CN1326766C - Apparatus and process of producing electronics level high purity hydrochloric acid - Google Patents
Apparatus and process of producing electronics level high purity hydrochloric acid Download PDFInfo
- Publication number
- CN1326766C CN1326766C CNB2004100911538A CN200410091153A CN1326766C CN 1326766 C CN1326766 C CN 1326766C CN B2004100911538 A CNB2004100911538 A CN B2004100911538A CN 200410091153 A CN200410091153 A CN 200410091153A CN 1326766 C CN1326766 C CN 1326766C
- Authority
- CN
- China
- Prior art keywords
- tower
- gas
- pure water
- work
- hydrochloric acid
- 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.)
- Expired - Fee Related
Links
Images
Abstract
The present invention relates to a gas absorption method for producing an electronic chemical-high pure hydrochloric acid and a production device for realizing the method. An electronic chemical-high pure hydrochloric acid can be directly produced by the method and the device of the present invention. The present invention solves the problem that hydrochloric acid gas is purified, and the large-scale production of the high pure hydrochloric acid can be realized by gas absorption. Metal impurities and an anion content of the high pure hydrochloric acid conform to requirements of an MOS grade and a BV-III (equal 3EML-C7) product standard for producing VLSI for metal impurities and anions.
Description
Technical field
The invention relates to the production method and the production equipment of electronic chemical product high purity hydrochloric acid, the electronic chemical product high purity hydrochloric acid of its production is mainly used in the production of microelectronic industry unicircuit, also can be used for the production of reagent grade hydrochloric acid.
Background technology
The production technology that the production of electronic chemical product high purity hydrochloric acid is now mainly adopted is a rectification method.There are shortcomings such as energy consumption height, output capacity is low, the discharging of waste liquid amount is bigger, and environmental pollution is serious in this method.
What the method for production high purity hydrochloric acid adopted mostly now is rectification method.(1) this method has the heating of resistance wire shell and tube, and energy consumption is very big, and tubulation is inner to influence heat conduction efficiency because long-time heated inner surface produces dirty shape thing, and very easily produces dangerous.(2) output capacity is low.Crude product hydrochloric acid is heated in the tower still and forms the azeotrope of about 20.2% (hydrogenchloride and water proportions constant) in the time of 108.5 ℃, raw material adds in the tower continuously in continuous production, and raffinate is also discharged continuously, the content nearly 20% of hydrogenchloride in the raffinate of discharging, output capacity only about 60%, the raffinate of discharging causes environmental pollution, also brings great burden to environmental protection facility.(3) rectification method production is difficult to form mass-producing.The material that rectifying device adopts is the scale that glass or quartzy its heat-supplying mode have in addition determined its equipment, and most of enterprise is that skinny device overlaps production more, and operator's preparation is again the potential risk of safety in production less.
Summary of the invention
The present invention has overcome hydrogen chloride gas bulk absorption method fully and rectification method is produced various weakness in the high purity hydrochloric acid, has realized continuous, efficient, pollution-free, large-scale production.
Energy consumption of the present invention is low, and the output capacity height near 100%, can be mass-produced, non-pollution discharge, and realized high-purity, high density (36～37%) hydrochloric acid of gas absorption method production, overcome the conventional gas absorption method and can only produce 31～32% hydrochloric acid.
In order to produce the electronic-grade high purity hydrochloric acid, the present invention has adopted three grades of gas purification.Gas absorption has adopted resistivity greater than 15M Ω cm
-1Second pure water as absorption liquid, absorption column of gas has adopted the Raschig ring mixed fillers of purified quartz and polypropylene material, utilizes hydrogen chloride gas as raw material.This device is simple, practical, easy handling.
The present invention relates to the gas absorption method and produce the production method of electronic chemical product high purity hydrochloric acid and the device of realizing this method.Its concrete feature is as follows:
1. the processing method of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, this method may further comprise the steps:
(1) adopting hydrogen chloride gas is raw material,
(2) hydrogenchloride of 0.15MPa is after variable valve ZQ-01 adjusts, and hydrogen chloride gas enters gas sweetening purification tower T-1 through mass flowmeter ZL-01,
(3) hydrogen chloride gas through in be filled with gac gas sweetening purification tower T-1, continuing to move ahead behind the organism that is contained in gac is removed gas enters gas purification washing tower T-2,
(4) hydrogen chloride gas enters the tower T-3 that the liquefied gas scavenging agent is housed after the purification through liquefied gas scavenging agent in the tower in tower T-2;
(5) hydrogen chloride gas enters the tower T-4 that the liquefied gas scavenging agent is housed after the purification through liquefied gas scavenging agent in the tower in tower T-3,
(6) tower 2, tower 3 and tower 4 built-in described liquefied gas scavenging agents are by the formulated acidic solution of potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or nitric acid,
(7) one times soft water is produced resistivity greater than 15M Ω .cm after the second pure water equipment clean
-1Second pure water, rely on the constant current water pump of second pure water equipment to be transported among the second pure water storage tank V-1,
(8) second pure water among the second pure water storage tank V-1 is transported to tower T-5 top by water transferpump GP-1,
(9) purify the hydrogen chloride gas of purifying through tower T-1, tower T-2, tower T-3 and tower T-4 and enter tower T-5 from tower T-5 bottom, the second pure water that flows into top of tower mixes mutually, reaction generates the electronic chemical product high purity hydrochloric acid after emitting a large amount of heats, content is greater than 36%, the electronic chemical product high purity hydrochloric acid that generates relies on the weight of self to flow into work in-process storage tank V-2
(10) refrigerated brine divides two parts to flow into the tower inner coil pipe from tower T-5 bottom side from the outflow of tower T-5 upper side through variable valve QL-51, variable valve QL-52 and under meter ZL-51, under meter ZL-52, and reaction heat is taken away, and the temperature of refrigerated brine is-5～10 ℃,
(11) work in-process among the work in-process storage tank V-2 go packing through work in-process transferpump GP-2 and electronic chemical product particle controlled filter device FV-1,
(12) work in-process among the work in-process storage tank V-2 link to each other with absorption tower T-5 to the ZX-5 of tower T-5 top variable valve through finished product transferpump GP-2 and variable valve GR-V2 and form a closed cycle.
2. a device that is used for the method for the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup is characterized in that this device comprises a cover second pure water equipment,
Second pure water equipment is connected with second pure water storage tank V-1; Second pure water storage tank V-1 is connected with tower T-5; Gas sweetening purification tower T-1, tower T-2, tower T-3 and tower T-4 are connected successively, gas sweetening purification tower T-1, interior filling gac; The built-in described liquefied gas scavenging agent of gas purification washing tower T-2, tower T-3 and tower T-4 is by the formulated acidic solution of potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or nitric acid; Absorption column of gas T-5, coil tube type cooling, the filler material is for being selected from glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material Raschig ring; Work in-process storage tank V-2; Work in-process transferpump GP-2, electronic chemical product particle controlled filter device FV-1; And above each single devices phase logotype pipeline and variable valve.
3. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, its resistivity of second pure water that it is characterized in that the second pure water device fabrication is greater than 15M Ω .cm
-1
4. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, the material that it is characterized in that second pure water storage tank V-1, tower T-1, tower T-2, tower T3, tower T-4 and tower T-5 adopt and are selected from glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material and make.
5. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, the gac that it is characterized in that filling in the gas sweetening purification tower T-1 is by the preparation of coconut husk class, through peracid treatment, and the liquefied gas scavenging agent of filling is with strong oxidizer potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or the formulated acidic solution of nitric acid in gas purification washing tower T-2, tower T-3 and the T-4.
6. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, it is characterized in that filling Raschig ring in the absorption column of gas T-5, its material is glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material, absorption column of gas T-5 adopts refrigerated brine, inlet water temperature is 0～10 ℃, temperature out is controlled at below 50 ℃, and work in-process storage tank V-2 is suitable for reading to be not less than 0.60 meter with tower T-5 liquid outlet difference of altitude.
7. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, what it is characterized in that filling in gas purification washing tower T-2, tower T-3 and the tower T-4 is the liquefied gas scavenging agent, wherein adds the Raschig ring of polyethylene or polypropylene material.
8. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, it is characterized in that work in-process storage tank V-2 adopts materials such as glass, quartz, polyethylene, polypropylene or tetrafluoroethylene to make, work in-process hydrochloric acid is transported to the purpose that tower T-5 top realizes that circulation absorbs through work in-process transferpump GP-2 and variable valve GR-V2 with work in-process electronics chemical high purity hydrochloric acid among the work in-process storage tank V-2, and what work in-process transferpump GP-2 adopted is tetrafluoroethylene material diaphragm metering pump.
9. the device of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, it is characterized in that the connection line between each single devices all makes with glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material, the total system regulated valve all adopts the tetrafluoroethylene diaphragm valve.
Utilize this law and production equipment can realize production extensive, high-level product; The key of producing high purity hydrochloric acid at first is the purifying of gas; Because high purity hydrochloric acid is the surface cleaning that is used for the production process of VLSI, ULSI; Metallic impurity individual event in the high purity hydrochloric acid is lower than 1～10ppb, and anion-content is lower than 200ppb; Therefore, the metals content impurity in the hydrogen chloride gas of Shi Yonging should be very low aborning, and the purification of hydrogen chloride gas is purified and is even more important; The overwhelming majority of present method and production equipment is used for the purifying hydrogen chloride gas; What fill among the tower T-1 is the gac of modification, the adsorbable organic substance that removes in the hydrogen chloride gas; The service temperature of this tower should be lower than 35 ℃; Otherwise the organism of charcoal absorption can parse in the system of reentering, thereby influences quality product; Thereby tower T-2 and tower T-3 adopt the strong acidic liquid gas purifying agent to meet the product that MOS level and BV-III grade standard require with the product of removing the extremely impurity of trace in the hydrogen chloride gas and guaranteeing that gas absorption is come out at the metallic impurity in the hydrogen chloride gas and negatively charged ion respectively;
The gas absorption method is produced a quality that key factor is used water quality of high purity hydrochloric acid; Pure water system mainly comprises former water pretreatment, 1 st pure water preparation, second pure water preparation;
Another key that the gas absorption method is produced high purity hydrochloric acid is the control of concentration of hydrochloric acid; The technology of hydrochloric acid production at present is very ripe, and the gas absorption fado adopts falling-film tower; Because hydrogen chloride gas can produce a large amount of heats when water-soluble; Untimely these heats are taken away the further absorption that can have a strong impact on hydrogenchloride, so prior art is many to produce 31% hydrochloric acid soln; Among the present invention absorption column of gas is redesigned, designed large-area heat exchange system in the tower T-5; Take away heat in the tower as early as possible by water coolant; Loaded in addition quartzy in the tower and polypropylene material mixed fillers has increased the gas-to-liquid contact area greatly, thereby realized the production of concentrated hydrochloric acid (36%～37%);
What the method for production high purity hydrochloric acid adopted mostly now is rectification method; (1) this method has the heating of resistance wire shell and tube, and energy consumption is very big, and tubulation is inner to influence heat conduction efficiency because long-time heated inner surface produces dirty shape thing, and very easily produces dangerous; (2) output capacity is low; Crude product hydrochloric acid is heated in the tower still and forms the azeotrope of about 20.2% (hydrogenchloride and water proportions constant) in the time of 108.5 ℃, raw material adds in the tower continuously in continuous production, and raffinate is also discharged continuously, the content nearly 20% of hydrogenchloride in the raffinate of discharging, output capacity only about 60%, the raffinate of discharging causes environmental pollution, also brings great burden to environmental protection facility; (3) rectification method production is difficult to form mass-producing; The material that rectifying device adopts is glass or quartz, and its heat-supplying mode has determined the scale of its equipment in addition, and most of enterprise is that skinny device overlaps production more, and operator's preparation is again the potential risk of safety in production less;
The present invention has overcome hydrogen chloride gas bulk absorption method fully and rectification method is produced various weakness in the high purity hydrochloric acid, has realized continuous, efficient, pollution-free, large-scale production;
Description of drawings
Accompanying drawing 1: electronic chemical product high purity hydrochloric acid technological process of production figure
1 ZQ-01 ZQ-02 gas control valve, 2 T-1 gas purification purifying columns, T-2, T-3 and T-4 gas purification scrubbing tower 3 JP-1 JP-2 JP-3 JP-4 ZP-1 ZP-2 ZP-3 ZP-4 ZP-5 ZP-6 ZX-1 ZX-2 ZX-3 ZX-4 ZX-6ZQ-5 ZF-6 enlarging straight-through valves 4 GP-1 finished product delivery pumps 5 GP-2 second pure water delivery pumps 6 ZL-01 gas flowmeters 7 GS-V11 GS-V12 GP-V21 GP-V2 GR-V2 ZC-V22 barrier film straight-through valves 8 T-5 absorption column of gas 9 T-6 suck-back-prevention type gas scrubbing fluid-tight towers 10 ZL-51 ZL-52 refrigerated brine flowmeters 11 QL-51 QL-52 direct-through valves 12 V-1 second pure water storage tanks 13 V-2 semi-finished product storage tanks 14 FV-1 electronic chemicals particle control filters
Accompanying drawing 2: tower T-6 suck-back-prevention type gas scrubbing fluid-tight tower
The inlet gas pipe 5 tower T-6 middle part glass partition of the pneumatic outlet 4 tower T-6 of the end opening 3 tower T-6 of the gas inlet 2 tower T-6 of 1 tower T-6
Accompanying drawing 3: second pure water system
1 activated carbon column, 2 ion exchange resin columns, 3 ion exchange resin columns, 4 contaminant filter, 5 electricity are led 6 threeways 7 of detection indicating system and are gone out water regulating valve 8 constant current water pumps
Embodiment
Technology specific embodiments of the present invention is as follows
The pressure of hydrogen chloride gas is 0.15MPa, through mass flowmeter ZL-01 metering, is connected with threeway through variable valve ZQ-01; Nitrogen gas pressure is that 0.15MPa is connected with threeway; Hydrogen chloride gas and nitrogen are mixed into scavenging tower T-1 in threeway, what load among the tower T-1 is coconut husk class modified activated carbon, gac can be removed the metallic impurity of the organic compound of oils in the unstripped gas and low-carbon (LC) and iron, copper, the working temperature of this tower should be lower than 35 ℃, otherwise the impurity of charcoal absorption can parse and enter next stage, or even has a strong impact on quality product in the absorption tower;
Begin all to adopt the web member of glass, quartz or tetrafluoroethylene material from tower T-1 to the connection of tower T-6; Because the index that high purity hydrochloric acid requires is very strict, therefore forbid in system, to use metal species web member or pipeline;
1. valve JP-1 is the enlarging through way valve, and material is glass, quartz or tetrafluoroethylene; Its technology characteristics:
1. this valve can help system emptying when system pressure is higher;
When 2. being negative pressure in the system, replenish virgin gas to system;
Can in tower T-2, replenish fresh liquefied gas scavenging agent by valve JP-1 when 3. the washings among the tower T-2 is not enough;
2. valve ZQ-1 is straight-through enlarging valve, and material is glass, quartz or tetrafluoroethylene, and its technology characteristics is the connection valve between tower T-1 and the tower T-2, when tower T-1 and tower T-2 are handled, adjust, maintenance etc. are disturbed mutually and are polluted preventing by valve ZQ-1;
3. tower T-2, tower T-3 and tower T-4 are the gas purification washing towers, the liquefied gas scavenging agent that adopts in tower T-2 and the tower T-3 tower, its technology characteristics is:
1.. the liquefied gas scavenging agent mainly is an acidic liquid;
2.. added strong oxidizer in the liquefied gas scavenging agent, in acidic medium, gas middle or low price attitude oxidation of impurities can have been become not volatile high price attitude material, it has been stayed in the washings, thereby reach the purpose that gas sweetening is purified; Strong oxidizer adopts potassium permanganate, persulfuric acid, sulfuric acid, hydrogen peroxide, potassium bichromate or nitric acid
3.. service temperature must be controlled at below 35 ℃
4. the pipeline of enlarging through way valve ZP-2 by glass, quartz or tetrafluoroethylene material links to each other with the residual liquid discharge pipe, needs the discharging of the washings among the tower T-2 totally in explained hereafter or during maintenance of the equipment, and just can open the tower maintenance after washing in the tower;
5. enlarging through way valve ZX-2, material is glass, quartz or tetrafluoroethylene, is connected with tower T-2 top; Its technology characteristics is:
1.. top links to each other with secondary water storage tank CV-1 with second pure water transferpump GP-1 by the secondary water pipe, after equipment installs, supplies pure water by the ZX-2 valve in tower, the filler in washing tower T-2 and the tower;
2.. when tower T-2 washings liquid level is on the low side, add the liquid level that second pure water improves washings in the tower T-2 by valve ZX-2;
3.. valve ZX-2 links to each other with tower T-6 top by four-way, when equipment is in nonproductive state, cause negative pressure in the tower T-2 owing to HCl in the gas phase in the tower T-2 is dissolved in liquid phase, the cooperation additional virgin gas in system by valve ZX-2 and tower T-6 makes the vapour-liquid two-phase reach balance;
6. link to each other by glass, quartz or tetrafluoroethylene pipeline between tower T-2 and tower T-3 two towers, and be connected with straight-through enlarging valve ZQ-2 with standpipe drain by valve JP-2;
7. the technology between tower T-3, tower T-4 and the tower T-5 connects, and is the same;
8. valve JP-2, valve JP-3 are identical with valve JP-1 with valve JP-4 technology characteristics;
9. valve ZQ-2, valve ZQ-3 and valve ZQ-4, technology characteristics is identical with valve ZQ-1;
10. valve ZP-3, valve ZP-4 are identical with valve ZP-2 with valve ZQ-6 technology characteristics;
11. valve ZX-3, valve ZX-4, valve ZX-5 are identical with valve ZX-2 with valve ZX-6 technology characteristics;
12. tower T-4 is a HCl gas purification washing tower, the washings in the tower T-4 is different with the washings of tower T-2 and tower T-3, does not put into oxygenant in the liquid phase; Because the back one-level is exactly the absorption tower, also be in order to prevent because the fluctuation of internal system working condition is brought the impurity of prime in the tower T-5 into;
13. add the Raschig ring that is made by macromolecular material in liquefied gas scavenging agent in tower T-2, the tower T-3 and the washings in the tower T-4, material is that polyethylene or polypropylene material are made, technology characteristics is a disturbance vapour-liquid mixed phase, increases vapour-liquid duration of contact;
14. being glass or quartzy material, makes tower T-5:
1.. hydrogen chloride gas purifies after valve ZQ-4 enters the absorption tower T-5 of gas from tower T-5 bottom through tower T-1, tower T-2, tower T-3 and tower T-4 level Four, and air-flow flows from bottom to top;
2.. secondary water pure water provides power by pump GP-1, and through way valve ZX-5 enters tower T-5 top through tower T-5 top, and water flows from top to bottom;
3.. tower T-5 indoor design is the big area tube exchanger, and inside is filled with Raschig ring and the quartz material Raschig ring that the polypropylene material is made, and filler is for huddling type; Filler is for increasing vapour-liquid duration of contact and contact area, so that hydrogen chloride gas is fully absorbed;
4.. water goes downstream at filling surface, contacts everywhere with upstream hydrogen chloride gas packing box inside pipe wall in tower etc., is combined into hydrochloric acid, and discharges a large amount of heat; Different heights can form a concentration gradient in the tower, increases successively from top to bottom; Obtain our needed 36%～37% high purity hydrochloric acid in tower T-5 bottom, the present invention realizes that concentration can regulate with interior 0～40%, by changing the cooling water flow in the tower T-5, processing condition such as vapor-liquid ratio realize in electronic chemical product high purity hydrochloric acid concentration 0～40% scope adjustable;
15. valve ZP-5 is the enlarging through way valve, by threeway and sampling valve GY-5, finished product is collected valve GC-V21 valve and is linked to each other, and then links to each other with work in-process storage tank V-2, generates purifying hydrochloric acid in the T-5 of absorption tower and flows into work in-process storage tank V-2 through this;
16. being the enlarging through way valve, valve ZQ-5 tower T-5 is connected with tower T-6 by pipeline;
By pipeline tower T-6 is connected 17. valve ZF-6 is the enlarging through way valve with the external world, technology characteristics is with the residual gas emptying in the system;
18. tower T-6 is the suck-back-prevention type gas scrubbing fluid-tight tower of being made by glass or quartzy material, structure is seen accompanying drawing 2;
Technology characteristics:
1.. tower T-6 bottom has 1/2～2/3, second pure water or diluted alkaline washings, the water that the unabsorbed hydrogen chloride gas of tower T-5 enters in tower T-6, the tower T-6 during ordinary production can prevent that hydrogen chloride gas from entering atmospheric environment and causing environmental pollution with hydrogen chloride gas bulk absorption wherein;
2.. when in case negative pressure appears in system, air in the outside atmosphere can suck in the tower T-6 by valve ZF-6, the liquid of tower T-6 bottom forms fluid-tight owing to negative pressure sucks top, and extraneous gas enters system after the washings washing thus, has prevented that introduced contaminants from entering system and polluted product;
19. be described as follows according to accompanying drawing 2:
1. .1 is the gas inlet of tower T-6; 2 is the end opening of tower T-6; 3 is the pneumatic outlet of tower T-6; 4 is the inlet gas pipe of tower T-6; 5 is tower T-6 middle part glass partition;
2.. its technology characteristics be gas through 1 enter tower T-6 glass partition 5 above in the cavity, enter the tower bottom through managing 4; Splendid attire 1/2～2/3 second pure water or diluted alkaline washings in the bottom, gas enter in the liquid of bottom through liquid scrubbing after 3 give off tower;
3.. when if negative pressure appears in system, the meeting suck-back of the liquid of tower bottom go into glass partition 5 above, the gas of suck-back can be through 3 and 4 tops that enter tower, intake system after this liquid scrubbing; Prevent that like this liquid from being gone into system by suck-back;
20. work in-process storage tank V-2 system is made by polypropylene or tetrafluoroethylene material, the resisting high-concentration hcl corrosion, and technology characteristics:
1.. work in-process hydrochloric acid is collected at this and is stored, and a certain amount of back enters ultra-clean chamber by liquid delivery pump GP-2 through through way valve ZC-V22, through filter FV-1 packing;
2.. open liquid delivery pump GP-2 when in case the work in-process concentration among the work in-process storage tank V-2 is on the low side, open through way valve ZR-V2 and valve ZX-5, the work in-process that concentration is on the low side pump into absorption tower T-5, and secondary absorbs and improves concentration of hydrochloric acid to required concentration;
21.0～10 ℃ refrigerated brine divides two parts to enter in the tower T-5 spiral coil cooling tube through variable valve QL-51, variable valve QL-52 and under meter ZL-51, under meter ZL-52; Flow out from the LQC valve.
Technology characteristics:
1.. by variable valve QL-51, variable valve QL-52 and under meter ZL-51, under meter ZL-52 the consumption of refrigerated brine is adjusted between 1100～1600L/h;
2.. the temperature out of refrigerated brine directly influences the concentration of finished product hydrochloric acid, can the refrigerated brine temperature out is controlled at below 45 ℃ by the flow of variable valve QL-51 and variable valve QL-52 adjustment refrigerated brine;
3.. refrigerated brine is supplied with according to the height segmentation of tower T-5;
22. secondary water storage tank V-1, its material is identical with work in-process storage tank V-2, links to each other with the secondary water system by pipeline; Second pure water among the secondary water storage tank V-1 pumps into tower T-5 through pump GP-1;
Valve GS-V11 is a through way valve, and its material is glass, quartz, tetrafluoroethylene or stainless steel;
Valve GS-V12 is a through way valve, and its material is glass, quartz, tetrafluoroethylene or stainless steel;
Pump GP-1 is a liquid delivery pump, and its material is the surge pump of tetrafluoroethylene or polyvinylidene difluoride (PVDF) material;
Pump GP-2 is a microprocessor pump drive; Its material is the surge pump of tetrafluoroethylene or polyvinylidene difluoride (PVDF) material;
23. second pure water system
The second pure water system is the necessaries of preparation second pure water; Be that a soft water further is refined into resistivity greater than 15M Ω cm
-1Second pure water; Be connected with second pure water storage tank V-1 by pipeline; In Fig. 3
1. .1 is activated carbon column shell useable glass, quartz, tetrafluoroethylene or stainless material preparation, and soft water can be removed the organic matter in soft water through the gac art;
2. negative resin and positive resin make .2 and 3 for ion exchange resin column is respectively; Shell prepares with glass, quartz, tetrafluoroethylene or stainless steel, and one time soft water is removed a small amount of negatively charged ion and the positively charged ion that contain in the water through (2) and (3);
3. .4 is a contaminant filter; Particle filtration in the water is fallen to reach service requirements;
4. .5 is that electricity is led the detection indicating system; The water quality of indication second pure water system outlet; In case the undesirable variable valve 7 of cutting out of water quality makes the native system self-circulation up to the requirement that reaches production;
5. .6 is threeway, and material is a stainless steel;
6. .7 is for going out water regulating valve; Material is stainless steel or tetrafluoroethylene material; The control water yield;
7. .8 is the constant current water pump; Material is a stainless steel; A small amount of negatively charged ion and positively charged ion that soft water is removed in anhydrating by ion exchange resin column 2 and ion exchange resin column 3 with the constant flow;
8.. the each several part connection line all adopts the pressure-resistant plastic pipeline;
Claims (9)
1. the processing method of the sub-chemical high purity hydrochloric acid of gas absorption legal system power backup, this method may further comprise the steps:
(1) adopting hydrogen chloride gas is raw material,
(2) hydrogenchloride of 0.15MPa is after variable valve ZQ-01 adjusts, and hydrogen chloride gas enters gas sweetening purification tower T-1 through mass flowmeter ZL-01,
(3) hydrogen chloride gas through in be filled with gac gas sweetening purification tower T-1, continuing to move ahead behind the organism that is contained in gac is removed gas enters gas purification washing tower T-2,
(4) hydrogen chloride gas enters the tower T-3 that the liquefied gas scavenging agent is housed after the purification through liquefied gas scavenging agent in the tower in tower T-2;
(5) hydrogen chloride gas enters the tower T-4 that the liquefied gas scavenging agent is housed after the purification through liquefied gas scavenging agent in the tower in tower T-3,
(6) tower 2, tower 3 and tower 4 built-in described liquefied gas scavenging agents are by the formulated acidic solution of potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or nitric acid,
(7) one times soft water is produced resistivity greater than 15M Ω .cm after the second pure water equipment clean
-1Second pure water, rely on the constant current water pump of second pure water equipment to be transported among the second pure water storage tank V-1,
(8) second pure water among the second pure water storage tank V-1 is transported to tower T-5 top by water transferpump GP-1,
(9) purify the hydrogen chloride gas of purifying through tower T-1, tower T-2, tower T-3 and tower T-4 and enter tower T-5 from tower T-5 bottom, the second pure water that flows into top of tower mixes mutually, reaction generates the electronic chemical product high purity hydrochloric acid after emitting a large amount of heats, content is greater than 36%, the electronic chemical product high purity hydrochloric acid that generates relies on the weight of self to flow into work in-process storage tank V-2
(10) refrigerated brine divides two parts to flow into the tower inner coil pipe from tower T-5 bottom side from the outflow of tower T-5 upper side through variable valve QL-51, variable valve QL-52 and under meter ZL-51, under meter ZL-52, and reaction heat is taken away, and the temperature of refrigerated brine is-5～10 ℃,
(11) work in-process among the work in-process storage tank V-2 go packing through work in-process transferpump GP-2 and electronic chemical product particle controlled filter device FV-1,
(12) work in-process among the work in-process storage tank V-2 link to each other with absorption tower T-5 to the ZX-5 of tower T-5 top variable valve through finished product transferpump GP-2 and variable valve GR-V2 and form a closed cycle.
2. device that is used to realize the method for claim 1, this device comprises a cover second pure water equipment,
Second pure water equipment is connected with second pure water storage tank V-1; Second pure water storage tank V-1 is connected with tower T-5; Gas sweetening purification tower T-1, tower T-2, tower T-3 and tower T-4 are connected successively, gas sweetening purification tower T-1, interior filling gac; The built-in described liquefied gas scavenging agent of gas purification Xian Di tower T-2, tower T-3 and tower T-4 is by the formulated acidic solution of potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or nitric acid; Absorption column of gas T-5, the coil tube type cooling, the filler material is for being selected from glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material Raschig ring; Work in-process storage tank V-2; Work in-process transferpump GP-2, electronic chemical product particle controlled filter device FV-1; And above each single devices phase logotype pipeline and variable valve.
3. according to the described device of claim 2, its resistivity of second pure water that it is characterized in that the second pure water device fabrication is greater than 15M Ω .cm
-1
4. according to the described device of claim 2, the material that it is characterized in that second pure water storage tank V-1, tower T-1, tower T-2, tower T-3, tower T-4 and tower T-5 adopts and is selected from glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material and makes.
5. according to the described device of claim 2, the gac that it is characterized in that filling in the gas sweetening purification tower T-1 is by the preparation of coconut husk class, through peracid treatment, and the liquefied gas scavenging agent of filling is with strong oxidizer potassium permanganate, persulfuric acid, potassium bichromate, hydrogen peroxide or the formulated acidic solution of nitric acid in gas purification washing tower T-2, tower T-3 and the T-4.
6. according to the described device of claim 2, it is characterized in that filling Raschig ring in the absorption column of gas T-5, its material is glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material, absorption column of gas T-5 adopts refrigerated brine, inlet water temperature is 0～10 ℃, temperature out is controlled at below 50 ℃, and work in-process storage tank V-2 is suitable for reading to be not less than 0.60 meter with tower T-5 liquid outlet difference of altitude.
7. according to the described device of claim 2, what it is characterized in that the interior filling of gas purification washing tower T-2, tower T-3 and tower T-4 is the liquefied gas scavenging agent, wherein adds the Raschig ring of polyethylene or polypropylene material.
8. according to the described device of claim 2, it is characterized in that work in-process storage tank V-2 adopts glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material to make, work in-process hydrochloric acid is transported to the purpose that tower T-5 top realizes that circulation absorbs through work in-process transferpump GP-2 and variable valve GR-V2 with work in-process electronics chemical high purity hydrochloric acid among the work in-process storage tank V-2, and what work in-process transferpump GP-2 adopted is tetrafluoroethylene material diaphragm metering pump.
9. according to the described device of claim 2, it is characterized in that the connection line between each single devices is all made with glass, quartz, polyethylene, polypropylene or tetrafluoroethylene material, the total system regulated valve all adopts the tetrafluoroethylene diaphragm valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100911538A CN1326766C (en) | 2004-11-22 | 2004-11-22 | Apparatus and process of producing electronics level high purity hydrochloric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100911538A CN1326766C (en) | 2004-11-22 | 2004-11-22 | Apparatus and process of producing electronics level high purity hydrochloric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1608975A CN1608975A (en) | 2005-04-27 |
| CN1326766C true CN1326766C (en) | 2007-07-18 |
Family
ID=34766270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100911538A Expired - Fee Related CN1326766C (en) | 2004-11-22 | 2004-11-22 | Apparatus and process of producing electronics level high purity hydrochloric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1326766C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398895A (en) * | 2010-09-16 | 2012-04-04 | 上海化学试剂研究所 | Production method of ultra-pure electronic grade chemical reagent |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017026260A1 (en) * | 2015-08-10 | 2017-02-16 | 昭和電工株式会社 | Method for producing hydrogen chloride |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1189787A (en) * | 1995-06-05 | 1998-08-05 | 斯塔泰克文切斯公司 | Point-of-use ammonia purifation for electronic component manufacture |
-
2004
- 2004-11-22 CN CNB2004100911538A patent/CN1326766C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1189787A (en) * | 1995-06-05 | 1998-08-05 | 斯塔泰克文切斯公司 | Point-of-use ammonia purifation for electronic component manufacture |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102398895A (en) * | 2010-09-16 | 2012-04-04 | 上海化学试剂研究所 | Production method of ultra-pure electronic grade chemical reagent |
| CN102398895B (en) * | 2010-09-16 | 2014-09-24 | 上海化学试剂研究所 | Production method of ultra-pure electronic grade chemical reagent |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1608975A (en) | 2005-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1083564C (en) | System and method for delivering vapor-phase product to place for using | |
| US6050283A (en) | System and method for on-site mixing of ultra-high-purity chemicals for semiconductor processing | |
| US5496778A (en) | Point-of-use ammonia purification for electronic component manufacture | |
| US5722442A (en) | On-site generation of ultra-high-purity buffered-HF for semiconductor processing | |
| KR100481256B1 (en) | Apparatus and method for point-of-use treatment of effluent gas streams | |
| EP0831978B1 (en) | On-site ammonia purification for semiconductor manufacture | |
| JPH1147584A (en) | Method and apparatus for manufacture of high purity chemical for microelectronics industry | |
| KR101775888B1 (en) | Method and device for treating fluorine-containing water | |
| CN104129762A (en) | Preparation method and preparation system of high-purity sulfuric acid solution | |
| CN109761196A (en) | A kind of method for producing electronic grade hydrochloric acid | |
| US20020081237A1 (en) | On-site generation of ultra-high-purity buffered-HF and ammonium fluoride | |
| CN204588694U (en) | A kind of production system of used in electronic industry hydrofluoric acid | |
| US6001223A (en) | On-site ammonia purification for semiconductor manufacture | |
| CN1326766C (en) | Apparatus and process of producing electronics level high purity hydrochloric acid | |
| CN104841195A (en) | Purification and recovery device for chlorosilane waste liquid and purification and recovery method for chlorosilane waste liquid | |
| CN207552067U (en) | The de- analysis apparatus of by-product hydrochloric acid in a kind of organic silicon monomer production process | |
| CN211998831U (en) | Electrolytic NF3Continuous pre-purification device | |
| WO1996039651A1 (en) | System and method for on-site mixing of ultra-high-purity chemicals for semiconductor processing | |
| CN108017039A (en) | Monochlorodifluoromethane by-product HCL produces the preparation method and device of high purity hydrochloric acid | |
| JPH11506411A (en) | On-site ammonia purification for electronic component manufacturing. | |
| KR19990022227A (en) | On-Site Generation System for Ultrathin Buffer-HF for Semiconductor Process | |
| CN205709899U (en) | A kind of ammonia gas purification device | |
| CN101071035B (en) | Method for delivering purity raised gas and purity improved overheat gas | |
| CN212356561U (en) | Preparation device of electronic grade ultrapure ammonia water | |
| CN103550948B (en) | To the method that waste gas and the waste liquid of chlorosilane rectification and purification operation process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20070718 Termination date: 20141122 |
|
| EXPY | Termination of patent right or utility model |