CN1303008C - Process for removing trace ammonia from high purity water - Google Patents
Process for removing trace ammonia from high purity water Download PDFInfo
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- CN1303008C CN1303008C CNB200410053426XA CN200410053426A CN1303008C CN 1303008 C CN1303008 C CN 1303008C CN B200410053426X A CNB200410053426X A CN B200410053426XA CN 200410053426 A CN200410053426 A CN 200410053426A CN 1303008 C CN1303008 C CN 1303008C
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 100
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000012498 ultrapure water Substances 0.000 title claims abstract description 15
- 230000008569 process Effects 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 65
- 150000003839 salts Chemical class 0.000 claims abstract description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- 238000011033 desalting Methods 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 11
- 238000010612 desalination reaction Methods 0.000 abstract 1
- 238000012544 monitoring process Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 11
- 239000012528 membrane Substances 0.000 description 9
- 241000047703 Nonion Species 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000011347 resin Substances 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 238000003556 assay Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000005684 electric field Effects 0.000 description 3
- 238000000909 electrodialysis Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 238000001223 reverse osmosis Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 210000002700 urine Anatomy 0.000 description 2
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 description 1
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 description 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000003011 anion exchange membrane Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000009615 deamination Effects 0.000 description 1
- 238000006481 deamination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
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- Water Treatment By Electricity Or Magnetism (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
一种去除高纯水中痕量氨的方法，涉及一种去除高纯水除氨工艺。先将氨浓度为20-250mg/L的水，按流量为1.0～2.0L/min泵入EDI。控制EDI电流1.0～3.0A，、进水(淡室、浓室、极室)流量分别为0.9～1.8L/min、0.1～0.2L/min和0.05L/min。EDI浓室加盐浓度满足电导率为1000μS/cm，浓室进水的电导率为61-266μS/cm等。随即监测淡室出水中总氨的浓度，能快速达到水中总氨含量＜0.5mg/L。本发明能同时去除水中离子态铵和非离子态氨，去除率达99.9%以上，且工艺简单，操作方便，可无人监控，无二次污染。设备占地而积少，适合核电站、太空、电子工业、分析实验室等各种场合和规模用于去除高纯水中痕量氨。
A method for removing trace amounts of ammonia in high-purity water relates to a process for removing ammonia from high-purity water. First pump water with an ammonia concentration of 20-250mg/L into the EDI at a flow rate of 1.0-2.0L/min. Control the EDI current to 1.0-3.0A, and the flow rate of the water inflow (dilute chamber, concentrated chamber, pole chamber) to be 0.9-1.8L/min, 0.1-0.2L/min and 0.05L/min respectively. The concentration of salt added to the EDI concentration chamber meets the conductivity of 1000μS/cm, and the conductivity of the water entering the concentration chamber is 61-266μS/cm. Immediately monitor the concentration of total ammonia in the effluent of the desalination chamber, and quickly reach the content of total ammonia in the water <0.5mg/L. The invention can simultaneously remove ionic ammonium and non-ionic ammonia in water, with a removal rate of over 99.9%, simple process, convenient operation, unattended monitoring and no secondary pollution. The equipment occupies a small area and is suitable for removing trace ammonia in high-purity water in various occasions and scales such as nuclear power plants, space, electronics industry, and analytical laboratories.
Description
Technical field
The present invention relates to a kind of technology of removing Trace Ammonia in the high purity water.
Background technology
At present, have many fields such as Nuclear power plants, universe space, electronic industry, assay laboratory etc. to need to use the high purity water of low ammonia, because its special equipment or environment or technology etc., they are to NH in the employed high purity water
3The requirement of content is very strict, can not contain ammonium ion and can not contain non-ion state ammon, only allows to contain the following Trace Ammonia of 0.5mg/L.As everyone knows, though it is a lot of to remove the method for ammonia in the water, all can not reach above-mentioned requirement to ammonia content.Exemplify 4 methods of removing ammonia in the water below.
One of method: with electrodialysis (ED) is to remove ammonium ion in the water, but effect is bad, generally can only be used for the processing that ammonium ion concentration is higher than the industry of 200mg/L.
Two of method: can remove ammonium ion in the water with reverse osmosis (RO), but can not remove non-ion state ammon.
Three of method: can remove ammonia with ion-exchange (LX), but need to select ammonia is had the resin of special selective adsorption, cost an arm and a leg.And no matter use which kind of ion exchange resin, and all need continuous regeneration, expensive big, the while contaminate environment.
Four of method: biological degradation (SBR) can only be removed to about 2mg/L at most.Be removed to＜0.5mg/L is unapproachable.And also be not suitable for for high strength ammonia, can only be below 50mg/L.
In a word, above method is except all existing separately some problems, and it is all undesirable to remove underwater trace ammonia, is difficult to satisfy the harsh requirement of above-mentioned field to low ammonia high purity water.
Summary of the invention
The objective of the invention is to disclose the method for Trace Ammonia in the removal high purity water that a kind of technology is simple, deamination is effective, speed is fast, floor space is little, working cost is low.
In order to achieve the above object, the present invention adopts the technology of electric desalting (EDI) and corresponding coupling that the high purity water that contains ammonia is handled, and makes ammonia content＜0.5mg/L in the water.Concrete steps are as follows:
At first, be the water of 20-200mg/L with ammonia concentration, be that 1.0～2.0L/min pumps into EDI by flow.Then, with the current control of EDI at 1.0～3.0A, with light chamber flow, the dense chamber flow of EDI with utmost point chamber flow is controlled at 0.9～1.8L/min, 0.1～0.2L/min respectively and 0.05L/min advances water.Then, adding NaCl and control the specific conductivity that adds in the salt water tank in adding salt water tank is 1000 μ S/cm, by with the salt volume pump with above-mentioned salt solution, pump into dense chamber water inlet place, enter EDI, making the specific conductivity of dense chamber water inlet is 61-266 μ S/cm, open dense water-circulating pump simultaneously, to discharge through the dense chamber of the part water outlet of EDI processing by dense water-circulating pump on the one hand, controlling dense chamber, to go out electrical conductivity of water be 250～300 μ S/cm, and dense on the other hand chamber current circulate with dense water-circulating pump.At last, monitor the concentration of total ammonia in the light chamber water outlet (product water), found that to reach total ammonia content＜0.5mg/L in the water fast.
Advantage of the present invention is as follows:
Because the inventive method adopts EDI, controls low current, with technologies such as salt circulations, therefore can remove water intermediate ion attitude ammonia and non-ion state ammon simultaneously, can make that ammonia content is dropped to＜0.5mg/L fast by 200mg/L in the water, clearance reaches more than 99.9%.
2. compare with RO, ED, LX, SBR method, it is thorough that present method is removed ammonia, minimum can reaching＜0.026mg/L, satisfy fully waters such as Nuclear power plants, space, electronic industry, assay laboratory (general tap water requires＜0.5mg/L) requirement.The utilization ratio height of water reaches 90～95% (ED＜50%, RO has only 50～75%).
Since in the inventive method the EDI module volume that uses less, and equipment is simple, floor space is few, is fit to as various occasions and scale uses such as Nuclear power plants, universe space, electronic industry, assay laboratory.
4. to remove the method technology of ammonia simple, easy to operate in the present invention, can no worker monitor, and non-secondary pollution.
Description of drawings
Fig. 1 is a process flow sheet of the present invention
Fig. 2 is that ammonia of the present invention is removed the reaction mechanism synoptic diagram
Embodiment
See also Fig. 1.At first, be the 20-250mg/L high purity water with ammonia concentration, put into the EDI water tank inlet, be that 1.0～2.0L/min pumps into EDI with the EDI intake pump with ammoniated water management flow in the water tank.Then, the EDI current control is at 1.0～3.0A, and light chamber flow, dense chamber flow and utmost point chamber flow are controlled at respectively under 0.9～1.8L/min, 0.1～0.2L/min and the 0.05L/min situation intakes.Then, add NaCl in adding salt water tank, the specific conductivity that control adds in the salt water tank is 1000 μ S/cm.Control adds the salt pump opening degree, and the specific conductivity of dense chamber water inlet is remained in the 61-266 μ S/cm scope.Dense chamber current circulate with the dense water-circulating pump of EDI, the part concentrated water discharge, and controlling dense chamber, to go out electrical conductivity of water be 250～300 μ S/cm.At last, monitor the concentration＜0.5mg/L of the total ammonia in the light chamber water outlet (product water), promptly reached purpose of the present invention.
Adopt aforesaid method to handle the result who contains ammoniacal liquor and see also table one and table two.
The non-ion state ammon content of table one: EDI water inlet solution
| pH | 10.91 | 10.80 | 10.78 | 10.76 |
| The total ammonia (mg/L) of intaking | 208.3 | 187.7 | 156.9 | 150.4 |
| Intake non-ion state ammon (mg/L) in total ammonia | 200.3 | 180.1 | 149.9 | 143.6 |
| The shared per-cent of the total ammonia of nonionic attitude (%) | 96.1 | 96.0 | 95.5 | 95.4 |
| The total ammonia of water outlet (mg/L) | 0.072 | 0.054 | ＜0.026 | ＜0.026 |
Annotate: the pH value in the table one is measured with pH meter, total ammonia usefulness 722S type spectrophotometric determination of intaking.By table one as can be seen, even the pH value in water inlet reaches at 10.91 o'clock (the pKa value 9.25 that is higher than ammonia), non-ion state ammon in water inlet this moment is 96.1%, basically be that form with non-ion state ammon exists, but after one-level EDI processing, total ammonia concentration that also can make high purity water is by 208.3mg/L removal dropping to 0.072mg/L.
The ionic state ammonia content of table two: EDI water inlet solution
| NH in the water inlet 4Cl concentration mg/L | Water inlet specific conductivity μ S/cm | NH in the water outlet 4 +Concentration mg/L |
| 20 | 61 | 0.0067 |
| 40 | 118.3 | 0.0081 |
| 60 | 173 | 0.0094 |
| 100 | 266 | 0.0158 |
NH in table two water outlet
4 +Concentration is according to experiment and calculating, as can be seen, and different water inlet ammonium ion concentration, NH in the water outlet
4 +Concentration is all lower.
It is as follows that ammonia is removed reaction mechanism:
EDI mainly is made up of ion exchange resin, ion selectivity exchange membrane and electrode, its principle of work is that electrode produces voltage to order about ion migration, because the selection perviousness of ion selectivity exchange membrane: negatively charged ion can only see through anion-exchange membrane (abbreviation cavity block), and can not see through cationic exchange membrane (abbreviation anode membrane); Positively charged ion can only see through anode membrane, and can not see through cavity block, makes the yin, yang ion migration to the ion selectivity exchange membrane and rest in the dense chamber like this.Can understand like this: after pending high purity water enters light chamber, ammonium ion enters into resinbed by diffusion, after the mobile ion exchange of going up mutually with resin, ammonium ion migrates to the ion selectivity exchange membrane at resin in mutually under effect of electric field, enter dense chamber by the ion selectivity exchange membrane at last, thereby reach the purpose of removing ammonium ion.
EDI is the membrane sepn process that DC electric field drives, and is filled with ion exchange resin in the light chamber, under certain operational condition, resin one water termination place generation " hydrolytic dissociation " in the light chamber (
) generation H
+And OH
-, the resin of filling is carried out electricity regeneration, make a part of resin be in good reproduced state all the time, abundant regenerated ion exchange resin can make nonionic attitude material be converted into the ionic state material (
), and then under the effect of DC electric field,, remove these nonionic attitude materials quickly and effectively by ion migration.Therefore can successive, economic operation is applied to total ammonia (nonionic attitude and ionic state ammonia) concentration from 200mgL
-1Drop to after the removal＜0.5mgL
-1Processing.When the waste liquid that discharges in the pressurised water reactors of space station water and nuclear reactor needs recycle, and electronic industry water and analyzing in the experimental water, EDI will be a kind of good ammonia-removal method.
Wherein: people's urine is the portion water resource in the space water.The urea of people's urine can resolve into gaseous ammonia and ammonium ion, degradation production such as three following chemical equations:
Ammonium ion generates as the degradation production of urinating in the formula, and constantly accumulation is increased its concentration, makes water no longer be fit to drinking of people.The EDI floor space is little, power consumption is low and can reach drinking-water with method treatment effect of the present invention at last requires (the total ammonia of water outlet＜0.5mg/L), satisfy the needs of space water fully.
Claims (1)
1. method of removing Trace Ammonia in the high purity water, it is characterized in that: at first, being the water of 20-250mg/L with ammonia concentration, is that 1.0～2.0L/min pumps into electric desalting by flow; Then, with the current control of electric desalting at 1.0～3.0A, with light chamber flow, the dense chamber flow of electric desalting with utmost point chamber flow is controlled at 0.9～1.8L/min, 0.1～0.2L/min respectively and 0.05L/min advances water; Then, adding NaCl and control the specific conductivity that adds in the salt water tank in adding salt water tank is 1000 μ S/cm, above-mentioned salt solution is pumped into dense chamber water inlet place enter electric desalting by adding salt pump, making the specific conductivity of dense chamber water inlet is 61-266 μ S/cm, open dense water-circulating pump simultaneously, to discharge through the dense chamber of the part water outlet of electric desalting processing by dense water-circulating pump on the one hand, controlling dense chamber, to go out electrical conductivity of water be 250～300 μ S/cm, and dense on the other hand chamber current circulate with dense water-circulating pump; At last, monitor the concentration of total ammonia in the water outlet of light chamber, found that to reach total ammonia content＜0.5mg/L in the water fast.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410053426XA CN1303008C (en) | 2004-08-04 | 2004-08-04 | Process for removing trace ammonia from high purity water |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200410053426XA CN1303008C (en) | 2004-08-04 | 2004-08-04 | Process for removing trace ammonia from high purity water |
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| Publication Number | Publication Date |
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| CN1587092A CN1587092A (en) | 2005-03-02 |
| CN1303008C true CN1303008C (en) | 2007-03-07 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20060091077A1 (en) * | 2004-10-29 | 2006-05-04 | Ecolochem, Inc. | Concentrate recycle loop with filtration module |
| CN111672327A (en) * | 2020-07-16 | 2020-09-18 | 上海核工程研究设计院有限公司 | A test system and method for the performance of steam generator blowdown ionization demineralization membrane stack |
| CN112981434A (en) * | 2021-02-08 | 2021-06-18 | 贵州荣福龙工程科技有限公司 | Method and system for preparing caustic soda and co-producing sulfuric acid from sodium sulfate |
| CN113277602A (en) * | 2021-07-02 | 2021-08-20 | 浙江浙能技术研究院有限公司 | Device and method for continuously removing cations in water for hydrogen conductivity measurement |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4969983A (en) * | 1988-07-11 | 1990-11-13 | Ionics, Incorporated | Apparatus and process for the removal of acidic and basic gases from fluid mixtures using bipolar membranes |
| WO2003055604A1 (en) * | 2001-12-27 | 2003-07-10 | Ebara Corporation | Electric demineralization apparatus |
| US20040060875A1 (en) * | 2002-08-06 | 2004-04-01 | Lin Yupo J. | Electrodionization method |
| CN1504428A (en) * | 2002-12-05 | 2004-06-16 | 彭昌盛 | Method and apparatus for preparing pure water by continuous electricity deionizing |
-
2004
- 2004-08-04 CN CNB200410053426XA patent/CN1303008C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4969983A (en) * | 1988-07-11 | 1990-11-13 | Ionics, Incorporated | Apparatus and process for the removal of acidic and basic gases from fluid mixtures using bipolar membranes |
| WO2003055604A1 (en) * | 2001-12-27 | 2003-07-10 | Ebara Corporation | Electric demineralization apparatus |
| US20040060875A1 (en) * | 2002-08-06 | 2004-04-01 | Lin Yupo J. | Electrodionization method |
| CN1504428A (en) * | 2002-12-05 | 2004-06-16 | 彭昌盛 | Method and apparatus for preparing pure water by continuous electricity deionizing |
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