CN103193203A - Method for improving quality of industrial grade hydrogen peroxide - Google Patents
Method for improving quality of industrial grade hydrogen peroxide Download PDFInfo
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- CN103193203A CN103193203A CN2013101434003A CN201310143400A CN103193203A CN 103193203 A CN103193203 A CN 103193203A CN 2013101434003 A CN2013101434003 A CN 2013101434003A CN 201310143400 A CN201310143400 A CN 201310143400A CN 103193203 A CN103193203 A CN 103193203A
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Abstract
The invention discloses a method for improving the quality of industrial grade hydrogen peroxide. The industrial grade hydrogen peroxide is used as a raw material; an asymmetric amide extraction agent is added for extraction, so that metal ion impurities are reduced or removed from the industrial grade hydrogen peroxide; and therefore, the hydrogen peroxide with improved quality is obtained. According to the hydrogen peroxide obtained by the method, the total organic carbon is less than 10 ppm, and the removal rate of the metal ion impurities such as Cd, Pb, Cu and Au is over 90 percent. By the method, the problem that the content of the metal ion impurities is overproof when the industrial grade hydrogen peroxide is used as the raw material for preparing the high-quality hydrogen peroxide is solved, and the quality of a product is stable; and furthermore, after being recycled, waste liquid of the asymmetric amide extraction agent containing the metal ion impurities is subjected to acidic washing, alkaline wash and salt water washing until the waste liquid is neutral and is decompressed and distilled so as to be reused.
Description
Technical field
The present invention relates to a kind of method that promotes technical grade hydrogen peroxide quality, particularly relate to a kind of method of utilizing asymmetric amides extraction agent extraction to promote technical grade hydrogen peroxide quality removal impurity metal ion.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals and fine chemical product.The electronic-grade hydrogen peroxide is ten minutes important electron chemical in the electronic industry, is widely used in microelectronics industry aspects such as large-scale integrated circuit (IC), film liquid crystal display (TFT-LCD), semi-conductor, and exploitation prospect is wide.
The production of ultrapure hydrogen peroxide adopts the hydrogen peroxide of technical grade as raw material usually, for the quality that guarantees ultrapure hydrogen peroxide and the stability of production, therefore, require the content of the impurity metal ion in the raw material hydrogen peroxide need remain on quite low-level particular requirement, thereby could make the ultrapure hydrogen peroxide that obtains reach the chemical material part SEMI standard of semiconductor equipment and material structure formulation.
In the prior art, because the hydrogen peroxide product of large-scale industrial production contains certain density various impurity metal ion, directly be not used for preparing ultrapure hydrogen peroxide if add processing, the impurity metal ion that exceeds standard will influence the quality of ultrapure hydrogen peroxide product and stability and the production capacity of production, therefore the technical grade hydrogen peroxide is promoted quality and to satisfy the preparation ultrapure hydrogen peroxide raw-material requirement is seemed very important.
The key that the electronic-grade hydrogen peroxide prepares is to control content and the cleanliness factor of impurity metal ion in the hydrogen peroxide, and the means of utilizing extraction reach the organic impurity in reduction or the removal hydrogen peroxide as pretreated method usually.The extraction agent that adopts has two types of liquids and gases, and liquid can use aromatic hydrocarbons and alcohols, and gas adopts high-pressure carbon dioxide.In the present processing method, use the hydrogen peroxide metal ion neutralization product impurity and the cleanliness factor that obtain after the extraction of liquid type extraction agent all undesirable, if it is use atmospheric carbon dioxide to make extraction agent, very high to the requirement of production unit.
Asymmetric acid amides is a kind of environmental protection extraction agent, can in the last handling process of nuclear fuel, use as extraction agent extracting metals ion, asymmetric acid amides is owing to be connected with the acid amides of small one and large one two different alkyl on the nitrogen-atoms, utilize the singularity of its chemical structure, namely the solvability in water is minimum, can extract impurity metal ion from water.Yet there are no utilization with asymmetric amides extraction agent extraction technical grade superoxol, to reduce or to remove the relevant report of impurity metal ion method.
Summary of the invention
Problem to be solved by this invention is to provide a kind of method that promotes technical grade hydrogen peroxide quality, utilize asymmetric amides extraction agent extraction, impurity metal ion in reduction or the removal technical grade hydrogen peroxide is to overcome the deficiency that impurity metal ion exceeds standard in the hydrogen peroxide extraction in the prior art.
Technical conceive of the present invention is such: be raw material with industrial hydrogen peroxide, add asymmetric amides extraction agent and extract, reduce or remove impurity metal ion in the industrial superoxol, thereby obtain the hydrogen peroxide of quality-improving.
Specifically, the method for lifting technical grade hydrogen peroxide quality of the present invention comprises the steps:
Asymmetric amides extraction agent is joined in the industrial hydrogen peroxide, stirred 8-12 hour under the room temperature, go to the skimmer standing demix, collect lower floor, the hydrogen peroxide of the quality that namely gets a promotion, it contains the recyclable recycling of asymmetric acid amides extraction agent waste liquid of impurity metal ion at the middle and upper levels.
According to aforesaid method, described asymmetric amides extraction agent is selected from: a kind of in N-methyl-N-octyl group decoylamide, N-methyl-N-octyl group decyl amide, the N-methyl-N-octyl group lauramide.
The weightmeasurement ratio of described asymmetric amides extraction agent and technical grade hydrogen peroxide is 0.10-0.15:1, g/ml.
Described industrial hydrogen peroxide is 35% the superoxol of conformance with standard GB1616-2003.
After testing, the hydrogen peroxide that adopts the inventive method to obtain, total organic carbon is less than 10ppm, and the clearance of impurity metal ion such as Cd, Pb, Cu, Au etc. is greater than 90%.
The present invention's beneficial effect compared with prior art:
The present invention extracts by add asymmetric amides extraction agent in the technical grade hydrogen peroxide, obtain the hydrogen peroxide of quality-improving, and the asymmetric amides extraction agent waste liquid of metal ion impurity reclaims by pickling, alkali cleaning, salt and is washed to neutral back underpressure distillation, and is reusable.Therefore, the problem of impurity metal ion content overproof when the inventive method efficiently solves the technical grade hydrogen peroxide as the high-quality hydrogen peroxide raw material of preparation has promoted the quality of hydrogen peroxide.
Embodiment
The present invention is described further below by specific embodiment, but embodiment does not limit protection scope of the present invention.Need to prove that following examples are only unrestricted in order to technical scheme of the present invention to be described.Although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement the technical scheme of invention, and not break away from the scope of technical solution of the present invention, it all should be encompassed in the claim scope of the present invention.
Embodiment 1
100g N-methyl-N-octyl group decoylamide extraction agent is joined in 35% the industrial hydrogen peroxide of 1000ml, stirred 8 hours under the room temperature, go to the skimmer standing demix, collect lower floor, namely obtain the hydrogen peroxide of quality-improving.Wherein, the N-of upper strata metal ion impurity methyl-recyclable recycling of N-octyl group decoylamide extraction agent waste liquid.
The above-mentioned hydrogen peroxide that obtains is carried out analyzing and testing, and detected result is as shown in table 1 below.
Table 1
| Project | The raw material measured value | The product measured value |
| Content H 2O 2，% | 35.5 | 35.1 |
| Total carbon content, % | 0.025 | 0.005 |
| Cadmium (Cd), % | 0.005 | 0.0003 |
| Plumbous (Pb), % | 0.005 | 0.0002 |
| Copper (Cu), % | 0.003 | 0.0001 |
| Gold (Au), % | 0.002 | 0.0001 |
Embodiment 2
120g N-methyl-N-octyl group decyl amide extraction agent is joined in 35% the industrial hydrogen peroxide of 1000ml, stirred 10 hours under the room temperature, go to the skimmer standing demix, collect lower floor, namely obtain the hydrogen peroxide of quality-improving.Wherein, the N-of upper strata metal ion impurity methyl-recyclable recycling of N-octyl group decyl amide extraction agent waste liquid.
The above-mentioned hydrogen peroxide that obtains is carried out analyzing and testing, and detected result is as shown in table 2 below.
Table 2
| Project | The raw material measured value | The product measured value |
| Content H 2O 2，% | 35.5 | 35.2 |
| Total carbon content, % | 0.025 | 0.002 |
| Cadmium (Cd), % | 0.005 | 0.0002 |
| Plumbous (Pb), % | 0.005 | 0.0001 |
| Copper (Cu), % | 0.003 | 0.0002 |
| Gold (Au), % | 0.002 | 0.0001 |
Embodiment 3
150g N-methyl-N-octyl group lauramide extraction agent is joined in 35% the industrial hydrogen peroxide of 1000ml, stirred 12 hours under the room temperature, go to the skimmer standing demix, collect lower floor, namely obtain the hydrogen peroxide of quality-improving.Wherein, the N-of upper strata metal ion impurity methyl-recyclable recycling of N-octyl group lauramide extraction agent waste liquid.
The above-mentioned hydrogen peroxide that obtains is carried out analyzing and testing, and detected result is as shown in table 3 below.
Table 3
| Project | The raw material measured value | The product measured value |
| Content H 2O 2，% | 35.5 | 35.0 |
| Total carbon content, % | 0.025 | 0.003 |
| Cadmium (Cd), % | 0.005 | 0.0001 |
| Plumbous (Pb), % | 0.005 | 0.0001 |
| Copper (Cu), % | 0.003 | 0.0002 |
| Gold (Au), % | 0.002 | 0.0002 |
From above-mentioned table 1, table 2, table 3 data as can be seen: the hydrogen peroxide that adopts the inventive method to obtain, total organic carbon is less than 10ppm, and the clearance of impurity metal ion such as Cd, Pb, Cu, Au etc. is greater than 90%.Thereby the problem of impurity metal ion content overproof when the inventive method efficiently solves the technical grade hydrogen peroxide as the high-quality hydrogen peroxide raw material of preparation has promoted the quality of hydrogen peroxide.
Claims (4)
1. a method that promotes technical grade hydrogen peroxide quality is characterized in that, comprises the steps:
Asymmetric amides extraction agent is joined in the industrial hydrogen peroxide, stirred 8-12 hour under the room temperature, go to the skimmer standing demix, collect lower floor, the hydrogen peroxide of the quality that namely gets a promotion.
2. method according to claim 1 is characterized in that, described asymmetric amides extraction agent is selected from: a kind of in N-methyl-N-octyl group decoylamide, N-methyl-N-octyl group decyl amide, the N-methyl-N-octyl group lauramide.
3. method according to claim 1 is characterized in that, the weightmeasurement ratio of described asymmetric amides extraction agent and technical grade hydrogen peroxide is 0.10-0.15:1, g/ml.
4. method according to claim 1 is characterized in that, the asymmetric acid amides extraction agent waste liquid recycling of impurity metal ion is contained on the upper strata.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310143400.3A CN103193203B (en) | 2013-04-23 | 2013-04-23 | A kind of method promoting quality of industrial grade hydrogen peroxide |
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| CN201310143400.3A CN103193203B (en) | 2013-04-23 | 2013-04-23 | A kind of method promoting quality of industrial grade hydrogen peroxide |
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| CN103193203A true CN103193203A (en) | 2013-07-10 |
| CN103193203B CN103193203B (en) | 2016-08-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271130A (en) * | 2015-09-18 | 2016-01-27 | 泰州市天平化工有限公司 | High production capacity no-pollution oxidant production line |
Citations (4)
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|---|---|---|---|---|
| CN1167507A (en) * | 1994-11-30 | 1997-12-10 | 联合讯号公司 | Use of a solvent impregnated crosslinked matrix for metal recovery |
| CN102424362A (en) * | 2011-10-13 | 2012-04-25 | 天津大沽化工股份有限公司 | Method for purifying hydrogen peroxide |
| CN102485642A (en) * | 2010-12-02 | 2012-06-06 | 上海化学试剂研究所 | Method for producing ultra-pure hydrogen peroxide |
| CN102858733A (en) * | 2010-04-19 | 2013-01-02 | 巴斯夫欧洲公司 | Purification of carboxylic esters by extractive distillation |
-
2013
- 2013-04-23 CN CN201310143400.3A patent/CN103193203B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1167507A (en) * | 1994-11-30 | 1997-12-10 | 联合讯号公司 | Use of a solvent impregnated crosslinked matrix for metal recovery |
| CN102858733A (en) * | 2010-04-19 | 2013-01-02 | 巴斯夫欧洲公司 | Purification of carboxylic esters by extractive distillation |
| CN102485642A (en) * | 2010-12-02 | 2012-06-06 | 上海化学试剂研究所 | Method for producing ultra-pure hydrogen peroxide |
| CN102424362A (en) * | 2011-10-13 | 2012-04-25 | 天津大沽化工股份有限公司 | Method for purifying hydrogen peroxide |
Non-Patent Citations (1)
| Title |
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| 崔玉等: ""新萃取剂N ,N′-不对称烷基酰胺的合成及表征"", 《济南大学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105271130A (en) * | 2015-09-18 | 2016-01-27 | 泰州市天平化工有限公司 | High production capacity no-pollution oxidant production line |
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Address after: 200333 No. 401 North Road, Shanghai, Putuo District Patentee after: SHANGHAI CHEMICAL REAGENT RESEARCH INSTITUTE Co.,Ltd. Address before: 200333 No. 401 North Road, Shanghai, Putuo District Patentee before: Shanghai Chemical Reagent Research Institute |