CN108636123A - A kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite - Google Patents
A kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite Download PDFInfo
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- CN108636123A CN108636123A CN201810347574.4A CN201810347574A CN108636123A CN 108636123 A CN108636123 A CN 108636123A CN 201810347574 A CN201810347574 A CN 201810347574A CN 108636123 A CN108636123 A CN 108636123A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/445—Ion-selective electrodialysis with bipolar membranes; Water splitting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
- B01D61/44—Ion-selective electrodialysis
- B01D61/46—Apparatus therefor
- B01D61/48—Apparatus therefor having one or more compartments filled with ion-exchange material, e.g. electrodeionisation
- B01D61/485—Specific features relating to the ion-exchange material
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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
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/165—Hypophosphorous acid; Salts thereof
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Abstract
The invention discloses a kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite, the method is：(1) configuration quality score is the sodium hypophosphite aqueous solution of 10wt%~30wt%；(2) sodium hypophosphite aqueous solution is added in material liquid tank, 3wt% metabisulfite solutions is added into pole flow container, and isometric pure water is added in alkali tank and sour tank；(3) bipolar membrane electrodialysis device is opened, voltage 10V~25V is controlled, control is each 20 DEG C~40 DEG C every indoor reaction temperature, carries out electrodialysis；When no longer being increased by hydrionic content in standard solution of sodium hydroxide Titrable acid room, it is considered as reaction end；(4) it takes the hypophosphorous acid solution in sour tank to carry out condensing crystallizing and obtains hypophosphorous acid crystal.The entire technique of the present invention realizes zero-emission substantially, and the bipolar membrane electrodialysis process provided, which prepares hypophosphorous acid, to be had in high yield, has significant environmental benefit and economic benefit.
Description
Technical field
The present invention relates to the preparation methods of hypophosphorous acid, and in particular to a kind of Bipolar Membrane electricity preparing hypophosphorous acid by sodium hypophosphite
Dialysis method.
Background technology
Hypophosphorous acid (H3PO2), colourless oil liquid, solid state is deliquescent crystallization.It is soluble in hot water, ethyl alcohol, second
Ether.130 DEG C are heated to, orthophosphoric acid and hydrogen phosphide are resolved into, is strong reductant.It can be used for chemical plating in capacitor production,
Catalyst, refrigerant for manufacturing organic reaction also can be used for food processing and produced with fresh-keeping and nickel/hydrogen battery cathode,
It is product critically important in phosphorous chemical industry for pharmaceutical industry etc..
The method of production hypophosphorous acid is mainly electroosmose process and ion-exchange at present, but since hypophosphorous acid has strong reduction
Property so that conventional electrodialysis method energy consumption is excessively high and purity is low；Ion exchange rule process complexity is cumbersome, is not suitable for high-volume
Production.Therefore, it is necessary to find a kind of new and effective method to avoid problem above.
As a result, from above problem, Bipolar Membrane is combined by the present invention with electrodialysis, is made a kind of novel bipolar
Membrane electrodialysis system (BMED), solves the problems such as conventional electrodialysis energy consumption is excessively high and process is cumbersome, and BMED have efficiently,
Green, the advantages that utilization rate is high.Currently, BMED technologies are widely used and develop, can give up such as in environmental protection industry (epi)
Object recycles, and produces food and medicine industry is ascorbic, organic acids and base etc. can be prepared in chemical industry.It can be seen that BMED
The appearance of technology makes each industry of society take on an entirely new look.Therefore, hypophosphorous acid is prepared using bipolar membrane electrodialysis to efficiently avoid time
The oxidation of phosphoric acid, and present invention obtains optimised process working conditions, it is easy to operate pollution-free.
Invention content
The purpose of the present invention is to provide a kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite, entire works
Skill realizes zero-emission substantially, and the bipolar membrane electrodialysis process provided, which prepares hypophosphorous acid, to be had in high yield, has significant ring
Border benefit and economic benefit.
To reach requirements above, technical solution of the present invention is as described below：
A kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite, the method use bipolar membrane electrodialysis
Prepared by device, the bipolar membrane electrodialysis device includes the membrane stack between two pieces of pole plates and two pieces of pole plates, and described two
Block pole plate be respectively the anode plate being connect with DC power anode and the cathode plate being connect with DC power cathode, the membrane stack by
One unit electrodialytic cell composition is composed in series by more than two unit electrodialytic cells, and each unit electrodialytic cell is from sun
Pole to cathode assembling sequence be Bipolar Membrane, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane, and adjacent two films it
Between separated by a partition board；Anode chamber and cathode chamber are constituted between the anode plate and cathode plate and adjacent Bipolar Membrane, often
In a unit electrodialytic cell Bipolar Membrane BM, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane BM be arranged in order constitute sour room,
Feed compartment and alkali room, the anion-exchange membrane be AHA type anion-exchange membranes, the anode chamber, cathode chamber, feed compartment,
Alkali room, sour room are equipped with inlet and liquid outlet；
The anode chamber and cathode chamber distinguish external pole flow container, and the outlet of the pole flow container is by pipeline via cycle
Pump a and valve a is connected with the inlet of anode chamber and cathode chamber respectively, and the liquid outlet of the anode chamber and cathode chamber leads to respectively
Piping is connected to the entrance of pole flow container；
The external material liquid tank of the feed compartment, the outlet of the material liquid tank by pipeline via circulating pump b and valve b with
The inlet of feed compartment is connected, and the outlet of the feed compartment is connected to by pipeline with the entrance of material liquid tank；
The external alkali tank of the alkali room, the outlet of the alkali tank is by pipeline via circulating pump c and valve c and alkali room
Inlet is connected, and the outlet of the alkali room is connected to by pipeline with the entrance of alkali tank；
The external sour tank of the sour room, the outlet of the sour tank is by pipeline via circulating pump d and valve d and sour room
Inlet is connected, and the outlet of the sour room is connected to by pipeline with the entrance of sour tank；
The method is：
(1) configuration quality score is the sodium hypophosphite aqueous solution of 10wt%~30wt%；
(2) the sodium hypophosphite aqueous solution that step (1) obtains is added in the material liquid tank, is added into pole flow container
3wt% metabisulfite solutions, and isometric pure water is added in alkali tank and sour tank；
(3) cathode of the bipolar membrane electrodialysis device is connected with the cathode of DC power supply, anode and DC power supply
Anode be connected, open each compartment circulating pump a, b, c and d, adjust the flow for flowing into each compartment to 20L/h, be then turned on Bipolar Membrane
Electrodialysis plant controls voltage 10V~25V, and control is each 20 DEG C~40 DEG C every indoor reaction temperature, in electrodialytic process
Hypophosphite ion in feed compartment is migrated by anion-exchange membrane to sour room is combined life with the Bipolar Membrane BM hydrogen ions generated
Sodium ion at hypophosphorous acid, while in feed compartment migrates the hydroxyl generated to alkali room and Bipolar Membrane BM through cation-exchange membrane
Ions binding generates sodium hydroxide；When no longer being increased by hydrionic content in standard solution of sodium hydroxide Titrable acid room, depending on
For reaction end；
(4) it takes the hypophosphorous acid solution in sour tank to carry out condensing crystallizing and obtains hypophosphorous acid crystal.
Further, the segment pipe being connect with the inlet of each compartment is placed in ice water, the feed liquid in pipeline is made to obtain
To being fully cooled.
Further, it is circulating coil to be placed in a segment pipe in ice water, being connect with the inlet of each compartment.
Further, the Bipolar Membrane uses FBM type Bipolar Membranes.
Further, the cation-exchange membrane is CMB type cation-exchange membranes.
Further, in step (1), the mass fraction of the sodium hypophosphite aqueous solution of preparation is 15%.
Further, in step (3), voltage 20V is controlled.
Compared with prior art, the beneficial effects of the present invention are：The present invention is by setting bipolar membrane electrodialysis device
Meter (especially to the screening of anion-exchange membrane) and process conditions are groped, and are provided bipolar membrane electrodialysis method and are prepared time phosphorus
The best manufacturing condition of acid, realizes that the high yield of hypophosphorous acid is produced, and by-product sodium hydroxide can be obtained；And it entirely gives birth to
Production. art realizes zero-emission substantially so that the method for the present invention has significant environmental benefit and economic benefit.
Description of the drawings
Fig. 1 is that bipolar membrane electrodialysis produces hypophosphorous acid experiment flow figure；
Fig. 2 is that bipolar membrane electrodialysis produces hypophosphorous acid schematic diagram of device；
Fig. 3 is that bipolar membrane electrodialysis produces hypophosphorous acid membrane stack fundamental diagram.
Specific implementation mode
Technical scheme of the present invention is further detailed with reference to specific example.
With reference to figure 1,2,3, wherein Fig. 3 has only drawn a unit electrodialytic cell, but practical membrane stack group for convenience
At being subject to described in embodiment.
The bipolar membrane electrodialysis device includes the membrane stack between two pieces of pole plates and two pieces of pole plates, described two pieces of pole plates
The anode plate respectively being connect with DC power anode and the cathode plate being connect with DC power cathode, the anode plate and cathode
Plate is all titanium plating ruthenium electrode plate；The membrane stack is composed in series by 5 unit electrodialytic cells, each unit electrodialytic cell from anode to
The assembling sequence of cathode be Bipolar Membrane, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane, and between adjacent two films by
One partition board separates；Wherein the Bipolar Membrane of membrane stack is FBM types Bipolar Membrane (Fuma-Tech Co, Germany), anion-exchange membrane
For AHA types anion-exchange membrane (ASTOM Co, Japan), cation-exchange membrane be CMB types cation-exchange membrane (ASTOM Co,
Japan), single film effective area 189cm2；Anode chamber is constituted between the anode plate and cathode plate and adjacent Bipolar Membrane
And cathode chamber, Bipolar Membrane BM, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane BM are arranged successively in each unit electrodialytic cell
Row constitute sour room, feed compartment and alkali room, the anode chamber, cathode chamber, feed compartment, alkali room, sour room and are equipped with inlet and go out liquid
Mouthful；
The anode chamber and cathode chamber distinguish external pole flow container, and the outlet of the pole flow container is by pipeline via cycle
Pump a and valve a is connected with the inlet of anode chamber and cathode chamber respectively, and the liquid outlet of the anode chamber and cathode chamber leads to respectively
Piping is connected to the entrance of pole flow container；The segment pipe being connect with the inlet of cathode chamber and anode chamber is circulating coil and follows
The ring disk pipe is placed in ice water, and the feed liquid in circulating coil is made to be adequately cooled；
The external material liquid tank of the feed compartment, the outlet of the material liquid tank by pipeline via circulating pump b and valve b with
The inlet of feed compartment is connected, and the outlet of the feed compartment is connected to by pipeline with the entrance of material liquid tank；With feed compartment into
One segment pipe of liquid mouth connection is circulating coil and circulating coil is placed in ice water, so that the feed liquid in circulating coil is obtained fully cold
But；
The external alkali tank of the alkali room, the outlet of the alkali tank is by pipeline via circulating pump c and valve c and alkali room
Inlet is connected, and the outlet of the alkali room is connected to by pipeline with the entrance of alkali tank；One section connect with the inlet of alkali room
Pipeline is circulating coil and circulating coil is placed in ice water, and the feed liquid in circulating coil is made to be adequately cooled；
The external sour tank of the sour room, the outlet of the sour tank is by pipeline via circulating pump d and valve d and sour room
Inlet is connected, and the outlet of the sour room is connected to by pipeline with the entrance of sour tank；One section connect with the inlet of sour room
Pipeline is circulating coil and circulating coil is placed in ice water, and the feed liquid in circulating coil is made to be adequately cooled；
Technical scheme is as follows：
(1) it is pumped into sodium hypophosphite solution in material liquid tank, is pumped into isometric pure water in alkali tank and sour tank, flow container is pumped into pole
3wt% metabisulfite solutions, open water pump after feed liquid start the cycle over, by by circulating coil be placed in ice water to the feed liquid in pipe into
Row is cooling to make feed liquid temperature before entering compartment reach within the scope of 20 DEG C~40 DEG C, opens electrodialysis plant power supply, control is suitable
Voltage, carry out producing for hypophosphorous acid.
(2) determination of experimental endpoints, in feed compartment hypophosphite ion through anion-exchange membrane enter sour room with it is bipolar
The hydrogen ion that film generates, which combines, generates hypophosphorous acid, and sodium ion is migrated through cation-exchange membrane to alkali room, is generated with Bipolar Membrane
Hydroxide ion, which combines, generates sodium hydroxide solution.It is sampled in sour tank, using phenolphthalein as indicator, uses standard solution of sodium hydroxide
Hydrionic content is titrated until when no longer rising, is considered as the arrival of experimental endpoints.
(3) pass through bipolar membrane electrodialysis to convert, hypophosphorous acid solution is generated in sour tank, concentrated crystallization obtains hypophosphorous acid crystalline substance
Body；Sodium hydroxide solution is generated in alkali tank, sodium hydroxide crystal can be made in concentration.
Embodiment 1
The membrane stack for taking FBM/AHA/CMB/FBM to form, is added to material liquid tank by the 15wt% sodium hypophosphite feed liquids of 0.5L, beats
Open cycle pump is pumped into the feed compartment of the bipolar membrane electrodialysis membrane stack of three compartments to 5 groups of 9cm × 21cm sizes, and will
Flow is adjusted to 20L/h；0.5L pure water is added to alkali tank and sour tank respectively, open circulating pump be pumped into membrane stack alkali room and
Flow is also adjusted to 20L/h by sour room；The 3wt% metabisulfite solutions of 0.5L are added to pole flow container, circulating pump is opened and is pumped into
It is run to the pole fluid chamber of membrane stack, and with the flow of 20L/h.DC power supply is opened, control voltage is 10V, reaction in compartment at this time
Temperature is reacted 150 minutes at 21.3 DEG C, and sour room generates hypophosphorous acid, and yield 63.34%, enriched chamber obtains 3.52% hydrogen-oxygen
Change sodium solution, current efficiency 53.78%, energy consumption 4.71kWh/kg.
Embodiment 2
The membrane stack for taking FBM/AHA/CMB/FBM to form adjusts voltage 15V, and compartment interior reaction temperature is 22.6 DEG C at this time,
His condition is same as Example 1, reacts 60 minutes, and sour room generates hypophosphorous acid, and yield 69.58%, enriched chamber obtains 3.80%
Sodium hydroxide solution, current efficiency 57.09%, energy consumption 5.09kWh/kg.
Embodiment 3
The membrane stack for taking FBM/AHA/CMB/FBM to form adjusts voltage 20V, and compartment interior reaction temperature is 23.3 DEG C at this time,
His condition is same as Example 1, reacts 40 minutes, and sour room generates hypophosphorous acid, and yield 80.06%, enriched chamber obtains 3.96%
Sodium hydroxide solution, current efficiency 58.41%, energy consumption 4.99kWh/kg.
Embodiment 4
The membrane stack for taking FBM/AHA/CMB/FBM to form adjusts voltage 25V, and compartment interior reaction temperature is 24.2 DEG C at this time,
His condition is same as Example 1, reacts 50 minutes, and sour room generates hypophosphorous acid, and yield 75.18%, enriched chamber obtains 3.88%
Sodium hydroxide solution, current efficiency 54.25%, energy consumption 6.40kWh/kg.
Embodiment 5
The membrane stack for taking FBM/AHA/CMB/FBM to form, is added to material liquid tank by the 10wt% sodium hypophosphite feed liquids of 0.5L, beats
Open cycle pump is pumped into the feed compartment to the bipolar membrane electrodialysis membrane stack of the double compartment of 5 groups of 9cm × 21cm sizes, and will
Flow is adjusted to 20L/h；0.5L pure water is added to alkali tank and sour tank respectively, open circulating pump be pumped into membrane stack alkali room and
Flow is also adjusted to 20L/h by sour room；The 3wt% metabisulfite solutions of 0.5L are added to pole flow container, circulating pump is opened and is pumped into
It is run to the pole fluid chamber of membrane stack, and with the flow of 20L/h.DC power supply is opened, control voltage is 20V, reaction in compartment at this time
Temperature is 23.1 DEG C, is reacted 40 minutes, and sour room generates hypophosphorous acid, and yield 77.64%, enriched chamber obtains 2.68% hydroxide
Sodium solution, current efficiency 40.96%, energy consumption 4.56kWh/kg.
Embodiment 6
The membrane stack for taking FBM/AHA/CMB/FBM to form, takes the 20wt% sodium hypophosphite feed liquids of 0.5L, reaction in compartment at this time
Temperature is 22.8 DEG C, and other conditions are same as Example 5, is reacted 60 minutes, and sour room generates hypophosphorous acid, and yield 79.90% is dense
Contracting room obtains 5.48% sodium hydroxide solution, current efficiency 60.29%, energy consumption 6.32kWh/kg.
Embodiment 7
The membrane stack for taking FBM/AHA/CMB/FBM to form, takes the 25wt% sodium hypophosphite feed liquids of 0.5L, reaction in compartment at this time
Temperature is 23.0 DEG C, and other conditions are same as Example 5, is reacted 60 minutes, and sour room generates hypophosphorous acid, and yield 77.97% is dense
Contracting room obtains 5.96% sodium hydroxide solution, current efficiency 57.53%, energy consumption 6.61kWh/kg.
Embodiment 8
The membrane stack for taking FBM/AHA/CMB/FBM to form, takes the 25wt% sodium hypophosphite feed liquids of 0.5L, reaction in compartment at this time
Temperature is 22.6 DEG C, and other conditions are same as Example 5, is reacted 70 minutes, and sour room generates hypophosphorous acid, and yield 75.29% is dense
Contracting room obtains 6.28% sodium hydroxide solution, current efficiency 58.68%, energy consumption 7.58kWh/kg.
Comparative example
The membrane stack for taking FBM/pK-5/CMB/FBM to form, anion-exchange membrane uses pK-5 type anion-exchange membranes in membrane stack
(Beijing Tingrun Membrane Technology Development Co., Ltd., China), remaining adds the 15wt% sodium hypophosphite feed liquids of 0.5L with embodiment 3
Enter to material liquid tank, opens circulating pump and be pumped into the bipolar membrane electrodialysis membrane stack to the double compartment of 5 groups of 9cm × 21cm sizes
Feed compartment, and flow is adjusted to 20L/h；0.5L pure water is added to alkali tank and sour tank respectively, circulating pump is opened and is pumped into
To the alkali room and sour room of membrane stack, flow is also adjusted to 20L/h；The 3wt% metabisulfite solutions of 0.5L are added to pole flow container, are opened
Circulating pump is pumped into the pole fluid chamber of membrane stack, and is run with the flow of 20L/h.DC power supply is opened, control voltage is 20V,
Compartment interior reaction temperature is 22.6 DEG C at this time, is reacted 50 minutes, and sour room generates hypophosphorous acid, and yield 76.41%, enriched chamber obtains
4.24% sodium hydroxide solution, current efficiency 53.95%, energy consumption 6.14kWh/kg.
Pass through the comparison of embodiment 3 and comparative example, it is evident that it can be seen that, it is secondary when using pK-5 type anion-exchange membranes
The yield of phosphoric acid drops to 76.41% by original 80.06%, and current efficiency drops to 53.95% by original 58.41%,
Energy consumption but rises to 6.14kWh/kg by original 4.99kWh/kg.When therefore, using AHA type anion-exchange membranes, it can obtain
The hypophosphorous acid of higher yield is obtained, and energy consumption is lower, economic benefit higher.Therefore, it can be seen that AHA types anion-exchange membrane is more
It is suitble to production hypophosphorous acid.
Obviously, embodiments described above is just to clearly express the case that the present invention is lifted, not to this hair
Bright embodiment sets qualifications.For those skilled in the art, can also have on the basis of the present invention
The variation and improvement of other form.It is all using equivalents or to belong to apparent change based on institute's lead-out process scheme of the present invention
It is dynamic to be within protection scope of the present invention.
Claims (8)
1. a kind of bipolar membrane electrodialysis process preparing hypophosphorous acid by sodium hypophosphite, the method is filled using bipolar membrane electrodialysis
It sets and is prepared, the bipolar membrane electrodialysis device includes the membrane stack between two pieces of pole plates and two pieces of pole plates, described two pieces
Pole plate is respectively the anode plate being connect with DC power anode and the cathode plate being connect with DC power cathode, and the membrane stack is by one
A unit electrodialytic cell composition is composed in series by more than two unit electrodialytic cells, and each unit electrodialytic cell is from anode
Assembling sequence to cathode is Bipolar Membrane, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane, and between adjacent two films
It is separated by a partition board；Anode chamber and cathode chamber are constituted between the anode plate and cathode plate and adjacent Bipolar Membrane, each
Bipolar Membrane BM, anion-exchange membrane, cation-exchange membrane, Bipolar Membrane BM, which are arranged in order, in unit electrodialytic cell constitutes sour room, material
Liquid chamber and alkali room, the anion-exchange membrane are AHA type anion-exchange membranes, the anode chamber, cathode chamber, feed compartment, alkali
Room, sour room are equipped with inlet and liquid outlet；
The anode chamber and cathode chamber distinguish external pole flow container, and the outlet of the pole flow container is by pipeline via circulating pump a
It is connected respectively with the inlet of anode chamber and cathode chamber with valve a, the liquid outlet of the anode chamber and cathode chamber passes through respectively
Pipeline is connected to the entrance of pole flow container；
The external material liquid tank of the feed compartment, the outlet of the material liquid tank is by pipeline via circulating pump b and valve b and feed liquid
The inlet of room is connected, and the outlet of the feed compartment is connected to by pipeline with the entrance of material liquid tank；
The outlet of the external alkali tank of the alkali room, the alkali tank passes through feed liquor of the pipeline via circulating pump c and valve c and alkali room
Mouth is connected, and the outlet of the alkali room is connected to by pipeline with the entrance of alkali tank；
The external sour tank of the sour room, the outlet of the sour tank pass through feed liquor of the pipeline via circulating pump d and valve d and sour room
Mouth is connected, and the outlet of the sour room is connected to by pipeline with the entrance of sour tank；
The method is：
(1) configuration quality score is the sodium hypophosphite aqueous solution of 10wt%~30wt%；
(2) the sodium hypophosphite aqueous solution that step (1) obtains is added in the material liquid tank, 3wt% is added into pole flow container
Metabisulfite solution, and isometric pure water is added in alkali tank and sour tank；
(3) cathode of the bipolar membrane electrodialysis device is connected with the cathode of DC power supply, anode and DC power supply are just
Extremely it is connected, opens each compartment circulating pump a, b, c and d, adjusts the flow for flowing into each compartment to 20L/h, be then turned on Bipolar Membrane electric osmose
Analysis apparatus controls voltage 10V~25V, and control is each 20 DEG C~40 DEG C every indoor reaction temperature, feed liquid in electrodialytic process
Hypophosphite ion in room is migrated by anion-exchange membrane is combined generation time to sour room with the Bipolar Membrane BM hydrogen ions generated
Phosphoric acid, while the sodium ion in feed compartment migrates the hydroxide ion generated to alkali room and Bipolar Membrane BM through cation-exchange membrane
In conjunction with generation sodium hydroxide；When no longer being increased by hydrionic content in standard solution of sodium hydroxide Titrable acid room, it is considered as anti-
Answer terminal；
(4) it takes the hypophosphorous acid solution in sour tank to carry out condensing crystallizing and obtains hypophosphorous acid crystal.
2. bipolar membrane electrodialysis process as described in claim 1, it is characterised in that：By what is connect with the inlet of each compartment
One segment pipe is placed in ice water, and the feed liquid in pipeline is made to be adequately cooled.
3. bipolar membrane electrodialysis process as claimed in claim 2, it is characterised in that：It is placed in ice water, with each compartment
One segment pipe of inlet connection is circulating coil.
4. the bipolar membrane electrodialysis process as described in one of claims 1 to 3, it is characterised in that：The Bipolar Membrane uses FBM
Type Bipolar Membrane.
5. the bipolar membrane electrodialysis process as described in one of claims 1 to 3, it is characterised in that：The cation-exchange membrane
For CMB type cation-exchange membranes.
6. bipolar membrane electrodialysis process as claimed in claim 4, it is characterised in that：The cation-exchange membrane is CMB types
Cation-exchange membrane.
7. bipolar membrane electrodialysis process as claimed in claim 6, it is characterised in that：In step (1), the sodium hypophosphite water of preparation
The mass fraction of solution is 15%.
8. bipolar membrane electrodialysis process as claimed in claim 7, it is characterised in that：In step (3), voltage 20V is controlled.
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| CN109336064A (en) * | 2018-11-06 | 2019-02-15 | 宜宾海丝特纤维有限责任公司 | A kind of viscose sodium sulfate waste liquor multi-level handling system |
| CN109589793A (en) * | 2018-12-28 | 2019-04-09 | 浙江蓝极膜技术有限公司 | A kind of bipolar membrane device producing hypophosphorous acid |
| CN109626347A (en) * | 2018-12-20 | 2019-04-16 | 常熟新特化工有限公司 | A kind of technique that bipolar membrane electrodialysis is used for sodium hypophosphite dealkalize |
| CN111138390A (en) * | 2019-12-30 | 2020-05-12 | 杭州蓝然环境技术股份有限公司 | Improved cleaning process for preparing vitamin C by membrane method |
| CN113441009A (en) * | 2021-06-22 | 2021-09-28 | 黑龙江新和成生物科技有限公司 | Vitamin C bipolar membrane acidification production process and device |
| CN114225702A (en) * | 2021-12-20 | 2022-03-25 | 宁夏百川科技有限公司 | Bipolar membrane electrodialysis device for preparing calcium formate and calcium formate preparation method |
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| US5431792A (en) * | 1993-12-20 | 1995-07-11 | Occidental Chemical Corporation | Method of making hypophosphorous acid |
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