CN103193203B - A kind of method promoting quality of industrial grade hydrogen peroxide - Google Patents
A kind of method promoting quality of industrial grade hydrogen peroxide Download PDFInfo
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- CN103193203B CN103193203B CN201310143400.3A CN201310143400A CN103193203B CN 103193203 B CN103193203 B CN 103193203B CN 201310143400 A CN201310143400 A CN 201310143400A CN 103193203 B CN103193203 B CN 103193203B
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Abstract
The invention discloses a kind of method promoting quality of industrial grade hydrogen peroxide.With industrial hydrogen peroxide as raw material, add asymmetric amide extractant and extract, the impurity metal ion reducing or removing in industrial hydrogen peroxide, thus obtain the hydrogen peroxide of quality-improving.The hydrogen peroxide obtained by the inventive method, total organic carbon is less than 10ppm, and the clearance of impurity metal ion Cd, Pb, Cu, Au etc. is more than 90%.Efficiently solve the problem that industrial grade hydrogen peroxide exceeds standard as foreign metal ion concentration during preparation high-quality hydrogen peroxide raw material, and the constant product quality obtained, additionally, after the asymmetric amide-type extractant devil liquor recovery of metal ion impurity, decompression distillation after pickling, alkali cleaning, salt are washed to neutrality, reusable.
Description
Technical field
The present invention relates to a kind of method promoting quality of industrial grade hydrogen peroxide, particularly relate to one and utilize asymmetric amide-type to extract
Take agent extraction and promote the method that quality of industrial grade hydrogen peroxide removes impurity metal ion.
Background technology
Hydrogen peroxide is a kind of important Inorganic Chemicals and fine chemical product.Semiconductor Hydrogen Peroxide is in electronics industry ten
Point important electronic chemical product, be widely used in large scale integrated circuit (IC), film liquid crystal display (TFT-LCD), half
The microelectronics industry aspects such as conductor, exploitation prospect is wide.
The hydrogen peroxide producing generally employing technical grade of ultrapure hydrogen peroxide is as raw material, in order to ensure the matter of ultrapure hydrogen peroxide
Amount and the stability produced, it is therefore desirable to the content of the impurity metal ion in raw material hydrogen peroxide need to be maintained at a fairly low level
Particular requirement, thus the ultrapure hydrogen peroxide that just can make reaches the chemical material that semiconductor equipment and material structure are formulated
Material part SEMI standard.
In prior art, owing to the hydrogen peroxide product of large-scale industrial production contains certain density various impurity metal ion,
If not adding process to be used directly to prepare ultrapure hydrogen peroxide, the impurity metal ion exceeded standard will affect ultrapure hydrogen peroxide product
Quality and the stability of production and production capacity, therefore industrial grade hydrogen peroxide being carried out promotes quality and prepares ultrapure peroxidating with satisfied
Hydrogen seems particularly significant to raw-material requirement.
Prepared by Semiconductor Hydrogen Peroxide it is critical only that content and the cleanliness factor controlling impurity metal ion in hydrogen peroxide, generally profit
By the means of extraction as the method for pretreatment, the organic impurities reducing or removing in hydrogen peroxide.The extractant used has
Liquids and gases two types, liquid can use aromatic hydrocarbons and alcohols, and gas uses high-pressure carbon dioxide.Current process
In, the hydrogen peroxide metal ion neutralization product impurity and the cleanliness factor that obtain after using the extraction of liquid type extractant are the most undesirable, if
Using atmospheric carbon dioxide to make extractant, the requirement to the equipment of production is the highest.
Asymmetric amide is a kind of environmental protection extractant, can in the last handling process of nuclear fuel as extractant extracting metals from
Son uses, and asymmetric amide has the amide of small one and large one two different alkyl owing to connecting on nitrogen-atoms, utilizes its chemical constitution
Particularity, i.e. dissolubility in water are minimum, can extract impurity metal ion from water.Yet there are no utilization with not
Symmetrical amides kind of extractants extraction industrial grade hydrogen peroxide solution, to reduce or to remove the relevant report of impurity metal ion method.
Summary of the invention
To be solved by this invention haveing a problem in that provides a kind of method promoting quality of industrial grade hydrogen peroxide, utilizes asymmetric amide
Kind of extractants extracts, and the impurity metal ion reducing or removing in industrial grade hydrogen peroxide, to overcome hydrogen peroxide in prior art
The deficiency that in extraction, impurity metal ion exceeds standard.
The technology design of the present invention is such that with industrial hydrogen peroxide as raw material, adds asymmetric amide-type extractant and extracts
Take, reduce or remove the impurity metal ion in industrial hydrogen peroxide solution, thus obtain the hydrogen peroxide of quality-improving.
Specifically, the method for lifting quality of industrial grade hydrogen peroxide of the present invention, comprise the steps:
Asymmetric amide-type extractant is joined in industrial hydrogen peroxide, stirs 8-12 hour under room temperature, go to liquor separator and stand
Layering, collects lower floor, the hydrogen peroxide of the quality that i.e. gets a promotion, and it contains the asymmetric amide extraction of impurity metal ion at the middle and upper levels
Take the recyclable recycling of agent waste liquid.
According to said method, described asymmetric amide-type extractant is selected from: N-methyl-N-octyl caprylamide, N-methyl-N-are pungent
One in base decyl amide, N-methyl-N-octyl lauramide.
Described asymmetric amide-type extractant is 0.10-0.15:1, g/ml with the w/v of industrial grade hydrogen peroxide.
Described industrial hydrogen peroxide is the hydrogenperoxide steam generator of the 35% of conformance with standard GB1616-2003.
After testing, use the hydrogen peroxide that obtains of the inventive method, total organic carbon less than 10ppm, impurity metal ion such as Cd,
The clearance of Pb, Cu, Au etc. is more than 90%.
Present invention beneficial effect compared with prior art:
The present invention extracts by adding asymmetric amide-type extractant in industrial grade hydrogen peroxide, obtains the mistake of quality-improving
It is washed to neutrality through pickling, alkali cleaning, salt after hydrogen oxide, and the asymmetric amide-type extractant devil liquor recovery of metal ion impurity
Rear decompression distillation, reusable.Therefore, the inventive method efficiently solves industrial grade hydrogen peroxide as preparation high-quality mistake
The problem of impurity metal ion content overproof during hydrogen oxide raw material, improves the quality of hydrogen peroxide.
Detailed description of the invention
Below by specific embodiment, the present invention is described further, but embodiment is not limiting as protection scope of the present invention.
It should be noted that following example are only in order to illustrate technical scheme and unrestricted.Although with reference to preferred embodiment pair
The present invention has been described in detail, and it will be understood by those within the art that, can modify the technical scheme of invention
Or equivalent, without deviating from the scope of technical solution of the present invention, it all should be contained in scope of the presently claimed invention.
Embodiment 1
100g N-methyl-N-octyl caprylamide extractant is joined in the industrial hydrogen peroxide of 35% of 1000ml, stir under room temperature
Mix 8 hours, go to liquor separator stratification, collect lower floor, i.e. obtain the hydrogen peroxide of quality-improving.Wherein, upper strata is containing gold
Belong to the N-methyl-N-octyl caprylamide recyclable recycling of extractant waste liquid of ionic impurity.
Hydrogen peroxide obtained above is analyzed detection, and testing result is as shown in table 1 below.
Table 1
| Project | Raw material measured value | Product measured value |
| Content H2O2, % | 35.5 | 35.1 |
| Total carbon content, % | 0.025 | 0.005 |
| Cadmium (Cd), % | 0.005 | 0.0003 |
| Lead (Pb), % | 0.005 | 0.0002 |
| Copper (Cu), % | 0.003 | 0.0001 |
| Gold (Au), % | 0.002 | 0.0001 |
Embodiment 2
120g N-methyl-N-octyl decyl amide extractant is joined in the industrial hydrogen peroxide of 35% of 1000ml, stir under room temperature
Mix 10 hours, go to liquor separator stratification, collect lower floor, i.e. obtain the hydrogen peroxide of quality-improving.Wherein, upper strata is containing gold
Belong to the N-methyl-N-octyl decyl amide recyclable recycling of extractant waste liquid of ionic impurity.
Hydrogen peroxide obtained above is analyzed detection, and testing result is as shown in table 2 below.
Table 2
| Project | Raw material measured value | Product measured value |
| Content H2O2, % | 35.5 | 35.2 |
| Total carbon content, % | 0.025 | 0.002 |
| Cadmium (Cd), % | 0.005 | 0.0002 |
| Lead (Pb), % | 0.005 | 0.0001 |
| Copper (Cu), % | 0.003 | 0.0002 |
| Gold (Au), % | 0.002 | 0.0001 |
Embodiment 3
150g N-methyl-N-octyl lauramide extractant is joined in the industrial hydrogen peroxide of 35% of 1000ml, under room temperature
Stir 12 hours, go to liquor separator stratification, collect lower floor, i.e. obtain the hydrogen peroxide of quality-improving.Wherein, upper strata contains
The N-methyl-N-octyl lauramide recyclable recycling of extractant waste liquid of impurity metal ion.
The above-mentioned hydrogen peroxide that obtains is analyzed detection, and testing result is as shown in table 3 below.
Table 3
| Project | Raw material measured value | Product measured value |
| Content H2O2, % | 35.5 | 35.0 |
| Total carbon content, % | 0.025 | 0.003 |
| Cadmium (Cd), % | 0.005 | 0.0001 |
| Lead (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 it can be seen that use the hydrogen peroxide that the inventive method obtains, total organic carbon is less than
10ppm, the clearance of impurity metal ion such as Cd, Pb, Cu, Au etc. is more than 90%.Thus, the inventive method efficient solution
Industrial grade hydrogen peroxide of having determined, as the problem of impurity metal ion content overproof during preparation high-quality hydrogen peroxide raw material, improves
The quality of hydrogen peroxide.
Claims (3)
1. the method promoting quality of industrial grade hydrogen peroxide, it is characterised in that comprise the steps:
Asymmetric amide-type extractant is joined in industrial hydrogen peroxide, stirs 8-12 hour under room temperature, go to liquor separator and stand
Layering, collects lower floor, the hydrogen peroxide of the quality that i.e. gets a promotion；Wherein, described asymmetric amide-type extractant and technical grade
The w/v of hydrogen peroxide is 0.10-0.15:1, g/ml.
Method the most according to claim 1, it is characterised in that described asymmetric amide-type extractant is selected from: N-methyl
One in-N-octyl group caprylamide, N-methyl-N-octyl decyl amide, N-methyl-N-octyl lauramide.
Method the most according to claim 1, it is characterised in that the asymmetric amide extraction of impurity metal ion is contained on upper strata
Agent devil liquor recovery recycles.
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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 CN103193203A (en) | 2013-07-10 |
| CN103193203B true CN103193203B (en) | 2016-08-24 |
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| 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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| CN102858733A (en) * | 2010-04-19 | 2013-01-02 | 巴斯夫欧洲公司 | Purification of carboxylic esters by extractive distillation |
| CN102485642B (en) * | 2010-12-02 | 2015-10-07 | 上海化学试剂研究所 | The production method of ultra-pure hydrogen phosphide |
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