CN106241746A - A kind of method of purification industrial hydrogen peroxide solution - Google Patents
A kind of method of purification industrial hydrogen peroxide solution Download PDFInfo
- Publication number
- CN106241746A CN106241746A CN201610711119.9A CN201610711119A CN106241746A CN 106241746 A CN106241746 A CN 106241746A CN 201610711119 A CN201610711119 A CN 201610711119A CN 106241746 A CN106241746 A CN 106241746A
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- Prior art keywords
- hydrogen peroxide
- peroxide solution
- industrial hydrogen
- adsorption resin
- purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/01—Hydrogen peroxide
- C01B15/013—Separation; Purification; Concentration
- C01B15/0135—Purification by solid ion-exchangers or solid chelating agents
Abstract
A kind of method that the invention discloses purification industrial hydrogen peroxide solution, using industrial hydrogen peroxide solution is raw material, is filtered by grade one filter and removes the 75 above large granular impurities of μm, and the material after filtration passes through adsorption resin column organics removal impurity；Then the alumina column connected by least one set and cation exchange resin column remove ionic impurity, and last material enters secondary filter and removes little granule foreign, thus prepares purifying hydrogen peroxide solution product.The method process conditions are gentle, it is easy to implement；Do not use anion exchange resin, eliminate it and produce organic peroxide or epoxide and contact the danger decomposed with hydrogen peroxide, serialization large-scale production can be realized.
Description
Technical field
The method that the present invention relates to purification industrial hydrogen peroxide solution.
Background technology
Anthraquinone is the current main production technology of industrial hydrogen peroxide solution.Owing to this technology production process needing add surely
Determine agent, extractant etc., and rely on metallic conduit, equipment to carry and store, make the industrial hydrogen peroxide solution of production contain
The impurity such as more Organic substance, inorganic matter and particulate matter.Organic impurities (in terms of total organic carbon) content 100～500ppm, its
Mainly include aromatic hydrocarbons, alkyl-anthraquinone, ester, alcohol, phenol, ketone compounds etc.；Inorganic impurity content 130～500ppm, it mainly wraps
Include metal cation and complex, inorganic acid radical anion etc..Miscellaneous to hydrogenperoxide steam generator of the field such as food, organic synthesis
Matter content has strict requirements, wherein organic carbon content≤80ppm, non-volatile matter≤60ppm, phosphate≤50ppm, metal
Ion≤10ppm.Therefore, industrial hydrogen peroxide solution needs through purification process, wants reaching to meet the quality of actual application
Ask.
In order to remove the impurity in industrial hydrogen peroxide solution, those skilled in the art develop many purification sides in succession
Method.At present, using relatively broad purification technique is adsorbent resin and the method for Ion Exchange Resin Phase combination, wherein, cloudy from
Sub-exchange resin is mainly used to remove the impurity such as phosphate radical.Owing to hydrogenperoxide steam generator has strong oxidizing property and faintly acid, its meeting
Destroy the framing structure of anion exchange resin so that it is lose ion-exchange capacity, may produce simultaneously organic peroxide or
Epoxide, even can cause heavy explosion time serious, so the application conditions of anion exchange resin is harsher, and its operation
Temperature is normally controlled in 5～10 DEG C, if operation temperature is beyond this scope, uses anion exchange resin to there is potential safety hazard, with
Time hydrogen peroxide exist decompose danger, along with temperature rise, hydrogen peroxide decomposition can aggravate, and even can set off an explosion.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method of purification industrial hydrogen peroxide solution.The method technique
Mild condition, it is easy to implement；Do not use anion exchange resin, eliminate its produce organic peroxide or epoxide and with mistake
Hydrogen oxide contacts the danger decomposed, and can realize serialization large-scale production.
The technical scheme is that employing industrial hydrogen peroxide solution is raw material, filtered by grade one filter and remove
The 75 above large granular impurities of μm, the material after filtration passes through adsorption resin column organics removal impurity；Then least one set is passed through
The alumina column of series connection and cation exchange resin column remove ionic impurity, and last material enters secondary filter and removes little granule
Impurity, thus prepare purifying hydrogen peroxide solution product.This product quality meets the domain requirement such as food, organic synthesis.
The adsorption resin column of above-mentioned organics removal impurity can use two kinds of absorption of single adsorption resin column or series connection
Resin column.Adsorbent resin is non-polar resin, or is the nonpolar of series connection and two kinds of adsorbent resiies of low pole.
The concentration of industrial hydrogen peroxide solution is generally 27.5%～50.0wt%.Alumina column operation temperature is 5～40
℃.Al in aluminium oxide2O3>=90wt%, its particle diameter is 1～4mm, specific surface area >=100m2/ g, pore volume 0.6～1.1cm3/g.Oxygen
Change and need before aluminum uses to use inorganic base, mineral acid, pure water to carry out pretreatment or regeneration.Inorganic base is that alkali metal hydroxide is water-soluble
Liquid, such as sodium hydroxide, potassium hydroxide aqueous solution etc., mineral acid is sulphuric acid, aqueous solution of nitric acid etc..Alkali metal hydroxide and inorganic
The concentration of aqueous acid is 0.1%～10wt%, usage amount 2～8BV, processing speed 1～8BV/h.
The method equipment is simple, process conditions are gentle, safety is high, product stability is good, it is extensive to realize serialization
Produce.
Compared to the prior art the present invention, has the advantage that solving hydrogen peroxide contacts with anion exchange resin
The technical barriers such as easily decomposition, operating condition harshness and process safety difference.Remove simultaneously effectively Organic substance in hydrogenperoxide steam generator,
Zwitterion and granule foreign, obtained refined hydrogenperoxide steam generator is that colourless transparent liquid, product stability are good, product quality
Meet the prescription in the field such as food, organic synthesis.
Detailed description of the invention
Below in conjunction with embodiment, the present invention will be further described.
Nonpolar adsorption resin, low pole adsorbent resin, aluminium oxide, the model of cation exchange resin and producer are respectively
(dawn, chemical research designing institute had for LSA-5/LSA-5BG (Xi-an Electric Power Resin Factory), AB-8 (Chemical Plant of Nankai Univ.), AO-18
Limit responsible company), LSA-101A (Xi-an Electric Power Resin Factory).Adsorption column a diameter of φ 133mm, exchange column a diameter of φ 100mm,
Load ratio of height to diameter 6.5, and cation exchange resin is Hydrogen.
Purifying process: by primary industry hydrogenperoxide steam generator, provide power to enter grade one filter by pump and remove big
Grain impurity, sequentially enters single or two kinds of adsorption resin columns of series connection after effusion meter controls flow, removes Organic substance in feed liquid
Impurity, feed liquid sequentially enters alumina column and the cation exchange resin column of series connection, removes ionic impurity, and last feed liquid enters two
Little granule foreign removed by level filter.
Embodiment 1
In the present embodiment, aluminium oxide pretreating process is as follows: be 0.5wt%'s initially with 4 times of bed volume, concentration
Sodium hydrate aqueous solution, processing aluminium oxide with 2.5BV/h flow velocity, then same volume, concentration are that the nitric acid of 10wt% is with identical
Flow velocity processes aluminium oxide, finally with pure water aluminium oxide to close to neutral.
Industrial hydrogen peroxide solution concentration is 35.8wt%.Aluminium oxide index is: Al2O3Content is 97.35wt%, granularity
It is 135m for 2.24mm, specific surface area2/ g, pore volume 0.93cm3/g。
Purifying process is as it has been described above, use two-stage filter to remove granule foreign, by adsorption resin column organics removal
Impurity, removes ionic impurity by alumina column and cation exchange resin column.Alumina column operation temperature is 30 DEG C, peroxidating
Hydrogen solution production per hour is 5 times of aluminium oxide volume, and its yield can be adjusted according to raw material and product demand quality.
The degree of stability of hydrogenperoxide steam generator is brought up to 98.2% by 90.9% before purification, and phosphate, lead and arsenic equal size do not detect, stannum
≤ 100ppb, ferrum≤15ppb, meet food, the impurity content requirement to hydrogenperoxide steam generator of the disinfectant field.
Embodiment 2
In the present embodiment aluminium oxide be regeneration after aluminium oxide, its regeneration technology is as follows: initially with 2 times of bed volume,
Concentration is the potassium hydroxide aqueous solution of 2wt%, processes aluminium oxide with 4BV/h flow velocity, then uses 1.25 times of bed volume, concentration
For the sulfuric acid solution of 0.5wt%, with 6BV/h flow velocity process aluminium oxide, finally with pure water alumina balls to close to neutral.Oxygen
The work adsorbance regeneration recovery rate changing aluminum can reach more than the 92% of aluminium oxide.
Alumina column operation temperature is 25 DEG C, and other are with embodiment 1.Product index is after purification: concentration 35.6wt.%,
Degree of stability 98.4%, acidity 0.016%, non-volatile matter 0.0046%, phosphate 0.0005%, total organic carbon 0.0030%, stannum
63ppb, ferrum 10ppb, lead and arsenic index do not detect.It meets food, the disinfectant field impurity content to hydrogenperoxide steam generator
Requirement.
Embodiment 3
In the present embodiment, aluminium oxide pretreating process is as follows: initially with 8 times of bed volume, 10wt.% sodium hydroxide
Aqueous solution, processing aluminium oxide with 8BV/h flow velocity, then same volume, 2.5wt.% sulphuric acid process aluminium oxide with identical flow velocity,
Afterwards with pure water aluminium oxide to close to neutral.
With 50% industrial grade hydrogen peroxide solution as raw material, the operation temperature of alumina column 10 DEG C, hydrogenperoxide steam generator is every
Hour volume of production is 5 times of aluminium oxide volume.Other are with embodiment 1.
Aluminium oxide and cation exchange resin remove phosphate and cation impurity effect is notable, and purified product meets organic
The impurity content requirement to hydrogenperoxide steam generator of the synthesis field.
Embodiment 4
In the present embodiment, aluminium oxide pretreating process is as follows: initially with 6 times of bed volume, 4wt.% potassium hydroxide
Aqueous solution, process aluminium oxide with 2.0BV/h flow velocity, then same volume, 2wt.% nitric acid, process aluminium oxide with identical flow velocity,
Finally with pure water aluminium oxide to close to neutral.
With 28.4wt.% industrial hydrogen peroxide solution as raw material, aluminium oxide index is: Al2O3>=95.4wt.%, granularity are
1.6mm, specific surface area are 150m2/ g, pore volume 0.85mL/g.The operation temperature of alumina column 40 DEG C, hydrogenperoxide steam generator is the least
Time volume of production be 6 times of aluminium oxide volume, and its yield can be adjusted according to raw material and product demand quality.Other are with implementing
Example 1.The degree of stability of products obtained therefrom hydrogenperoxide steam generator is improved, and its quality meets food, disinfectant field to hydrogen peroxide
The impurity content requirement of solution.
Claims (9)
1. a method for purification industrial hydrogen peroxide solution, using industrial hydrogen peroxide solution is raw material, passes through single filter
Device filters removes the 75 above large granular impurities of μm, and the material after filtration passes through adsorption resin column organics removal impurity；Then lead to
Alumina column and the cation exchange resin column of crossing least one set series connection remove ionic impurity, and last material enters secondary filter
Remove little granule foreign, thus prepare purifying hydrogen peroxide solution product.
The method of purification industrial hydrogen peroxide solution the most according to claim 1, is characterized in that adsorption resin column uses single
One adsorption resin column or two kinds of adsorption resin columns of series connection.
The method of purification industrial hydrogen peroxide solution the most according to claim 2, is characterized in that single adsorption resin column is inhaled
Attached resin is non-polar resin, and two kinds of adsorption resin column adsorbent resiies of series connection are nonpolar adsorption resin and low pole absorption tree
Fat.
The method of purification industrial hydrogen peroxide solution the most according to claim 1, is characterized in that Al in aluminium oxide2O3≥
90wt%, its particle diameter is 1～4mm, specific surface area >=100m2/ g, pore volume 0.6～1.1cm3/g。
The method of purification industrial hydrogen peroxide solution the most according to claim 1, is characterized in that alumina column operates temperature
At 5～40 DEG C.
The method of purification industrial hydrogen peroxide solution the most according to claim 1, is characterized in that aluminium oxide uses before using
Inorganic base, mineral acid, pure water carry out pretreatment or regeneration.
The method of purification industrial hydrogen peroxide solution the most according to claim 6, is characterized in that inorganic base is alkali metal hydrogen
Oxide water solution, mineral acid is sulphuric acid or aqueous solution of nitric acid.
The method of purification industrial hydrogen peroxide solution the most according to claim 7, it is characterized in that alkali metal hydroxide and
The concentration of inorganic acid aqueous solution is 0.1%～10wt%, usage amount 2～8BV, processing speed 1～8BV/h.
9., according to the method for the purification industrial hydrogen peroxide solution one of claim 1～8 Suo Shu, it is characterized in that industry peroxidating
The concentration of hydrogen solution is 27.5%～50wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205572A (en) * | 2017-06-30 | 2019-01-15 | 中国石油化工股份有限公司 | A method of purifying hydrogen peroxide |
| CN109850851A (en) * | 2019-02-26 | 2019-06-07 | 苏州晶瑞化学股份有限公司 | The control method of particle in a kind of ultra-pure hydrogen phosphide |
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| CN1684904A (en) * | 2002-09-30 | 2005-10-19 | 德古萨股份公司 | Novel aqueous hydrogen peroxide solutions |
| CN101239704A (en) * | 2008-03-14 | 2008-08-13 | 华南理工大学 | Method for purifying hydrogen peroxide solution |
| CN103842288A (en) * | 2011-09-30 | 2014-06-04 | 三菱瓦斯化学株式会社 | Method for producing aqueous hydrogen peroxide solution |
-
2016
- 2016-08-18 CN CN201610711119.9A patent/CN106241746A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1684904A (en) * | 2002-09-30 | 2005-10-19 | 德古萨股份公司 | Novel aqueous hydrogen peroxide solutions |
| CN101239704A (en) * | 2008-03-14 | 2008-08-13 | 华南理工大学 | Method for purifying hydrogen peroxide solution |
| CN103842288A (en) * | 2011-09-30 | 2014-06-04 | 三菱瓦斯化学株式会社 | Method for producing aqueous hydrogen peroxide solution |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109205572A (en) * | 2017-06-30 | 2019-01-15 | 中国石油化工股份有限公司 | A method of purifying hydrogen peroxide |
| CN109205572B (en) * | 2017-06-30 | 2021-03-05 | 中国石油化工股份有限公司 | Method for purifying hydrogen peroxide |
| CN109850851A (en) * | 2019-02-26 | 2019-06-07 | 苏州晶瑞化学股份有限公司 | The control method of particle in a kind of ultra-pure hydrogen phosphide |
| CN109850851B (en) * | 2019-02-26 | 2020-11-24 | 苏州晶瑞化学股份有限公司 | Method for controlling particles in ultra-high-purity hydrogen peroxide |
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Application publication date: 20161221 |