CN109809964A - A method of neopentyl glycol is purified using bipolar membrane electrodialysis system - Google Patents
A method of neopentyl glycol is purified using bipolar membrane electrodialysis system Download PDFInfo
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Abstract
The present invention provides a kind of method using bipolar membrane electrodialysis system purification neopentyl glycol, comprising: a, building bipolar membrane electrodialysis system, bipolar membrane electrodialysis system includes membrane stack;Membrane stack includes the cathode plate set gradually, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane and anode plate;And cathode chamber, alkaline chamber, feed compartment, acid compartment and anode chamber are sequentially formed between adjacent component on from cathode plate to anode plate direction in membrane stack;B, the neopentyl glycol solution circulation pump containing sodium formate is entered into feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;Acid compartment solution circulation pump is entered into acid compartment;Electrolyte solution is recycled respectively and is pumped into cathode chamber and anode chamber;C, it opens power supply and carries out electrodialysis, recording voltage and electric current, and detect the conductivity of acid compartment, alkaline chamber, cathode chamber, anode chamber and feed compartment, until cutting off the power after the stable conductivity of feed compartment, obtaining neopentyl glycol.This method can purify neopentyl glycol, and the purity of neopentyl glycol is higher.
Description
Technical field
The invention belongs to electrodialysis purification technique field more particularly to a kind of use bipolar membrane electrodialysis system purifications new penta
The method of glycol.
Background technique
Neopentyl glycol (abbreviation NPG)) it is a kind of typical neopentyl dihydric alcohol, white crystal, soluble easily in water, aromatic hydrocarbon,
It is halogenated etc..NPG is widely used in producing the chemical materials such as powdery paints, photosensitive material polyester resin, polyurethane, it may also be used for
Medicine, agronomy, lubricating oil, plasticizer etc..Wherein mainly for the production of resin, it is prepared at resin there is good stabilization
Property, heat resistance and it is corrosion-resistant the advantages that.
Preparation of industrialization NPG mainly has disproportionation processes and hydrogenation technique in the world at present, and in China, most manufacturers are equal
NPG is produced using disproportionation processes, changes method preparation simple process, but a large amount of byproduct formic acids can be generated while producing NPG
Sodium.NPG is extracted using purified petroleum benzin in the prior art, destilling tower is then reused and separates benzene and NPG, production technology it is complicated and
Energy consumption is very high, causes the production cost of NPG high;In the byproduct formic acid sodium product that the technique produces simultaneously
Containing certain density NPG, cause product quality not high, it is difficult to meet Chemical Manufacture demand.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of sides using bipolar membrane electrodialysis system purification neopentyl glycol
Method, this method can purify neopentyl glycol, and purity is higher.
The present invention provides a kind of methods using bipolar membrane electrodialysis system purification neopentyl glycol, comprising the following steps:
A), bipolar membrane electrodialysis system is constructed, the bipolar membrane electrodialysis system includes membrane stack;
The membrane stack includes the cathode plate set gradually, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane
And anode plate;
And cathode chamber, alkaline chamber, material are sequentially formed between adjacent component on from cathode plate to anode plate direction in the membrane stack
Liquid chamber, acid compartment and anode chamber;
B), the neopentyl glycol solution circulation pump containing sodium formate is entered into feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;It will
Acid compartment solution circulation pump enters acid compartment;Electrolyte solution is recycled respectively and is pumped into cathode chamber and anode chamber;
C), open power supply and carry out electrodialysis, recording voltage and electric current, and detect acid compartment, alkaline chamber, cathode chamber, anode chamber and
The conductivity of feed compartment, until cutting off the power after the stable conductivity of feed compartment, obtaining neopentyl glycol.
Preferably, the model Neosepta BP-1 of the Bipolar Membrane.
Preferably, the model Fumasep FAS-PET-30 of the anion-exchange membrane.
Preferably, the alkaline chamber solution is selected from sodium sulphate, sodium nitrate, potassium sulfate, potassium nitrate, sodium hydroxide solution or originally
Water;
The acid compartment solution is selected from sodium sulphate, sodium nitrate, potassium sulfate, potassium nitrate, formic acid solution or tap water.
Preferably, the electrolyte solution is selected from ammonium sulfate, sodium sulphate, sodium nitrate, potassium sulfate or potassium nitrate.
Preferably, the flow velocity of the neopentyl glycol solution containing sodium formate is not less than 5mL/min.
Preferably, the concentration of sodium formate is not less than 0.1mol/L in the neopentyl glycol solution containing sodium formate.
Preferably, the concentration of sodium formate is 0.4mol/L in the neopentyl glycol solution containing sodium formate.
Preferably, the electrodialytic current density is 10~50mA/cm2。
Preferably, the electrodialytic current density is 30m A/cm2。
The present invention provides a kind of methods using bipolar membrane electrodialysis system purification neopentyl glycol, comprising the following steps:
A), bipolar membrane electrodialysis system is constructed, the bipolar membrane electrodialysis system includes membrane stack;The membrane stack includes the yin set gradually
Pole plate, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane and anode plate;And from cathode plate Zhiyang in the membrane stack
Cathode chamber, alkaline chamber, feed compartment, acid compartment and anode chamber are sequentially formed on pole plate direction between adjacent component;B), sodium formate will be contained
Neopentyl glycol solution circulation pump enter feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;Acid compartment solution circulation pump is entered into acid compartment;It will
Electrolyte solution recycles be pumped into cathode chamber and anode chamber respectively;C), open power supply and carry out electrodialysis, recording voltage and electric current, and
Detect acid compartment, alkaline chamber, cathode chamber, anode chamber and feed compartment conductivity, until feed compartment stable conductivity after, cutting electricity
Source obtains neopentyl glycol.The present invention can purify neopentyl glycol using bipolar membrane electrodialysis system, and the purity of neopentyl glycol compared with
It is high.With traditional benzene extraction process, method of purification provided by the invention is environmentally protective, can be completed without using other chemical reagent
Purify operation;Energy consumption is lower, can significantly reduce production cost;While removing the sodium formate in neopentyl glycol, generate not
Impure formic acid and sodium hydroxide, by-product quality is higher, improves added value of product, on the other hand, formic acid and hydroxide
Sodium is also the required raw material of disproportionation processes production neopentyl glycol, and the endless-chain of technique may be implemented.The results showed that new penta
The purity of glycol is 99% or more;84% or more is obtained in wider sodium formate concentrations and wider current density range
High current efficiency;10~50mA/cm2The lower energy consumption for decomposing sodium formate is 6.1~27.2kWh/kg.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of membrane stack in the bipolar membrane electrodialysis system of the invention used;
Fig. 2 is the current efficiency and energy consumption column schematic diagram of the embodiment of the present invention 1~3;
Fig. 3 is the current efficiency and energy consumption column schematic diagram of the embodiment of the present invention 4~6.
Specific embodiment
The present invention provides a kind of methods using bipolar membrane electrodialysis system purification neopentyl glycol, comprising the following steps:
A), bipolar membrane electrodialysis system is constructed, the bipolar membrane electrodialysis system includes membrane stack;
The membrane stack includes the cathode plate set gradually, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane
And anode plate;
And cathode chamber, alkaline chamber, material are sequentially formed between adjacent component on from cathode plate to anode plate direction in the membrane stack
Liquid chamber, acid compartment and anode chamber;
B), the neopentyl glycol solution circulation pump containing sodium formate is entered into feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;It will
Acid compartment solution circulation pump enters acid compartment;Electrolyte solution is recycled respectively and is pumped into cathode chamber and anode chamber;
C), open power supply and carry out electrodialysis, recording voltage and electric current, and detect acid compartment, alkaline chamber, cathode chamber, anode chamber and
The conductivity of feed compartment, until cutting off the power after the stable conductivity of feed compartment, obtaining neopentyl glycol.
The present invention can purify neopentyl glycol using bipolar membrane electrodialysis system, and the purity of neopentyl glycol is higher.With biography
The benzene extraction process of system, method of purification provided by the invention is environmentally protective, and purification can be completed without using other chemical reagent and make
Industry;Energy consumption is lower, can significantly reduce production cost;While removing the sodium formate in neopentyl glycol, generate free from foreign meter
Formic acid and sodium hydroxide, by-product quality is higher, improve added value of product, on the other hand, formic acid and sodium hydroxide are also
Disproportionation processes produce the required raw material of neopentyl glycol, and the endless-chain of technique may be implemented.
Referring to Fig. 1, Fig. 1 is the structural schematic diagram of membrane stack in the bipolar membrane electrodialysis system of the invention used;Wherein, 1 is
Cathode plate, 2a are Bipolar Membrane, and 3 be cation-exchange membrane, and 4 be anion-exchange membrane, and 2b is Bipolar Membrane, and 5 be anode plate.
The bipolar membrane electrodialysis system further includes that power supply (not shown in figure 1) and liquid circulating apparatus (do not show in Fig. 1
Out);The liquid circulating apparatus includes electrode chamber circulator, alkaline chamber circulator, feed compartment circulator and acid compartment circulation
Device.
The membrane stack includes the cathode plate set gradually, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane
And anode plate;It is denoted as cathode plate-Bipolar Membrane-cation-exchange membrane-anion-exchange membrane-Bipolar Membrane-anode plate;In the present invention
In, the cation-exchange membrane, anion-exchange membrane and Bipolar Membrane can also repeat to be arranged, i.e., membrane stack is cathode plate-Bipolar Membrane-
[cation-exchange membrane-anion-exchange membrane-Bipolar Membrane]nAnode plate, wherein n is the natural number greater than 1.
During bipolar membrane electrodialysis system works, by feed compartment circulator by the neopentyl glycol containing sodium formate
Solution circulation pump enters feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber by alkaline chamber circulator;It will by acid compartment circulator
Acid compartment solution circulation pump enters acid compartment;Electrolyte solution is recycled respectively by electrode chamber circulator and is pumped into cathode chamber and anode
Room.Above-mentioned each circulator includes the original parts such as pipeline, valve, pipe fitting and circulating pump, is the prior art, does not go to live in the household of one's in-laws on getting married herein
It states.
In the present invention, the model of the Bipolar Membrane is preferably Neosepta BP-1.The model of the anion-exchange membrane
Preferably Fumasep FAS-PET-30.
In the present invention, the material of the anode plate is that titanium applies ruthenium;The material of the cathode plate is stainless steel.
In the present invention, the alkaline chamber solution be selected from sodium sulphate, sodium nitrate, potassium sulfate, potassium nitrate, sodium hydroxide solution or
Tap water;
The acid compartment solution is selected from sodium sulphate, sodium nitrate, potassium sulfate, potassium nitrate, formic acid solution or tap water.
The electrolyte solution is selected from ammonium sulfate, sodium sulphate, sodium nitrate, potassium sulfate or potassium nitrate.The electrolyte solution
Concentration be not less than 0.1mol/L.
In the present invention, the flow velocity of the neopentyl glycol solution containing sodium formate is not less than 5mL/min.It is described to contain first
The concentration of sodium formate is preferably not less than 0.1mol/L in the neopentyl glycol solution of sour sodium.The neopentyl glycol containing sodium formate is molten
The concentration of sodium formate is 0.4mol/L in liquid.The transformation efficiency of sodium formate in neopentyl glycol solution containing sodium formate is with electricity
The increase of current density and increase, when current density be 50mA/cm2Current density only need the time of hour can be all
Remove sodium formate.When sodium formate concentrations are 0.1~0.5mol/L, over time, conversion ratio can break through 90%.
It opens power supply and carries out electrodialysis, recording voltage and electric current, and detect acid compartment, alkaline chamber, cathode chamber, anode chamber and feed liquid
The conductivity of room, until cutting off the power after the stable conductivity of feed compartment, obtaining neopentyl glycol.In the present invention, electrodialysis
Cheng Zhong, electrodialytic current density are 10~50mA/cm2.In the specific embodiment of the invention, the electrodialytic current density
For 10mA/cm2、30mA/cm2Or 50mA/cm2.10~50mA/cm in electrodialytic process2Current density voltage drop can be caused
Influence: over time, voltage can reduce first, then as the time passage and keep stable, it is electric after a period of time
Pressure can rapidly rise to a stable numerical value again and remain unchanged.Meanwhile current density is higher, the numerical value of voltage knee is also got over
It is high.It is very small in the indoor conductivity of soda acid when reaction starts, so as to cause relatively high voltage, once Bipolar Membrane occurs
Electrodialysis will generate a large amount of hydroxide ion and hydrogen ion in bipolar membrane interface, and reduce rapidly voltage.Later period, due to
Conductivity constantly reduces in feed compartment, and voltage increases continuously until a stationary value, at this point, reaction terminates.
In order to further illustrate the present invention, below with reference to embodiment to provided by the invention a kind of using bipolar membrane electrodialysis
The method of system purification neopentyl glycol is described in detail, but they cannot be interpreted as to the limit to the scope of the present invention
It is fixed.
Fig. 2 is the current efficiency and energy consumption column schematic diagram of the embodiment of the present invention 1~3;Embodiment 1 is current density 10A/
cm2Histogram;Embodiment 2 is current density 30A/cm2Histogram;Embodiment 3 is current density 50A/cm2Histogram;
Fig. 3 is the current efficiency and energy consumption column schematic diagram of the embodiment of the present invention 4~6;Wherein, embodiment 4 is sodium formate
The histogram of concentration 0.1mol/L;Embodiment 5 is the histogram of sodium formate concentrations 0.2mol/L;Embodiment 6 is sodium formate concentrations
The histogram of 0.5mol/L.
Embodiment 1
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.3mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.3mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation in 10A/cm2, reaction
After, by detecting and calculating, current efficiency 99.8%, the energy consumption for decomposing sodium formate is 6.1kWh/kg.
Embodiment 2
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.3mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.3mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation 30A/cm2, reaction knot
Shu Hou, by detecting and calculating, current efficiency 95.3%, the energy consumption for decomposing sodium formate is 16.5kWh/kg.
Embodiment 3
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.3mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.3mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation 50A/cm2, reaction knot
Shu Hou, by detecting and calculating, current efficiency 87.3%, the energy consumption for decomposing sodium formate is 27.2kWh/kg.
Embodiment 4
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.3mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.1mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation 30A/cm2, reaction knot
Shu Hou, by detecting and calculating, current efficiency 91.2%, the energy consumption for decomposing sodium formate is 25kWh/kg.
Embodiment 5
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.2mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.2mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation 30A/cm2, reaction knot
Shu Hou, by detecting and calculating, current efficiency 85.3%, the energy consumption for decomposing sodium formate is 25.3kWh/kg.
Embodiment 6
Device assembly is finished as before, in the first that 100mL pure water is added in acid compartment and 1mL concentration is 0.3mol/L
Acid 100mL pure water is added in alkaline chamber and sodium hydroxide that 1mL concentration is 0.2mol/L, and feed compartment is the formic acid of neopentyl glycol containing
Sodium mixed solution, wherein the concentration of sodium formate is 0.5mol/L, and ammonium sulfate (or the sulfuric acid that concentration is 0.3mol/L is added in electrode chamber
Sodium) solution.After opening liquid circulating apparatus 5min, the scale of its initial graduated cylinder is recorded.By current regulation 30A/cm2, reaction knot
Shu Hou, by detecting and calculating, current efficiency 84.9%, the energy consumption for decomposing sodium formate is 15.1kWh/kg.
From Examples 1 to 6 it can be seen that in sodium formate concentrations between 0.1~0.5mol/L, current efficiency can be maintained
84% or more, for current density in 0.1~5mol/L, the energy consumption for decomposing sodium formate is to be reduced to about from about 25kWh/kg
15.1kWh/kg;In different current density (10~50mA/cm2) under, 87% can be maintained above in larger operation interval
Current efficiency, with the increase of electric current, energy-output ratio is stepped up, and the energy consumption for decomposing sodium formate is about 6.1-
27.2kWh/kg。
As seen from the above embodiment, the present invention provides a kind of sides using bipolar membrane electrodialysis system purification neopentyl glycol
Method, comprising the following steps: a), construct bipolar membrane electrodialysis system, the bipolar membrane electrodialysis system includes membrane stack;The membrane stack
Including cathode plate, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane and the anode plate set gradually;And the film
Cathode chamber, alkaline chamber, feed compartment, acid compartment and anode are sequentially formed between adjacent component on from cathode plate to anode plate direction in heap
Room;B), the neopentyl glycol solution circulation pump containing sodium formate is entered into feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;By acid compartment
Solution circulation pump enters acid compartment;Electrolyte solution is recycled respectively and is pumped into cathode chamber and anode chamber;C), open power supply and carry out electric osmose
Analysis, recording voltage and electric current, and the conductivity of acid compartment, alkaline chamber, cathode chamber, anode chamber and feed compartment is detected, until feed compartment
It after stable conductivity, cuts off the power, obtains neopentyl glycol.The present invention can purify new penta 2 using bipolar membrane electrodialysis system
Alcohol, and the purity of neopentyl glycol is higher.With traditional benzene extraction process, method of purification provided by the invention is environmentally protective, does not make
Purification operation can be completed with other chemical reagent;Energy consumption is lower, can significantly reduce production cost;In removing neopentyl glycol
While sodium formate, formic acid and sodium hydroxide free from foreign meter are generated, by-product quality is higher, added value of product is improved,
On the other hand, formic acid and sodium hydroxide are also the required raw material of disproportionation processes production neopentyl glycol, and following for technique may be implemented
Loop chain.The results showed that the purity of neopentyl glycol is 99% or more;In wider sodium formate concentrations and wider current density
84% or more high current efficiency is obtained in range;10~50mA/cm2It is lower decompose sodium formate energy consumption be 6.1~
27.2kWh/kg。
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of method using bipolar membrane electrodialysis system purification neopentyl glycol, comprising the following steps:
A), bipolar membrane electrodialysis system is constructed, the bipolar membrane electrodialysis system includes membrane stack;
The membrane stack includes the cathode plate set gradually, Bipolar Membrane, cation-exchange membrane, anion-exchange membrane, Bipolar Membrane and sun
Pole plate;
And sequentially formed between adjacent component on from cathode plate to anode plate direction in the membrane stack cathode chamber, alkaline chamber, feed compartment,
Acid compartment and anode chamber;
B), the neopentyl glycol solution circulation pump containing sodium formate is entered into feed compartment;Alkaline chamber solution circulation pump is entered into alkaline chamber;By acid compartment
Solution circulation pump enters acid compartment;Electrolyte solution is recycled respectively and is pumped into cathode chamber and anode chamber;
C), open power supply and carry out electrodialysis, recording voltage and electric current, and detect acid compartment, alkaline chamber, cathode chamber, anode chamber and feed liquid
The conductivity of room, until cutting off the power after the stable conductivity of feed compartment, obtaining neopentyl glycol.
2. the method according to claim 1, wherein the model Neosepta BP-1 of the Bipolar Membrane.
3. the method according to claim 1, wherein the model Fumasep FAS- of the anion-exchange membrane
PET-30。
4. the method according to claim 1, wherein the alkaline chamber solution is selected from sodium sulphate, sodium nitrate, sulfuric acid
Potassium, potassium nitrate, sodium hydroxide solution or tap water;
The acid compartment solution is selected from sodium sulphate, sodium nitrate, potassium sulfate, potassium nitrate, formic acid solution or tap water.
5. the method according to claim 1, wherein the electrolyte solution is selected from ammonium sulfate, sodium sulphate, nitric acid
Sodium, potassium sulfate or potassium nitrate.
6. the method according to claim 1, wherein the flow velocity of the neopentyl glycol solution containing sodium formate is not
Less than 5mL/min.
7. the method according to claim 1, wherein sodium formate in the neopentyl glycol solution containing sodium formate
Concentration be not less than 0.1mol/L.
8. the method according to claim 1, wherein sodium formate in the neopentyl glycol solution containing sodium formate
Concentration be 0.4mol/L.
9. the method according to claim 1, wherein the electrodialytic current density is 10~50mA/cm2。
10. the method according to claim 1, wherein the electrodialytic current density is 30m A/cm2。
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CN113603565A (en) * | 2021-07-15 | 2021-11-05 | 浙江蓝波新材料科技有限公司 | Novel process for separating pentaerythritol and byproduct sodium formate by membrane method |
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CN113603565A (en) * | 2021-07-15 | 2021-11-05 | 浙江蓝波新材料科技有限公司 | Novel process for separating pentaerythritol and byproduct sodium formate by membrane method |
CN114031508A (en) * | 2021-11-12 | 2022-02-11 | 浙江工业大学 | Method for preparing (R) -3-aminobutanol and recycling D-tartaric acid by using bipolar membrane electrodialysis |
CN114230441A (en) * | 2021-11-26 | 2022-03-25 | 南通百川新材料有限公司 | Electrodialysis membrane separation method for sodium formate in trimethylolpropane |
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