CN101187034B - Bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid - Google Patents
Bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid Download PDFInfo
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- CN101187034B CN101187034B CN2007100712059A CN200710071205A CN101187034B CN 101187034 B CN101187034 B CN 101187034B CN 2007100712059 A CN2007100712059 A CN 2007100712059A CN 200710071205 A CN200710071205 A CN 200710071205A CN 101187034 B CN101187034 B CN 101187034B
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Abstract
Disclosed is a bipolar type non-membrane device of electrolytic synthesis of butanedioic acid, which comprises an electrolysis bath, a fluid distribution inlet pipe and a fluid collecting pipe which are communicated with the electrolysis bath, and an electrolyte fluid storage tank, a heat exchanger and an elevated tank with which the electrolysis bath forms a circle. The elevated tank and the fluid distribution inlet pipe are communicated, and the fluid collecting pipe is connected with the electrolyte fluid storage tank. The butanedioic acid synthesis device further comprises bipolar type electrodes which are of plate shape and installed in the electrolysis bath, unit electrolyzers are arranged between two adjacent bipolar type electrodes, each unit electrolyzer is provided with an electrolyte inlet and an electrolyte outlet, each electrolyte inlet is connected with the fluid distribution inlet pipe, each electrolyte outlet is connected with the fluid collecting pipe, and the bipolar type electrodes arranged at both ends of the electrolysis bath are respectively connected with a positive electrode and a negative electrode of power supply. The invention is economical in investment and suitable in mass electrolysis, and reduces the energy consumption.
Description
Technical field
The present invention relates to the electrolytic synthesis of amber acid device, relate in particular to a kind of electrolyzer of large-scale industrial production Succinic Acid.
Background technology
Succinic Acid is a kind of important synthesis intermediates and food-flavoring comps.Be widely used in fields such as medicine, agricultural chemicals, fine chemistry industry, Synolac, in recent years, Succinic Acid is obtained widespread use in fields such as biological degradation plastics poly butylene succinate (PBS) organic coatings.
It is the electrolytic oxidation of raw material that the main method of industrial preparation Succinic Acid has maleic acid catalytic reduction method, succinonitrile hydrolysis method, cis-butenedioic anhydride electrolytic reduction and ethene and carbon monoxide, wherein electrolytic process is the main method of producing Succinic Acid at present, but the electrolyzer of current electrolysis synthesizing succinic acid generally adopts the acyclic type device, and there is following shortcoming in such:
(1) electrolyzer and number of electrodes are many, and the electrode investment is big, is difficult for extensive electrolysis;
When (2) large-current electric is separated, electrode connection request height, line drop height, power consumption increase.
Summary of the invention
Big for the investment of the electrolytic synthesis of amber acid acyclic type device that overcomes, be difficult for extensive electrolysis, deficiency that power consumption is high, the invention provides a kind of bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid of saving investment, suitable extensive electrolysis, cutting down the consumption of energy.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid, fluid distribution inlet pipe that comprise electrolyzer, is communicated with and fluid collecting pipe with electrolyzer, and constitute round-robin electrolytic solution storage tank, interchanger and header tank with electrolyzer; Described header tank is communicated with the fluid distribution inlet pipe, described fluid remittance abroad pipe coupling electrolytic solution storage tank, described device for synthesizing succinic acid also comprises the multipole type electrode that is installed in the electrolyzer, described multipole type electrode is tabular, between two adjacent multipole type electrodes is unit groove, each unit groove is provided with electrolytic solution import and electrolyte outlet, each electrolytic solution import connects the fluid distribution inlet pipe, each electrolyte outlet connects the fluid collecting pipe, and the multipole type electrode at electrolyzer two ends connects the positive pole and the negative pole of power supply respectively.
As preferred a kind of scheme: the front/rear end of described electrolyzer and the cell wall of bottom surface have groove, and described multipole type electrode inserts in the groove.
Further, described multipole type electrode is a slab construction.
Perhaps, described multipole type electrode is the foam type sheet structure, and its anode sides is provided with the plumbic oxide coating, and its cathode side is provided with paste lead powder coated side and is provided with prismatic or strip bulge.
Further, the side of described multipole type electrode is provided with prismatic or strip bulge.
Described multipole type electrode is the lead alloy electrode, and alloying constituent is a multicomponent lead alloy, and its expression formula is Pb
1-x-y-zSb
xAg
yM
z, M=Cu wherein, Sn, Cd, Fe, Ti, Re, Co or Ni, x=0～0.15; Y=0～0.05; Z=0～0.01, wherein x, y, z are atomic ratio.
As preferred another scheme: described header tank connects and is used to control the flow of each unit groove and the fluid of fluid pressure balance distributes control device, and described fluid distributes control device to connect the fluid distribution inlet pipe.
Further, described fluid distributes control device to be provided with valve, also can adopt the valveless structure.
Described unit groove is 1～200 group.Series connection mutually between each unit groove.
The pipeline of described electrolytic solution storage tank and header tank is provided with transferpump, is provided with water cooler in the conduit entrance of header tank.
Technical conceive of the present invention is: the integral type cell construction that adopts the band groove, the both sides of electrolyzer and bottom cell wall have groove, a plurality of multipole type lead alloy electrodes insert groove, as dividing plate electrolyzer is divided into several unit grooves, divide electrolytic solution import and electrolyte outlet in each unit groove, the electrolytic solution import is connected fluid distribution inlet pipe and fluid collecting pipe respectively with electrolyte outlet.
Described electrolytic solution can be joined control device by the fluid distribution inlet pipe and is dispensed to each unit groove, and each unit groove electrolytic solution to the fluid collecting pipe, connects electrolytic solution storage tank, interchanger and header tank through electrolyte outlet, constitutes circulation.
Described multipole type electrode is combined into one anode and negative electrode, and both as reaction electrode, again as the dividing plate between the electrolyzer monomer, electrode no longer needs the connection by other any way when installing.Further, electrode is slab construction or foam type sheet structure, electrode surface can have the projection of prismatic, bar shaped or other shape, or employing paste lead powder full-filling (cathode plane) of foam type electrode both sides and titanium dioxide lead powder full-filling (anode surface), to increase electrode surface area.
Multipole type electrode, its alloying constituent are multicomponent lead alloy, and its expression formula is Pb
1-x-y-zSb
xAg
yM
z, M=Cu wherein, Sn, Cd, Fe, Ti, Re (rare earth), Co, Ni etc., x=0～0.15; Y=0～0.05; Z=0～0.01 (x, y, z are atomic ratio);
Described fluid distributes control device to be provided with valve or valveless structure, can control the flow and the fluid pressure balance of each unit groove.
The present invention is directed to the shortcoming of above electrolytic synthesis of amber acid acyclic type electrolyzer, with the lead alloy plate is electrode, adopts sheet frame multipole type electrolyzer electrolytic synthesis of amber acid, has saved the electrode investment, reducing power consumption, is a kind of electrolyzer of extensive electrolytic synthesis of amber acid.
Beneficial effect of the present invention mainly shows: 1, adopt the multipole type structure, the lead alloy electrode as the dividing plate between the electrolyzer monomer, has been simplified connection again both as reaction electrode, has reduced power consumption, has improved process safety; 2, electrode utilization ratio height, long service life, easy realization of large-scale production, the technology non-wastewater discharge is a kind of industrial electro synthesizing succinic acid technology of green; 3, compact construction is attractive in appearance, and floor space is little, and investment reduces significantly; Particularly have the product purity height, bath voltage is low, is the electrolyzer that a kind of energy is suitable for different scales suitability for industrialized production Succinic Acid, has good versatility.
Description of drawings
Fig. 1 is an electrolyzer cell body synoptic diagram of the present invention.
Fig. 2 is the schematic cross-section of Fig. 1.
Fig. 3 is an electrolysis process synoptic diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing the present invention is further described.
With reference to Fig. 1～Fig. 3, a kind of bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid, comprise electrolyzer 1, fluid distribution inlet pipe 8 that is communicated with electrolyzer 1 and fluid collecting pipe 7, and constitute round-robin electrolytic solution storage tank 9 with electrolyzer, interchanger and header tank 10, described header tank 10 is communicated with fluid distribution inlet pipe 8, described fluid remittance abroad pipe 7 connects electrolytic solution storage tank 9, described device for synthesizing succinic acid also comprises the multipole type electrode 4 that is installed in the electrolyzer, described multipole type electrode 4 is tabular, between two adjacent multipole type electrodes 4 is unit groove, each unit groove is provided with electrolytic solution import 5 and electrolyte outlet 6, each electrolytic solution import 5 connects fluid distribution inlet pipe 8, each electrolyte outlet 6 connects fluid collecting pipe 7, and the multipole type electrode 4 at the two ends of described electrolyzer 1 connects the positive pole 2 and the negative pole 3 of direct supply respectively.
Described multipole type is divided into several unit grooves not only as electrode but also as dividing plate with electrolyzer.The front/rear end of described electrolyzer 1 and the cell wall of bottom surface have groove, and described multipole type electrode 4 inserts in the groove.Described multipole type electrode 4 is a slab construction.Perhaps, described multipole type electrode 4 is the foam type sheet structure, and its anode sides is provided with the plumbic oxide coating, and its cathode side is provided with paste lead powder coating.The side of described multipole type electrode 4 is provided with prismatic or strip bulge.Described multipole type electrode 4 is the lead alloy electrode, and alloying constituent is a multicomponent lead alloy, and its expression formula is Pb
1-x-y-zSb
xAg
yM
z, M=Cu wherein, Sn, Cd, Fe, Ti, Re, Co or Ni, x=0～0.15; Y=0～0.05; Z=0～0.01, wherein x, y, z are atomic ratio.
Described header tank 10 connects and is used to control the flow of each unit groove and the fluid distribution control device of fluid pressure balance, and described fluid distributes control device to connect fluid distribution inlet pipe 8.Fluid distributes control device to be provided with valve, also can adopt the valveless structure.Described unit groove is 1～200 group.Series connection mutually between each unit groove.Described electrolytic solution storage tank 9 is provided with transferpump with the pipeline of header tank 10, is provided with water cooler in the conduit entrance of header tank.
In the present embodiment, comprise the electrolyzer 1 that is in series by 40 groups of unit grooves, comprise compositions such as lead alloy multipole type electrode 4 (Pb-0.05Sb-0.0075Ag electrode), electrolytic solution import 5, electrolyte outlet 6, fluid distribution inlet pipe 8, fluid collecting pipe 7.Described electrolytic solution is defeated through supercooler by pump by electrolytic solution storage tank 9, deliver to header tank 10, the electrolytic solution of header tank distributes control device to be dispensed to each unit groove by fluid, each unit groove electrolytic solution is confluxed to the fluid collecting pipe by outlet through after the electrolytic reaction, and the fluid collecting pipe connects electrolytic solution storage tank 10.Water cooler can be controlled electrolyte temperature.
When the Succinic Acid electrolysis production, in the electrolytic solution storage tank saturated Succinic Acid mother liquor 3000L (sulfuric acid of 5-10%), constitute circulation by pump delivery to header tank; Disposable adding MALEIC ANHYDRIDE 300kg when electrolysis begins, be delivered to header tank and water cooler by recycle pump, be delivered to fluid distribution inlet pipe 8 again, behind electrolytic reduction on the multipole type electrode 4, electrolytic solution after the electrolysis confluxes to fluid through electrolyte outlet 6 and confluxes 7, flows into electrolytic solution storage tank 9 again.At electrolyte temperature is 50-60 ℃, and current density is 100-800A/m
2Condition under electrolysis.After electrolysis finished, electrolytic solution was through decolouring, crystallisation by cooling 4-24 hour, filtered, drying obtains colourless Succinic Acid crystal 3 29kg.Fusing point 184.3-186.1 ℃, bath voltage 2.5-3.0V, electrolysis unit consumption 911.8kg cis-butenedioic anhydride/ton Succinic Acid, current efficiency 91.2%.
With reference to Fig. 1～Fig. 3, the unit groove of present embodiment is 90 groups, adopts lead alloy multipole type electrode 4 (Pb-0.05Sb-0.01Ag).The saturated mother liquor 6000L of Succinic Acid (sulfuric acid of 5-10%) constitutes circulation by pump delivery to header tank; Disposable adding MALEIC ANHYDRIDE 600kg when electrolysis begins, be delivered to header tank and water cooler by recycle pump, be delivered to fluid distribution inlet pipe 8 again, behind electrolytic reduction on the multipole type electrode 4, electrolytic solution after the electrolysis confluxes to fluid through electrolyte outlet 6 and confluxes 7, flows into the electrolytic solution storage tank again.At electrolyte temperature is 50-60 ℃, and current density is 300-500A/m
2Condition under electrolysis.After electrolysis finished, electrolytic solution was through decolouring, crystallisation by cooling 4-6 hour, filtered, drying obtains colourless Succinic Acid crystal 6 65kg.Fusing point 184.8-186.4 ℃, bath voltage 2.4-3.2V, electrolysis unit consumption 902.2kg cis-butenedioic anhydride/ton Succinic Acid, current efficiency 90.6%.
Other structures of present embodiment are identical with embodiment 1.
With reference to Fig. 1～Fig. 3, the unit groove of present embodiment is 40 groups, adopts lead alloy multipole type electrode 4 (Pb-0.05Sb-0.0075Ag-0.01Cu), and paste lead powder full-filling (cathode plane) and titanium dioxide lead powder full-filling (anode surface) are adopted in the electrode both sides.When the Succinic Acid electrolysis production, in the electrolytic solution storage tank saturated Succinic Acid mother liquor 3000L (sulfuric acid of 5-10%), constitute circulation by pump delivery to header tank; Disposable adding MALEIC ANHYDRIDE 300kg when electrolysis begins, be delivered to header tank and water cooler by recycle pump, be delivered to fluid distribution inlet pipe 8 again, be coated with on the cream electrode 4 behind the electrolytic reduction at lead alloy, electrolytic solution after the electrolysis confluxes to fluid through electrolyte outlet 6 and confluxes 7, flows into the electrolytic solution storage tank again.At electrolyte temperature is 50-60 ℃, and current density is 100-800A/m
2Condition under electrolysis.After electrolysis finished, electrolytic solution was through decolouring, crystallisation by cooling 4-24 hour, filtered, drying obtains colourless Succinic Acid crystal 3 28kg.Fusing point 185.0-186.1 ℃, bath voltage 2.3-3.0V, electrolysis unit consumption 897.3kg cis-butenedioic anhydride/ton Succinic Acid, current efficiency 92.4%.
Other structures of present embodiment are identical with embodiment 1.
Claims (9)
1. a bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid comprises electrolyzer, and constitutes round-robin electrolytic solution storage tank, interchanger and header tank with electrolyzer; Described device for synthesizing succinic acid also comprises the multipole type electrode, described multipole type electrode is tabular, the side of described multipole type electrode is respectively anode, negative electrode, between two adjacent multipole type electrodes is unit groove, the multipole type electrode at electrolyzer two ends connects the positive pole and the negative pole of power supply respectively, described each unit groove is provided with electrolytic solution import and electrolyte outlet, and each electrolytic solution import connects the fluid distribution inlet pipe, and each electrolyte outlet connects the fluid collecting pipe; It is characterized in that: described device for synthesizing succinic acid also comprises fluid distribution inlet pipe and the fluid collecting pipe that is communicated with electrolyzer, described header tank is communicated with the fluid distribution inlet pipe, described fluid remittance abroad pipe coupling electrolytic solution storage tank, described header tank connects and is used to control the flow of each unit groove and the fluid distribution control device of fluid pressure balance, and described fluid distributes control device to connect the fluid distribution inlet pipe.
2. bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid as claimed in claim 1 is characterized in that: the front/rear end of described electrolyzer and the cell wall of bottom surface have groove, and described multipole type electrode inserts in the groove.
3. bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid as claimed in claim 2 is characterized in that: described multipole type electrode is a slab construction.
4. bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid as claimed in claim 2, it is characterized in that: described multipole type electrode is the foam type sheet structure, its anode sides is provided with the plumbic oxide coating, and its cathode side is provided with paste lead powder coated side and is provided with prismatic or strip bulge.
5. as the described bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid of one of claim 1-4, it is characterized in that: the side of described multipole type electrode is provided with prismatic or strip bulge.
6. bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid as claimed in claim 5 is characterized in that: described multipole type electrode is the lead alloy electrode, and alloying constituent is a multicomponent lead alloy, and its expression formula is Pb
1-x-y-zSb
xAg
yM
z, M=Cu wherein, Sn, Cd, Fe, Ti, Re, Co or Ni, x=0～0.15; Y=0～0.05; Z=0～0.01, wherein x, y, z are atomic ratio.
7. as the described bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid of one of claim 1-4, it is characterized in that: described fluid distributes control device to be provided with valve or valveless.
8. bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid as claimed in claim 7 is characterized in that: described unit groove is 1～200 group.
9. as the described bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid of one of claim 1-4, it is characterized in that: the pipeline of described electrolytic solution storage tank and header tank is provided with transferpump, is provided with water cooler in the conduit entrance of header tank.
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| CN2007100712059A CN101187034B (en) | 2007-09-06 | 2007-09-06 | Bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid |
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| CN2007100712059A CN101187034B (en) | 2007-09-06 | 2007-09-06 | Bipolar type diaphragm-free type electrolysis device for synthesizing succinic acid |
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| CN101187034B true CN101187034B (en) | 2010-12-08 |
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| CN102021604B (en) * | 2010-10-15 | 2012-07-25 | 福建师范大学 | Method for preparing succinic acid based on alloy wire mesh-bipolar film combined electrode technology |
| CN102691070A (en) * | 2011-03-22 | 2012-09-26 | 王惟华 | Energy-efficient series electrolytic device with electrolyte circulation outlet and inlet isolated slots |
| CN103374732A (en) * | 2012-04-11 | 2013-10-30 | 王惟华 | Anode scrap-free tandem electrolyzing device with anode material storing box |
| CN103233242B (en) * | 2013-03-30 | 2016-04-13 | 浙江工业大学 | A kind of DSA/ lead alloy combined electrode and its preparation method and application |
| CN104947138B (en) * | 2015-05-19 | 2017-04-12 | 浙江工业大学 | Method for electrolytic synthesis of butanedioic acid and fixed bed electrochemical reaction device |
| CN110818028A (en) * | 2018-08-08 | 2020-02-21 | 江阴顶立环保科技有限公司 | Three-dimensional electrolytic catalytic oxidation device |
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| CN2651267Y (en) * | 2003-11-04 | 2004-10-27 | 马世金 | Non-diaphragm continuous electrolytic succinic acid producing apparatus |
| CN201087216Y (en) * | 2007-09-06 | 2008-07-16 | 浙江工业大学 | Complex pole type non diaphragm device for electrolysis synthesizing succinic acid |
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2007
- 2007-09-06 CN CN2007100712059A patent/CN101187034B/en not_active Expired - Fee Related
Patent Citations (4)
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| EP1036874A2 (en) * | 1999-03-14 | 2000-09-20 | C.S.E.M. Centre Suisse D'electronique Et De Microtechnique Sa | Cell for bleaching and disinfecting and use of this cell in laundry washing machines |
| CN2517752Y (en) * | 2002-01-11 | 2002-10-23 | 孙金和 | Synthetized butanedioic acid bipolar type electrolyzer |
| CN2651267Y (en) * | 2003-11-04 | 2004-10-27 | 马世金 | Non-diaphragm continuous electrolytic succinic acid producing apparatus |
| CN201087216Y (en) * | 2007-09-06 | 2008-07-16 | 浙江工业大学 | Complex pole type non diaphragm device for electrolysis synthesizing succinic acid |
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