CN105947994A - Production device and production method for MOS-grade sulfuric acid used for microelectronics - Google Patents
Production device and production method for MOS-grade sulfuric acid used for microelectronics Download PDFInfo
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- CN105947994A CN105947994A CN201610276602.9A CN201610276602A CN105947994A CN 105947994 A CN105947994 A CN 105947994A CN 201610276602 A CN201610276602 A CN 201610276602A CN 105947994 A CN105947994 A CN 105947994A
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- sulphuric acid
- acid
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- desorption
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention relates to a production device and a production method for MOS-grade sulfuric acid used for microelectronics. The production device comprises an absorption unit, a reabsorption unit, a desorption unit, a sulfuric acid product tank and a tail gas recovery unit. The method prepares the MOS-grade sulfuric acid used for microelectronics through a series of purification, absorption, cooling and desorption processes to sulfur trioxide mixed gas in an industrial production system by using the above-mentioned device. The invention has the following advantages: system stability is high; and production cost is effectively reduced.
Description
Technical field
The present invention relates to the process units of a kind of sulphuric acid, especially relate to the production dress of a kind of microelectronics MOS level sulphuric acid
Put, the invention still further relates to the production method of a kind of sulphuric acid, especially relate to the production method of a kind of microelectronics MOS level sulphuric acid.
Background technology
POV, as one of fine chemicals, is widely used in the industry such as telecommunications, medicine, also serves as chemistry examination
Agent and the raw material of accumulator, wherein the MOS stage in chip production process, it is also desirable to use sulphuric acid to realize this technique,
And the purity of sulphuric acid is had higher requirement, i.e. MOS level sulphuric acid, MOS level sulphuric acid refers in sulphuric acid ferrum element concentration not
Concentrated sulphuric acid more than 100PPb.
In prior art, the method producing employing industrial sulphuric acid distillation mostly of MOS level sulphuric acid and the liquid of employing finished product
Sulfur trioxide gas is produced by absorption process, and this method has the disadvantage that one, uses the way of distillation or uses finished product
Liquid sulphur trioxide, its energy consumption and production cost are the highest, and two, the production safety coefficient of both approaches is relatively low；Three, to sulphuric acid
Concentration precision controlling not accurate enough, be difficult to reach production requirement.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art, the present invention provides the life of a kind of microelectronics MOS level sulphuric acid
Produce device and production method, highly purified microelectronics MOS level sulphuric acid can not only be produced, there is relatively low production cost simultaneously
Higher system reliability energy, and there is relatively simple operating process, it is effectively improved economic benefit.
In order to realize foregoing invention purpose, the technical scheme that the present invention provides is as follows:
The process units of a kind of microelectronics MOS level sulphuric acid, this device includes: absorption plant, weight absorption plant, desorption receive dress
Put, sulphuric acid pan tank and device for recovering tail gas；Absorption plant, this absorption plant includes the first absorption tower, sulphuric acid circulating slot, sulphuric acid
Circulating pump, the first sulfuric acid cooler, preheater, sulfur trioxide evaporator, defecator and waste liquid tank, set on the first absorption tower
There are the first air inlet, first row QI KOU, the first inlet and the first liquid outlet, in described sulphuric acid circulating slot, are provided with sulphuric acid circulation
Pump, is provided with sulphuric acid circulating pump liquid outlet and sulphuric acid circulating pump inlet on described sulphuric acid circulating pump, cold at described first sulphuric acid
But device is provided with cooler inlet, cooler liquid outlet, recirculated cooling water water inlet and recirculated cooling water outlet, described
Preheater is provided with cold acid import, cold acid outlet, hot acid import and hot acid outlet, is provided with steaming in described sulfur trioxide evaporator
Send out device inlet, vaporizer liquid outlet, heating steam inlet, condensation-water drain and sulfur trioxide gas outlet, filter dress described
Putting and be provided with filtered inlet, filtering outlet and leakage fluid dram, described defecator is cage structure, is provided with filter in defecator
Net, described first air inlet is connected with industrial sulphuric acid production system by pipeline, and described first row QI KOU passes through pipeline and work
Industry sulfuric acid production system is connected, and is provided with the first sulphuric acid spray thrower, described first sulphuric acid spray thrower and in the first absorption tower
One inlet is connected, and described first liquid outlet is connected with sulphuric acid circulating slot by pipeline, described sulphuric acid circulating pump inlet
Being connected with sulphuric acid circulating slot, described sulphuric acid circulating pump liquid outlet is connected with cooler inlet and heated acid import respectively
Logical, described cooler liquid outlet and the first inlet are connected, described recirculated cooling water water inlet and recirculated cooling water outlet
Being connected with circulating water inlet and return pipe respectively, described heated acid import is connected with heated acid outlet, described quilt
Cooling acid outlet is connected with vaporizer inlet, and described vaporizer liquid outlet is connected with cooled acid import, described cold
But acid import is connected with cooled acid outlet, and described cooled acid exports and is connected with sulphuric acid circulating slot, described in add vapours
Import is connected with condensation-water drain, and described sulfur trioxide gas outlet is connected with pneumatic filter import, described gas filtration
Device leakage fluid dram is communicated to waste liquid tank；
Weight absorption plant, this heavy absorption plant includes that second absorption tower, MOS absorb acid circulating slot, MOS absorbs acid circulating pump and the
Two sulfuric acid coolers, are provided with the second air inlet, second exhaust port, the second inlet and the second liquid outlet on second absorption tower,
Be provided with MOS absorption acid circulating slot import on described MOS absorption acid circulating slot, MOS absorbs sour circulating slot outlet and ultra-pure water enters
Mouthful, absorb at described MOS and be provided with input and outfan on acid circulating pump, described second sulfuric acid cooler is provided with cooler
Sulphuric acid import, the outlet of cooler sulphuric acid, circulating cooling water inlet and circulating cooling water out, described second air inlet passes through pipeline
Be connected with filtering outlet, at described second air inlet, be provided with gas dilution device, described second exhaust port by pipeline with
Device for recovering tail gas is connected, and is provided with the second sulphuric acid spray thrower, described second sulphuric acid spray thrower and second in second absorption tower
Inlet is connected, and described MOS absorbs acid circulating slot import and is connected with the second liquid outlet, and described MOS absorbs acid circulating slot and goes out
Mouth is connected with input, and described outfan is connected with cooler sulphuric acid import, and the outlet of described cooler sulphuric acid is entered with second
Liquid mouth is connected, and described circulating cooling water inlet is connected with circulating cooling outlet；
Desorption receiving apparatus, this desorption device includes desorption tower, MOS desorption acid circulating slot, MOS desorption acid circulating pump, sulphuric acid finished product
Groove and noble gas generator, be provided with the 3rd air inlet, the 3rd air vent, the 3rd inlet, circulation feed liquor on desorption tower
Mouth and the 3rd liquid outlet, be provided with MOS desorption acid circulating slot import and MOS desorption acid circulation on described MOS desorption acid circulating slot
Groove exports, and is provided with MOS desorption acid circulating pump import and the outlet of MOS desorption acid circulating pump, institute on described MOS desorption acid circulating pump
State the outlet of the 3rd inlet and cooler sulphuric acid to be connected, on described desorption tower in be additionally provided with the 3rd sulphuric acid spray thrower, described
3rd sulphuric acid spray thrower is connected with the 3rd inlet and circulation inlet respectively, and described 3rd liquid outlet follows with MOS desorption acid
Annular groove import is connected, and the outlet of described MOS desorption acid circulating slot is connected with MOS desorption acid circulating pump import, described MOS desorption
Acid circulating pump outlet is connected with circulating inlet, and described 3rd air inlet is connected with noble gas generator, and described the
Three air vents are connected with device for recovering tail gas；
Sulphuric acid pan tank, this sulphuric acid pan tank is connected with the outlet of MOS desorption acid circulating pump by pipeline；
Device for recovering tail gas, this device for recovering tail gas is connected with industrial sulphuric acid production system.
In the process units of above-mentioned microelectronics MOS level sulphuric acid of the present invention, described process units connects with sulphuric acid
The position touched is all covered with Fluorine-lined material, it is possible to effectively prevent concentrated sulphuric acid to the corrosion of equipment and the purity of guarantee concentrated sulphuric acid.
Present invention also offers a kind of method utilizing above-mentioned production equipment to produce microelectronics MOS level sulphuric acid, the method
Comprise the following steps:
The first step, selects the sulfur trioxide mixed gas of conversion procedure, sulfur trioxide mixed gas in industrial sulphuric acid production system
Entering in the first absorption tower by the first air inlet, concentrated sulphuric acid enters the first sulphuric acid spray thrower, the first sulfur by the first inlet
Acid spray thrower absorbs sulfur trioxide in concentrated sulphuric acid is sprayed into the first absorption tower, and unabsorbed mixed gas passes through first exhaust
Mouth is expelled in industrial sulphuric acid production system, absorbs complete concentrated sulphuric acid and enters sulphuric acid circulating slot through the first liquid outlet；
Second step, obtain in the first step absorbs complete and enters the concentrated sulphuric acid in sulphuric acid circulating slot, and a portion is at sulphuric acid
Under the effect of circulating pump, enter in the first sulfuric acid cooler, by recirculated cooling water, above-mentioned concentrated sulphuric acid is cooled down, by
One inlet enters in the first absorption tower, and another part enters in preheater by sulphuric acid circulating pump, enters the dense sulfur of preheater
Sulfur trioxide evaporator is sent in acid after preheating, heats by adding vapours, goes out from condensed water after adding vapours condensation
Mouthful flow out, concentrated sulphuric acid through heating after sulfur trioxide gas therein be heated after overflow, the sulfur trioxide gas of spilling entered
Filter device, the concentrated sulphuric acid after pervaporation is flow in preheater by back of pipeline, enters the concentrated sulphuric acid that wherein temperature is relatively low
Row preheating, is then flow in sulphuric acid circulating slot by back of pipeline；
3rd step, the sulfur trioxide gas obtained in above-mentioned second step removes the impurity such as acid mist after defecator, after purification
Sulfur trioxide gas entered second absorption tower from the second air inlet by pipeline, impurity flows into waste liquid tank by leakage fluid dram
In；
4th step, after the sulfur trioxide gas obtained in the 3rd step enters second absorption tower, by gas dilution device by three oxygen
Change sulfur gas concentration to reduce, spray concentrated sulphuric acid by the second sulphuric acid spray thrower and absorb sulfur trioxide, unabsorbed minimum gas
It is expelled to device for recovering tail gas by second exhaust port, absorbs complete concentrated sulphuric acid and follow through the second liquid outlet entrance MOS absorption acid
Annular groove；
5th step, the concentrated sulphuric acid obtained in the 4th step maintains concentration 96～98% through ultra-pure water dilution, then absorbs acid through MOS
Circulating pump is transported in the second sulfuric acid cooler cool down, and the concentrated sulphuric acid part after cooling enters the by the second inlet
Recycling in two absorption towers, another part concentrated sulphuric acid then flows in desorption tower；
6th step, the concentrated sulphuric acid of inflow desorption device after desorption purifies, enters MOS desorption acid circulating slot in desorption tower
In, a part enters in sulphuric acid pan tank by MOS desorption acid circulating pump, and another part enters in desorption tower and recycles.
In the production method of above-mentioned a kind of microelectronics MOS level sulphuric acid, the collection in described device for recovering tail gas
In gas entrance industrial sulphuric acid drying device after going acid-mist-removing to process, it is delivered in industrial sulphuric acid production system be circulated
Utilize.
According to technique scheme, have the advantage that relative to prior art
One, the sulfur trioxide mixed gas during the present invention utilizes industrial sulphuric acid production system produces, and effectively reduces production
Cost.
Two, the device for recovering tail gas of the present invention has carried out recycling to waste gas therein, is " green " circulation industrial
Skill, reduces production cost simultaneously, the productivity effect of raising.
Three, the process units of the present invention combines production method, has higher system stability and safety, it is ensured that raw
The purity of the MOS level sulphuric acid produced meets production requirement.
Accompanying drawing explanation
Fig. 1 is the flow sheet of microelectronics MOS sulphuric acid plant of the present invention.
Fig. 2 is the structural representation on the first absorption tower in the present invention.
Fig. 3 is the structural representation of sulphuric acid circulating slot in the present invention.
Fig. 4 is the structural representation of sulphuric acid circulating pump in the present invention.
Fig. 5 is the structural representation of the first cooler in the present invention.
Fig. 6 is the structural representation of preheater in the present invention.
Fig. 7 is the structural representation of sulfur trioxide evaporator in the present invention.
Fig. 8 is the structural representation of defecator in the present invention.
Fig. 9 is the structural representation of second absorption tower in the present invention.
Figure 10 is the structural representation that MOS of the present invention absorbs acid circulating slot.
Figure 11 is the structural representation that MOS of the present invention absorbs acid circulating pump.
Figure 12 is the structural representation of the present invention the second cooler.
Figure 13 is the structural representation of desorption tower of the present invention.
Figure 14 is the structural representation of MOS desorption acid circulating slot of the present invention.
Figure 15 is the structural representation of MOS desorption acid circulating pump of the present invention.
Detailed description of the invention
The process units to microelectronics MOS level sulphuric acid of the present invention and producer is come below in conjunction with the accompanying drawings with concrete example
Method is further elaborated, and in the hope of being more fully apparent from understands its structure composition and working method, but can not come with this
Limit the protection domain of patent of the present invention.
As shown in Fig. 1 15, the process units of a kind of microelectronics MOS level sulphuric acid, this device includes: a kind of microelectronics is used
The process units of MOS level sulphuric acid, this device includes: absorption plant, weight absorption plant, desorption receiving apparatus, sulphuric acid pan tank and tail
Gas recovering device；Absorption plant, this absorption plant includes the first absorption tower 2, sulphuric acid circulating slot 3, sulphuric acid circulating pump the 4, first sulfur
Acid cooler 5, preheater 6, sulfur trioxide evaporator 7, defecator 8 and waste liquid tank 9；Described first absorption tower 2 is used to inhale
Sulfur trioxide gas in mixed gas in industry of knocking off sulfuric acid production system 1, it is possible to effectively sulfur trioxide is absorbed；Sulfur
Acid circulating slot 3 is used for storing the concentrated sulphuric acid absorbing sulfur trioxide gas in the first absorption tower 2；Sulphuric acid circulating pump 4 be used to by
Concentrated sulphuric acid in sulphuric acid circulating slot 3 is transported to the first sulfuric acid cooler 5 respectively to carry out heating in cooling and preheater 6；The
The concentrated sulphuric acid that one sulfuric acid cooler 5 is used for transport being come is delivered to realize recycling in the first absorption tower 2 after cooling down；In advance
Hot device 6 is used for that sulphuric acid circulating pump 4 is transported the concentrated sulphuric acid come and tentatively heats, it is possible to realizes the effective utilization to heat energy, subtracts
Few wasting of resources；Sulfur trioxide evaporator 7 is used for heating the concentrated sulphuric acid transported from preheater 6, obtains the purest
Clean sulfur trioxide gas；Defecator 8 is cage structure, is inside provided with filter screen, is used for the acid that will contain in sulfur trioxide gas
The impurity such as mist remove, and improve the purity of sulfur trioxide gas.
Be provided with the first air inlet 201 on the first absorption tower 2, first row QI KOU the 202, first inlet 203 and first goes out
Liquid mouth 204, is provided with sulphuric acid circulating pump 4 in described sulphuric acid circulating slot 3, is provided with sulphuric acid circulating pump on described sulphuric acid circulating pump 4
Liquid outlet 402 and sulphuric acid circulating pump inlet 401, be provided with cooler inlet 501, cold on described first sulfuric acid cooler 5
But device liquid outlet 502, recirculated cooling water water inlet 503 and recirculated cooling water outlet 504, described preheater 6 is provided with by
Add hot acid import 601, cooled acid outlet 602, cooled acid import 603 and heated acid outlet 604, at described sulfur trioxide
Vaporizer 7 is provided with vaporizer inlet 701, vaporizer liquid outlet 702, heating steam inlet 703, condensation-water drain 704 and
Sulfur trioxide gas outlet 705, is provided with filtered inlet 801, filtering outlet 802 and leakage fluid dram 803, institute on described defecator 8
State the first air inlet 201 to be connected with industrial sulphuric acid production system 1 by pipeline, described first row QI KOU 202 by pipeline and
Industrial sulphuric acid production system 1 is connected, and is provided with the first sulphuric acid spray thrower 205, described first sulphuric acid spray in the first absorption tower 2
Device 205 is connected with the first inlet 203, and described first liquid outlet 204 is connected with sulphuric acid circulating slot 3 by pipeline, described
Sulphuric acid circulating pump inlet 401 is connected with sulphuric acid circulating slot 3, and described sulphuric acid circulating pump liquid outlet 402 enters with cooler respectively
Liquid mouth 501 is connected with cold acid import 601, and described cooler liquid outlet 502 is connected with the first inlet 203, described circulation
Cooling water intake 503 is connected with recirculated cooling water outlet 504, and described cold acid import 601 is connected with hot acid outlet 604
Logical, described hot acid outlet 604 is connected with vaporizer inlet 701, described vaporizer liquid outlet 702 and hot acid import 603 phase
Connection, described hot acid import 603 is connected with cold acid outlet 602, and described cold acid outlet 602 is connected with sulphuric acid circulating slot 3, institute
Stating heating steam inlet 703 to be connected with condensation-water drain 704, described sulfur trioxide gas outlet 705 is connected with filtered inlet 801
Logical, described leakage fluid dram 803 is communicated to waste liquid tank 9；
Weight absorption plant, this heavy absorption plant includes that second absorption tower 10, MOS absorb acid circulating slot 11, MOS absorbs acid circulating pump
12 and second sulfuric acid cooler 13, described second absorption tower 10 is used for absorbing and filtering device 8 and transports the sulfur trioxide gas come,
Obtain the concentrated sulphuric acid of higher concentration；MOS absorbs acid circulating slot 11 and is used for using the concentrated sulphuric acid transported from second absorption tower 10
Ultra-pure water is diluted, and obtains MOS sulphuric acid；MOS absorbs acid circulating pump 12 and is used to absorb in acid circulating slot 11 MOS transport
MOS sulphuric acid be transported in the second sulfuric acid cooler 13；3rd sulfuric acid cooler is used to that MOS absorbs acid circulating pump 12 and transports
The MOS sulphuric acid come cools down, and is transported in second absorption tower 10 be circulated utilization by MOS sulphuric acid one tunnel after cooling,
One tunnel is transported in desorption tower.
Second absorption tower 10 is provided with the second air inlet 1001, second exhaust port the 1002, second inlet 1003 and
Two liquid outlets 1004, described MOS absorb acid circulating slot 11 on be provided with MOS absorb acid circulating slot import 1101, MOS absorb acid follow
Annular groove outlet 1102 and ultra-pure water import 1103, absorb at described MOS and be provided with input 1201 and outfan on acid circulating pump 12
1202, described second sulfuric acid cooler 13 is provided with cooler sulphuric acid import 1301, cooler sulphuric acid outlet 1302, circulate cold
But water inlet 1303 and circulating cooling water out 1304, described second air inlet 1001 is connected with filtering outlet 802 by pipeline
Logical, at described second air inlet 1001, it is provided with gas dilution device 1006, described second exhaust port 1002 is by pipeline and tail
Gas recovering device 19 is connected, and is provided with the second sulphuric acid spray thrower 1005, described second sulphuric acid spray thrower in second absorption tower 10
1005 are connected with the second inlet 1003, and described MOS absorbs acid circulating slot import 1101 and is connected with the second liquid outlet 1004,
Described MOS absorbs acid circulating slot outlet 1102 and is connected with input 1201, described outfan 1202 and cooler sulphuric acid import
1301 are connected, and described cooler sulphuric acid outlet 1302 is connected with the second inlet 1003, described circulating cooling water inlet
1303 are connected with circulating cooling water out 1304.
Desorption receiving apparatus, this desorption device includes desorption tower 14, MOS desorption acid circulating slot 15, MOS desorption acid circulating pump
16, sulphuric acid pan tank 17 and noble gas generator 18；Desorption tower 14 is used to transport in the second sulfuric acid cooler 13
MOS sulphuric acid carry out desorption purification；MOS desorption acid circulating slot 15 is intended for desorption tower 14 and transports the MOS sulphuric acid come
Store and transferring device；The MOS sulphuric acid that MOS desorption acid circulating slot 15 transports is divided into two-way by MOS desorption acid circulating pump 16, and one
Road is transported to sulphuric acid pan tank 17 and stores, and a road is transported in desorption tower 14 be circulated utilization.
Desorption tower 14 is provided with the 3rd air inlet the 1401, the 3rd air vent the 1402, the 3rd inlet 1403, circulation feed liquor
Mouth 1404 and the 3rd liquid outlet 1405, be provided with MOS desorption acid circulating slot import 1501 He on described MOS desorption acid circulating slot 15
MOS desorption acid circulating slot outlet 1502, is provided with MOS desorption acid circulating pump import 1601 on described MOS desorption acid circulating pump 16
Exporting 1602 with MOS desorption acid circulating pump, described 3rd inlet 1403 is connected, described with cooler sulphuric acid outlet 1302
Be additionally provided with the 3rd sulphuric acid spray thrower 1406 on desorption tower 14, described 3rd sulphuric acid spray thrower 1406 respectively with the 3rd inlet
1403 are connected with circulation inlet 1404, and described 3rd liquid outlet 1405 is connected with MOS desorption acid circulating slot import 1501,
Described MOS desorption acid circulating slot outlet 1502 is connected with MOS desorption acid circulating pump import 1601, and described MOS desorption acid circulates
Pump discharge 1602 is connected with circulation inlet 1404, and described 3rd air inlet 1401 is connected with noble gas generator 18
Logical, described 3rd air vent 1402 is connected with device for recovering tail gas 19；
Sulphuric acid pan tank 17, this sulphuric acid pan tank 17 is connected with MOS desorption acid circulating pump outlet 1602 by pipeline；
Device for recovering tail gas 19, this device for recovering tail gas 19 is connected with industrial sulphuric acid production system 1.
In the process units of above-mentioned microelectronics MOS level sulphuric acid of the present invention, described process units connects with sulphuric acid
The position touched is all covered with Fluorine-lined material, it is possible to effectively prevent concentrated sulphuric acid to the corrosion of equipment and the purity of guarantee concentrated sulphuric acid.
Present invention also offers a kind of method utilizing above-mentioned production equipment to produce microelectronics MOS level sulphuric acid, the method
Comprise the following steps:
The first step, selects the sulfur trioxide mixed gas of conversion procedure, sulfur trioxide mixed gas in industrial sulphuric acid production system 1
Entering in the first absorption tower 2 by the first air inlet 201, concentrated sulphuric acid enters the first sulphuric acid spray thrower by the first inlet 203
205, the first sulphuric acid spray thrower 205 absorbs sulfur trioxide, unabsorbed gaseous mixture in concentrated sulphuric acid is sprayed into the first absorption tower 2
Body is expelled in industrial sulphuric acid production system 1 by first row QI KOU 202, absorbs complete concentrated sulphuric acid through the first liquid outlet 204
Enter sulphuric acid circulating slot 3；
Second step, obtain in the first step absorbs complete and enters the concentrated sulphuric acid in sulphuric acid circulating slot 3, and a portion is at sulphuric acid
Under the effect of circulating pump 4, enter in the first sulfuric acid cooler 5, by recirculated cooling water, above-mentioned concentrated sulphuric acid is cooled down, pass through
First inlet 203 enters in the first absorption tower 2, and another part enters in preheater 6 by sulphuric acid circulating pump 4, enters preheating
The concentrated sulphuric acid of device 6 sends into sulfur trioxide evaporator 7 after preheating, heats by adding vapours, after adding vapours condensation
Flow out from condensation-water drain 704, concentrated sulphuric acid through heating after sulfur trioxide gas therein be heated after overflow, three oxidations of spilling
Sulfur gas enters defecator 8, and the concentrated sulphuric acid after pervaporation is flow in preheater 6 by back of pipeline, relative to wherein temperature
Relatively low concentrated sulphuric acid preheats, and is then flow in sulphuric acid circulating slot 3 by back of pipeline；
3rd step, the sulfur trioxide gas obtained in above-mentioned second step removes the impurity such as acid mist after defecator 8, after purification
Sulfur trioxide gas enter second absorption tower 10 from the second air inlet 1001 by pipeline, impurity is flowed by leakage fluid dram 803
Enter in waste liquid tank 9；
4th step, after the sulfur trioxide gas obtained in the 3rd step enters second absorption tower 10, by gas dilution device 1006
Sulfur trioxide gas bulk concentration is reduced, prevents owing to sulfur trioxide excessive concentration causes absorption rate too fast so that process is difficult to
Control, and the concentration precision of MOS is difficult to control to, spray concentrated sulphuric acid by the second sulphuric acid spray thrower 1005 and absorb sulfur trioxide, not
Absorbed minimum gas is expelled to device for recovering tail gas 19 by second exhaust port 1002, absorbs complete concentrated sulphuric acid through second
Liquid outlet 1004 enters MOS and absorbs acid circulating slot 11；
5th step, the concentrated sulphuric acid obtained in the 4th step maintains concentration 96～98% through ultra-pure water dilution, with removing ferrum, chlorine, aluminum etc.
The ultra-pure water of ion can be prevented effectively from the purity to sulphuric acid and impact, then absorbs acid circulating pump 12 through MOS and be transported to the
Cooling down in two sulfuric acid coolers 13, the concentrated sulphuric acid part after cooling enters second absorption tower by the second inlet 1003
Recycling in 10, another part concentrated sulphuric acid then flows in desorption tower 14；
6th step, the concentrated sulphuric acid of inflow desorption device after desorption purifies, enters MOS desorption acid circulating slot in desorption tower 14
In 15, a part enters in sulphuric acid pan tank 17 by MOS desorption acid circulating pump 16, and another part enters in desorption tower 14 and circulates
Utilize.
The gas of the collection in described device for recovering tail gas 19 enters in industrial sulphuric acid drying device through going at acid-mist-removing
After reason, be delivered in industrial sulphuric acid production system 1 be circulated utilization, on the one hand prevent waste gas to environment, simultaneously
The wasting of resources can be reduced, save production cost.
Certainly, the process units of microelectronics MOS level sulphuric acid of the present invention and production method are in addition to examples detailed above
Also have other similar structure composition and occupation modes.Sum it up, the process units of microelectronics MOS level sulphuric acid of the present invention and
Production method also includes other obvious conversion and replacements for those skilled in the art of the present technique.
Claims (4)
1. the microelectronics process units of MOS level sulphuric acid, it is characterised in that this device includes: absorption plant, heavily absorb dress
Put, desorption receiving apparatus, sulphuric acid pan tank and device for recovering tail gas；
Absorption plant, this absorption plant includes the first absorption tower (2), sulphuric acid circulating slot (3), sulphuric acid circulating pump (4), the first sulphuric acid
Cooler (5), preheater (6), sulfur trioxide evaporator (7), defecator (8) and waste liquid tank (9), in the first absorption tower (2)
It is provided with the first air inlet (201), first row QI KOU (202), the first inlet (203) and the first liquid outlet (204), described
It is provided with sulphuric acid circulating pump (4) in sulphuric acid circulating slot (3), described sulphuric acid circulating pump (4) is provided with sulphuric acid circulating pump liquid outlet
(402) and sulphuric acid circulating pump inlet (401), described first sulfuric acid cooler (5) is provided with cooler inlet (501),
Cooler liquid outlet (502), recirculated cooling water water inlet (503) and recirculated cooling water outlet (504), at described preheater
(6) heated acid import (601), cooled acid outlet (602), cooled acid import (603) and heated acid outlet it are provided with
(604), described sulfur trioxide evaporator (7) is provided with vaporizer inlet (701), vaporizer liquid outlet (702), heating steaming
Vapor inlet (703), condensation-water drain (704) and sulfur trioxide gas outlet (705), be provided with filtration on described defecator (8)
Import (801), filtering outlet (802) and leakage fluid dram (803), described defecator (8) is cage structure, in defecator (8)
Inside being provided with filter screen (804), described first air inlet (201) is connected with industrial sulphuric acid production system (1) by pipeline, and described the
One air vent (202) is connected with industrial sulphuric acid production system (1) by pipeline, is provided with the first sulfur in the first absorption tower (2)
Acid spray thrower (205), described first sulphuric acid spray thrower (205) is connected with the first inlet (203), described first liquid outlet
(204) it is connected with sulphuric acid circulating slot (3) by pipeline, described sulphuric acid circulating pump inlet (401) and sulphuric acid circulating slot (3) phase
Connection, the sour import heated with cooler inlet (501) and preheater respectively of described sulphuric acid circulating pump liquid outlet (402)
(601) being connected, described cooler liquid outlet (502) is connected with the first inlet (203), described recirculated cooling water water inlet
(503) it is connected with circulating water inlet and return pipe respectively with recirculated cooling water outlet (504), described heated acid import
(601) being connected with heated acid outlet (604), described heated acid outlet (604) is connected with vaporizer inlet (701)
Logical, described vaporizer liquid outlet (702) is connected with cooled acid import (603), and described cooled acid import (603) is with cold
But acid outlet (602) is connected, and described cooled acid outlet (602) is connected with sulphuric acid circulating slot (3), described in add vapours and enter
Mouth (703) is connected with condensation-water drain (704), and described sulfur trioxide gas outlet (705) is connected with filtered inlet (801),
Described leakage fluid dram (803) is communicated to waste liquid tank (9)；
Weight absorption plant, this heavy absorption plant includes that second absorption tower (10), MOS absorb acid circulating slot (11), MOS absorbs acid and follows
Ring pump (12) and the second sulfuric acid cooler (13), be provided with the second air inlet (1001), second exhaust on second absorption tower (10)
Mouth (1002), the second inlet (1003) and the second liquid outlet (1004), absorb at described MOS and be provided with in acid circulating slot (11)
MOS absorbs acid circulating slot import (1101), MOS absorbs acid circulating slot outlet (1102) and ultra-pure water import (1103), described
MOS absorbs acid circulating pump (12) and is provided with input (1201) and outfan (1202), described second sulfuric acid cooler (13)
It is provided with cooler sulphuric acid import (1301), cooler sulphuric acid outlet (1302), circulating cooling water inlet (1303) and circulation cold
But water out (1304), described second air inlet (1001) is connected with filtering outlet (802) by pipeline, enters described second
QI KOU (1001) place is provided with gas dilution device (1006), and described second exhaust port (1002) passes through pipeline and device for recovering tail gas
(19) it is connected, in second absorption tower (10), is provided with the second sulphuric acid spray thrower (1005), described second sulphuric acid spray thrower
(1005) being connected with the second inlet (1003), described MOS absorbs acid circulating slot import (1101) and the second liquid outlet
(1004) being connected, described MOS absorbs acid circulating slot outlet (1102) and is connected with circulating pump input (1201), described circulation
Pump output terminal (1202) is connected with cooler sulphuric acid import (1301), described cooler sulphuric acid outlet (1302) and the second feed liquor
Mouthful (1003) are connected, described circulating cooling water inlet (1303) and circulating cooling outlet (1304) respectively with the entering of recirculated water
Water pipe and return pipe are connected；
Desorption receiving apparatus, this desorption device includes desorption tower (14), MOS desorption acid circulating slot (15), MOS desorption acid circulating pump
(16) and noble gas generator (18), desorption tower (14) is provided with the 3rd air inlet (1401), the 3rd air vent
(1402), the 3rd inlet (1403), circulation inlet (1404) and the 3rd liquid outlet (1405), follow in described MOS desorption acid
Annular groove (15) is provided with MOS desorption acid circulating slot import (1501) and MOS desorption acid circulating slot outlet (1502), at described MOS
Desorption acid circulating pump (16) is provided with MOS desorption acid circulating pump import (1601) and MOS desorption acid circulating pump outlet (1602), institute
State the 3rd inlet (1403) to be connected with cooler sulphuric acid outlet (1302), in described desorption tower (14) is upper, is additionally provided with the 3rd
Sulphuric acid spray thrower (1406), described 3rd sulphuric acid spray thrower (1406) respectively with the 3rd inlet (1403) and circulation inlet
(1404) being connected, described 3rd liquid outlet (1405) is connected with MOS desorption acid circulating slot import (1501), and described MOS takes off
Inhaling acid circulating slot outlet (1502) to be connected with MOS desorption acid circulating pump import (1601), described MOS desorption acid circulating pump exports
(1602) being connected with circulation inlet (1404), described 3rd air inlet (1401) is connected with noble gas generator (18)
Logical, described 3rd air vent (1402) is connected with device for recovering tail gas (19)；
Sulphuric acid pan tank (17), this sulphuric acid pan tank (17) is connected with MOS desorption acid circulating pump outlet (1602) by pipeline；
Device for recovering tail gas (19), this device for recovering tail gas (19) is connected with industrial sulphuric acid production system (1).
The process units of microelectronics MOS level sulphuric acid the most according to claim 1, it is characterised in that described process units
In have the position contacted to be all covered with Fluorine-lined material with sulphuric acid.
3. one kind utilizes the method that equipment produces microelectronics MOS level sulphuric acid that produces described in claim 1, it is characterised in that should
Method comprises the following steps:
The first step, selects the sulfur trioxide mixed gas of conversion procedure, sulfur trioxide gaseous mixture in industrial sulphuric acid production system (1)
Body enters in the first absorption tower (2) by the first air inlet (201), and concentrated sulphuric acid enters the first sulfur by the first inlet (203)
Acid spray thrower (205), the first sulphuric acid spray thrower (205) absorbs sulfur trioxide in concentrated sulphuric acid is sprayed into the first absorption tower (2), not
Absorbed mixed gas is expelled in industrial sulphuric acid production system (1) by first row QI KOU (202), absorbs complete dense sulfur
Acid enters sulphuric acid circulating slot (3) through the first liquid outlet (204)；
Second step, the absorption obtained in the first step is complete and enters the concentrated sulphuric acid in sulphuric acid circulating slot (3), and a portion is at sulfur
Under the effect of acid circulating pump (4), enter in the first sulfuric acid cooler (5), by recirculated cooling water, above-mentioned concentrated sulphuric acid is carried out cold
But, entering in the first absorption tower (2) by the first inlet (203), another part enters preheater by sulphuric acid circulating pump (4)
(6), in, the concentrated sulphuric acid entering preheater (6) sends into sulfur trioxide evaporator (7) after preheating, adds by adding vapours
Heat, flows out from condensation-water drain (704) after adding vapours condensation, and concentrated sulphuric acid is part sulfur trioxide gas therein after heating
Separating out after being heated, the sulfur trioxide gas of precipitation enters defecator (8), and the concentrated sulphuric acid after pervaporation is flow to by back of pipeline
In preheater (6), the concentrated sulphuric acid that wherein temperature is relatively low is preheated, then flow to sulphuric acid circulating slot by back of pipeline
(3) in；
3rd step, the sulfur trioxide gas obtained in above-mentioned second step removes the impurity such as acid mist after defecator (8), purifies
After sulfur trioxide gas entered second absorption tower (10) from the second air inlet (1001) by pipeline, impurity passes through leakage fluid dram
(803) flow in waste liquid tank (9)；
4th step, after the sulfur trioxide gas obtained in the 3rd step enters second absorption tower (10), by gas dilution device
(1006) sulfur trioxide gas bulk concentration is reduced, sprays concentrated sulphuric acid by the second sulphuric acid spray thrower (1005) and absorb sulfur trioxide,
Unabsorbed minimum gas is expelled to device for recovering tail gas (19) by second exhaust port (1002), absorbs complete concentrated sulphuric acid
Enter MOS through the second liquid outlet (1004) and absorb acid circulating slot (11)；
5th step, the concentrated sulphuric acid obtained in the 4th step maintains concentration 96～98% through ultra-pure water dilution, then absorbs acid through MOS
Circulating pump (12) is transported in the second sulfuric acid cooler (13) cool down, and the concentrated sulphuric acid part after cooling passes through the second feed liquor
Mouth (1003) enters in second absorption tower (10) and recycles, and another part concentrated sulphuric acid then flows in desorption tower (14)；
6th step, the concentrated sulphuric acid of inflow desorption device after desorption purifies, enters MOS desorption acid circulation in desorption tower (14)
In groove (15), a part enters in sulphuric acid pan tank (17) by MOS desorption acid circulating pump (16), and another part enters desorption tower
(14) recycle in.
The production method of microelectronics MOS level sulphuric acid the most according to claim 3, it is characterised in that described tail gas recycle
The tail gas of the collection in device (19) enters in industrial sulphuric acid drying device, after going acid-mist-removing to process, is delivered to industrial sulphuric acid
Production system is circulated utilization in (1).
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| CN108793089A (en) * | 2018-09-03 | 2018-11-13 | 中国瑞林工程技术股份有限公司 | A kind of technique of sulfuric acid plant's production refined sulfuric acid |
| CN112079337A (en) * | 2020-09-19 | 2020-12-15 | 韶关高科祥高新材料有限公司 | Production method of electronic grade high-purity ultra-clean sulfuric acid |
| CN112320768A (en) * | 2021-01-04 | 2021-02-05 | 联仕(昆山)化学材料有限公司 | Production method of electronic-grade sulfuric acid |
| CN112850657A (en) * | 2021-02-06 | 2021-05-28 | 岷山环能高科股份公司 | Flue gas separation and purification system for producing electronic-grade sulfuric acid |
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| CN105947994B (en) | 2018-10-09 |
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Effective date of registration: 20201012 Address after: Cuihu 6th Road, Wusong Town, Yi'an District, Tongling City, Anhui Province Patentee after: Tongling Yuanli Electronic Chemicals Co., Ltd Address before: 200241 No. 4600, Wu Long Road, Shanghai, Minhang District Patentee before: SHANGHAI JINGTENG CHEMICAL Co.,Ltd. |