cooler one, and into surge tank one, cooling medium is Cooling water or air, at 38 DEG C, one temperature of surge tank is controlled at 36 DEG C the control of sulfur trioxide drop temperature;
(2) sulfur trioxide in surge tank one is delivered to absorption tower, and is passed through ultrapure water and is absorbed, and it is slow that absorbing liquid enters bottom Tank two is rushed, the sulfuric acid in surge tank two is delivered to cooler two by cyclic acid pump, and part of sulfuric acid after cooling returns to absorption tower Cyclic absorption, part of sulfuric acid are produced to stripping tower;Wherein temperature is controlled at 85 DEG C in absorbing tower;Two sulfuric acid of cooler discharging acid Temperature control system is at 55 DEG C;
(3) it is aerated into the sulfuric acid of stripping tower using high-purity compressed air, the control of high pure air tolerance is exposed in 480L/min Product after gas enters finished product storage tank.
Through detecting, metal ion < 60ppt, anion concentration < 100ppb, readily oxidizable substance concentration in electronic-grade sulfuric acid < 2ppm, sulfuric acid concentration 96%~97%.

Claims (8)

1. a kind of device of electronic-grade sulfuric acid production, which is characterized in that including sulfur trioxide raw material storage tank (1), vaporizer one (3), demister (4), cooler one (5), surge tank one (6), vaporizer two (8), absorption tower (9), surge tank two (12), cooling Device two (14), stripping tower (15), sulfur trioxide raw material storage tank (1) are connected to through raw material pump (2) with vaporizer one (3), vaporizer one (3) top connect with demister (4), is connect at the top of demister (4) with cooler one (5) top, cooler one (5) bottom with delay Tank one (6) connection is rushed, surge tank one (6) is connected through feed pump (7) with vaporizer two (8), vaporizer two (8) and absorption tower (9) Connection, absorption tower (9) bottom are connect with surge tank two (12), and surge tank two (12) bottom is through cyclic acid pump (13) and cooler two (14) it connects, cooler two (14) is connected to stripping tower (15), and stripping tower (15) is connected to electronic-grade sulfuric acid storage tank.
2. the device of electronic-grade sulfuric acid production according to claim 1, which is characterized in that cooler two (14) and absorption tower (9) it connects and is connect with the spray thrower (10) in absorption tower (9), the absorption tower (9) top is provided at least two-stage tower tray (16), tower tray has drip tray (11), displays providing holes (17) in drip tray (11).
3. the device of electronic-grade sulfuric acid production according to claim 1, which is characterized in that described absorption tower (9) top It is provided with ultrapure water and enters pipe;Air, which is provided with, on the stripping tower (15) enters pipe.
4. a kind of method of electronic-grade sulfuric acid production, using electronic-grade sulfuric acid as claimed in any one of claims 1 to 3 production Device, comprising the following steps:
(1) three oxygen of the sulfur trioxide in sulfur trioxide raw material storage tank by raw material pump transport to vaporizer one, in vaporizer one Enter demister after changing sulphur evaporation, carry out gas-liquid separator, gaseous sulfur trioxide enters cooler one and be condensed into liquid, into slow Rush tank one;
(2) sulfur trioxide in surge tank one is delivered to absorption tower through feed pump after vaporizer two carries out gas-liquid separation, and It is passed through ultrapure water to be absorbed, absorbing liquid enters bottom surge tank two, and the sulfuric acid in surge tank two is delivered to by cyclic acid pump Cooler two, part of sulfuric acid after cooling return to absorption tower cyclic absorption, and part of sulfuric acid is produced to stripping tower;
(3) it is aerated into the sulfuric acid of stripping tower using high-purity compressed air, subsequently into sulfuric acid storage tank, SEMI- can be obtained The electronic-grade sulfuric acid of C12 rank.
5. the method for electronic-grade sulfuric acid production as claimed in claim 4, which is characterized in that sulfur trioxide raw material stores up in step (1) The temperature control of tank, surge tank one is at 32 DEG C~40 DEG C;Vaporizer uses coil pipe hot water or heat-conducting oil heating, one temperature of vaporizer Degree control is at 50 DEG C~70 DEG C, and two temperature of vaporizer is controlled at 40 DEG C~55 DEG C, and there are temperature difference, purposes for vaporizer one, two It is that one higher temperature of vaporizer vaporizes, can with the most liquid impurities of demisting, two temperature of vaporizer is lower, vaporizes and brings into Droplet is few, guarantees the quality for entering absorption tower sulfur trioxide;Cooler one using cooling water or air as cooling medium, three Sulfur oxide drop temperature is controlled at 32 DEG C~40 DEG C.
6. the method for electronic-grade sulfuric acid as claimed in claim 4 production, which is characterized in that step (2) sulfur trioxide gas is from suction It receives tower bottom to enter, ultrapure water sprays under first piece of tower tray on absorption tower top;In absorbing tower temperature control 70 DEG C~ 110℃;Two sulfuric acid of cooler discharges sour temperature control system at 40 DEG C~70 DEG C.
7. the method for electronic-grade sulfuric acid production as claimed in claim 4, which is characterized in that the ultrapure water is electric at 25 DEG C Resistance rate is the >=ultrapure water of 18M Ω * cm.
8. the method for electronic-grade sulfuric acid as claimed in claim 4 production, which is characterized in that step (3) sulfuric acid is from stripper-overhead Into high pure air enters from stripping tower lower part;Stripping tower aeration control is in 450 L/min~650L/min.
CN201910636090.6A 2019-07-15 2019-07-15 A kind of apparatus and method of electronic-grade sulfuric acid production Withdrawn CN110255506A (en)

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CN114275743A (en) * 2021-12-10 2022-04-05 湖北兴福电子材料有限公司 Method for producing high-purity liquid sulfur trioxide for electronic-grade sulfuric acid
CN114348972A (en) * 2021-12-10 2022-04-15 湖北兴福电子材料有限公司 Intelligent vaporization and energy recycling method and device for electronic-grade sulfuric acid production
CN116281876A (en) * 2023-03-09 2023-06-23 山东鲁东化学研究院有限公司 Preparation method and production system of electronic grade sulfuric acid

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