CN110055550A - A kind of anode membrane electrolysis unit preparing tetra-alkyl ammonium hydroxide and method - Google Patents
A kind of anode membrane electrolysis unit preparing tetra-alkyl ammonium hydroxide and method Download PDFInfo
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- CN110055550A CN110055550A CN201910473169.1A CN201910473169A CN110055550A CN 110055550 A CN110055550 A CN 110055550A CN 201910473169 A CN201910473169 A CN 201910473169A CN 110055550 A CN110055550 A CN 110055550A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B3/00—Electrolytic production of organic compounds
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B9/00—Cells or assemblies of cells; Constructional parts of cells; Assemblies of constructional parts, e.g. electrode-diaphragm assemblies; Process-related cell features
- C25B9/17—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof
- C25B9/19—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms
- C25B9/23—Cells comprising dimensionally-stable non-movable electrodes; Assemblies of constructional parts thereof with diaphragms comprising ion-exchange membranes in or on which electrode material is embedded
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Abstract
The invention discloses a kind of system and method that anode membrane electrolysis method prepares tetra-alkyl ammonium hydroxide.Using content for 10%-30% (wt) tetra-alkyl-phosphonium halide aqueous ammonium as raw material, by electrolysis unit generate content be 8%-25% (wt) tetra-alkyl ammonium hydroxide.Anode membrane electrolysis unit includes that raw material (by-product) room and product chambers and homogeneous anode membrane, wherein negative electrode plate and homogeneous anode membrane form raw material (by-product) room, homogeneous anode membrane and positive electrode plate formation product chambers；After the ionization of tetra-alkyl-phosphonium halide aqueous ammonium, cationic R4N+Enter product chambers by anode membrane, and anion X‑It cannot be left on feed chamber by homogeneous anode membrane, feed chamber becomes by-product room in turn.Its simple process, it is easy to operate, it is at low cost, it is pollution-free.
Description
Technical field
The invention belongs to electrochemical technology fields, and in particular to a kind of anode membrane electrolysis unit for preparing tetra-alkyl ammonium hydroxide
And method.
Background technique
Electrolysis refers to the process of that electric current causes chemical change by substance.It is widely used in non-ferrous metal metallurgy, chlor-alkali
With production of inorganic and Organic Chemical Industry.Electrolytic process is carried out in electrolytic cell.Electrolytic cell is by being immersed in respectively
Two electrodes of yin, yang in solution containing positive and negative ion are constituted.Electric current flows into negative electrode (cathode), positively charged in solution
Cation move to cathode, and in conjunction with electronics, become neutral element or molecule；Negatively charged anion moves to separately
One electrode (anode), provides electronics, becomes neutral element or molecule.
Tetra-alkyl ammonium hydroxide is common template, and template plays structure guide work in the preparation process of catalyst
With tetra-alkyl ammonium hydroxide can be used as the template of the important molecules such as ZSM-5, pure silicon molecular sieve, Titanium Sieve Molecular Sieve sieve.
Currently, industrial tetra-alkyl ammonium hydroxide is mainly prepared by corresponding quaternary ammonium salt, common method has three
Kind, including silver oxide method, ion-exchange-resin process and electrolysis method.
Silver oxide method mainly utilize tetraalkyl bromination ammonium salt under conditions of heating with oxidation silver reaction, generate AgBr and
Tetra-alkyl ammonium hydroxide.The tetra-alkyl ammonium hydroxide product purity of this method production can satisfy to be wanted as the use of corrosion reagent
It asks, but since the method is using costly containing silver material, production cost is higher, and yield is small.
Ion-exchange carries out ion exchange using tetraalkyl ammonium bromide as raw material in ion exchange resin and lye.It should
Method is limited by ion-exchange reactions balance, and the conversion ratio of product is lower, molten so as to cause the tetra-alkyl ammonium hydroxide in production
Contain certain density tetra-alkyl ammonium hydroxide in liquid, product purity is difficult to meet the requirement in terms of high-end technology；And
And it is long reaction time using ion-exchange production, exchanger resin easily entrains Na+ ion when regenerating, and Na+ ion concentration is high
It is low that molecular sieve performance is had a major impact；Furthermore ion-exchange production technology is used, a large amount of waste water can be generated.
There is the technique using three Room, two membrane electrolysis electrolysis 4-propyl bromide preparation tetrapropylammonium hydroxide in the country at present,
The present invention is simpler with respect to other techniques, easy to operate, at low cost, pollution-free.
Summary of the invention
The present invention provides it is a kind of with monofilm technology preparation high-purity tetra-alkyl ammonium hydroxide electrolysis system and method,
The current multimembrane electrolysis system solved is erroneous for installation, and save the cost.
The present invention provides a kind of anode membrane electrolysis unit for preparing tetra-alkyl ammonium hydroxide, it is characterised in that, the anode membrane electricity
Solution device is made of membrane stack, product slot, raw material/by-product slot, magnetic drive pump and high frequency electric source；The membrane stack include by negative electrode plate and
Homogeneous anode membrane forms product chambers；Comprising forming raw material/by-product room by homogeneous anode membrane and positive electrode plate, wherein negative electrode plate and positive electricity
Pole plate is respectively in the two sides of homogeneous anode membrane.
Further, in the above-mentioned technical solutions, strap is respectively equipped on the outside of the membrane stack two；The strap
Inside is respectively equipped with polyethylene insulation plate；The homogeneous anode membrane two sides are closely connected with elastic baffle.
Further, in the above-mentioned technical solutions, the negative electrode plate is closely connected with bullet towards homogeneous anode membrane side
Property partition；It is equipped with PVC partition in the product chambers, contains PE fill-net on the PVC partition；In the PVC partition be equipped with into
Pipe material and discharge pipe, the feed pipe and discharge pipe are separately connected product slot.
Further, in the above-mentioned technical solutions, the positive electrode plate is closely connected with bullet towards homogeneous anode membrane side
Property partition；It is equipped with PVC partition in the raw material/by-product room, contains PE fill-net on the PVC partition；It is set in the PVC partition
There are feed pipe and discharge pipe, the feed pipe and discharge pipe are separately connected raw material/by-product slot.
Further, in the above-mentioned technical solutions, in the membrane stack successively include product chambers, raw material/by-product room, raw material/
By-product room, product chambers form a unit, and two neighboring raw material/by-product room shares a positive electrode plate.
It further, in the above-mentioned technical solutions, successively include raw material/by-product room, product chambers, product in the membrane stack
Room, raw material/by-product room form a unit, and two neighboring product chambers share a negative electrode plate.
Further, in the above-mentioned technical solutions, be successively arranged 1-20 unit in the membrane stack, two neighboring unit it
Between using insulation board connect.
Further, in the above-mentioned technical solutions, the positive electrode plate is Ti-Ru electrode web plate.
The present invention separately provides a kind of method that cavity block electrolysis method prepares tetra-alkyl ammonium hydroxide, using above-mentioned apparatus, to contain
The tetra-alkyl-phosphonium halide aqueous ammonium that amount is 10-30wt% is electrolyte raw material input raw material/by-product room, after connecting direct current, is led to
Crossing electrolysis unit and generating content in product chambers is 8-25wt% tetra-alkyl ammonium hydroxide.After the ionization of tetra-alkyl-phosphonium halide aqueous ammonium,
Cationic R4N+ enters product chambers by anode membrane, and anion X-It cannot be left on feed chamber by homogeneous anode membrane, raw material
Room becomes by-product room in turn.
Further, in the above-mentioned technical solutions, quaternary alkylammonium halides be selected from tetramethyl ammonium chloride, etamon chloride,
4-propyl ammonium chloride, tetrabutylammonium chloride, 4 bromide, tetraethylammonium bromide, 4-propyl bromide, tetrabutyl phosphonium bromide
Ammonium.
Detailed description of the invention
Fig. 1 is the anode membrane electrolysis unit structural schematic diagram for preparing tetra-alkyl ammonium hydroxide；
Fig. 2 is membrane stack schematic diagram of internal structure in Fig. 1；
1, membrane stack；2, raw material/by-product slot；3, product slot；4, magnetic drive pump；11, negative electrode plate；12, homogeneous anode membrane；13 positive electricity
Pole plate.
Specific embodiment
The invention will be further described for following embodiment, but content not thereby limiting the invention.
Chloride ion content is surveyed by Polarized energy dispersion X-ray fluorescence spectrometer (SPECTROXEPOS) in following embodiment
It is fixed.
As shown in Figure 1, a kind of cavity block electrolysis unit for preparing tetra-alkyl ammonium hydroxide, the cavity block electrolysis unit is by membrane stack
1, raw material/by-product slot 2, product slot 3, magnetic drive pump 4 and high frequency electric source composition；As shown in Fig. 2, the membrane stack includes by negative electrode plate
11 and homogeneous anode membrane 12 formed product chambers；Comprising forming raw material/by-product room by homogeneous anode membrane 12 and positive electrode plate 13, wherein positive electricity
Pole plate 13 and negative electrode plate 11 are respectively in the two sides of homogeneous anode membrane 12.
Strap is respectively equipped on the outside of the membrane stack two；Polyethylene insulation plate is respectively equipped on the inside of the strap；
The homogeneous anode membrane two sides are closely connected with elastic baffle.
The negative electrode plate is closely connected with elastic baffle towards homogeneous anode membrane side；PVC is equipped in the product chambers
Partition contains PE fill-net on the PVC partition；Feed pipe and discharge pipe, the feed pipe are equipped in the PVC partition
Road and discharge pipe are separately connected product slot.
The positive electrode plate is closely connected with elastic baffle towards homogeneous anode membrane side；The raw material/by-product is set in room
There is PVC partition, contains PE fill-net on the PVC partition；Feed pipe and discharge pipe are equipped in the PVC partition, it is described
Feed pipe and discharge pipe are separately connected raw material/by-product slot.
As shown in Fig. 2, successively being formed including product chambers, raw material/by-product room, raw material/by-product room, product chambers in the membrane stack
One unit, two neighboring raw material/by-product room share a positive plate.
The positive electrode plate is Ti-Ru electrode web plate.
Embodiment 1
Etamon chloride is diluted to the aqueous solution of 10% (wt) with deionized water.Electricity is added in aqueous solution after dilution
It solves in raw material/by-product slot, product slot is added in the deionized water of half raw material volume.Electrolysis installation is opened, allows material in pipeline
And 10min is recycled in membrane stack.High frequency electric source is opened, electric current is adjusted to 70A.After equipment runs 1h, four in sampling analysis product slot
Ammonium hydroxide concentration 8.8% (wt), wherein Cl-Content is less than 2.0ppm.
Embodiment 2
Etamon chloride is diluted to the aqueous solution of 15% (wt) with deionized water.Electricity is added in aqueous solution after dilution
It solves in raw material/by-product slot, product slot is added in the deionized water of half raw material volume.Electrolysis installation is opened, allows material in pipeline
And 10min is recycled in membrane stack.High frequency electric source is opened, electric current is adjusted to 70A.After equipment runs 1.5h, in sampling analysis product slot
Tetramethylammonium hydroxide concentration 13.9% (wt), wherein Cl-Content is less than 2.0ppm.
Embodiment 3
Etamon chloride is diluted to the aqueous solution of 20% (wt) with deionized water.Electricity is added in aqueous solution after dilution
It solves in raw material/by-product slot, product slot is added in the deionized water of half raw material volume.Electrolysis installation is opened, allows material in pipeline
And 10min is recycled in membrane stack.High frequency electric source is opened, electric current is adjusted to 70A.After equipment runs 1.5h, in sampling analysis product slot
Tetramethylammonium hydroxide concentration 17.9% (wt), wherein Cl-Content is less than 2.0ppm.
Embodiment 4
Tetramethyl ammonium chloride is diluted to the aqueous solution of 12% (wt) with deionized water.Electricity is added in aqueous solution after dilution
It solves in raw material/by-product slot, product slot is added in the deionized water of half raw material volume.Electrolysis installation is opened, allows material in pipeline
And 10min is recycled in membrane stack.High frequency electric source is opened, electric current is adjusted to 70A.After equipment runs 1h, four in sampling analysis product slot
Ammonium hydroxide concentration 10.1% (wt), wherein Cl-Content is less than 2.0ppm.
Embodiment 5
4-propyl ammonium chloride is diluted to the aqueous solution of 12% (wt) with deionized water.Electricity is added in aqueous solution after dilution
It solves in raw material/by-product slot, product slot is added in the deionized water of half raw material volume.Electrolysis installation is opened, allows material in pipeline
And 10min is recycled in membrane stack.High frequency electric source is opened, electric current is adjusted to 70A.After equipment runs 1.5h, in sampling analysis product slot
Tetramethylammonium hydroxide concentration 10.5% (wt), wherein Cl-Content is less than 2.0ppm.
Claims (10)
1. a kind of anode membrane electrolysis unit for preparing tetra-alkyl ammonium hydroxide, it is characterised in that: the anode membrane electrolysis unit by membrane stack,
Raw material/by-product slot, product slot, magnetic drive pump and high frequency electric source composition；The membrane stack includes to be formed by positive electrode plate and homogeneous anode membrane
Raw material/by-product room；Comprising forming product chambers by homogeneous anode membrane and negative electrode plate, wherein negative electrode plate and positive electrode plate are respectively equal
The two sides of phase anode membrane.
2. device according to claim 1, it is characterised in that: be respectively equipped with strap on the outside of the membrane stack two；It is described solid
Polyethylene insulation plate is respectively equipped on the inside of clamp plate；The homogeneous anode membrane two sides are closely connected with elastic baffle.
3. device according to claim 1, it is characterised in that: the negative electrode plate is closely connected towards homogeneous anode membrane side and set
Flexible partition；It is equipped with PVC partition in the product chambers, contains PE fill-net on the PVC partition；It is set in the PVC partition
There are feed pipe and discharge pipe, the feed pipe and discharge pipe are separately connected product slot.
4. device according to claim 1, it is characterised in that: the positive electrode plate is closely connected towards homogeneous anode membrane side and set
Flexible partition；It is equipped with PVC partition in the raw material/by-product room, contains PE fill-net on the PVC partition；The PVC partition
In be equipped with feed pipe and discharge pipe, the feed pipe and discharge pipe are separately connected raw material/by-product slot.
5. device according to claim 1, it is characterised in that: in the membrane stack successively include product chambers, raw material/by-product room,
Raw material/by-product room, product chambers form a unit, and two neighboring raw material/by-product room shares a positive electrode plate.
6. device according to claim 1, it is characterised in that: in the membrane stack successively include raw material/by-product room, product chambers,
Product chambers, raw material/by-product room form a unit, and two neighboring product chambers share a negative electrode plate.
7. according to claim 5 or 6 described devices, it is characterised in that: it is successively arranged 1-20 unit in the membrane stack, adjacent two
It is connected between a unit using insulation board.
8. device according to claim 1, it is characterised in that: the positive electrode plate is Ti-Ru electrode web plate.
9. a kind of method that anode membrane electrolysis method prepares tetra-alkyl ammonium hydroxide, it is characterised in that: any using claim 1~8
One described device inputs raw material/by-product as electrolyte raw material for the tetra-alkyl-phosphonium halide aqueous ammonium of 10-30wt% using content
Room, after connecting 50A -200A direct current, generating content in product chambers by electrolysis unit is 8-25wt% tetraalkylphosphonium hydroxide
Ammonium.
10. the method that anode membrane electrolysis method as claimed in claim 9 prepares tetra-alkyl ammonium hydroxide, which is characterized in that tetraalkyl
Ammonium halide is selected from tetramethyl ammonium chloride, etamon chloride, 4-propyl ammonium chloride, tetrabutylammonium chloride, 4 bromide, four
Ethyl phosphonium bromide ammonium, 4-propyl bromide, tetrabutylammonium bromide.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526224A (en) * | 2013-09-22 | 2014-01-22 | 镇江润晶高纯化工有限公司 | Method for preparing high-purity tetraethylammonium hydroxide by continuous electrolysis |
| CN105112934A (en) * | 2015-09-16 | 2015-12-02 | 青岛润兴光电材料有限公司 | Preparation method for tetra-alkyl ammonium hydroxide |
| CN106801233A (en) * | 2017-01-11 | 2017-06-06 | 浙江工业大学 | A kind of electrolysis prepares the system and method for high-purity TPAOH |
-
2019
- 2019-05-31 CN CN201910473169.1A patent/CN110055550A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103526224A (en) * | 2013-09-22 | 2014-01-22 | 镇江润晶高纯化工有限公司 | Method for preparing high-purity tetraethylammonium hydroxide by continuous electrolysis |
| CN105112934A (en) * | 2015-09-16 | 2015-12-02 | 青岛润兴光电材料有限公司 | Preparation method for tetra-alkyl ammonium hydroxide |
| CN106801233A (en) * | 2017-01-11 | 2017-06-06 | 浙江工业大学 | A kind of electrolysis prepares the system and method for high-purity TPAOH |
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