CN103879977B - A kind of continuous production method of high pure nitric acid and production equipment - Google Patents
A kind of continuous production method of high pure nitric acid and production equipment Download PDFInfo
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- CN103879977B CN103879977B CN201410133101.6A CN201410133101A CN103879977B CN 103879977 B CN103879977 B CN 103879977B CN 201410133101 A CN201410133101 A CN 201410133101A CN 103879977 B CN103879977 B CN 103879977B
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Abstract
The present invention relates to a kind of continuous production method and production equipment of high pure nitric acid, the method comprises the operation of nitric acid material being carried out to pressure regulation rectifying, absolute pressure in pressure regulation rectifying tower reactor is between 1 ~ 200KPa, and be not normal pressure, at the bottom of pressure regulation rectifying tower reactor, temperature is 50 ~ 200 DEG C, reflux ratio is 1:1 ~ 6, nitric acid material is obtained by atmospheric distillation 69 ~ 71wt% industrial concentrated acid with through two-stage filter core circulating filtration, in this nitric acid material >=0.1 μm of granule content≤25/mL, individual event metal ion content≤5ppb.The continuous voltage regulating rectifying mode that the inventive method adopts, takes full advantage of the advantage of various high-purity equipment material, has evaded various shortcoming, the heavy in nitric acid, light impurities component can be removed, prepare the high pure nitric acid of individual event metal content lower than 50ppt.In addition, the present invention adopts explained hereafter condition simple, easy to maintenance, is applicable to continuous prodution.
Description
Technical field
The present invention relates to a kind of high pure nitric acid continuous production method and device, gained high pure nitric acid is mainly used in the IC industry of microfabrication.
Background technology
Along with China's electronic industry is fast-developing, chip manufacturing level rapidly promotes, and semiconductor equipment material industry association formulates harsher SEMIC12 standard.As the guardian technique material of chip manufacturing---the technical requirements of the clean electronic chemical product of ultrapure height progressively promotes, and the purity of electronic chemical product directly affects the electrical property of chip, yield rate and reliability.Nitric acid, as a kind of strong acid with oxidisability, can remove most of metal, metal oxide and organism, in a large number for cleaning and the etching of chip.
At present, domestic production manufacturer adopts the techniques such as rectification method, resin filter, membrane filtration to reduce metal content in nitric acid material, and product meets SEMIC8 standard.Adopt above-mentioned production technique, operating procedure complicated difficult, with production control quality, obtains stability product.Along with IC memory capacity progressively increases, the oxide film as insulation layer becomes thinner, and the alkali metal impurity in electron chemistry kind can dissolve in oxide film, thus causes insulation voltage to reduce; Beavy metal impurity can be attached on silicon wafer surface and P-N junction proof voltage can be made to reduce.To the IC Technology of different live width, need the high pure electronic chemical reagent of supporting different stage.
Chinese patent CN101264869B discloses a kind of ultra-high pure nitric acid continuous production method, technical grade nitric acid and diallyl 18-are preced with-6 ether organosilicon macromolecule complexing agents to mix mutually in pretreater, direct draught passes through micro-filtrate membrane filtration, filtrate passes in rectifying tower carries out rectifying, collect the cut of tower head, dilute with ultrapure water in air mix facilities, then in decoloration device, drive free nitrogen peroxide out of with high pure nitrogen, after decolouring, after nanofiltration membrane, namely obtain ultra-high pure nitric acid again.
Chinese patent CN102001635B discloses a kind of ultra-high pure nitric acid preparation technology, nitric acid metal-salt is added reaction in technical grade nitric acid and removes Cl
-and SO
4 2-, carry out rectification and purification after membrane filtration, blow blow with purifying air in White Tower white after, blow white liquid and enter crude product groove, after membrane filtration, obtain high pure nitric acid.
In sum, existing various technology is not all to the low cost of high pure nitric acid, and in enormous quantities, continuous production processes and equipment are introduced.Make a general survey of the preparation technology of existing high pure nitric acid, the content of individual event metal ion higher (being all greater than 0.1ppb) in gained high pure nitric acid product, and along with the increasing of high pure nitric acid amount of product throughput, the content of metal ion is higher (see Chinese patent CN102001635B specification sheets table 2, the highest 2.5kg/h that is no more than of suitable entering tower flow rate of the high pure nitric acid of SEMI-C8 standard-required can be reached, so greatly limit production efficiency, make production cost higher.
Summary of the invention
Technical problem to be solved by this invention overcome the deficiencies in the prior art, a kind of continuous production method of high pure nitric acid is provided, the method technique is simple, production efficiency is high, cost is lower, gained high pure nitric acid constant product quality, and wherein the content of individual event metal ion can be reduced to below 50ppt.
The present invention also provides a kind of continuous production device of high pure nitric acid simultaneously, and this device is arranged simply, utilize its can continous-stable produce high pure nitric acid product.
For overcoming the above problems, a kind of technical scheme that the present invention takes is:
A kind of continuous production method of high pure nitric acid, this production method comprises the operation of nitric acid material being carried out to pressure regulation rectifying, when carrying out pressure regulation rectifying, absolute pressure in pressure regulation rectifying tower reactor is between 1 ~ 200KPa, and be not normal pressure, at the bottom of pressure regulation rectifying tower reactor, temperature is 50 ~ 200 DEG C, and reflux ratio is 1:1 ~ 6, in described nitric acid material >=0.1 μm of granule content≤25/mL, individual event metal ion content≤5ppb.
Preferably, the absolute pressure in described pressure regulation rectifying tower reactor is 1 ~ 90KPa or 110 ~ 150KPa.
According to the present invention, when carrying out described pressure regulation rectifying, the entering tower flow rate of nitric acid material can be 350 ~ 450L/h, preferably 390 ~ 420L/h.
According to further embodiment of the present invention: the equipment that described pressure regulation rectifying adopts comprises nitric acid material tank, pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser.Nitric acid material tank is liner ptfe plastic material, condensation tower head and the finished product intermediate collection tank of pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material or steel lining tetrafluoro plastics, and described method also comprises and being connected with finished product packing bucket by finished product intermediate collection tank.
According to a concrete aspect: condensation tower head and the finished product intermediate collection tank of described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material, and described pressure regulation rectifying device also comprises vacuum system.
Preferably, described pressure regulation rectifying tower plates number is 10-20 column plate.In a concrete and preferred implementation, described pressure regulation theoretical number of plates of rectifying tower is 14.2 column plates.
Preferably, the step that it is nitric acid material described in raw material continuous production that described production method also comprises with the massfraction industrial concentrated acid that is 69 ~ 71wt%, the preparation of described nitric acid material comprises the atmospheric distillation operation and circulating filtration operation of carrying out successively.
According to a concrete and preferred aspect, when carrying out described atmospheric distillation, the feed rate of rectifying tower is 350 ~ 450L/h, collect tower head cut and be stored in atmospheric distillation holding tank, described atmospheric distillation reflux ratio is 1:1 ~ 3, adopts coil pipe heating, uses steam as heating source, vapor pressure is 0.10 ~ 0.35MPa, and cooling water flow is 6 ~ 10m
3/ h.
According to another concrete and preferred aspect, in described circulating filtration operation, the nitric acid that atmospheric distillation is collected carries out the circulating filtration of 1 ~ 3h successively through 0.2 μm of filter core and 0.1 μm of filter core, then squeeze in described nitric acid material tank.
According to a concrete and preferred aspect of the present invention, the reflux ratio controlling pressure regulation rectifying is 1:3 ~ 5, absolute pressure in pressure regulation rectifying tower reactor is 20 ~ 90KPa or 110 ~ 120KPa, the entering tower flow rate of nitric acid material is 390 ~ 420L/h, and in gained nitric acid finished product like this, individual event metal ion content is less than 50ppt.
The another technical scheme that the present invention takes is: a kind of continuous production device of high pure nitric acid, and it comprises the atmospheric distillation equipment, circulating filtration equipment, pressure regulation rectifying device and the finished product packing bucket that set gradually,
Described atmospheric distillation equipment comprise connect successively industrial nitric acid raw material tank, heating tower reactor, atmospheric distillation tower, atmospheric distillation condenser, atmospheric distillation holding tank;
Described circulating filtration equipment comprises the fluorine plastic tube and the pumping set gradually on described fluorine plastic tube, 0.2 μm of filter core and 0.1 μm of filter core that both ends are communicated with described atmospheric distillation holding tank respectively;
Described pressure regulation rectifying device comprises nitric acid material tank, pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser, counter flow controller, finished product water cooler, finished product intermediate collection tank and connecting tube, the reflux ratio of described counter flow controller was controlled by the magnet switching electricity time, described nitric acid material tank is liner tetrafluoro material, condensation tower head and the finished product intermediate collection tank of described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material or steel lining tetrafluoro plastic material, and described connecting tube adopts PFA pipe.
According to the present invention, described pressure regulation rectifying can be high-pressure rectification or rectification under vacuum or the combination of the two.Pressure regulation rectifying device can take high-pressure rectification equipment or rectification under vacuum equipment or the combination of the two accordingly.
Due to the employing of above technical scheme, the present invention compared with prior art has following advantage:
The inventive method adopts pressure regulation rectifying to purify nitric acid, pressure during by selecting suitable raw material and controlling pressure regulation rectifying in tower, can obtain that colourity < 5 is black once, individual event metal ion content is lower than the nitric acid finished product of 50ppt.Compared with existing method, the inventive method technology and equipment is simple, and production efficiency is high, constant product quality, and energy consumption is low, and product meets even more than the requirement of SEMIC12 standard, can be used for cleaning and the etching of highly integrated chip.
Apparatus of the present invention are simple, energy consumption is low, are suitable for continuous seepage and meet even more than the high pure nitric acid product of SEMIC12 standard-required.
Accompanying drawing explanation
Fig. 1 is the structural representation of continuous production device of the present invention;
Wherein: 1, industrial nitric acid raw material tank; 2, tower reactor is heated; 3, atmospheric distillation tower; 4, atmospheric distillation condenser; 5, waste gas treatment equipment; 6, atmospheric distillation holding tank; 7,0.2 μm of filter core recycle system; 8,0.1 μm of filter core recycle system; 9, nitric acid material tank; 10, pressure regulation rectifying tower reactor; 11, pressure regulation rectifying king-post; 12, pressure regulation rectifying condenser; 13, counter flow controller; 14, finished product water cooler; 15, finished product intermediate collection tank; 16 is finished product packing bucket; 17, vacuum system; 18, waste liquor treatment equipment.
Embodiment
The present invention conceives and is mainly: by carrying out pressure regulation rectifying to suitable nitric acid material, obtains and meets even more than the high pure nitric acid product of SEMIC12 standard-required.A specific embodiment is as follows: be that 69 ~ 71wt% industrial concentrated acid is as raw material using mass ratio, remove most of metal ion in raw material by atmospheric distillation and obtain work in-process, particle is removed to work in-process circulating filtration and obtains described suitable nitric acid material, then, in pressure regulation rectifying tower, obtain by regulating tower reactor internal pressure, column bottom temperature, reflux ratio the pressure regulation rectifying tower top cut removing oxynitride without the need to decolouring.The processing step of whole method simply, at utmost reduce the secondary pollution introduced in purification process, compared with prior art, the method can obtain higher-quality target product with lower energy consumption, higher productive rate.
High pure nitric acid continuous production method of the present invention, can adopt the production equipment shown in Fig. 1 to carry out.See Fig. 1, this production equipment mainly comprises atmospheric distillation equipment, circulating filtration equipment, pressure regulation rectifying device, finished product packing bucket 16, waste gas treatment equipment 5 and waste liquor treatment equipment 18.
Atmospheric distillation equipment mainly comprise connect successively industrial nitric acid raw material tank 1, heating tower reactor 2, atmospheric distillation tower 3, atmospheric distillation condenser 4, atmospheric distillation holding tank (work in-process tank) 6.Crouch tank as atmospheric distillation holding tank 6 using steel lining tetrafluoro plastics.
Described circulating filtration equipment mainly comprises the fluorine plastic tube (PFA manages) and the pumping set gradually on fluorine plastic tube, 0.2 μm of filter core 7 and 0.1 μm of filter core 8 that both ends are communicated with atmospheric distillation holding tank 6 respectively.
Pressure regulation rectifying device mainly comprises nitric acid material tank 9, pressure regulation rectifying tower reactor 10, pressure regulation rectifying king-post 11, pressure regulation rectifying condenser 12, counter flow controller 13, finished product water cooler 14, finished product intermediate collection tank 15 and connecting tube, the reflux ratio of counter flow controller 13 was controlled by the magnet switching electricity time.Nitric acid material tank 9 is the storage tank of liner PTFE.When pressure regulation rectifying device is used for rectification under vacuum, it also comprises vacuum system 17.
The concrete implementation step of the inventive method is as follows: industrial nitric acid is passed into heating tower reactor.Atmospheric distillation uses steam source, and steam is by coil pipe to heating material, and Steam pressure control is at 0.10 ~ 0.35MPa; Nitric acid vapor carries out heat exchange at overhead condenser place, enters work in-process tank through cooling tube.Work in-process after 0.2 μm and 0.1 μm of filter core circulating filtration, squeeze into nitric acid material tank successively.When pressure regulation is for decompression, in unlatching vacuum pump maintenance pressure regulation rectifying device, absolute pressure is at 1 ~ 90KPa, and preferably 20 ~ 80KPa opens feed valve and sucked by work in-process in nitric acid material tank in pressure regulation rectifying tower reactor; Control Heating temperature at 70 ~ 110 DEG C, regulate between top reflux rates 1:1 ~ 1:6, namely obtain high pure nitric acid product.
Nitric acid content of the present invention adopts chemical titration analysis, and metal ion content adopts icp ms (ICP-MS, ThermoX-7series) to detect, and particle is detected by liquid particle instrument (LPC).
Below in conjunction with specific embodiment, the present invention is described in further details.Should be understood that these embodiments are for illustration of ultimate principle of the present invention, principal character and advantage, and the present invention does not limit by the scope of following examples.The implementation condition adopted in embodiment can do further adjustment according to specific requirement, and not marked implementation condition is generally the condition in normal experiment.
Embodiment 1
This example provides a kind of atmospheric distillation method of industrial nitric acid, is implemented as follows:
By mass content be 69% industrial nitric acid squeeze into heating tower reactor; Open cooling circulating water, cooling water flow controls at 6 ~ 10m
3/ h; Open steam valve, control vapour pressure at 0.10 ~ 0.35MPa; After equipment steady running, controlling material feeding flow is 390 ~ 420L/h, collects phlegma and is work in-process.Work in-process detected result is as shown in table 1.
Every metal ion detection result in table 1 atmospheric distillation raw material and atmospheric distillation work in-process
As shown in Table 1, industrial nitric acid is the highest 5ppb that is no more than of individual event metal ion content after above-mentioned atmospheric distillation, and anion-content is no more than 200ppb.
Embodiment 2
This example provides a kind of nitric acid half-finished circulating filtration method, be implemented as follows: open pumping and the work in-process obtained according to embodiment 1 method are driven into circulated filter system from work in-process tank, work in-process are back to work in-process tank successively after two-stage filter core, the circulating filtration time is 1 ~ 3h, is squeezed in nitric acid batch can by work in-process after circulating filtration completes through two-stage filter core.Sample detection in nitric acid batch can: >=0.1 μm of granule content < 20/mL.
Embodiment 3
This example provides a kind of pressure regulation (decompression) rectificating method of nitric acid, is implemented as follows: open vacuum system, and maintaining absolute pressure in pressure regulation rectifying tower reactor is 20KPa, opens tower reactor feed valve, closes tower reactor feed valve when liquid level arrives tower reactor capacity 1/2 ~ 2/3.Open cooling recirculation system.Open heating system, collect finished product.Open tower reactor feed valve, maintain inlet amount 390 ~ 420L/h.
Product checking result is see table 3.
Embodiment 4
This example provides a kind of pressure regulation (high pressure) rectificating method of nitric acid, and processing parameter is as follows:
In pressure regulation rectifying tower, absolute pressure maintains 120KPa;
Heating temperature 200 DEG C
Reflux ratio is 1:3;
Inlet amount 390 ~ 420L/h.
Product checking result is see table 3.
Embodiment 5
This example provides a kind of pressure regulation (decompression) rectificating method of nitric acid, and step is substantially with embodiment 3, and processing parameter is as follows:
In pressure regulation rectifying tower, absolute pressure maintains 80KPa;
Heating temperature 110 DEG C
Reflux ratio is 1:3;
Inlet amount 390 ~ 420L/h.
Product checking result is see table 3.
The detected result of table 3 embodiment 3 ~ 5
Above to invention has been detailed description; its object is to allow the personage being familiar with this art can understand content of the present invention and be implemented; can not limit the scope of the invention with this; the equivalence change that all spirit according to the present invention are done or modification, all should be encompassed in protection scope of the present invention.
Claims (10)
1. the continuous production method of a high pure nitric acid, it is characterized in that: described production method comprises the operation of nitric acid material being carried out to pressure regulation rectifying, when carrying out described pressure regulation rectifying, absolute pressure in pressure regulation rectifying tower reactor is between 1 ~ 200KPa, and be not normal pressure, at the bottom of pressure regulation rectifying tower reactor, temperature is 50 ~ 200 DEG C, and reflux ratio is 1:1 ~ 6, in described nitric acid material >=0.1 μm of granule content≤25/mL, individual event metal ion content≤5ppb.
2. the continuous production method of high pure nitric acid according to claim 1, is characterized in that: the absolute pressure in described pressure regulation rectifying tower reactor is 1 ~ 90KPa or 110 ~ 150KPa.
3. the continuous production method of high pure nitric acid according to claim 1, is characterized in that: when carrying out described pressure regulation rectifying, and the entering tower flow rate of described nitric acid material is 350 ~ 450L/h.
4. the continuous production method of high pure nitric acid according to claim 1, it is characterized in that: the equipment that described pressure regulation rectifying adopts comprises nitric acid material tank, described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser and finished product intermediate collection tank, described nitric acid material tank is steel lining tetrafluoro material storage tank, and condensation tower head and the finished product intermediate collection tank of described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material or steel lining tetrafluoro plastics.
5. the continuous production method of high pure nitric acid according to claim 4, is characterized in that: described pressure regulation rectifying king-post stage number is 10 ~ 20 column plates.
6. the continuous production method of high pure nitric acid according to claim 4, it is characterized in that: condensation tower head and the finished product intermediate collection tank of described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material, and described pressure regulation rectifying device also comprises vacuum system.
7. the continuous production method of high pure nitric acid according to claim 4, it is characterized in that: the step that it is nitric acid material described in raw material continuous production that described production method also comprises with the massfraction industrial concentrated acid that is 69 ~ 71wt%, the preparation of described nitric acid material comprises the atmospheric distillation operation and circulating filtration operation of carrying out successively.
8. the continuous production method of high pure nitric acid according to claim 7, it is characterized in that: when carrying out described atmospheric distillation, the feed rate of rectifying tower is 350 ~ 450L/h, collect tower head cut and be stored in atmospheric distillation holding tank, described atmospheric distillation reflux ratio is 1:1 ~ 3, adopts coil pipe heating, use steam as heating source, vapor pressure is 0.10 ~ 0.35MPa, and atmospheric distillation adopts horizontal condenser, and cooling water flow is 6 ~ 10m
3/ h.
9. the continuous production method of high pure nitric acid according to claim 7, it is characterized in that: in described circulating filtration operation, the nitric acid that atmospheric distillation is collected carries out the circulating filtration of 1 ~ 3h successively through two-stage filter core, then squeezed in described nitric acid material tank by pumping.
10. a continuous production device for high pure nitric acid, is characterized in that: described production equipment comprises the atmospheric distillation equipment, circulating filtration equipment, pressure regulation rectifying device and the finished product packing bucket that set gradually,
Described atmospheric distillation equipment comprise connect successively industrial nitric acid raw material tank, heating tower reactor, atmospheric distillation tower, atmospheric distillation condenser, atmospheric distillation holding tank;
Described circulating filtration equipment comprises the fluorine plastic tube and the pumping set gradually on described fluorine plastic tube, 0.2 μm of filter core and 0.1 μm of filter core that both ends are communicated with described atmospheric distillation holding tank respectively;
Described pressure regulation rectifying device comprises nitric acid material tank, pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser, counter flow controller, finished product water cooler, finished product intermediate collection tank and connecting tube, the reflux ratio of described counter flow controller was controlled by the magnet switching electricity time, described nitric acid material tank is the storage tank of liner PTFE, condensation tower head and the finished product intermediate collection tank of described pressure regulation rectifying tower reactor, pressure regulation rectifying king-post, pressure regulation rectifying condenser are quartzy material or steel lining tetrafluoro plastic material, and described connecting tube adopts PFA pipe.
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| CN108744572B (en) * | 2018-05-14 | 2021-04-20 | 南华大学 | Device and method for recovering nitric acid from nitric acid-containing waste liquid |
| CN115028147A (en) * | 2022-06-30 | 2022-09-09 | 江苏淮河化工有限公司 | Process for continuously preparing electronic-grade nitric acid by rectification and stripping integrated method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1544317A (en) * | 1976-12-30 | 1979-04-19 | Poudres & Explosifs Ste Nale | Process for the continuous treatment of used nitric acid |
| US6214173B1 (en) * | 1996-06-05 | 2001-04-10 | Air Liquide Electronics Chemicals & Services, Inc. | On-site manufacture of ultra-high-purity nitric acid |
| US20050074389A1 (en) * | 2001-04-12 | 2005-04-07 | Paul Hofmann | Method for the production of highly pure nitric acid |
| CN101941683A (en) * | 2010-08-12 | 2011-01-12 | 上海华谊微电子材料有限公司 | Continuous preparation method of ultra pure nitric acid |
| CN103601163A (en) * | 2013-12-02 | 2014-02-26 | 上海化学试剂研究所有限公司 | Preparation method for high purity nitric acid |
-
2014
- 2014-04-03 CN CN201410133101.6A patent/CN103879977B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1544317A (en) * | 1976-12-30 | 1979-04-19 | Poudres & Explosifs Ste Nale | Process for the continuous treatment of used nitric acid |
| US6214173B1 (en) * | 1996-06-05 | 2001-04-10 | Air Liquide Electronics Chemicals & Services, Inc. | On-site manufacture of ultra-high-purity nitric acid |
| US20050074389A1 (en) * | 2001-04-12 | 2005-04-07 | Paul Hofmann | Method for the production of highly pure nitric acid |
| CN101941683A (en) * | 2010-08-12 | 2011-01-12 | 上海华谊微电子材料有限公司 | Continuous preparation method of ultra pure nitric acid |
| CN103601163A (en) * | 2013-12-02 | 2014-02-26 | 上海化学试剂研究所有限公司 | Preparation method for high purity nitric acid |
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