CN101264869A - Continuous producing technique for ultra-high pure nitric acid - Google Patents
Continuous producing technique for ultra-high pure nitric acid Download PDFInfo
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- CN101264869A CN101264869A CNA2008100235389A CN200810023538A CN101264869A CN 101264869 A CN101264869 A CN 101264869A CN A2008100235389 A CNA2008100235389 A CN A2008100235389A CN 200810023538 A CN200810023538 A CN 200810023538A CN 101264869 A CN101264869 A CN 101264869A
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Abstract
The invention relates to a process for continuously producing extra high purity nitric acid, which comprises the following steps: first, industrial grade 80-90% nitric acid raw material and double allyl 18-crown-6 ether organosilicon macromolecular complexing agent accounting for 0.2-2% of the weight of nitric acid raw material are mixed in a pretreater, then, the mixture is filtered by a micro-filtration membrane under a working pressure of 0.1-0.2 Mpa, the filtrate enters a rectification tower, and the semi-finished product going through the rectification tower is diluted by ultra pure water in a dilution device; after the dilution is finished, the dissociative NO2 is expelled by high pure nitrogen in a whitening device, and the obtained finished product is filtered by a nanometer filter membrane and enters a finished product receiver under the working pressure of 0.5-0.8 Mpa; wherein, the aperture of the micro filtration membrane is 0.2 to 0.8 Mu m, and the aperture of the nanometer filter membrane is 0.5 to 1.5 nm. In the prepared ultra high purity nitric acid, the content of single cation is lower than 1 ppb, the content of single anion is lower than 100 ppb, and the content of the dust particle larger than 0.5 Mu m is lower than 5 per milliliter. The production process for extra high purity nitric acid has the advantages of simple technique, low production costs, high purity of products, low content of impurity ions, and applicability for large-scale mass production.
Description
Technical field
The present invention relates to the high-purity chemical reagent of a kind of ultra-clean, especially relate to a kind of ultra-high pure nitric acid quantity-produced technology.Ultra-high pure nitric acid is applicable to that mainly microelectronics industry makes in the large-scale integrated circuit semiconducter device industry as cleaning and the usefulness of corrosion.
Background technology
The high-purity chemical reagent of ultra-clean claims microelectronics chemistry product again, it is one of key basic chemical industry material indispensable in the electronic technology microfabrication making processes, be mainly used in the cleaning and the corrosion of chip, its purity and cleanliness factor have very great influence to yield rate, electrical property and the reliability of unicircuit.Along with improving constantly of chip (IC) storage content, capacity is also constantly increasing, thereby the oxide film of chip surface becomes thinner.But the alkali metal impurity in the microelectronics chemistry product, can dissolve in and go in the oxide film as sodium (Na), calcium impurity such as (Ca), thereby caused the decline of anti-insulation voltage, beavy metal impurity such as copper (Cu), iron (Fe), chromium (Cr), silver (Ag) etc., if attached to silicon wafer surface, the proof voltage of silicon wafer P-N knot is reduced.Therefore, also more and more higher to the requirement of the granule content of microelectronics chemistry product and metals content impurity.
Ultra-high pure nitric acid is a kind of crucial microelectronics chemistry reagent, and being that feed purification is refining with technical grade nitric acid normally forms, and technical grade nitric acid has various metals and nonmetallic impurity.The preparation technology of ultra-high pure nitric acid mainly contains sub-boiling distillation method, rectification method etc. at present, and scale production nitric acid mainly adopts continuous rectification method.The nitric acid of 95% above concentration has higher volatility and stability, and wherein impurities is nitrate mostly, has very high boiling point, can separate in the tower still in rectifying, but indivedual impurity close with the nitric acid volatility is difficult to remove.So general industry nitric acid by rectifying after, its foreign matter content still can't reach the standard of super-pure nitric acid.
Summary of the invention
The objective of the invention is to overcome that metal ion and the impurity close with the nitric acid volatility are difficult to removal in the prior art, the deficiency that difficult quality meets the demands provides that a kind of technology is continuously strong, good separating effect, purity height, ultra-high pure nitric acid quantity-produced technology that foreign matter content is low.
The object of the present invention is achieved like this: a kind of ultra-high pure nitric acid quantity-produced technology, it is characterized in that described technology may further comprise the steps: earlier 80～98% nitric acid material of technical grade are mixed in pre-place device with diallyl 18-hat-6 ether organosilicon macromolecule complexing agents that account for nitric acid material weight 0.2%～2%, under the operating pressure of 0.1～0.2MPa, filter again through the microfiltration membrane in the micro-filter, filtrate enters into rectifying tower, the work in-process that go out rectifying tower dilute with the ultrapure water of 15～18M Ω cm in air mix facilities, after treating that dilution finishes, in blowing white device, catch up with free NO with high pure nitrogen
2, the gained work in-process enter the finished product susceptor after the nanofiltration membrane in the nanofiltration device under the operating pressure of 0.5～0.8MPa is filtered, and the aperture of described microfiltration membrane is 0.2～0.8 μ m, and the nanofiltration membrane aperture is 0.5～1.5nm.
Ultra-high pure nitric acid quantity-produced technology of the present invention, described microfiltration membrane, nanofiltration membrane are the high density polyethylene(HDPE) material; Rectifying tower is quartzy material; Blowing white equipment is the hard glass material.
The present invention improves on the basis of conventional art.At first, utilize the complexing of metal ion agent that raw material has been carried out pre-treatment, and in purification process, having added microfiltration membrane separates with nanofiltration membrane, better removed and be difficult to isolating metallic impurity, single cations is lower than 1ppb in the prepared ultra-high pure nitric acid, and single anion-content is lower than 100ppb, dust granules greater than 0.5 μ m is lower than 5/milliliter, production cost is low, the product purity height, and impurity ion content is low, and production technique is easy, is fit to large-scale industrial production.
Description of drawings
Fig. 1 is technological process of production figure of the present invention.
Among the figure: raw material tank 1, pump 2, pretreater 3, micro-filtration strainer 4, valve 5, rectifying tower 6, air mix facilities 7, blow white device 8, nanofiltration device 9 and finished product susceptor 10.
Embodiment
Embodiment 1:
Ultra-high pure nitric acid quantity-produced technology of the present invention following (referring to Fig. 1): nitric acid (98%) raw material with technical grade mixes in pre-place device with the organosilicon macromolecule complexing agent of diallyl 18-hat-6 ethers that account for nitric acid material weight 0.5%～1% earlier, under the operating pressure of 0.15MPa, filter again through the microfiltration membrane in the micro-filter, filtrate enters into rectifying tower, the work in-process that go out rectifying tower dilute with the ultrapure water of 18M Ω cm in air mix facilities, after treating that dilution finishes, in blowing white device, catch up with free NO with high pure nitrogen
2, the gained work in-process enter the finished product susceptor after the nanofiltration membrane in the nanofiltration device under the operating pressure of 0.6MPa is filtered.In the present embodiment, the pressure the during micro-filtrate membrane filtration in the micro-filter is chosen as: 0.1,0.15 or 0.2MPa; Pressure when nanofiltration membrane in the nanofiltration device is filtered is chosen as: 0.5,0.6 or 0.8MPa, and described microfiltration membrane, nanofiltration membrane are the high density polyethylene(HDPE) material, and rectifying tower is quartzy material, and blowing white equipment is the hard glass material.The aperture of described microfiltration membrane is 0.2～0.8 μ m, and for example: the aperture of microfiltration membrane is 0.2,0.5 or 0.8 μ m; Described nanofiltration membrane aperture is 0.5～1.5nm for the nanofiltration membrane aperture, and for example: the nanofiltration membrane aperture is 0.5,1.0 or 1.5nm.
The ultra-high pure nitric acid analysis of present embodiment production is adopted and is divided method, and nitric acid content adopts gas chromatographic analysis in the product, and positively charged ion adopts ICP-MS to analyze, and negatively charged ion adopts ion chromatography, and dust granules adopts the laser particle calculating instrument to measure.Analytical results such as table 1.
Table 1
| Classification | The SEMI-C8 standard | Embodiment 1 |
| HNO 3Content (%) | 70.0±1.0％ | 70.3％ |
| Particle (〉=0.2 μ m≤0.5 μ m, individual/ml), max | 5 | 2 |
| Colourity; APHA, max | 10 | 5 |
| Muriate (Cl); Ppb, max | 200 | 100 |
| Vitriol (SO 4)；ppb，max | 200 | 100 |
| Low NOx (N 2O 3)；ppb，max | 200 | 100 |
| Phosphoric acid salt (PO 4)；ppb，max | 200 | 100 |
| Aluminium (Al); Ppb, max | 1 | 0.2 |
| Arsenic (As); Ppb, max | 1 | 0.1 |
| Gold (Au); Ppb, max | 1 | 0.5 |
| Silver (Ag); Ppb, max | 1 | / do not detect |
| Barium (Ba); Ppb, max | 1 | 0.1 |
| Boron (B); Ppb, max | 1 | 0.5 |
| Cadmium (Cd); Ppb, max | 1 | / do not detect |
| Calcium (Ca); Ppb, max | 1 | 0.7 |
| Chromium (Cr); Ppb, max | 1 | 0.6 |
| Cobalt (Co); Ppb, max | 1 | 0.1 |
| Copper (Cu); Ppb, max | 1 | 0.1 |
| Iron (Fe); Ppb, max | 1 | 0.7 |
| Gallium (Ga); Ppb, max | 1 | 0.5 |
| Germanium (Ge); Ppb, max | 1 | 0.6 |
| Potassium (K); Ppb, max | 1 | 0.2 |
| Indium (In); Ppb, max | 1 | 0.6 |
| Lithium (Li); Ppb, max | 1 | / do not detect |
| Magnesium (Mg); Ppb, max | 1 | 0.5 |
| Manganese (Mn); Ppb, max | 1 | / do not detect |
| Molybdenum (Mo); Ppb, max | 1 | / do not detect |
| Sodium (Na); Ppb, max | 1 | 0.6 |
| Nickel (Ni); Ppb, max | 1 | / do not detect |
| Platinum (Pt); Ppb, max | 1 | 0.5 |
| Plumbous (Pb); Ppb, max | 1 | 0.4 |
| Antimony (Sb); Ppb, max | 1 | 0.6 |
| Tin (Sn); Ppb, max | 1 | 0.2 |
| Strontium (Sr); Ppb, max | 1 | / do not detect |
| Titanium (Ti); Ppb, max | 1 | 0.1 |
| Zinc (Zn); Ppb, max | 1 | 0.2 |
| Zirconium (Zr); Ppb, max | 1 | / do not detect |
| Vanadium (V); Ppb, max | 1 | / do not detect |
Claims (2)
1, a kind of ultra-high pure nitric acid quantity-produced technology, it is characterized in that described technology may further comprise the steps: earlier 80～98% nitric acid material of technical grade are mixed in pre-place device with diallyl 18-hat-6 ether organosilicon macromolecule complexing agents that account for nitric acid material weight 0.2%～2%, under the operating pressure of 0.1～0.2MPa, filter again through the microfiltration membrane in the micro-filter, filtrate enters into rectifying tower, the work in-process that go out rectifying tower dilute with the ultrapure water of 15～18M Ω cm in air mix facilities, after treating that dilution finishes, in blowing white device, catch up with free NO with high pure nitrogen
2, the gained work in-process enter the finished product susceptor after the nanofiltration membrane in the nanofiltration device under the operating pressure of 0.5～0.8MPa is filtered, and the aperture of described microfiltration membrane is 0.2～0.8 μ m, and the nanofiltration membrane aperture is 0.5～1.5nm.
2, a kind of ultra-high pure nitric acid quantity-produced technology according to claim 1 is characterized in that described microfiltration membrane, nanofiltration membrane are the high density polyethylene(HDPE) material; Rectifying tower is quartzy material; Blowing white equipment is the hard glass material.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870460A (en) * | 2010-07-21 | 2010-10-27 | 上海华谊微电子材料有限公司 | Method for preparing super-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 |
| CN102001635A (en) * | 2010-12-27 | 2011-04-06 | 上海化学试剂研究所 | Process for preparing ultrapure nitric acid |
| CN102139864A (en) * | 2011-02-21 | 2011-08-03 | 上海正帆科技有限公司 | Method for producing electronic-grade nitric acid |
| CN102399140A (en) * | 2010-09-17 | 2012-04-04 | 上海华谊微电子材料有限公司 | Production method of ultra-clean and high-purity electronic grade acetic acid |
| CN102557071A (en) * | 2012-01-06 | 2012-07-11 | 中国石油大学(华东) | ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof |
| CN103523761A (en) * | 2013-10-15 | 2014-01-22 | 苏州市晶协高新电子材料有限公司 | Continuous nitric acid discoloring device and method thereof |
| CN104291281A (en) * | 2014-06-12 | 2015-01-21 | 西陇化工股份有限公司 | Method for preparing ultraclean and highly pure nitric acid |
| CN113426270A (en) * | 2021-08-10 | 2021-09-24 | 联仕(昆山)化学材料有限公司 | White blowing device and white blowing process for producing electronic-grade nitric acid |
Family Cites Families (3)
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| CN1102443A (en) * | 1994-04-24 | 1995-05-10 | 抚顺市高新技术开发服务部 | Technology method for refining waste concentrated nitric acid with flash vaporization |
| CN1217854C (en) * | 2002-12-27 | 2005-09-07 | 四川泸天化股份有限公司 | Spiral thick nitricacid bleaching tower and preparation of thick nitric-acid |
| CN100546903C (en) * | 2007-08-06 | 2009-10-07 | 江阴市润玛电子材料有限公司 | Purifying method of ultrahigh pure hydrofluoric acid |
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2008
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101870460A (en) * | 2010-07-21 | 2010-10-27 | 上海华谊微电子材料有限公司 | Method for preparing super-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 |
| CN102399140B (en) * | 2010-09-17 | 2015-04-15 | 联仕(上海)电子化学材料有限公司 | Production method of ultra-clean and high-purity electronic grade acetic acid |
| CN102399140A (en) * | 2010-09-17 | 2012-04-04 | 上海华谊微电子材料有限公司 | Production method of ultra-clean and high-purity electronic grade acetic acid |
| CN102001635A (en) * | 2010-12-27 | 2011-04-06 | 上海化学试剂研究所 | Process for preparing ultrapure nitric acid |
| CN102001635B (en) * | 2010-12-27 | 2013-08-28 | 上海化学试剂研究所 | Process for preparing ultrapure nitric acid |
| CN102139864B (en) * | 2011-02-21 | 2013-01-23 | 上海正帆科技有限公司 | Method for producing electronic-grade nitric acid |
| CN102139864A (en) * | 2011-02-21 | 2011-08-03 | 上海正帆科技有限公司 | Method for producing electronic-grade nitric acid |
| CN102557071B (en) * | 2012-01-06 | 2013-08-21 | 中国石油大学(华东) | ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof |
| CN102557071A (en) * | 2012-01-06 | 2012-07-11 | 中国石油大学(华东) | ZSM-11 molecular sieve with hierarchical porous structure and preparation method thereof |
| CN103523761A (en) * | 2013-10-15 | 2014-01-22 | 苏州市晶协高新电子材料有限公司 | Continuous nitric acid discoloring device and method thereof |
| CN103523761B (en) * | 2013-10-15 | 2015-08-05 | 苏州市晶协高新电子材料有限公司 | A kind of nitric acid continuous stripping devices and methods therefor |
| CN104291281A (en) * | 2014-06-12 | 2015-01-21 | 西陇化工股份有限公司 | Method for preparing ultraclean and highly pure nitric acid |
| CN104291281B (en) * | 2014-06-12 | 2016-03-09 | 西陇科学股份有限公司 | A kind of method preparing super-clean high-purity nitric acid |
| CN113426270A (en) * | 2021-08-10 | 2021-09-24 | 联仕(昆山)化学材料有限公司 | White blowing device and white blowing process for producing electronic-grade nitric acid |
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Address after: 214423, No. 1, Changqing North Road, Jiangyin Industrial Park, Zhouzhuang Town, Jiangsu, China Patentee after: Jiangyin Runma Electronic Material Co., Ltd. Address before: 214423, No. 1, Changqing North Road, Jiangyin Industrial Park, Zhouzhuang Town, Jiangsu, China Patentee before: Jiangyin Runma Electronic Material Co., Ltd. |