CN108163811A - A kind of preparation method of hydroiodic acid - Google Patents
A kind of preparation method of hydroiodic acid Download PDFInfo
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- CN108163811A CN108163811A CN201810064286.8A CN201810064286A CN108163811A CN 108163811 A CN108163811 A CN 108163811A CN 201810064286 A CN201810064286 A CN 201810064286A CN 108163811 A CN108163811 A CN 108163811A
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- membrane
- room
- bipolar membrane
- hydroiodic acid
- alkali
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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
- C01B7/00—Halogens; Halogen acids
- C01B7/13—Iodine; Hydrogen iodide
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The present invention relates to a kind of methods that hydroiodic acid is prepared using bipolar membrane electrodialysis.By the way that IodineSodium Solution is put into the feed chamber being made of Bipolar Membrane；Cation-exchange membrane and anion-exchange membrane are respectively arranged on the left side and the right side in feed chamber, the Bipolar Membrane of cation-exchange membrane and feed chamber forms alkali room, the Bipolar Membrane of anion-exchange membrane and feed chamber forms sour room, and feed chamber forms bipolar membrane electrodialysis device with sour room, alkali room；Then under electric field, sour room adds in distilled water, and alkali room adds in aqueous sulfuric acid；For the NaOH solubility of detection reaction generation to when stablizing, stopping reaction sour room and alkali room obtain hydriodic acid aqueous solution and sodium hydrate aqueous solution respectively, will obtain hydroiodic acid after hydriodic acid aqueous solution distillation and concentration.The hydriodic acid concentration that method by the present invention is prepared is 2.4% solution mixed above, and mixed solution obtained is obtained the higher hydroiodic acid solution of concentration after distillation；Alkali room obtains a concentration of more than 2% sodium hydroxide solution, can be used as by-product recovery.
Description
Technical field
The invention belongs to application of the bipolar membrane electrodialysis technology in chemical field, and in particular to a kind of to utilize Bipolar Membrane electricity
The method that dialysis prepares hydroiodic acid.
Background technology
Hydroiodic acid is the aqueous solution of hydrogen iodide, has the tart flavour of intense irritation, belongs to strong acid, is in "dead" oxygen-free acid
It is acid most strong, free-iodine is precipitated easily by oxidation in air, is reproducibility most powerhouse in halogen acids.Hydroiodic acid to skin,
Eyes and mucous membrane have strong stimulation effect.Hydroiodic acid is mainly used for the raw material of analytical reagent and reducing agent, medicine intermediate, fungicide
And the preparation of organic iodide.In the prior art, there are direct synthesis technique, iodine and red phosphorus synthesis about the preparation method of hydroiodic acid
Method, vulcanization hydrogen reduction method.
(1) direct synthesis technique：It is directly synthesized through platinum black or platinized asbestos catalysis with hydrogen and iodine：H2+I2=2HI, this reaction can
Inverse, this method is reacted under conditions of 500 DEG C or more, severe reaction conditions, to equipment requirement height, the disposable throwing of equipment
Enter greatly, and the catalyst Pt needed for it is expensive so that the cost of entire synthesis technology is higher.
(2) iodine and red phosphorus synthetic method：Its reaction equation is：2P+3I2+6H2O=6HI+2H3PO3, iodine is with red phosphorus in deionization
It is reacted in water, generates hydroiodic acid and phosphorous acid, acquired solution after filtering, are distilled, then Fractional Collections hydroiodic acid
Fraction, at present, this method is in the lab using more.
(3) vulcanize hydrogen reduction method：Displacement occurs with iodine with hydrogen sulfide to react, H2S+I2=2HI+S ↓, the shortcomings that this method
Be hydrogen sulfide gas preparation speed it is slow, technique line length, and if hydrogen sulfide gas control it is improper it is easy leak, thus
Worker is made to be poisoned, is not easy large-scale production.
Chinese patent CN101935021A discloses a kind of production method of hydrogen iodide, using red phosphorus method, includes successively anti-
It answers step, filtration step and distilation steps, in reaction step, deionized water is added in into consersion unit, adds red phosphorus and iodine
Afterwards, the proportion of reaction material liquid is measured, controlling its proportion, hydroiodic acid steam is absorbed with water spray pump, filtration step two in 1.2-1.4
Secondary filtering although the invention solves the problems, such as that large-scale production is not easy to realize, controls the generation of explosion, and production efficiency is high,
But complex steps, the time is long, and energy consumption is big, of high cost, and product purity is not high, should be noted filtering red phosphorus in process of production, no
Then there is some potential safety problems, and by-product phosphorous acid is not disposable.
Chinese patent CN102674253A discloses a kind of preparation method of hydroiodic acid, using sodium iodide and pure water as raw material,
It is reacted in the presence of solid phosphorous acid, target product hydroiodic acid is collected from organic phase.Although the hydrogen iodine that the present invention obtains
Sour purity is more than 99%, more than 90% yield, but the raw materials used sodium iodide of this method is expensive, time added in distillation process
It is easily decomposed in phosphorous acid distillation process, there is security risk.
Chinese patent CN103523753A discloses a kind of method that high-purity hydrogen acid iodide is prepared using Biodine, it is
Be raw material using Biodine, restore by elemental iodine, desulfurization, defluorinate, concentration and etc. after prepare high-purity hydrogen acid iodide, product
Purity is up to more than 98%, although the present invention overcomes security risk existing for traditional handicraft process, production cost is low, production
Quality is stablized, but prepares hydroiodic acid with sodium sulfite reduction, and when reaction easily disengages sulfur dioxide, and desulfurization is plus certain carbon
Sour barium, and barium carbonate category heavy metal compound, are unfavorable for environmental protection.
United States Patent (USP) US5520793A synthesizes hydroiodic acid using electrolysis, this patent is opened by USA New York Electrosynthesis Co., Inc.
Hair.Electrolytic cell is separated into cathodic region, anode region and middle area with anion-exchange membrane and cation-exchange membrane, middle area between
Between anion-exchange membrane and cation-exchange membrane.Iodine is reduced to iodide ion on cathode, the oxidation generation hydrogen ion on anode,
Then iodide ion and hydrogen ion are complex as hydroiodic acid in middle area, and key reaction is：
Cathodic region：I2+2e-=2I-
Anode region：2H2O-4e-=O2+4H+
Middle area：H++I-=HI
In place of this method plays the same tune on different musical instruments with chlor-alkali production, and whole process liquid phase circulation uses, and theoretically raw material point is complete
Portion converts, and no waste liquid generates, very environmentally friendly, but needs to increase the input of electrode in industrialized production, and project investment is larger.
Above preparation process exists respectively insufficient, it is therefore necessary to which existing technology is improved.
Bipolar Membrane is a kind of amberplex with specific function, its wherein interbed under electric field action hydrolyzes
From generation H+And OH-Ion.And this specific function is exactly combined in common electrodialysis by bipolar membrane electrodialysis technology, so as to
It can realize production/regeneration of instant acid/base or be acidified and/or alkalize.
Invention content
For deficiency existing for hydroiodic acid technique made above, the present invention provides a kind of rate of recovery height, and production cost is low,
No three industrial wastes generate, and product quality is high, and can obtain the hydroiodic acid production technology of the by-product sodium hydroxide of high quality.
The present invention realizes object above, the technical scheme is that：
A kind of preparation method of hydroiodic acid, includes the following steps：
(1) IodineSodium Solution is put into the feed chamber being made of Bipolar Membrane；
(2) cation-exchange membrane and anion-exchange membrane, the cation are respectively arranged on the left side and the right side in the feed chamber
The Bipolar Membrane of exchange membrane and feed chamber forms the Bipolar Membrane composition sour room of alkali room, the anion-exchange membrane and feed chamber, described
Feed chamber forms bipolar membrane electrodialysis device with sour room, alkali room；
(3) under electric field, sour room adds in distilled water, and alkali room adds in aqueous sulfuric acid；
(4) NaOH concentration of detection reaction generation stops reaction to when stablizing；
(5) sour room and alkali room obtain hydriodic acid aqueous solution and sodium hydrate aqueous solution respectively, and hydriodic acid aqueous solution is distilled
Hydroiodic acid is obtained after concentration.
Further, the speed that distilled water is added in described in step (3) is 35~40L/h, and alkali room adds in aqueous sulfuric acid
Speed be 35~40L/h.
Further, the mass concentration that aqueous sulfuric acid is added in described in step (3) is 2~3%.
Further, the current density of electric field described in step (3) is 20~50mA/cm2。
Further, anion-exchange membrane is one kind of heterogeneous membrane, half homogeneous membrane or homogeneous membrane, and cation-exchange membrane is different
One kind of phase film, half homogeneous membrane or homogeneous membrane.
Further, the bipolar membrane electrodialysis device in step (2) can also be：
Two compartments of sour (salt)/alkali：Using the electrodialytic salt/sour room of two compartments of Bipolar Membrane+anode membrane+anode membrane+Bipolar Membrane；
Three compartments of acid/salt/alkali：Using three compartment electrodialysis salt rooms of Bipolar Membrane+cavity block+anode membrane+Bipolar Membrane.
When three compartments design of the bipolar membrane electrodialysis device using acid/salt/alkali, it is water-soluble that salt room is pumped into sodium iodide
Liquid, sour room be pumped into pure water either 0.1% hydroiodic acid solution alkali room be pumped into pure water or 0.1% sodium hydroxide solution；
When two compartments design of the bipolar membrane electrodialysis device using sour (salt)/alkali, sour (salt) room is pumped into sodium iodide aqueous solution, alkali room pump
Enter pure water or 0.1% sodium hydroxide solution；
Further, the electrodialysis compartment that the bipolar membrane electrodialysis device uses is by 1~500 group of unit group arranged in series
Composition, can form bipolar membrane electrodialysis equipment by 2~50 bipolar membrane electrodialysis device serial or parallel connections.
The hydriodic acid concentration that method by the present invention is prepared is 2.4% solution mixed above, by mixing obtained
Solution obtains the higher hydroiodic acid solution of concentration after distillation；Alkali room obtains a concentration of more than 2% sodium hydroxide solution, can make
For by-product recovery.
Specific embodiment
The present invention is described further below by way of specific embodiment.
Embodiment 1
It prepares hydroiodic acid to carry out using bipolar membrane electrodialysis equipment, the bipolar membrane electrodialysis equipment is by pole room, hydrochlorate
Room, alkali room are formed.The bipolar membrane electrodialysis device mode of two cell structures is used as shown in Figure 1, the area of every film is 90mm
× 210mm mainly has two Bipolar Membranes, three cationic membrane compositions.Anode electrolysis room (1) is equipped with anode electrode and anode electrolysis
Liquid, equipped with cathode electrode, film A, C, D are cationic membrane for catholyte chamber (6), and film B, E are Bipolar Membrane.The electrodialysis compartment
It is alternatively arranged by Bipolar Membrane and cation-exchange membrane and forms hydrochlorate room and alkali room unit group and by 5 unit group arranged in series groups
Into.
Using sodium iodide aqueous solution as raw material, into the feed liquid room of bipolar membrane electrodialysis device.By 500mL 1mol/L's
Sodium iodide aqueous solution enters the hydrochlorate room of two compartment bipolar membrane electrodialysis devices with the flow velocity of 40L/h, with the stream of 40L/h in alkali room
Speed adds in distilled water solution 500mL, and the flow velocity of 40L/h adds in the aqueous sulfuric acid 400mL of 0.3mol/L in the liquid chamber of pole, and control is double
The current density of pole membrane electrodialysis device is 50mA/cm2, bring into operation, 1mL NaOH being taken to carry out titration survey every 10min, its is dense
Degree, out of service when NaOH concentration remains unchanged, hydrochlorate room and alkali room obtain hydroiodic acid, sodium iodide mixed aqueous solution respectively
And sodium hydrate aqueous solution.By hydroiodic acid, sodium iodide mixed aqueous solution distillation and concentration, start to collect fraction in 127 DEG C, obtain hydrogen
Acid iodide；Sodium hydroxide solution is regarded into by-product recovery.The hydroiodic acid of acquisition is analyzed, testing result is shown in Table 1.
Embodiment 2
With embodiment 1, it is 20mA/cm only to change current density2, testing result is shown in Table 1.
Embodiment 3
With embodiment 1, only change a concentration of 3mol/L of IodineSodium Solution, testing result is shown in Table 1.
1 Examples 1 to 3 testing result of table
The hydroiodic acid prepared by the present invention can be seen that by the testing result to Examples 1 to 3, the rate of recovery is high, raw
Produce it is at low cost, while the method without three industrial wastes generate, no environmental protection pressure.
Claims (7)
1. a kind of preparation method of hydroiodic acid, it is characterised in that：Include the following steps：
(1) IodineSodium Solution is put into the feed chamber being made of Bipolar Membrane；
(2) cation-exchange membrane and anion-exchange membrane, the cation exchange are respectively arranged on the left side and the right side in the feed chamber
The Bipolar Membrane of film and feed chamber forms the Bipolar Membrane composition sour room of alkali room, the anion-exchange membrane and feed chamber, the raw material
Room forms bipolar membrane electrodialysis device with sour room, alkali room；
(3) under electric field, sour room adds in distilled water, and alkali room adds in aqueous sulfuric acid；
(4) NaOH concentration of detection reaction generation stops reaction to when stablizing；
(5) sour room and alkali room obtain hydriodic acid aqueous solution and sodium hydrate aqueous solution respectively, by hydriodic acid aqueous solution distillation and concentration
After obtain hydroiodic acid.
2. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：It adds in and steams described in step (3)
The speed of distilled water is 35~40L/h, and the speed that alkali room adds in aqueous sulfuric acid is 35~40L/h.
3. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：Step adds in sulphur described in (3)
The mass concentration of aqueous acid is 2~3%.
4. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：Electric field described in step (3)
Current density is 20~50mA/cm2。
5. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：Anion-exchange membrane is out-phase
One kind of film, half homogeneous membrane or homogeneous membrane, cation-exchange membrane are one kind of heterogeneous membrane, half homogeneous membrane or homogeneous membrane.
6. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：Bipolar Membrane electricity in step (2)
Electrodialysis apparatus can also be：
Two compartments of acid/base or salt/alkali：Using the electrodialytic salt/sour room of two compartments of Bipolar Membrane+anode membrane+anode membrane+Bipolar Membrane；
Three compartments of acid/salt/alkali：Using three compartment electrodialysis salt rooms of Bipolar Membrane+cavity block+anode membrane+Bipolar Membrane.
7. a kind of preparation method of hydroiodic acid according to claim 1, it is characterised in that：The bipolar membrane electrodialysis device
The electrodialysis compartment of use is made of 1~500 group of unit group arranged in series.
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| CN201810064286.8A CN108163811A (en) | 2018-01-23 | 2018-01-23 | A kind of preparation method of hydroiodic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658044A (en) * | 2018-08-10 | 2018-10-16 | 太仓沪试试剂有限公司 | A kind of purification process of hydroiodic acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009023847A (en) * | 2007-06-20 | 2009-02-05 | Godo Shigen Sangyo Kk | Method for producing hydriodic acid |
-
2018
- 2018-01-23 CN CN201810064286.8A patent/CN108163811A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009023847A (en) * | 2007-06-20 | 2009-02-05 | Godo Shigen Sangyo Kk | Method for producing hydriodic acid |
Non-Patent Citations (2)
| Title |
|---|
| J. MICHAEL ROBINSON ET AL.: "Electrohydrolysis recycling of waste iodide salts into hydriodic acid for the chemical conversion of biomass into liquid hydrocarbons", 《JOURNAL OF MEMBRANE SCIENCE》 * |
| 高艳荣 等: "双极膜电渗析解NaCl清洁制备酸碱的实验研究", 《膜科学与技术》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108658044A (en) * | 2018-08-10 | 2018-10-16 | 太仓沪试试剂有限公司 | A kind of purification process of hydroiodic acid |
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Effective date of registration: 20200103 Address after: 212006 No. 88 Qiusuo Road, Jingkou District, Zhenjiang City, Jiangsu Province Applicant after: Jiangsu Sopo Chemical Co.,Ltd. Applicant after: Jiangsu Thorpe Engineering Technology Co., Ltd. Address before: No. 101, Jingkou Road, Zhenjiang, Jiangsu, Jiangsu Applicant before: Jiangsu Soap (Group) Co., Ltd. Applicant before: Jiangsu Thorpe Engineering Technology Co., Ltd. |
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Application publication date: 20180615 |