CN104495877A - Method for removing trace quantity of iodine from ion membrane caustic soda raw material brine - Google Patents
Method for removing trace quantity of iodine from ion membrane caustic soda raw material brine Download PDFInfo
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- CN104495877A CN104495877A CN201410694358.9A CN201410694358A CN104495877A CN 104495877 A CN104495877 A CN 104495877A CN 201410694358 A CN201410694358 A CN 201410694358A CN 104495877 A CN104495877 A CN 104495877A
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Abstract
The invention provides a method for removing a trace quantity of iodine from ion membrane caustic soda raw material brine, and belongs to the field of industrial caustic soda production. The method comprises the following steps: 1, detecting the content of iodide ions in the raw material brine; 2, adding NaNO2 and Al2O3 into the raw material brine, adjusting the pH value to 1-4, magnetically stirring for 15-45min, and filtering to obtain a filtrate, wherein a molar ratio of NaNO2 to I<-> is 8.8*10<4>-9.8*10<4>, and a molar ratio of Al2O3 to I<-> is 1.3*10<5>-1.4*10<5>:1; and 3, adding the filtrate to an active carbon chromatography column, and carrying out chromatography for 15min. The method for removing a trace quantity of iodine from ion membrane caustic soda raw material brine has the advantages of operation at normal temperature under normal pressure, simple process and good adsorption effect; the content of iodine in treated brine is not greater than 0.15mg/L, and the lowest content can reach 0.111mg/L; an adsorbent can be recycled, so the production cost is reduced; and the removal method does not pollute the raw material brine.
Description
Technical field
The invention belongs to industrial alkaline field, be specifically related to a kind of method removing ionic membrane alkaline raw material salt Trace Iodine in Water.
Background technology
China has been the first in the world production of caustic soda big country, and shooting up of caustic industry facilitates the flourish of related industries, but still has certain gap compared with the advanced level of World Developed Countries, and particularly the ion-exchange membrane lifetime of ionic membrane alkali works use is short.One of prime cost of ion film caustic soda is ionic membrane, and not only itself is expensive, and its whether normal energy consumption and running cost directly determining production process.Iodide ion content height in raw material salt (halogen) water is one of important factor affecting service life of ion-exchange membrane.
In recent years, external each heavy ion film manufacturer, the E.I.Du Pont Company of the such as U.S., the chlorine engineering of Japan and Asahi Kasei Corporation find successively, and often containing more iodide ion and iodide in ionic membrane alkaline raw material salt solution, during electrolysis, these iodide ions and iodide can be oxidized to IO in anolyte
3 -, can IO be oxidized in film
4 -, the Ca in salt solution
2+, Mg
2+, Sr
2+, Ba
2+natively can reduce current efficiency and the voltage of ionic membrane Deng metal ion, iodate enters the alkaline environment in ionic membrane, and namely iodate is oxidized to periodate, and and Ca
2+, Mg
2+, Sr
2+, Ba
2+in conjunction with generating insoluble Periodic acid calcium and Periodic acid magnesium, Periodic acid strontium, barium periodate.Even if Ca
2+, Mg
2+, Sr
2+, Ba
2+content extremely low, the periodate in film also can precipitate with its formation, is deposited on ionic membrane, reduces the current efficiency of ionic membrane and voltage, shortens the work-ing life of ionic membrane.Iodide ion content generally in halogen (salt) water is more than the impact can accelerated during 0.4mg/L ionic membrane, and therefore, when Introduced From Abroad ionic membrane product, producer is proposed when using ionic membrane and requires that iodine content is lower than 0.2mg/L.
Developing multiple bittern both at home and abroad takes off iodine technology at present, for reducing the iodide ion content of raw material salt (halogen) water, and then can reduce the content of anolyte meso-periodic acid root and iodate, thus improves the life-span of ionic membrane.The bittern of current use takes off iodine technology and mainly contains several technology such as ion-exchange-resin process, Air blowing method and molecular sieve adsorption, wherein ion-exchange-resin process technology is relatively ripe, except iodine effect is better, but its resin dedicated relative price costly, running cost is higher, and resin regeneration process can produce a large amount of regeneration waste liquids, causes environmental pollution; Air blowing method is simple to operate, but only can remove the high price iodide ion in medium, iodine content can not be reduced to very low concentration range; It is good that molecular sieve adsorption removes iodine effectiveness comparison, but molecular sieve is unstable at aouatic structure, reclaims more difficult.Therefore, develop a kind of simple to operate, cost is low, the method that can remove ionic membrane alkaline raw material salt Trace Iodine in Water is well significant.
Summary of the invention
The object of this invention is to provide a kind of method removing ionic membrane alkaline raw material salt Trace Iodine in Water.
Based on above-mentioned purpose, the present invention adopts following technical scheme: a kind of method removing ionic membrane alkaline raw material salt Trace Iodine in Water, and step is:
(1) iodide ion content in raw material salt solution is detected;
(2) in raw material salt solution, NaNO is added
2and Al
2o
3, NaNO
2with I
-mol ratio be 8.8 × 10
4~ 9.8 × 10
4: 1, Al
2o
3be 1.3 × 10 with the mol ratio of iodide ion
5~ 1.4 × 10
5: 1, regulate pH=1 ~ 4, filter after magnetic agitation 15 ~ 45 min, obtain filtrate;
(3) filtrate is placed in chromatography 15 ~ 120min in activated carbon chromatography post.
NaNO in step (2)
2with Al
2o
3mass ratio be 1:1.
PH=1 is regulated in step (2).
Salt acid for adjusting pH is used in step (2).
Step (3) described gac is cocoanut active charcoal.
Step (3) described gac is used rear 0.05mol/L sodium hydroxide to carry out processing rear recirculation and is used.
In method provided by the invention, in salt solution, add Al
2o
3and NaNO
2after, under magnetic agitation effect, Al
2o
3and NaNO
2can by I
-be processed into elemental iodine (I
2) form, that is: 2I
--2e=I
2, I
2easily be attracted on granulated active carbon, by charcoal absorption elemental iodine (I
2), thus reach the object except iodine.
Compared with prior art, the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention operates at normal temperatures and pressures, technique is simple, advantages of good adsorption effect, salt solution iodine content≤0.15 mg/L after process, minimumly reaches 0.111 mg/L, and sorbent material can recycle, reduce production cost, meanwhile, removal methods provided by the invention can not pollute former bittern.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
embodiment 1 determination of the content of iodine is tested
The arsenic cerium catalytic water iodine detection kit using Wuhan all living creatures company to provide measures iodine content, and its principle utilizes iodine to the katalysis of arsenic cerium redox reaction: H
3asO
3+ 2Ce
4++ H
2o → H
3asO
4+ 2Ce
3++ 2H
+.Ce yellow in reaction
4+colourless Ce is reduced into by arsenus acid
3+, iodine content is higher, reacts faster, remaining Ce
4+then fewer, control temperature of reaction and time, remaining Ce in mensuration system under certain wavelength
4+absorbancy, can iodine content be obtained.
Concrete steps are: (1) gets iodine standard application serial solution respectively and each 0.2mL of water sample is placed in glass test tube, then adds 3.5mL arsenic chloride solution, and fully mixing is placed on 15min in 30 DEG C of waters bath with thermostatic control;
(2) use manual time-keeping, often pipe interval accurately adds 0.5mL ammonium cerous sulfate solution to each pipe in 15 ~ 30 seconds in order, mixes immediately, puts back in water-bath;
(3) when the first pipe adds accurate response 15min after ammonium cerous sulfate solution, often 1cm cuvette is used in 15 ~ 30 seconds in pipe interval under 420nm wavelength in order, measures the absorbancy of each pipe.
Quantitative relationship between iodine content C and the A of absorbancy is C=a+blnA, calculates the regression equation of typical curve, and the absorbance of sample is substituted into this equation, can obtain the iodine concentration of sample.
embodiment 2
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected according to the method for embodiment 1
-content, its measurement result is 0.152 mg/L.
(2) 1.0 g Al are added in every 100 ml salt solution
2o
3with 1.0 g NaNO
2, add hydrochloric acid and regulate pH=4, magnetic agitation 15min, filter to get filtrate.
(3) filtrate is divided into 3 groups, after the chromatography column chromatographic adsorption 15min that normal activated carbon, active fruit shell carbon, cocoanut active charcoal be housed, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculating the concentration of iodide ion in chromatographic solution, concrete outcome is in table 1.
Described raw material salt solution is from Haohua Yuhang Chemical Co., Ltd..
The adsorption effect of the different sorbing material of table 1
As can be seen from Table 1, after adopting the chromatography column absorption that cocoanut active charcoal is housed, in salt solution, the concentration of iodide ion is 110.6ug/L, and adsorption effect is best.Gac has good absorption property and chemical stability; apply more a kind of nonpolar sorbent material; thus the apolar substance that solubleness is little is easily adsorbed; iodine is concentrated integrated one deck adsorption layer (or claiming adsorption film) on activated carbon surface, and the internal surface of coconut husk granulated active carbon is maximum.
The coconut husk granulated active carbon used is from Heng Tai filter material factory of Gongyi City, and the performance perameter of this cocoanut active charcoal is in table 2.
The performance perameter of table 2 cocoanut active charcoal
embodiment 3
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected
-content, its measurement result is 0.152 mg/L.
(2) get 5 groups of samples, often organizing sample is 100 ml salt solution, adds 1.0 g Al in salt solution
2o
3with 1.0 g NaNO
2, in 4 groups of samples, add hydrochloric acid respectively regulate pH=1,2,3,4, the 5th group of sample does not add hydrochloric acid, and magnetic agitation 15 min, filters to get filtrate;
(3) after 5 groups of filtrates being used respectively the chromatography column chromatographic adsorption 15min that cocoanut active charcoal is housed, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution.
Use the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention, under condition of different pH, carry out aforesaid operations, concrete outcome is in table 3.
Experimental result under table 3 different pH condition
As can be seen from Table 3 as pH=1, the concentration of iodide ion is minimum, and concentration is 104.8ug/L, and the effect removing iodine is best.According to reaction principle
4H + + 2NaNO 2 + 4I -
===I 2 + 2NO+2NaI+H 2 oknown, this experiment x needs to carry out in acid condition, adopts salt acid for adjusting pH value, can reach required acidity, can not introduce impurity again in bittern.
embodiment 4
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected
-content, its measurement result is 0.152 mg/L.
(2) 1.0 g Al are added in every 100 ml salt solution
2o
3with 1.0 g NaNO
2, add hydrochloric acid and regulate pH=1, sample after magnetic agitation 15 min, 30 min, 45 min respectively, filter to get filtrate.
(3) after 3 groups of filtrates being used respectively chromatography column chromatographic adsorption 15 min that cocoanut active charcoal is housed, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution.
Use the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention, the magnetic agitation time on the impact of iodide ion removal effect in table 4.
The table 4 magnetic agitation time is on the impact of iodide ion removal effect
Magnetic agitation 15 min as can be seen from Table 4, the concentration of iodide ion is minimum, and concentration is 104.2 ug/L, and the effect removing iodine is best.When this experiment adopts Sodium Nitrite to make oxygenant, its oxidation rate is fast, and energy consumption is low, and the time, more long-acting fruit was bad on the contrary.
embodiment 5
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected
-content, its measurement result is 0.152 mg/L.
(2) 1.0 g Al are added in every 100 ml salt solution
2o
3with 1.0 g NaNO
2, add hydrochloric acid and regulate pH=1, after magnetic agitation 15min, filter to get filtrate.
(3) filtrate is divided into 6 groups, often organize after using respectively chromatography column chromatographic adsorption 15 min, 30 min of cocoanut active charcoal, 45 min, 60 min, 90 min, 120 min being housed, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution..
Use the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention, adsorption time on the impact of iodide ion removal effect in table 5.
Table 5 adsorption time is on the impact of iodide ion removal effect
As can be seen from Table 5, use that the concentration of iodide ion after the chromatography column chromatographic adsorption 15min of cocoanut active charcoal is housed is minimum, concentration is 103.7ug/L, and the effect removing iodine is best.
When 15 min, adsorptive capacity is maximum, extend adsorptive capacity along with adsorption time and diminish, this is because the process of activated carbon adsorption iodine belongs to physical adsorption, the speed of activated carbon adsorption iodine quickly, reach the adsorption equilibrium time used short, activated carbon particle diameter is less simultaneously, and iodine is short in the diffusion length of activated carbon surface, diffusional resistance is little, and rate of adsorption is fast.
embodiment 6
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected
-content, its measurement result is 0.152 mg/L.
(2) get 5 groups of samples, often organizing sample is 100 ml salt solution, first in salt solution, adds 1.0 g Al
2o
3, then in 5 groups of samples, add 0.2 g, 0.4 g, 0.6 g, 0.8 g, 1.0 g NaNO respectively
2, add hydrochloric acid and regulate pH=1, after magnetic agitation 15 min, filter to get filtrate.
(3) after adsorbing 15 min respectively in chromatography column filtrate being placed in being equipped with cocoanut active charcoal, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution.
Use the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention, Sodium Nitrite add-on on the impact of iodide ion removal effect in table 6.
Table 6 Sodium Nitrite add-on is on the impact of iodide ion removal effect
As can be seen from Table 6, NaNO
2addition when being 1.0g, i.e. NaNO
2with Al
2o
3mass ratio when being 1:1, I
-concentration minimum, concentration is 103.1ug/L, and the effect removing iodine is best.
embodiment 7
Remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, step is:
(1) I in raw material salt solution is detected
-content, its measurement result is 0.152 mg/L.
(2) get 5 groups of samples, often organizing sample is 100 ml salt solution, adds 0.2 g, 0.4 g, 0.6 g, 0.8 g, 1.0 g Al respectively often organizing in sample
2o
3, then in 5 groups of samples, all add 1.0 g NaNO
2, add hydrochloric acid and regulate pH=1, after magnetic agitation 15 min, filter to get filtrate.
(3) after adsorbing 15 min respectively in chromatography column filtrate being placed in being equipped with cocoanut active charcoal, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution.
Use the method removing ionic membrane alkaline raw material salt Trace Iodine in Water provided by the invention, Al
2o
3add-on on the impact of iodide ion removal effect in table 7.
Table 7 aluminum oxide add-on is on the impact of iodide ion removal effect
As can be seen from Table 7, aluminum oxide plays a driving role, when the addition of aluminum oxide is 1.0g, i.e. and Sodium Nitrite and Al
2o
3mass ratio when being 1:1, the concentration of iodide ion is minimum, and concentration is 103.1ug/L, and the effect removing iodine is best.
embodiment 8 measures iodine absorption number and cocoanut active charcoal magnitude relation is tested
The relation between iodine absorption number and cocoanut active charcoal consumption is measured according to following steps:
(1) in salt solution, add 1ppm iodide ion, the concentration measuring iodide ion is 1126.2 ug/L.
(2), in experimentation, in every 300 ml salt solution, 2.7 ~ 3.0 grams of Al are added
2o
3with 2.7 ~ 3.0 grams of NaNO
2, add hydrochloric acid and regulate pH=1, after magnetic agitation 15 min, filter to get filtrate.
(3) filtrate is divided into 3 groups, use different model that the chromatography column chromatographic adsorption of cocoanut active charcoal is housed respectively, control salt solution flow velocity, after adsorbing 15 min, use UV, visible light spectrophotometer (WFZ UV-2000, outstanding Nico Shanghai Instrument Ltd.) measure the absorbancy of chromatographic solution, and then calculate the concentration of iodide ion in chromatographic solution..
The relation test-results of iodine absorption number and cocoanut active charcoal consumption is in table 8.
The relation of table 8 iodine absorption number and cocoanut active charcoal consumption
In process of the test, 30 g cocoanut active charcoal chromatography columns often adsorb 100 mL salt solution, with 0.05 M sodium hydroxide 200 mL process once; 93 g cocoanut active charcoal chromatography columns often adsorb 400 mL salt solution, with sodium hydroxide 0.05 M 600 mL process once; 347 g cocoanut active charcoal chromatography columns often adsorb 1100 mL salt solution, with 0.05 M sodium hydroxide 2200 mL process once.
As can be seen from Table 8, iodine absorption becomes quantitative relationship with the amount of cocoanut active charcoal.
Claims (6)
1. remove a method for ionic membrane alkaline raw material salt Trace Iodine in Water, it is characterized in that, step is:
(1) iodide ion content in raw material salt solution is detected;
(2) in raw material salt solution, NaNO is added
2and Al
2o
3, NaNO
2with I
-mol ratio be 8.8 × 10
4~ 9.8 × 10
4: 1, Al
2o
3be 1.3 × 10 with the mol ratio of iodide ion
5~ 1.4 × 10
5: 1, regulate pH=1 ~ 4, filter after magnetic agitation 15 ~ 45 min, obtain filtrate;
(3) filtrate is placed in chromatography 15 ~ 120min in activated carbon chromatography post.
2. remove the method for ionic membrane alkaline raw material salt Trace Iodine in Water according to claim 1, it is characterized in that, NaNO in step (2)
2with Al
2o
3mass ratio be 1:1.
3. according to claim 1 or 2, remove the method for ionic membrane alkaline raw material salt Trace Iodine in Water, it is characterized in that, in step (2), regulate pH=1.
4. remove the method for ionic membrane alkaline raw material salt Trace Iodine in Water according to claim 3, it is characterized in that, in step (2), use salt acid for adjusting pH.
5. remove the method for ionic membrane alkaline raw material salt Trace Iodine in Water according to claim 4, it is characterized in that, step (3) described gac is cocoanut active charcoal.
6. remove the method for ionic membrane alkaline raw material salt Trace Iodine in Water according to claim 5, it is characterized in that, step (3) described gac is used rear 0.05mol/L sodium hydroxide to carry out processing rear recirculation and is used.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293526A (en) * | 2015-10-26 | 2016-02-03 | 天津科技大学 | Method for purifying iodine in saline water of ionic membrane caustic soda production process |
| CN105293779A (en) * | 2015-11-24 | 2016-02-03 | 天津科技大学 | Purification device of iodine in brine by ionic membrane caustic soda production process and operating method thereof |
| CN105905927A (en) * | 2016-06-20 | 2016-08-31 | 中盐金坛盐化有限责任公司 | Brine purification device and method for removing strontium element from sodium sulfate type brine |
| CN106082278A (en) * | 2016-06-20 | 2016-11-09 | 中盐金坛盐化有限责任公司 | A kind of Galuber's salt type brine removes the purification method of strontium element |
| WO2019039759A1 (en) * | 2017-08-23 | 2019-02-28 | 에스케이케미칼 주식회사 | Method for producing mono-iodobenzene and mono-iodobenzene produced therefrom |
| CN111307746A (en) * | 2019-12-16 | 2020-06-19 | 哈尔滨医科大学 | Kit for detecting iodine concentration |
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| CN1807245A (en) * | 2005-01-18 | 2006-07-26 | 新汶矿业集团有限责任公司 | Removal of minim iodine ion from brine liquor which is material of caustic soda produced by ion membrane method |
| CN103305863A (en) * | 2013-06-19 | 2013-09-18 | 北京化工大学 | Deep iodine removing method for brine by ionic membrane caustic soda |
-
2014
- 2014-11-27 CN CN201410694358.9A patent/CN104495877B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807245A (en) * | 2005-01-18 | 2006-07-26 | 新汶矿业集团有限责任公司 | Removal of minim iodine ion from brine liquor which is material of caustic soda produced by ion membrane method |
| CN103305863A (en) * | 2013-06-19 | 2013-09-18 | 北京化工大学 | Deep iodine removing method for brine by ionic membrane caustic soda |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105293526A (en) * | 2015-10-26 | 2016-02-03 | 天津科技大学 | Method for purifying iodine in saline water of ionic membrane caustic soda production process |
| CN105293779A (en) * | 2015-11-24 | 2016-02-03 | 天津科技大学 | Purification device of iodine in brine by ionic membrane caustic soda production process and operating method thereof |
| CN105905927A (en) * | 2016-06-20 | 2016-08-31 | 中盐金坛盐化有限责任公司 | Brine purification device and method for removing strontium element from sodium sulfate type brine |
| CN106082278A (en) * | 2016-06-20 | 2016-11-09 | 中盐金坛盐化有限责任公司 | A kind of Galuber's salt type brine removes the purification method of strontium element |
| WO2019039759A1 (en) * | 2017-08-23 | 2019-02-28 | 에스케이케미칼 주식회사 | Method for producing mono-iodobenzene and mono-iodobenzene produced therefrom |
| CN111307746A (en) * | 2019-12-16 | 2020-06-19 | 哈尔滨医科大学 | Kit for detecting iodine concentration |
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|---|---|
| CN104495877B (en) | 2016-06-08 |
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