CN101864578B - Method for preparing peroxysulfuric acid by sonoelectrochemical method - Google Patents

Method for preparing peroxysulfuric acid by sonoelectrochemical method Download PDF

Info

Publication number
CN101864578B
CN101864578B CN2010101451359A CN201010145135A CN101864578B CN 101864578 B CN101864578 B CN 101864578B CN 2010101451359 A CN2010101451359 A CN 2010101451359A CN 201010145135 A CN201010145135 A CN 201010145135A CN 101864578 B CN101864578 B CN 101864578B
Authority
CN
China
Prior art keywords
ultrasonic
electrolysis
anode
sulphuric acid
peroxy
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN2010101451359A
Other languages
Chinese (zh)
Other versions
CN101864578A (en
Inventor
洪涛
李林波
薛娟琴
张毅
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Xian University of Architecture and Technology
Original Assignee
Xian University of Architecture and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Xian University of Architecture and Technology filed Critical Xian University of Architecture and Technology
Priority to CN2010101451359A priority Critical patent/CN101864578B/en
Publication of CN101864578A publication Critical patent/CN101864578A/en
Application granted granted Critical
Publication of CN101864578B publication Critical patent/CN101864578B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Abstract

The invention discloses a method for preparing peroxysulfuric acid by a sonoelectrochemical method, which is characterized in that in the method, a sulphuric acid solution is placed in an electrolyzer; pure platinum serves as an anode, and a lead board or thermal shock graphite serves as a cathode; the cathode and the anode are separated by a sulfonic group anion selecting membrane; an ultrasonic is added at the bottom of the electrolyzer; the electrolysis temperature is 0-40 DEG C, and the electrolysis voltage is kept between 3V and 7V, and the current density is 1000A/m<2>-6000A/m<2>; the frequency of the added ultrasonic is 20kHz-100kHz, the sound intensity of the ultrasonic is 5-20W/m<2>, and the electrolysis time of the ultrasonic is 1-5 hours; and sulfate radicals in the sulphuric acid solution at the anode zone is subject to an oxidation reaction to produce the peroxysulfuric acid. Compared with the conventional method for preparing peroxysulfuric acid by the high concentration synthesis method, the invention has the advantages of simple method, reduced energy consumption, shortened reaction time, higher activity of a generated oxidant and the like.

Description

Utilize ultrasonic electrochemical to prepare the method for peroxy-monosulfuric acid
Technical field
The present invention relates to a kind of preparation of oxygenant, particularly a kind of method of utilizing ultrasonic electrochemical to prepare peroxy-monosulfuric acid.
Background technology
In the high-level oxidation technology of hydrometallurgy flow process and environmental engineering, oxygenant is used by a large amount of.Existing oxygenant mainly contains permanganate, oxygen, perferrate, chlorine, ozone, hypochlorite etc.; But problems such as the toxic height of these oxygenants, oxidizing potential is low, the reagent consumption is big, cost is high, residual reagent contamination environment; And used oxygenant or be solid or for gas, oxidation efficiency is low in solution; Therefore for reaching the purpose of effective processing, often add a large amount of oxygenants and follow repeatedly oxidation, cause subsequent disposal extremely difficult.
Peroxy-monosulfuric acid is compared the oxidizing potential that has more than 2.0 as a kind of novel oxygenant with other oxygenant, and oxidation activity is good, oxidation efficiency is high, is used for the aqueous solution and has good result; According to reports, the foreign scholar adopts 60-70% hydrogen peroxide and the synthetic peroxy-monosulfuric acid of the vitriol oil, but synthesis condition is harsh, and synthesis temperature need be controlled at below 0 ℃, and is restive as far as this exothermic process.Domestic also have the scholar to utilize hydrogen peroxide and the synthetic peroxy-monosulfuric acid of the vitriol oil, but because the domestic production concentration that is difficult to is higher than 30% hydrogen peroxide, therefore synthesizes and do not see successfully report.
Summary of the invention
Defective or deficiency to prior art exists the objective of the invention is to, and a kind of method of utilizing ultrasonic electrochemical to prepare peroxy-monosulfuric acid is provided.This method can make sulphuric acid soln electrolysis under relatively mild condition generate the novel oxygenant of peroxy-monosulfuric acid with in the ultrasonic introducing electrolyzer.
For realizing above-mentioned task, the present invention takes following technical solution scheme:
A kind of ultrasonic electrochemical prepares the method for peroxy-monosulfuric acid, it is characterized in that, this method places electrolyzer with sulphuric acid soln; Pure platinum is anode, and negative electrode is stereotype or thermal shock graphite, and sulfonic group negatively charged ion selective membrane is separated anode and cathode; Bottom of electrolytic tank adds UW; Electrolysis temperature is 0-40 ℃, and electrolysis voltage remains on 3V~7V, and current density is 1000A/m 2-6000A/m 2, the ultrasonic frequency that is added is 20kHz~100kHz, the ultrasonic sound intensity is 5-20W/m 2, the ultrasonic electrolysis time is 1~5 hour, sulfate radical generation oxidizing reaction in the sulphuric acid soln of positive column generates peroxy-monosulfuric acid.
The present invention adopts the intensified by ultrasonic wave electrochemical process, prepares novel oxygenant peroxy-monosulfuric acid.Adopt the intensified by ultrasonic wave electrochemical process, noble potential, high-energy can be provided, help strengthening and flow, improve mass transfer, reduce concentration polarization; Effectively shorten the reaction times, improve synthetic yield, can reduce voltage simultaneously, improve current efficiency.
Description of drawings
Fig. 1 is for realizing equipment structure chart of the present invention.
Below in conjunction with accompanying drawing and embodiment the present invention is done further explain.
Embodiment
As shown in Figure 1, sulphuric acid soln is placed electrolyzer, pure platinum is anode; Negative electrode is stereotype or thermal shock graphite, and sulfonic group negatively charged ion selective membrane is separated anode and cathode, and bottom of electrolytic tank adds ultrasonic generation systems; There is ultrasonic transducer ultrasonic generation systems inside; Electrolysis temperature is 0-40 ℃, and electrolysis voltage remains on 3V~7V, and current density is 1000-6000A/m 2, sulphuric acid soln (electrolytic solution) concentration is 20-45%, and the ultrasonic frequency that is added is 20kHz~100kHz, and the ultrasonic sound intensity is 5-20W/m 2, the ultrasonic electrolysis time is 1~5 hour, sulfate radical generation oxidizing reaction in the sulphuric acid soln of positive column generates peroxy-monosulfuric acid.
The mode that the present invention adopts ultrasonic electrochemical to combine with the negatively charged ion selective membrane is carried out electrolysis; The peroxy-monosulfuric acid that anode generates under the effect of anionic membrane in the positive column concentration improve constantly, sulfuric acid constantly is dissociated into hydrogen ion in the cathodic area, generation hydrogen under cathodic process.
Below be the embodiment that the contriver provides, need to prove that these embodiment are the preferable examples of the present invention, the invention is not restricted to these embodiment.
Embodiment 1:
With concentration is that 20% sulphuric acid soln adds in the electrolyzer, and pure platinum is anode, and negative electrode is a stereotype, and the sulfonic group anionic membrane separates the negative and positive district, and bottom of electrolytic tank adds UW, and electrolysis voltage is 3V, current density 1500A/m 2, ultrasonic frequency is 20kHz, ultrasonic sound intensity 10W/m 2, temperature of reaction is 0 ℃, ultrasonic electrolysis 4 hours, and the oxygenant peroxy-monosulfuric acid concentration that makes is 0.9mol/L.
Embodiment 2:
With concentration is that 30% sulphuric acid soln adds in the electrolyzer, and pure platinum is anode, and negative electrode is a stereotype, and the sulfonic group anionic membrane separates the negative and positive district, and electrolysis voltage is 5V, current density 2500A/m 2, adding UW at bottom of electrolytic tank, ultrasonic frequency is 60kHz, ultrasonic sound intensity 5W/cm 2, temperature of reaction is 20 ℃, ultrasonic electrolysis 3 hours, and the oxygenant peroxy-monosulfuric acid concentration that makes is 0.95mol/L.
Embodiment 3:
With concentration is that 45% sulphuric acid soln adds in the electrolyzer, and pure platinum is anode, and negative electrode is a stereotype, and the sulfonic group anionic membrane separates the negative and positive district, and electrolysis voltage is 6V, current density 5000A/m 2, adding UW at bottom of electrolytic tank, ultrasonic frequency is 100kHz, ultrasonic sound intensity 20W/cm 2, temperature of reaction is 40 ℃, ultrasonic electrolysis 2 hours, and the oxygenant peroxy-monosulfuric acid concentration that makes is 1mol/L.

Claims (1)

1. a ultrasonic electrochemical prepares the method for peroxy-monosulfuric acid, it is characterized in that this method places electrolyzer with sulphuric acid soln; Pure platinum is anode, and negative electrode is stereotype or thermal shock graphite, and sulfonic group negatively charged ion selective membrane is separated anode and cathode; Bottom of electrolytic tank adds UW; Electrolysis temperature is 0-40 ℃, and electrolysis voltage remains on 3V~7V, and current density is 1000A/m 2-6000A/m 2, the ultrasonic frequency that is added is 20kHz~100kHz, the ultrasonic sound intensity is 5-20W/m 2, the ultrasonic electrolysis time is 1~5 hour, sulfate radical generation oxidizing reaction in the sulphuric acid soln of positive column generates peroxy-monosulfuric acid;
The concentration of described sulphuric acid soln is 20%-45%.
CN2010101451359A 2010-04-12 2010-04-12 Method for preparing peroxysulfuric acid by sonoelectrochemical method Expired - Fee Related CN101864578B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN2010101451359A CN101864578B (en) 2010-04-12 2010-04-12 Method for preparing peroxysulfuric acid by sonoelectrochemical method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN2010101451359A CN101864578B (en) 2010-04-12 2010-04-12 Method for preparing peroxysulfuric acid by sonoelectrochemical method

Publications (2)

Publication Number Publication Date
CN101864578A CN101864578A (en) 2010-10-20
CN101864578B true CN101864578B (en) 2012-02-01

Family

ID=42956496

Family Applications (1)

Application Number Title Priority Date Filing Date
CN2010101451359A Expired - Fee Related CN101864578B (en) 2010-04-12 2010-04-12 Method for preparing peroxysulfuric acid by sonoelectrochemical method

Country Status (1)

Country Link
CN (1) CN101864578B (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104109878B (en) * 2014-07-21 2017-02-15 河南省科学院高新技术研究中心 Process for synthesizing rubber vulcanization accelerator CBS by electrolytic method in water phase
CN106830214A (en) * 2017-03-28 2017-06-13 西安建筑科技大学 A kind of device and method for processing acidic arsenic-containing solution
CN108048864B (en) * 2017-12-26 2019-10-25 扬州大学 Common cathode ultrasonic electrochemical device

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4020856C2 (en) * 1990-06-29 1992-04-23 Degussa Ag, 6000 Frankfurt, De
CN1528660A (en) * 2003-10-16 2004-09-15 陶华西 Method for preparing permonosulfuric hydrogen-pottassium compound salt
CN1781846A (en) * 2004-12-01 2006-06-07 宋海鹏 Process for preparing potassium hydrogen persulfate composite salts

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4020856C2 (en) * 1990-06-29 1992-04-23 Degussa Ag, 6000 Frankfurt, De
CN1528660A (en) * 2003-10-16 2004-09-15 陶华西 Method for preparing permonosulfuric hydrogen-pottassium compound salt
CN1781846A (en) * 2004-12-01 2006-06-07 宋海鹏 Process for preparing potassium hydrogen persulfate composite salts

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王杰等.过一硫酸氢钾三复盐的研制.《无机盐工业》.2004,(第06期), *
田淑芳.过一硫酸的合成及其在铀水冶中的应用.《铀矿冶》.1992,(第04期), *

Also Published As

Publication number Publication date
CN101864578A (en) 2010-10-20

Similar Documents

Publication Publication Date Title
CN101634035B (en) Electrochemical method and electrochemical device for synergistically generating ozone and hydrogen peroxide in neutral medium
CN105483747B (en) A kind of method and device of water electrolysis hydrogen production gas
US9297084B2 (en) Electrochemical production of hydrogen
CN105951117B (en) A kind of electrolytic method of low cost production high purity of hydrogen peroxide and hydrogen
Grotheer et al. Industrial electrolysis and electrochemical engineering
CN101713078B (en) Device and method for preparing potassium ferrate through electrolysis
JP2015091572A (en) Biogas producing system and method of producing biogas and carbon dioxide reduced product using biogas producing system
CN101864578B (en) Method for preparing peroxysulfuric acid by sonoelectrochemical method
CN112725823B (en) Coupling process for efficiently utilizing electric energy to perform coal oxidation and carbon dioxide reduction
CN101864577B (en) Method for electrochemically preparing peroxysulfuric acid
CN103866344A (en) Method for preparing nitric acid through electrolysis
CN108722437A (en) The preparation method and ferronickel composite catalyst of ferronickel composite catalyst
Chaenko et al. Indirect electrosynthesis of peracetic acid using hydrogen peroxide generated in situ in a gas diffusion electrode
CN205204884U (en) Handle many diaphragm electrolysis of multi -electrode groove of high salt industrial waste water
CN106048641A (en) Process method of electrochemically preparing Fe3+ and H2 in pair
CN105696017A (en) Novel technical method for reducing nitrobenzene by using iron
CN215517653U (en) Device for producing hydrogen by electrolyzing recovered plastic
KR20160038363A (en) Electrochemical reduction method of carbon dioxide and apparatus therefor
CN114059086A (en) Device and method for two-step electrolytic hydrogen production based on acidic electrolyte
KR20140036436A (en) Automatic oxygen generator by water electrolysis and hydrogen fuel cell
CN110965071B (en) Metal catalyst for electrochemical reduction of carbon dioxide and preparation and application thereof
WO2006113463A3 (en) Apparatus and method for the controllable production of hydrogen at an accelerated rate
JP2016029199A (en) Method and apparatus for producing chemical by electrochemical process
CN102241430B (en) Method for removing bromine ions in drinking water by utilizing electrolytic cell
CN117488317A (en) Coal slime oxidation auxiliary method for reducing hydrogen production energy consumption by water electrolysis

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20120201

Termination date: 20160412

CF01 Termination of patent right due to non-payment of annual fee