CN103879977A - Continuous production method and device for high-purity nitric acid - Google Patents
Continuous production method and device for high-purity nitric acid Download PDFInfo
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Abstract
The invention relates to a continuous production method and device for high-purity nitric acid. The method comprises the steps: carrying out pressure-regulating and rectifying processes on a nitric acid raw material, wherein the absolute pressure in a pressure-regulating and rectifying tower is 1-200KPa and is not the normal pressure, the temperature of the bottom of the pressure-regulating and rectifying tower is 50-200 DEG C, and the reflux ratio is 1:(1-6); carrying out normal-pressure rectifying on 69-71wt% industrial concentrated nitric acid, and carrying out two-stage filter core circulating filtration to prepare the nitric acid raw material, wherein the content of particles having the grain diameters more than or equal to 0.1 micron in the nitric acid raw material is less than or equal to 25 per mL, and the single metal ion content is less than or equal to 5ppb. The method has the beneficial effects that by utilizing the continuous pressure-regulating and rectifying manners, the advantages of textures of various high-purity devices are adequately utilized, various disadvantages are evaded, heavy and light impurity components in the nitric acid can be removed, and the high-purity nitric acid of which the single metal ion content is less than 50ppt is prepared; and besides, the utilized process is simple in production condition, is convenient to maintain and is suitable for continuous production.
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 fast development, chip manufacturing level rapidly promotes, and semiconductor equipment material industry association formulates harsher SEMI C12 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 electrical property, yield rate and the reliability of chip.Nitric acid, as a kind of strong acid with oxidisability, can be removed most of metal, metal oxide and organism, a large amount of cleaning and etchings for 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 SEMI C8 standard.Adopt above-mentioned production technique, operating procedure complicated difficult, with production control quality, obtains stability product.Along with IC memory capacity progressively increases, become thinner as the oxide film of insulation layer, the alkali metal impurity in electron chemistry kind can dissolve in oxide film, thereby causes insulation voltage to reduce; Beavy metal impurity can be attached on silicon wafer surface and can make P-N knot proof voltage reduce.To the IC Technology of different live widths, 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, by mixed mutually in pretreater to technical grade nitric acid and diallyl 18-hat-6 ether organosilicon macromolecule complexing agents, direct draught passes through micro-filtrate membrane filtration, filtrate passes into carries out rectifying in rectifying tower, collect the cut of tower head, in air mix facilities, dilute with ultrapure water, then in decoloration device, drive free nitrogen peroxide out of with high pure nitrogen, after decolouring, after nanofiltration membrane is filtered, obtain ultra-high pure nitric acid again.
Chinese patent CN102001635B discloses a kind of ultra-high pure nitric acid preparation technology, adds reaction in technical grade nitric acid to remove Cl nitric acid metal-salt
-and SO
4 2-, after membrane filtration, carry out rectification and purification, blow in White Tower, blow with purifying air white after, blow white liquid and enter crude product groove, after membrane filtration, obtain high pure nitric acid.
In sum, all low costs to high pure nitric acid not of existing various technology, 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 (referring to Chinese patent CN102001635B specification sheets table 2, can reach the highest 2.5kg/h of being no more than of suitable entering tower flow rate of the high pure nitric acid of SEMI-C8 standard-required, so greatly limit production efficiency, made 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 arranges simply, and that utilizes that it can continous-stable produces 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, while 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 ℃, and reflux ratio is 1:1～6, in described nitric acid material >=and 0.1 μ m 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, while 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 finished product intermediate collection tank and finished product packing bucket are connected.
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, described production method also comprises industrial concentrated acid take massfraction as the 69～71wt% step as nitric acid material described in raw material continuous production, and the preparation of described nitric acid material comprises atmospheric distillation operation and the circulating filtration operation of carrying out successively.
According to a concrete and preferred aspect, while 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, make nitric acid that atmospheric distillation is collected carry out successively the circulating filtration of 1～3h through 0.2 μ m filter core and 0.1 μ m filter core, then squeeze in described nitric acid material tank.
According to a concrete and preferred aspect of the present invention, the reflux ratio of 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 so in gained nitric acid finished product, 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 comprises the industrial nitric acid raw material tank, heating tower reactor, atmospheric distillation tower, atmospheric distillation condenser, the atmospheric distillation holding tank that connect successively;
Described circulating filtration equipment comprises the fluorine plastic tube that both ends are communicated with described atmospheric distillation holding tank respectively and the pumping setting gradually on described fluorine plastic tube, 0.2 μ m filter core and 0.1 μ m filter core;
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 be taked 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 the pressure regulation rectifying nitric acid of purifying, and the pressure when selecting suitable raw material and control 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 the requirement that even exceedes SEMI C12 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 producing continuously meeting the high pure nitric acid product that even exceedes SEMI C12 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, heating tower reactor; 3, atmospheric distillation tower; 4, atmospheric distillation condenser; 5, waste gas treatment equipment; 6, atmospheric distillation holding tank; 7, the 0.2 μ m filter core recycle system; 8, the 0.1 μ m 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 mainly and is: carry out pressure regulation rectifying by the nitric acid material to suitable, obtain and meet the high pure nitric acid product that even exceedes SEMI C12 standard-required.A specific embodiment is as follows: using mass ratio as 69～71wt% industrial concentrated acid is as raw material, remove most of metal ion in raw material by atmospheric distillation and obtain work in-process, work in-process circulating filtration is removed to particle and obtain described suitable nitric acid material, then in pressure regulation rectifying tower, by regulating tower reactor internal pressure, column bottom temperature, reflux ratio to obtain the pressure regulation rectifying tower top cut of removing oxynitride without decolouring.The processing step of whole method simply, at utmost the secondary pollution that reduces to introduce 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.Referring to 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 comprises the industrial nitric acid raw material tank 1, heating tower reactor 2, atmospheric distillation tower 3, atmospheric distillation condenser 4, the atmospheric distillation holding tank (work in-process tank) 6 that connect successively.Using the sleeping tank of steel lining tetrafluoro plastics as atmospheric distillation holding tank 6.
Described circulating filtration equipment mainly comprises the fluorine plastic tube (PFA pipe) that both ends are communicated with atmospheric distillation holding tank 6 respectively and the pumping setting gradually on fluorine plastic tube, 0.2 μ m filter core 7 and 0.1 μ m filter core 8.
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.In the time that 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 μ m and 0.1 μ m filter core circulating filtration, are squeezed into nitric acid material tank successively.In the time that pressure regulation is decompression, open vacuum pump and maintain the interior absolute pressure of pressure regulation rectifying device at 1～90KPa, preferably 20～80KPa, opens feed valve by work in-process suction pressure regulation rectifying tower reactor in nitric acid material tank; Control Heating temperature at 70～110 ℃, between adjusting tower tops reflux ratio 1:1～1:6, 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, Thermo X-7series) to detect, and particle detects by liquid particle instrument (LPC).
Below in conjunction with specific embodiment, the present invention is described in further details.Should be understood that these embodiment are for ultimate principle of the present invention, principal character and advantage are described, and the present invention is not limited by the scope of following examples.The implementation condition adopting in embodiment can be done 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:
The industrial nitric acid that is 69% by mass content is squeezed into heating tower reactor; Open cooling circulating water, cooling water flow is controlled 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 the work in-process that obtain 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, after circulating filtration completes, work in-process is squeezed in nitric acid batch can through two-stage filter core.Sample detection in nitric acid batch can: 20/mL of >=0.1 μ m granule content <.
Embodiment 3
This example provides a kind of pressure regulation (decompression) rectificating method of nitric acid, is implemented as follows: open vacuum system, maintaining absolute pressure in pressure regulation rectifying tower reactor is 20KPa, opens tower reactor feed valve, and liquid level arrives tower reactor capacity and closes tower reactor feed valve at 1/2～2/3 o'clock.Open cooling recirculation system.Open heating system, collect finished product.Open tower reactor feed valve, maintain inlet amount 390～420L/h.
Product detected result is referring to 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;
200 ℃ of Heating temperatures
Reflux ratio is 1:3;
Inlet amount 390～420L/h.
Product detected result is referring to 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;
110 ℃ of Heating temperatures
Reflux ratio is 1:3;
Inlet amount 390～420L/h.
Product detected result is referring to table 3.
The detected result of table 3 embodiment 3～5
Above the present invention is described in detail; its object is to allow the personage who is 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 that all spirit according to the present invention are done changes or modifies, and 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, while 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 ℃, and reflux ratio is 1:1～6, in described nitric acid material >=and 0.1 μ m 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: while carrying out described pressure regulation rectifying, 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: described production method also comprises industrial concentrated acid take massfraction as the 69～71wt% step as nitric acid material described in raw material continuous production, and the preparation of described nitric acid material comprises atmospheric distillation operation and the 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: while 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, make the nitric acid of atmospheric distillation collection carry out successively the circulating filtration of 1～3h through two-stage filter core, then squeeze 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 comprises the industrial nitric acid raw material tank, heating tower reactor, atmospheric distillation tower, atmospheric distillation condenser, the atmospheric distillation holding tank that connect successively;
Described circulating filtration equipment comprises the fluorine plastic tube that both ends are communicated with described atmospheric distillation holding tank respectively and the pumping setting gradually on described fluorine plastic tube, 0.2 μ m filter core and 0.1 μ m filter core;
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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108744572A (en) * | 2018-05-14 | 2018-11-06 | 南华大学 | The device and method of nitric acid is recycled from containing nitric acid waste |
| 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 |
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| 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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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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108744572A (en) * | 2018-05-14 | 2018-11-06 | 南华大学 | The device and method of nitric acid is recycled from containing nitric acid waste |
| 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 |
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| CN103879977B (en) | 2015-12-09 |
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Address after: Cheng lake road Wuzhong Economic Development Zone of Suzhou City, Jiangsu Province, No. 3 215168 Applicant after: SUZHOU JINGRUI CHEMICAL CO., LTD. Address before: Cheng lake road Wuzhong Economic Development Zone of Suzhou City, Jiangsu Province, No. 3 215168 Applicant before: Suzhou Jingrui Chemical Co.,Ltd. |
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