CN102002725B - Bipolar membrane device for producing gluconic acid - Google Patents
Bipolar membrane device for producing gluconic acid Download PDFInfo
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- CN102002725B CN102002725B CN2010102984524A CN201010298452A CN102002725B CN 102002725 B CN102002725 B CN 102002725B CN 2010102984524 A CN2010102984524 A CN 2010102984524A CN 201010298452 A CN201010298452 A CN 201010298452A CN 102002725 B CN102002725 B CN 102002725B
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Abstract
The invention discloses a mechanical device, and in particular relates to a device for producing gluconic acid. The device comprises a clamping steel plate, a polar liquid flow channel plate, a platinum electrode, a bipolar membrane, an elastic partition plate, a hydroxyl difficult penetrating homogeneous phase cationic membrane, and the like, wherein the electrode adopts a titanium alloy or platinum electrode with higher efficiency; an elastic coating is coated on the elastic partition plate for sealing; a material liquid inlet, a material liquid outlet, a sodium hydroxide liquid outlet and a sodium hydroxide inlet are arranged on the clamping steel plate, which is beneficial to the safety in the transportation process; and a liquid guide hole is improved and adopts an elliptic liquid guide hole. The invention has the advantages of high yield, no pollution, low running cost, convenience for transportation, and the like and can be widely applied to a glucose producing enterprise.
Description
Technical field
The present invention relates to a kind of mechanism, specifically be meant a kind of device that is used to produce glucono-.
Technical background
Gluconic acid derivatives is the material that is obtained through certain combination reaction by glucono-.Gluconic acid derivatives series product such as Zinc Gluconate, Ferrous Gluconate, copper gluconate, glucono delta lactone or the like are one type of of great value products, are foodstuff additive and the nutrition accessory agents harmless, effective, safe, necessary fully to human body.The main products of its verivate has obtained using comparatively widely at industrial circles such as medicine food, chemical industry, buildings.
Over 20 years, China's gluconic acid derivatives Application and Development has obtained significant achievement, and Products Development is more and more faster, and large-tonnage product has been walked out the gateway of a country.At present, domestic gluconic acid derivatives develops into present many kinds from more single kind of past, and scale has developed into the level of 260,000 tons of present annual outputs from lower last kiloton YO of past.If produce the present traditional processing technology of glucono-replacement to bipolar embrane method, will be in energy-saving and emission-reduction, produce unusual effect aspect reducing production costs, improving the quality of products.Because the exploitation of domestic production to Bipolar Membrane, related device relatively lags behind always, cause this technology to fail effectively to promote.
Bipolar Membrane is a kind of ion-exchange membrane with specific function, and water decomposition takes place in its middle layer under electric field action, produces H+ and OH
-Ion.And the bipolar membrane electrodialysis technology is compound to this specific function in the common electrical dialysis exactly, thereby can realize the production/regeneration of instant acid/alkali, perhaps acidifying and/or alkalization.The bipolar membrane electrodialysis technology is applied to not only can realize the conversion of Sunmorl N 60S in traditional glucono-production process, and the NaOH that produces can be back to the catalyzed oxidation of glucose.Like this then spent acid that can reduce greatly in the ion exchange resin regeneration process pollutes, and realizes the technology internal recycle of material, improves the quality of glucono-product and reduces production costs, and this significantly is superior to existing glucono-production technique.
Though the method that the Bipolar Membrane legal system is equipped with glucono-someone for a long time proposes, also do many researchs, and obtained many achievements, up to the present, domestic also do not have to be used for the Bipolar Membrane equipment that glucono-is produced.Its reason is exactly that many researchists have only carried out experimental study and PREPARATIOM OF BIPOLAR MEMBRANE to this method, the appliance arrangement of bipolar embrane method production glucono-is not developed.
The objective of the invention is to fill up the at present domestic manufacturing technology that does not also have to be used to produce the bipolar devices of glucono-.If the at present domestic Bipolar Membrane device that is used for laboratory test directly amplifies, can exist: 1 running current density is too little, generally is not more than 400A/m
2, can't use big electric current operation, make the device membrane area that equates treatment capacity excessive; The solution of feed liquid chambers 2 and sodium hydroxide chamber is gone here and there each other Lou and is directed at shortcomings such as current efficiency is too low, grape acid product transformation efficiency is low excessively, concentration caustic lye of soda is low excessively, energy consumption is too big; 3 do not select the difficult homogeneous phase anode membrane that sees through of suitable hydroxide radical for use, and the concentration of caustic lye of soda can't be improved, and the glucono-that also makes sodium hydroxide see through anode membrane and generation neutralizes again and makes operational efficiency low; 4 dividing plates selected for use only are applicable to heterogeneous membrane, directly are used for the Bipolar Membrane device, can cause interior leakage, leak outside; The loss of 5 glucono-s is too high, and the glucose acid group can see through Bipolar Membrane or anode membrane to the sodium hydroxide chamber, thus the loss of formation glucono-.
We are to above present situation; On the basis of forefathers' research,, series of studies and exploitation have been carried out to the particular requirement of Bipolar Membrane production equipment; Through many-sided experimental study; Finally developed have leak in anti-with anti-ly leak outside, anti-creeping Bipolar Membrane is at a distance from analysing, and fully solved the disturbing influence of many externalitiess, the accuracy of warranty test data and repeatability; On this basis; Produce the requirement of glucono-according to bipolar embrane method; Continuation to Bipolar Membrane, one pole anode membrane, electrode, gripping unit, heat sink, runner design, current density, flow velocity is studied and optimize, finally develop to be used for the large-scale Bipolar Membrane device that glucono-is produced.
Summary of the invention
The present invention is directed to deficiency of the prior art, a kind of manufacturing technology that existing Bipolar Membrane device can not be realized glucono-economy, batch process that overcomes is provided.Can carry out the operating parameter of the bipolar embrane method production glucono-of economy, environmental protection.
The present invention is achieved through following technical proposals:
A kind of Bipolar Membrane device of producing glucono-; It comprises clamping steel plate, utmost point flow guidance tape, platinum electrode, elastic baffle, homogeneous phase anode membrane; Bipolar Membrane, holding bolt, liquor inlet, utmost point flow guidance tape, anode terminal, cathode terminal, circular delivery hole, net septum cordis net; It is characterized in that
Cathode terminal is vertical with negative electrode to be welded, and anode terminal is vertical with anode to be welded; Between negative electrode and anode, form a membrane stack space;
In the membrane stack space, place the film group, being placed as of film group: homogeneous phase anode membrane, elastic baffle, Bipolar Membrane, elastic baffle are arranged in order; Film group in the membrane stack space is 1～500 group; Between diaphragm, be placed with net septum cordis net; On the frame of elastic baffle, have half elliptic delivery hole and runner, oval delivery hole, utmost point liquid delivery hole; The two-layer homogeneous phase anode membrane that is of the outermost of membrane stack promptly after the installation of film group, adds one deck homogeneous phase anode membrane again;
Some groups of film groups are clamped by a pair of utmost point flow guidance tape; Anolyte import, catholyte import, anolyte outlet, catholyte outlet are arranged on utmost point flow guidance tape; Outside at utmost point flow guidance tape is clamped, fixes through holding bolt by a pair of clamping steel plate;
Anode terminal, cathode terminal lay respectively at the middle position that clamps steel plate;
Liquor inlet, material liquid outlet, caustic lye of soda outlet, caustic lye of soda import are arranged on the clamping steel plate.
As preferably, the electrode described in the above-mentioned Bipolar Membrane device is the pure titanium of 1～3 mm thick, or electroplates the platinum layer of 1～5 micron thick on the titanium alloy substrate, or the platinum plate.
As preferably, the anode terminal in the above-mentioned Bipolar Membrane device, cathode terminal adopt the titanium screw mandrel of direct 14～24mm to be vertically welded on the diagonal lines mid point of the electrode back side respectively.As better selection, have a terminal stud duct on titanium screw mandrel top.
As preferably; Be coated with one deck elastic coating on the elastic baffle in the above-mentioned Bipolar Membrane device, elastic coating is with one or more materials in silicon rubber type, liquid polysulfide rubber type, urethanes type, acrylic elastomer type, viton type, polyisobutylene rubber, flexible PVC, the elastic epoxy glue.
The present invention is directed to the problem that running current density can not improve, from improving electrode performance, reduce the terminal stud contact resistance, carrying out aspect such as electrode sealing and improve current density.Electroplate the platinum layer of 1-5 micron thick among the present invention on the pure titanium of preferred 1-3 mm thick or the titanium alloy substrate; Adopt the titanium screw mandrel of M14-M24 to be vertically welded on the diagonal lines mid point of the titanium electrode back side; Make distribution of current more even, utmost point flow guidance tape is passed outwardly in the other end, and outwardly one; Make a call to a dark endoporus and be used for external connection, reduce the contact resistance of wiring for the M6 of 10-20 millimeters deep or M8; Sealing between electrode and the utmost point flow guidance tape adopts resilient silicone glue or elastic epoxy glue to seal, and stops the leakage of utmost point liquid.Thereby can make the electric current of operation significantly bring up to 1000A/m
2More than.Device membrane area in same treatment greatly lowers, and is the 1/2-1/4 of the membrane area of common current density, reduces the cost of investment of device greatly.
Utmost point liquid draining plate of the present invention adopts the side utmost point liquid of coming in and going out, and anode and cathode liquid is circulation separately separately, and 6 utmost point liquid delivery holes are adopted on every limit, make the utmost point flow of electrode surface moving more even, effectively reduce the voltage loss of electrode surface.
The rapid-acting coupling of materials processeds such as the corrosion resistant acetate that contracts, tetrafluoro is adopted in the import and export of feed liquid of the present invention and the import and export of caustic lye of soda; Water pipe adopts the PE flexible pipe of health level; Do not influencing under the flow rate conditions, effectively raising the convenience that corrosion resistance and membrane stack are installed, transported.
The present invention is directed to the shortcoming that present Bipolar Membrane device feed liquid chamber is gone here and there each other Lou, leaked outside, leaks electricity, adopted Bipolar Membrane dedicated elas-tic dividing plate, this dividing plate is on the basis at the elastic baffle of patent 200920201823.5; Delivery hole is improved, adopted oval delivery hole, thereby do not reducing under the efficient situation of film; Increase the flow of delivery hole; Also make the runner number of each delivery hole more, can reach the 8-10 road, each width of flow path is 0.15-0.25mm; 3-4 delivery hole used on every limit, like this more than the surface current scooter 10cm/s that makes film under the situation of pressure less than 0.1MPa.And the top coat to dividing plate has carried out modification, in coating formula, adds softening agent, like soft PVC, silica gel etc., make this dividing plate can be used in large-scale Bipolar Membrane device, and its sealing effectiveness is not worse than dingus.
The present invention is directed to Bipolar Membrane and produce the characteristics of glucono-; Adopted the difficult homogeneous membrane that sees through of hydroxide radical, like commercialization homogeneous phase anode membranes such as CSV, HSV, CSO, common relatively homogeneous phase anode membrane; It is higher to the rate that stops hydroxy, makes the concentration of sodium hydroxide chamber higher, the rate of loss of glucono-is lower.
The present invention adopts two compartment mounting means to make the preparation membrane stack of glucono-.The glucono-radical ion will see through cavity block in the three compartment bipolar membrane electrodialysis processes; Because the radius of glucono-radical ion is excessive, excessive through the resistance of cavity block, water temperature rise is very fast in the process of the test; Cavity block distortion is also relatively more serious, only in current density less than 300A/m
2The time film distortion just not obvious.Though so three compartment bipolar membrane electrodialysis have the advantage of separating glucose,, have that membrane lifetime is too short, the film cost is high, test conditions shortcoming rambunctious with respect to two compartments.Therefore the present invention adopts the membrane stack array mode of two compartments.
Among the present invention, individual film is of a size of 400*800mm or 550*1100mm, and the effective film area of single membrane stack can reach 60m
2Or 120m
2, the throughput for preparing 40% glucono-can reach 20 ton per days or 40 ton per days.Operational conditions is that the concentration of Sunmorl N 60S feed concentration 5-40%, sodium hydroxide chamber can reach 2-15%, current density 300-1000A/cm
2, film surface velocity 3-15cm/s, feed pressure be that 0.06-0.12MPa, pipe flow speed are that 0.5-1.5m/s, delivery hole flow velocity are 0.3-0.7m/s, through trouble free operation more than 500 hours.Its current efficiency 85-95%, glucono-transformation efficiency are more than 98.5%, and the relieving haperacidity energy consumption is lower than the acid of 400 degree/tons, and the integrated operation cost is far below traditional technology.
Beneficial effect: Bipolar Membrane device involved in the present invention is used to produce glucono-; The transformation efficiency that can make Sunmorl N 60S is more than 98.5%, current efficiency reaches more than 88%, the relieving haperacidity energy consumption is lower than 400 degree/tons, sour production cost far below traditional technology, no spent acid and salkali waste discharge, the alkali of output can circulate and be used for the production of Sunmorl N 60S; Realize favorable economic benefit and social benefit; And damaging can not appear in processes such as transportation, installation in device; Even there are parts that damage is arranged; Also change easily, and traditional device the damage that the parts damages meeting causes whole device occurs because the layout of material liquid outlet, caustic lye of soda outlet is unreasonable in transportation.
Description of drawings
The principle schematic of Fig. 1 Bipolar Membrane device
Fig. 2 Bipolar Membrane device schematic cross-section
Fig. 3 Bipolar Membrane device side schematic view
Fig. 4 elastic baffle, net septum cordis net assembly structure synoptic diagram
Fig. 5 electrode, clamping steel plate assembly structure synoptic diagram
Fig. 6 the present invention is process flow sheet in process of production
Fig. 7 tradition method is produced the process flow sheet of glucono-
1; Anolyte import 2; Homogeneous phase anode membrane 3; Elastic baffle 4; Bipolar Membrane 5; Catholyte import 6; Holding bolt 7; Liquor inlet 8; Utmost point flow guidance tape 9; Anode terminal 10; Clamp steel plate 11; Material liquid outlet 12; Caustic lye of soda outlet 13; Cathode terminal 14; Caustic lye of soda import 15; Frame 16; Half elliptic delivery hole and runner 17; Oval delivery hole 18; Net septum cordis net 19; Elastic coating 20; Utmost point liquid delivery hole 21; Terminal stud duct 22; Electrode 23; Anolyte outlet 24; The catholyte outlet
Embodiment
Below in conjunction with accompanying drawing, enforcement of the present invention is specified:
Press structure shown in Fig. 2, Fig. 3, Fig. 4, Fig. 5; A Bipolar Membrane device is installed; Comprise and clamp steel plate 10, utmost point flow guidance tape 8, electrode 22, elastic baffle 3, homogeneous phase anode membrane 2; Bipolar Membrane 4, holding bolt 6, liquor inlet 7, utmost point flow guidance tape 8, anode terminal 9, cathode terminal 13, oval delivery hole 17, net septum cordis net 18, cathode terminal 13 is connected with negative electrode, and anode terminal 9 is connected with anode; Between negative electrode and anode, form a membrane stack space; In the membrane stack space, place the film group, being placed as of film group: homogeneous phase anode membrane 2, elastic baffle 3, Bipolar Membrane 4, elastic baffle 3, homogeneous phase anode membrane 2 are arranged in order; Between diaphragm, be placed with net septum cordis net 18; On the frame 15 of elastic baffle 3, have half elliptic delivery hole and runner 16, circular delivery hole 17, utmost point liquid delivery hole 20; Some groups of film groups are clamped by a pair of utmost point flow guidance tape 8; Anolyte import 1, catholyte import 5, anolyte outlet 23, catholyte outlet 24 are arranged on utmost point flow guidance tape 8; Outside at utmost point flow guidance tape 8 is clamped, fixes through holding bolt 6 by a pair of clamping steel plate 10; Anode terminal 9, cathode terminal 13 lay respectively at the middle position that clamps steel plate 10; Liquor inlet 7, material liquid outlet 11, caustic lye of soda outlet 12, caustic lye of soda import 14 are arranged on clamping steel plate 10.
Electrode 22 wherein is the pure titanium of 3 mm thick; Anode terminal 9, cathode terminal 13 adopt the titanium screw mandrel of direct 16mm to be vertically welded on electrode 22 back side diagonal lines mid points respectively.Have one 10 millimeters deep on titanium screw mandrel top, directly be the terminal stud duct 21 of 6mm, wherein elastic coating 19 is flexible PVCs, and homogeneous phase anode membrane 2 wherein is the impervious homogeneous phase anode membrane 2 of hydroxide radical.
Adopt the film of 400*800 specification, totally 50 groups, 12.5 squares of effective film areas; Adopt homemade Bipolar Membrane, anode membrane to adopt the HSF film; Block board thickness is 0.7mm, 3 groups arranged side by side of delivery hole, and the runner of each delivery hole is 8 roads; Width of flow path is 0.2mm, Sunmorl N 60S feed concentration 40%, the concentration 15% of sodium hydroxide chamber, current density 1000A/cm
2Constant current operation, film surface velocity 12cm/s, feed pressure are that 0.08MPa, pipe flow speed are that 1.0m/s, delivery hole flow velocity are 0.5m/s, and the membrane stack locking torque is 25 Ns. rice, move 500 hours continuously.In operational process, except feed temperature rising need cooling processing, there are not faults such as leakage, current efficiency decline, voltage rising to occur.Operation result is: glucono-transformation efficiency 99.0%, relieving haperacidity energy consumption are lower than the acid of 385 degree/tons, and 720 yuan/ton of integrated operation costs are far below about 1400 yuan/ton of traditional technologys.
Embodiment 2
Adopt device among the embodiment 1, wherein elastic coating 19 is urethanes type, the film that adopts the 400*800 specification, totally 150 groups; 37.5 squares of effective film areas, electrode 22 are the platinum layer of electroplating 1 micron thick on the 2 mm thick titanium alloy substrates, adopt homemade Bipolar Membrane, anode membrane to adopt the CSO film; Block board thickness is 0.7mm, 3 groups arranged side by side of delivery hole, and the runner of each delivery hole is 8 roads; Width of flow path is 0.2mm, Sunmorl N 60S feed concentration 30%, the concentration 10% of sodium hydroxide chamber, current density 600A/cm
2Constant current operation, film surface velocity 8cm/s, feed pressure are that 0.06MPa, pipe flow speed are that 1.0m/s, delivery hole flow velocity are 0.5m/s, and the membrane stack locking torque is 45 Ns. rice, move 50 hours continuously.In operational process, except feed temperature rising need cooling processing, there are not faults such as leakage, current efficiency decline, voltage rising to occur.Operation result is: glucono-transformation efficiency 99.0%, relieving haperacidity energy consumption are lower than the acid of 370 degree/tons, and 705 yuan/ton of integrated operation costs are far below traditional technology.
Embodiment 3
Adopt the device among the embodiment 1, be coated with one deck silicon rubber type on the elastic baffle 3: the liquid polysulfide rubber type: 2: 1: 0.5 elastic coating of mass ratio 19 is pressed in the blend of flexible PVC elasticity.Adopt the film of 550*1100 specification, totally 50 groups, 25 squares of effective film areas; Electrode 22 is 2 mm thick platinum plates, adopts homemade Bipolar Membrane, anode membrane to adopt the HSF film, and block board thickness is 0.7mm; 4 groups arranged side by side of delivery hole; The runner of each delivery hole is 8 roads, and width of flow path is 0.2mm, Sunmorl N 60S feed concentration 30%, the concentration 10% of sodium hydroxide chamber, current density 600A/cm
2Constant current operation, film surface velocity 9cm/s, feed pressure are that 0.07MPa, pipe flow speed are that 1.0m/s, delivery hole flow velocity are 0.5m/s, and the membrane stack locking torque is 35 Ns. rice, move 50 hours continuously.In operational process, except feed temperature rising need cooling processing, there are not faults such as leakage, current efficiency decline, voltage rising to occur.Operation result is: glucono-transformation efficiency 98.8%, and the acid of relieving haperacidity energy consumption 360 degree/tons, 710 yuan/ton of integrated operation costs are far below traditional technology.
Claims (6)
1. Bipolar Membrane device of producing glucono-; It comprises clamping steel plate (10), utmost point flow guidance tape (8), electrode (22), elastic baffle (3), homogeneous phase anode membrane (2); Bipolar Membrane (4), holding bolt (6), liquor inlet (7), utmost point flow guidance tape (8), anode terminal (9), cathode terminal (13), oval delivery hole (17), net septum cordis net (18); It is characterized in that
Cathode terminal (13) is vertical with negative electrode to be welded, and anode terminal (9) is vertical with anode to be welded; Between negative electrode and anode, form a membrane stack space;
In the membrane stack space, place the film group, being placed as of film group: homogeneous phase anode membrane (2), elastic baffle (3), Bipolar Membrane (4), elastic baffle (3) are arranged in order; Film group in the membrane stack space is 1～500 group; Between diaphragm, be placed with net septum cordis net (18); On the frame (15) of elastic baffle (3), have half elliptic delivery hole and runner (16), oval delivery hole (17), utmost point liquid delivery hole (20); The two-layer homogeneous phase anode membrane (2) that is of the outermost of membrane stack;
Some groups of film groups are clamped by a pair of utmost point flow guidance tape (8); Anolyte import (1), catholyte import (5), anolyte outlet (23), catholyte outlet (24) are arranged on utmost point flow guidance tape (8); Outside at utmost point flow guidance tape (8) is clamped, fixes through holding bolt (6) by a pair of clamping steel plate (10);
Anode terminal (9), cathode terminal (13) lay respectively at the middle position that clamps steel plate (10);
Liquor inlet (7), material liquid outlet (11), caustic lye of soda outlet (12), caustic lye of soda import (14) are arranged on clamping steel plate (10).
2. a kind of Bipolar Membrane device according to claim 1 is characterized in that described electrode (22) is the pure titanium of 1～3 mm thick, or electroplates the platinum layer of 1～5 micron thick on the titanium alloy substrate, or the platinum plate.
3. a kind of Bipolar Membrane device according to claim 1 is characterized in that described anode terminal (9), cathode terminal (13) adopt the titanium screw mandrel of diameter 14～24mm to be vertically welded on the diagonal lines mid point of electrode (22) back side respectively.
4. a kind of Bipolar Membrane device according to claim 3 is characterized in that having one 10～20 millimeters deep, diameter on titanium screw mandrel top the terminal stud duct (21) that is 6～8mm.
5. a kind of Bipolar Membrane device according to claim 1; It is characterized in that being coated with one deck elastic coating (19) on the said elastic baffle (3), elastic coating (19) is with one or more materials in silicon rubber type, liquid polysulfide rubber type, urethanes type, acrylic elastomer type, viton type, polyisobutylene rubber, flexible PVC, the elastic epoxy glue.
6. a kind of Bipolar Membrane device according to claim 1 is characterized in that said homogeneous phase anode membrane (2) is the impervious homogeneous phase anode membrane of hydroxide radical (2).
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103981533A (en) * | 2014-05-30 | 2014-08-13 | 李欣 | Cathode fastening spring bearer plate structure of electrolysis ozonator |
| CN104313633B (en) * | 2014-07-22 | 2016-09-07 | 宜宾丝丽雅集团有限公司 | A kind of Bipolar Membrane method prepares the production technology of gluconic acid |
| CN104328452B (en) * | 2014-07-22 | 2017-02-01 | 宜宾丝丽雅集团有限公司 | Producing technology of gluconic acid through bipolar membrane electrodialysis method |
| CN104445534B (en) * | 2014-12-05 | 2016-06-08 | 杭州水处理技术研究开发中心有限公司 | The homogeneous membrane electrodialysis group device of a kind of band pH regulator |
| CN111118532B (en) * | 2019-11-21 | 2021-12-10 | 华南师范大学 | Method for preparing zinc gluconate based on photo-enhanced fruit fuel cell |
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| FR2729305A1 (en) * | 1995-01-18 | 1996-07-19 | Atochem Elf Sa | REGENERATION OF STRONG ORGANIC ACIDS BY BIPOLAR MEMBRANES |
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| CN1081120A (en) * | 1992-07-09 | 1994-01-26 | 清华大学 | The equipment and technology of preparing organic acid with bipolar film electrodialysis method |
| CN1204549A (en) * | 1997-01-17 | 1999-01-13 | 阿切尔丹尼尔斯密德兰公司 | Electrodialysis apparatus |
| CN201565259U (en) * | 2009-12-07 | 2010-09-01 | 杭州水处理技术研究开发中心有限公司 | Inside and outside leakage-proof and electric leakage-proof bipolar membrane electrodialysis baffle plate |
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