CN2688725Y - Electrolyzer for synthesis of alkyl azanol salt - Google Patents
Electrolyzer for synthesis of alkyl azanol salt Download PDFInfo
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- CN2688725Y CN2688725Y CN200420020638.3U CN200420020638U CN2688725Y CN 2688725 Y CN2688725 Y CN 2688725Y CN 200420020638 U CN200420020638 U CN 200420020638U CN 2688725 Y CN2688725 Y CN 2688725Y
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Abstract
The utility model provides an electrolyser for electrolysing synthesized alkyl azanol salt, comprising an electric tank, a cathode electrolyte storage slot, a catholyte storage slot, a cathode elevated tank and an anode elevated tank. Wherein the electric tank is composed of unit troughs which are connected in series, and the electric tank is placed on a pressing frame via a supporting frame. The unit trough comprises a cathode chamber, an anode chamber, a cathode chamber, an anode, a membrane, a cathode liquid;catholyte inlet, a catholyte outlet, a catholyte outlet, a cathode liquid; catholyte outlet, a cathode gas outlet, an anodic gas outlet and a unit trough slot wall. The unit trough slot wall is an insulated plate frame. The utility model has the advantages of high current efficiency, high space-time efficiency, high product purity and low energy consumption, being adapted to the industrial production of alkyl azanol salt.
Description
(1) technical field
The utility model relates to a kind of electrolyzer that is used for electrolytic synthesis alkyl hydroxylammonium salt, relates in particular to a kind of electrolyzer of suitability for industrialized production alkyl hydroxylammonium salt.
(2) background technology
The alkyl hydroxylammonium salt is the important organic synthesis intermediate of a class, is widely used in the synthetic of agricultural chemicals, medicine etc.The alkyl hydroxylammonium salt generally adopts chemical method synthetic, uses conventional chemical reaction and separating device, adopts electrolytic process synthesis of alkyl hydroxylammonium salt, does not obtain suitability for industrialized production both at home and abroad as yet.Domesticly applied to industrialized electrolyzer and be mainly chlor-alkali electrolytic cells, this device only is applicable in the basic solution, its barrier film adopts alkali proof asbestos film or perfluor type ionic membrane, can not be applicable to hydrochloric acid or sulfuric acid medium that electrolytic process production alkyl hydroxylammonium salt is adopted, electrode and barrier film are corroded easily; Other electrochemical reactors, as electrolyzers such as sheet frame acyclic type, sheet frame multipole type, fixed bed, rotating electrode reactors, all can not directly carry out the suitability for industrialized production of the rudimentary hydroxylammonium salt of electrolytic synthesis effectively, have that technology and material horizontal are low, the industrialization maturity is low, a shortcoming such as electrode and barrier film are not corrosion-resistant.
(3) summary of the invention
The purpose of this utility model is to provide a kind of hydrochloric acid or sulfuric acid medium of being applicable to, thereby the electrolytic reduction alkyl nitro compounds realizes the electrolyzer of suitability for industrialized production alkyl hydroxylammonium salt, especially in order to produce hydrochloride or the vitriol as alkyl azanols such as methyl hydroxylamine, ethyl azanol, isopropylhydroxyla, n-propyl azanol, normal-butyl azanol, n-pentyl azanol, n-hexyl azanol, cyclohexyl azanols.
For achieving the above object, the utility model provides a kind of electrolyzer that is used for electrolytic synthesis alkyl hydroxylammonium salt, comprise electrolyzer, catholyte storage tank, anolyte storage tank, negative electrode header tank, anode header tank, wherein said electrolyzer is in series by unit groove, and electrolyzer places on the hold-down frame by bracing frame; Described unit groove comprises cathode compartment, anolyte compartment, negative electrode, anode, barrier film, catholyte import, anolyte import, anolyte outlet, catholyte outlet, cathode gas outlet, anodic gas outlet, unit groove cell wall; Described unit groove cell wall is the insulation sheet frame; Described anolyte import is by total pipe coupling anode header tank, and the outlet of the anolyte of described unit groove connects the anolyte storage tank, and the anolyte storage tank is connected to the anode header tank by recycle pump; Described catholyte import is by total pipe coupling negative electrode header tank, and the outlet of the catholyte of described unit groove connects the catholyte storage tank, and the catholyte storage tank is connected to the negative electrode header tank by recycle pump.
Above-mentioned insulation sheet frame one of can be preferably following the sheet frame of material: polypropylene sheet frame, polyethylene sheet frame, synthetic glass sheet frame, polyvinyl chloride sheet frame and ABS resin sheet frame, more preferably polypropylene sheet frame.
In electrolyzer described in the utility model, the electrolyzer that unit groove is in series places on the hold-down frame by bracing frame, and hold-down frame compresses sealing with electrolyzer.Especially, described hold-down frame is the hold-down frame of plate-and-frame filter press.
Because it is that 0～70 ℃, negative electrode and anolyte are under 1～30% hydrochloric acid or the vitriolic operating mode that ionic membrane is operated in electrolyte temperature, and electrolytic solution exists and contains certain density oxygen or chlorine in certain flow velocity and the electrolytic solution in the electrolytic process, so adopts acid proof cationic membrane under this operating mode.These ionic membranes have the hydrochloric acid of being applicable to or sulfuric acid medium, have certain oxidation-resistance, and the corrosion of resistance to chlorine or oxygen has lower membrane voltage and falls, and have preferably characteristics such as physical strength.In order further to improve the work-ing life of ionic membrane, in the electrolyzer design, be provided with negative electrode porous plate and anode porous plate, diaphragm clip from the pressure of header tank and recycle pump, helps membranous operation steady in a long-term on the minimizing unit surface between porous plate.
Above-mentioned acid proof cationic membrane can be sulfonate film or carboxylic acid membrane, as available perfluoro sulfonic acid membrane or perfluorocarboxylic acid film plasma film.
Especially, described anolyte import is provided with adjustable valve, can each anolyte compartment's flow of electrolyte of independent regulation.The anolyte import imports hydrochloric acid or sulphuric acid soln, and electrolytic solution is analysed oxygen or analysed chlorine on anode, and the anolyte outlet of unit groove is derived electrolytic solution after the electrolysis separately to anode electrolytic solution storage tank, constitutes circulation by pump delivery Zhiyang utmost point header tank.
Especially, described catholyte import is provided with adjustable valve, can each cathode compartment flow of electrolyte of independent regulation.The catholyte import imports hydrochloric acid or sulphuric acid soln, the catholyte outlet of unit groove is derived reacted electrolytic solution separately to negative electrode electrolytic solution storage tank, is furnished with the reaction mass device in the catholyte storage tank, the material alkyl nitro compounds makes an addition in the catholyte storage tank with continuous or mode intermittently, be delivered to the negative electrode header tank through recycle pump, being delivered to the catholyte import again, is corresponding alkyl hydroxylammonium salt by electrolytic reduction on negative electrode.Cathode compartment and anolyte compartment also are provided with pneumatic outlet, derive the gas that negative electrode and anode produce respectively.
Above-mentioned alkyl nitro compounds can be Nitromethane 99Min., nitroethane, 1-nitropropane, 2-nitropropane, 1-nitrobutane, 1-nitropentane, 1-nitro hexane or nitrocyclohexane.
In order to reduce electrolytic energy consumption, negative electrode adopts the insoluble metallic cathode (as copper, copper-amalgam) or the Graphite Electrodes of acid corrosion-resistant, and electrode is preferably netted or tabular porous electrode, favourable gas evolution and electrolysis mass transfer; The anode of electrolyzer adopts the insoluble metal anode or the Graphite Electrodes of analysing chlorine (as DSA) or analysing oxygen (as lead alloy) of acid corrosion-resistant, and electrode is preferably netted or tabular porous electrode, favourable gas evolution and electrolysis mass transfer.
The utility model compare with electrolyzers such as existing relevant chlorine industry, sheet frame multipole type, fixed bed, rotating electrode reactors have the current efficiency height, spatiotemporal efficiency height, product purity height and advantage of low energy consumption, simultaneously described electrolyzer has adjustable, compact construction applied widely, independent, characteristics easy to maintenance, is specially adapted to electrolysis production alkyl hydroxylammonium salt in hydrochloric acid or sulfuric acid medium.
(4) description of drawings
Fig. 1 is a structural representation of the present utility model.
Fig. 2 is a schematic perspective view of the present utility model.
(5) embodiment
Below in conjunction with accompanying drawing the utility model is further described, but technical parameter related in the scheme can not be interpreted as restriction of the present utility model.
Embodiment 1
A kind of electrolyzer that is used for electrolytic synthesis alkyl hydroxylammonium salt comprises the electrolyzer that is in series by 12 groups of unit grooves, and electrolyzer places on the hold-down frame 13 by bracing frame 16.The unit groove of electrolyzer comprises cathode compartment 1, anolyte compartment 2, negative electrode 3, anode 4, barrier film 5, negative electrode porous plate 6, anode porous plate 7, anolyte import 8, anolyte outlet 9, cathode gas outlet 10, anodic gas outlet 11, unit groove cell wall 12, catholyte import 14, catholyte outlet 15.Anode 4 adopts improved ruthenium titanium oxide electrode (DSA), and negative electrode 3 adopts copper electrode, and barrier film 5 adopts polystyrolsulfon acid type ionic membrane, and unit groove cell wall 12 adopts the polypropylene sheet frame.Anolyte import 8 is through the total pipe coupling anode of anolyte header tank, and the electrolytic solution after the anolyte outlet 9 derivation electrolysis is to anode electrolytic solution storage tank, and the anolyte storage tank is connected to the anode header tank by recycle pump simultaneously; Catholyte import 14 is through the total pipe coupling negative electrode of catholyte header tank, and the catholyte outlet is derived reacted electrolytic solution to negative electrode electrolytic solution storage tank, and the catholyte storage tank is connected to the negative electrode header tank by recycle pump.
As when the methyl hydroxylamine hydrochloride is produced, in the anolyte storage tank, add 36% hydrochloric acid continuously, constitute circulation by pump delivery Zhiyang utmost point header tank; Add Nitromethane 99Min. simultaneously in the catholyte storage tank continuously, be delivered to the negative electrode header tank by recycle pump, be delivered to catholyte import 14 again, behind electrolytic reduction on the negative electrode 3, electrolytic solution after the electrolysis exports the catholyte storage tank to by catholyte outlet 15.Anolyte compartment's electrolytic solution is 18% hydrochloric acid, and cathode compartment electrolytic solution is 18% hydrochloric acid, is 40 ℃ at electrolyte temperature, and current density is 1500A/m
2Condition under electrolysis.After electrolysis finished, it was 20% methyl hydroxylamine hydrochloride solution that cathode compartment 1 obtains concentration.This group electrolyzer yearly capacity is 20～30 tons.
Embodiment 2
In embodiment 1, unit groove is replaced by 15 groups, anode 4 is replaced by the lead alloy electrode, and barrier film 5 is replaced by perfluorinated sulfonic acid type ionic membrane, and unit groove cell wall 12 is replaced by the polyethylene sheet frame.
As when producing the n-pentyl hydroxylamine sulfate, anolyte compartment's electrolytic solution is replaced by 15% sulphuric acid soln, and cathode compartment electrolytic solution is replaced by 15% sulphuric acid soln,, in the catholyte storage tank, add the 2-nitropropane continuously, all the other conditions are constant.After electrolysis finished, it was 18% isopropylhydroxyla sulfate liquor that cathode compartment 1 obtains concentration.This electrolyzer yearly capacity is 20～30 tons.
Claims (10)
1, a kind of electrolyzer that is used for electrolytic synthesis alkyl hydroxylammonium salt, comprise electrolyzer, catholyte storage tank, anolyte storage tank, negative electrode header tank, anode header tank, it is characterized in that: described electrolyzer is in series by unit groove, and electrolyzer places on the hold-down frame by bracing frame; Described unit groove comprises cathode compartment, anolyte compartment, negative electrode, anode, barrier film, catholyte import, anolyte import, anolyte outlet, catholyte outlet, cathode gas outlet, anodic gas outlet, unit groove cell wall; Described unit groove cell wall is the insulation sheet frame; Described anolyte import is by total pipe coupling anode header tank, and the outlet of the anolyte of described unit groove connects the anolyte storage tank, and the anolyte storage tank is connected to the anode header tank by recycle pump; Described catholyte import is by total pipe coupling negative electrode header tank, and the outlet of the catholyte of described unit groove connects the catholyte storage tank, and the catholyte storage tank is connected to the negative electrode header tank by recycle pump.
2, electrolyzer according to claim 1 is characterized in that also being provided with anode porous plate and negative electrode porous plate in the described electrolyzer, and described diaphragm clip is between porous plate.
3, electrolyzer according to claim 1 and 2 is characterized in that described insulation sheet frame is one of following:
1. 2. 3. 4. 5. ABS resin sheet frame of polyvinyl chloride sheet frame of synthetic glass sheet frame of polyethylene sheet frame of polypropylene sheet frame.
4, electrolyzer according to claim 1 is characterized in that described negative electrode and anolyte import are provided with adjustable valve.
5, electrolyzer according to claim 3 is characterized in that described barrier film is acid proof cationic membrane.
6, electrolyzer according to claim 5 is characterized in that described barrier film is one of following:
1. 2. carboxylic acid membrane of sulfonate film.
7, electrolyzer according to claim 1 is characterized in that described unit groove number is the 1-20 group.
8, electrolyzer according to claim 1 is characterized in that described negative electrode is the high overpotential of hydrogen evolution electrode of acid corrosion-resistant; Described anode is the low chlorine or the low overpotential for oxygen evolution electrode of analysing of acid corrosion-resistant.
9, electrolyzer according to claim 8 is characterized in that described negative electrode is netted or tabular porous metal electrode or Graphite Electrodes.
10, electrolyzer according to claim 8 is characterized in that described anode is netted or tabular porous metal electrode or Graphite Electrodes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200420020638.3U CN2688725Y (en) | 2004-03-05 | 2004-03-05 | Electrolyzer for synthesis of alkyl azanol salt |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200420020638.3U CN2688725Y (en) | 2004-03-05 | 2004-03-05 | Electrolyzer for synthesis of alkyl azanol salt |
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| CN2688725Y true CN2688725Y (en) | 2005-03-30 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776525A (en) * | 2012-08-20 | 2012-11-14 | 云南天恒通泰腐植酸有限公司 | Method for electrolyzing and recycling chromium containing waste liquid generated during oxidation decoloration of montan wax, deresinated montan wax, peat wax or deresinated peat wax |
| CN112759036A (en) * | 2020-12-28 | 2021-05-07 | 云南驰宏国际锗业有限公司 | Method for treating hydrochloric acid wastewater by electrolysis method and electrolytic cell for hydrochloric acid wastewater electrolysis |
-
2004
- 2004-03-05 CN CN200420020638.3U patent/CN2688725Y/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102776525A (en) * | 2012-08-20 | 2012-11-14 | 云南天恒通泰腐植酸有限公司 | Method for electrolyzing and recycling chromium containing waste liquid generated during oxidation decoloration of montan wax, deresinated montan wax, peat wax or deresinated peat wax |
| CN102776525B (en) * | 2012-08-20 | 2015-07-15 | 云南尚呈生物科技有限公司 | Method for electrolyzing and recycling chromium containing waste liquid generated during oxidation decoloration of montan wax, deresinated montan wax, peat wax or deresinated peat wax |
| CN112759036A (en) * | 2020-12-28 | 2021-05-07 | 云南驰宏国际锗业有限公司 | Method for treating hydrochloric acid wastewater by electrolysis method and electrolytic cell for hydrochloric acid wastewater electrolysis |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20050330 Termination date: 20100305 |