CN103030224B - A kind of deionized water does the circulating water treatment method of moisturizing - Google Patents
A kind of deionized water does the circulating water treatment method of moisturizing Download PDFInfo
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Abstract
The present invention relates to a kind of circulating water treatment method that deionized water does moisturizing.It comprises the following steps: a) pH value of controlled circulation water is at 9-11.5; B) add type oxide film inhibiter, described type oxide film inhibiter is the mixture of at least two kinds of salt being selected from tungstate, molybdate, vanadate; C) add environment-friendly type sterilant, described environment-friendly type sterilant is hydrogen peroxide and ozone.Circulating water treatment method of the present invention is applicable to the sewage after second-stage treatment as the recirculating cooling water system process of moisturizing after bi-membrane method process, can effectively control corrosion rate and microorganism growth.
Description
Technical field
The present invention relates to a kind of circulating water treatment method, relate in particular to a kind of circulating water treatment method doing moisturizing with deionized water.
Background technology
As everyone knows, in industries such as petrochemical complex, thermal power generation, metallurgy, need to use large water gaging, wherein water coolant accounts for significant proportion, as petroleum chemical enterprise's water coolant water accounts for more than 80% of water of productive use.Nowadays water resources shortage, water saving becomes world theme.Sewage and Treated sewage reusing will be reduced the consumption of fresh water greatly in recirculated water, even realize spot patch fresh water.
The U.S. achieved in the sixties in 20th century can discharge urban sewage recycling in power generation cycle water system, and the nineties achieves qualified discharge Waste Water Reuse and petrochemical equipment circulating water system.The method taked is that sewage is carried out advanced treatment, reduces COD, suspended substance and microorganism concn in qualified discharge sewage, then uses corrosion and scaling and the microorganism of water conditioner operating device.
Sewage and Treated sewage reusing have two kinds in the method for recirculated water.One is advanced treatment, by sewage reuse after coagulation, precipitation, filtration, sterilization again after second-stage treatment.Another kind is bi-membrane method, passes into ultrafiltration reverse osmosis device by the water after second-stage treatment after coagulation, precipitation, filtration, and water outlet is deionized water.Bi-membrane method investment cost is large, but, because there is no the fouling factor in deionized water, be applied to circulating cooling make-up water, scale problems can be ignored, and therefore greatly can improve cycles of concentration, but also save the expense of Scale inhibitors, and in addition can also extension device working life, save overhaul of the equipments expense.Visible employing deionized water can reduce later stage expense.Deionized water does circulating cooling make-up water needs the problem solved to be corrosion and microbiological manipulation.
CN1338433A discloses and in the sewage of qualified discharge, adds sterilant carry out disinfection, and adds alkaline matter and makes pH value control to carry out inhibition at 9.5-14.Its shortcoming is: because there is dissolved oxygen in water, and depending merely on adjust ph can not control corrosion rate effectively.
CN1524806A discloses and the water of high oily(waste)water after oil removal, sedimentation is introduced circulating water system, meanwhile, adds inorganic base substance and makes pH value reach 7-11, add sterilant and corrosion inhibiting and descaling agent.The chlorine such as clorox, trichloroisocyanuric acid series bactericidal agent selected by sterilant, corrosion inhibiting and descaling agent selects organophosphorus, Sodium hexametaphosphate 99, Sodium orthomolybdate etc.Its shortcoming is: chlorine series bactericidal agent can lose efficacy in the basic conditions, if the phosphorus containg substances such as organophosphorus, Sodium hexametaphosphate 99 can cause body eutrophication with sewage discharge.
CN1393411A have studied a kind of composite corrosion inhibitor for deionized water, and composition is made up of deionized water, polyetheramides, silicate.Form different from inhibiter of the present invention, and the present invention is circulating water treatment method.
Summary of the invention
A kind of deionized water is the object of the present invention is to provide to do the circulating water treatment method of moisturizing.
For reaching above object, the invention provides a kind of circulating water treatment method using deionized water as moisturizing, comprising the following steps: a) pH value of controlled circulation water is at 9-11.5; B) add type oxide film inhibiter, described type oxide film inhibiter is the mixture of at least two kinds of salt being selected from tungstate, molybdate, vanadate; C) add environment-friendly type sterilant, described environment-friendly type sterilant is hydrogen peroxide or ozone.
The present invention preferably uses the pH value of alkaline matter controlled circulation water, the one of described alkaline matter preferably in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood.
Consider price factor, when effect is close, the general particular certain cancers inhibiter of the present invention.
Tungstate of the present invention is selected from tungstate and is selected from sodium wolframate and potassium wolframate; Molybdate is selected from Sodium orthomolybdate and potassium molybdate; Vanadate is selected from ortho-vanadate and metavanadate.Tungstate is preferably from anhydrous wolframic acid sodium, tungstate dihydrate acid sodium and anhydrous wolframic acid potassium; Molybdate is preferably from anhydrous molybdic acid sodium, Sodium Molybdate Dihydrate and five water potassium molybdates; Vanadate is preferably from 12 water sodium orthovanadates, ortho-vanadic acid potassium, two water sodium metavanadates, anhydrous sodium metavanadate, potassium metavanadate.
Composite corrosion inhibitor of the present invention relative to the effective concentration of each component of pending aqueous solution total amount is: molybdate is 20-50mg/L, and tungstate is 20-50mg/L, and vanadate is 20-50mg/L
Ozone of the present invention is produced by ozonizer, and the after-odour oxygen content control in water is at 0.05-0.1mg/L; The frequency that adds of hydrogen peroxide is that every 2-4 days adds once, and adding concentration is 20mg/L.
Inhibiter b) described in step of the present invention can add in the mode of single dose, also first can be mixed with composite corrosion inhibitor, is more once added in recirculated water by composite scale-inhibiting corrosion inhibitor, preferably carries out in the mode of the latter.Using conventional procedures prepares composite corrosion inhibitor of the present invention, and the reinforced order of each component is unimportant, such as, by vanadate, molybdate, tungstate and water by the mixing of predetermined concentration, can obtain required composite corrosion inhibitor.
The addition step of circulating water treatment method of the present invention is unimportant, can be undertaken successively, also can carry out a)-c by other arbitrary orders by a), b) and c) step) step, these three steps can also be carried out simultaneously.
Method of the present invention is applicable to the recirculating cooling water system process as moisturizing after bi-membrane method process of the sewage after second-stage treatment, can effectively control corrosion rate and microorganism growth.Inhibiter toxicity used is low, generates oxygen G&W environmentally safe after sterilant degraded used.
Embodiment
Corrosion inhibitor formula embodiment below will contribute to the present invention is described, but not limit to its scope.Test water is deionized water, and carbon steel test piece is 20# steel.Test water water quality is in table 1.
Table 1 quality of de-ionized water
| Specific conductivity/(us/cm) | PH value | Total molten solid/ppb |
| 2 | 6.0 | 300 |
The measuring method of water quality is with reference to as follows:
PH value: GB/T 6920-1986 " the mensuration glass electrode method of water pH value "
Specific conductivity: GB/T 6908-2008 " mensuration of boiler feed water river water coolant analytical procedure specific conductivity "
Total molten solid: the GB/T 14415-2007 mensuration of solid matter " in industrial circulating cooling water and the boiler feed water ".
Corrosion inhibition and the bactericidal property assessment method of following embodiment gained are as follows:
corrosion inhibitionthe test piece of 20# qualitative carbon steel be fixed on lacing film instrument, put into the test water being added with the drug concentration added by embodiment, steady temperature 45 ± 1 DEG C, keep rotating speed 75rpm to rotate 72h, the weight of test piece before and after record test, calculates average corrosion rate.
Average corrosion rate calculation formula is: F=(C × △ W)/(A × T × ρ)
C: computational constant, during with mm/a (millimeter/year) for unit, C=8.76 × 10
7
△ W: the corrosion weight loss (g) of test specimen
A: the area (cm of test specimen
2)
T: corrosion test time (h)
ρ: the density (kg/m of material for test
3).
the mensuration of heterotrophic bacterium:get test water, in sterilisable chamber, adopt former water 10 times of dilution technologies, test water is diluted to suitable multiple, and the water sample of corresponding extension rate is inoculated in culture dish.Then aseptic culture medium being poured in culture dish, mix with water sample, cultivating 72 ± 4h etc. being inverted after culture medium solidifying to be placed in the incubator of 29 ± 1 DEG C.After cultivation, take out culture dish, select those culture dish with 30-300 bacterium colony to count, colony number is multiplied by the heterotrophic bacterium number that corresponding dilution training number is this water sample.
adhere to the mensuration of speed:be positioned on by test tube in the bypass of interchanger, take out test tube after off-test, after cleaning test tube outer wall, constant temperature drying, takes the heavy (W of band bur test tube
1).Then inboard wall of test tube bur is cleaned, dry, take the heavy (W of test tube
2), calculate and adhere to speed F '.
F’=7.2×10
5×(W
1-W
2)/（A×t）
A: the area (cm of test specimen
2)
T: corrosion test time (h).
Embodiment 1
Taking 35.0g anhydrous molybdic acid sodium and 50.5g tungstate dihydrate acid sodium, to join 114.5g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of Sodium orthomolybdate and sodium wolframate is respectively 35 mg/L, 45mg/L, by potassium hydroxide control ph 10.5, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0341mm/a.
Embodiment 2
Taking 29.4g Sodium Molybdate Dihydrate and 77.4g 12 water sodium orthovanadate, to join 93.2g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of Sodium orthomolybdate and sodium orthovanadate is respectively 25mg/L, 35mg/L, by sodium hydroxide control ph 11.2, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0401mm/a.
Embodiment 3
Taking 35.0g anhydrous wolframic acid sodium and the anhydrous sodium metavanadate of 45.0g, to join 120.0g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of wooden sodium wolframate and sodium metavanadate is respectively 35 mg/L, 45mg/L, by potassium hydroxide control ph 10.5, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0395mm/a.
Embodiment 4
Taking 62.0g five water potassium molybdate and 35.0g potassium metavanadate, to join 103.0g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of potassium molybdate and potassium metavanadate is respectively 45mg/L, 35mg/L, by salt of wormwood control ph 10.0, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0395mm/a.
Embodiment 5
Taking 30.0g anhydrous wolframic acid potassium and 30.0g ortho-vanadic acid potassium, to join 140.0g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of potassium wolframate and ortho-vanadic acid potassium is respectively 30mg/L, 30mg/L, by potassium hydroxide control ph 11.0, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0400mm/a.
Embodiment 6
Take 35.3g Sodium Molybdate Dihydrate, 28.1g tungstate dihydrate acid sodium and 31.6g bis-water sodium metavanadate and join 105.0g deionized water for stirring evenly, be made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of Sodium orthomolybdate, sodium wolframate, sodium metavanadate is respectively 30mg/L, 25mg/L, 25mg/L, by sodium carbonate control ph 9.20, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0218mm/a.
Comparative example 1
Take 80.0g anhydrous molybdic acid sodium and join 120.0g deionized water for stirring evenly, be made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of Sodium orthomolybdate is respectively 80mg/L, by sodium hydroxide control ph 10.5, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.0926mm/a.
Comparative example 2
Taking 52.9g Sodium Molybdate Dihydrate and 44.2g 12 water sodium orthovanadate, to join 102.9g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of Sodium orthomolybdate and sodium orthovanadate is respectively 45mg/L, 35mg/L, not adjust pH is 45 DEG C in temperature, and rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.3210mm/a.
Comparative example 3
Taking 35.0g anhydrous wolframic acid sodium and the anhydrous sodium metavanadate of 45.0g, to join 120.0g deionized water for stirring even, is made into inhibiter 200.0g of the present invention.
The inhibiter of the present embodiment and deionized water are carried out rotary hanging plate experiment, in water, the concentration that effectively adds of wooden sodium wolframate and sodium metavanadate is respectively 35 mg/L, 45mg/L, not adjust pH, be 45 DEG C in temperature, rotating speed is that to record erosion rate after running 72h under 75r/min condition be 0.3158mm/a.
Comparative example 4
Carrying out control corrosion rate separately through with sodium hydroxide adjust pH, is 45 DEG C in temperature, and rotating speed is record corrosion data as table 2 after running 72h under 75r/min condition.
Table 2 pH value is on the impact of corrosion of carbon steel
| PH value | 10.0 | 11.0 | 12.0 |
| Erosion rate (mm/a) | 1.0345 | 0.0483 | 0.0722 |
Embodiment 6
In order to simulated field, carry out dynamic analog test.Dynamic analog test method is undertaken by People's Republic of China (PRC) chemical industry standard HG/T2160-2008, and controling parameters is as follows.
Test water quality: test water (deionized water)
Flow velocity: 1.0m/s
Temperature in: 32 ± 1 DEG C of temperature difference: 10 DEG C
Days running: 15 days.
A tower: first add the composite corrosion inhibitor in embodiment 1, the effective concentration of Sodium orthomolybdate and sodium wolframate in water is made to be respectively 35 mg/L, 45mg/L, then adding the effective concentration that hydrogen peroxide makes it in water is 20mg/L, be 10.5 by potassium hydroxide adjust ph simultaneously, density of corrosion inhibitor will be controlled in real time afterwards and pH value remains unchanged.Hydrogen peroxide added once every three days.Analog result is in table 3, table 4.
B tower: first pass into ozone with ozonizer in recirculated water, the ozone concn in water is made to reach 0.05mg/L, then the composite corrosion inhibitor in embodiment 3 is added, the effective concentration of sodium wolframate and sodium metavanadate in water is made to be respectively 35mg/L, 45mg/L, be 10.5 by potassium hydroxide adjust ph simultaneously, will control density of corrosion inhibitor in real time afterwards and pH value remains unchanged, Residual ozone concentration maintains 0.05-0.1mg/L.Analog result is in table 3, table 4.
C tower: by sodium carbonate adjust ph to 9.2, then the composite corrosion inhibitor in embodiment 5 is added, the effective concentration of Sodium orthomolybdate in water, sodium wolframate and sodium metavanadate is made to be respectively 30 mg/L, 25mg/L, 25mg/L, then in recirculated water, ozone is passed into ozonizer, the ozone concn in water is made to reach 0.05mg/L, will control density of corrosion inhibitor in real time afterwards and pH value remains unchanged, Residual ozone concentration maintains 0.05-0.1mg/L.Analog result is in table 3, table 4.
Table 3 dynamic analog test test tube result
Table 4 heterotrophic bacterium monitoring result
| Sample time | 3rd day | 6th day | 9th day | 12nd day | 15th day |
| A tower | 3.3×10 4 | 5.4×10 3 | 3.5×10 3 | 3.5×10 4 | 6.4×10 3 |
| B tower | 4.2×10 3 | 7.1×10 3 | 3.1×10 3 | 4.0×10 3 | 2.3×10 3 |
| C tower | 2.3×10 3 | 2.7×10 3 | 3.4×10 3 | 2.6×10 3 | 8.3×10 3 |
Heterotrophic bacterium number unit: individual/mL.
Regulation in standard GB/T 50050-2007 " Code for design of industrial recirculating cooling water treatment ", the corrosion speed of the carbon steel tube wall of open type system is less than or equal to 0.125mm/a; In " water coolant analysis and the test method " of production department of China PetroChemical Corporation and development division establishment, " the small-sized experimental analogic method of testing laboratory " specifies that the corrosion speed of carbon steel is " very well " level at 0-0.028mm/a, being " good " level between 0.028-0.056mm/a, is " can allow " level at 0.056-0.070mm/a; Adhesion speed is " very well " level at 0-6mcm, and being " good " level at 6-15mcm, is " can allow " level at 15-20mcm.Heterotrophic bacterium controls 10
5be below qualified.
As can be seen here, apply circulating water treatment prescription of the present invention to be applied to deionized water and to do in circulating cooling make-up water, the erosion rate of each tower test tube of A, B, C is all lower than 0.05mm/a, reach China Petrochemical Industry's " good level " standard, adhere to speed all lower than 8mcm, reach " good level " standard, heterotrophic bacterium is all being less than 1.0 × 10
5in span of control.
Claims (12)
1. the circulating water treatment method using deionized water as moisturizing, it comprises the following steps: a) pH value of controlled circulation water is at 9-11.5; B) add type oxide film inhibiter, described type oxide film inhibiter is the mixture of tungstate and vanadate, or the mixture of molybdate and vanadate; C) add environment-friendly type sterilant, described environment-friendly type sterilant is hydrogen peroxide or ozone.
2. circulating water treatment method according to claim 1, is characterized in that the pH value with alkaline matter controlled circulation water.
3. circulating water treatment method according to claim 2, is characterized in that described alkaline matter is be selected from the one in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood.
4. circulating water treatment method according to claim 1, is characterized in that tungstate is selected from sodium wolframate and potassium wolframate; Molybdate is selected from Sodium orthomolybdate and potassium molybdate; Vanadate is selected from ortho-vanadate and metavanadate.
5. circulating water treatment method according to claim 4, is characterized in that tungstate is selected from anhydrous wolframic acid sodium, tungstate dihydrate acid sodium and anhydrous wolframic acid potassium; Molybdate is selected from anhydrous molybdic acid sodium, Sodium Molybdate Dihydrate and five water potassium molybdates; Vanadate is selected from 12 water sodium orthovanadates, ortho-vanadic acid potassium, two water sodium metavanadates, anhydrous sodium metavanadate, potassium metavanadate.
6. the circulating water treatment method according to any one of claim 1-5, it is characterized in that relative to the effective concentration of each component of pending aqueous solution total amount be: molybdate is 20-50mg/L, and tungstate is 20-50mg/L, and vanadate is 20-50mg/L.
7. the circulating water treatment method according to any one of claim 1-5, is characterized in that ozone is produced by ozonizer, and the after-odour oxygen content control in water is at 0.05-0.1mg/L.
8. circulating water treatment method according to claim 6, is characterized in that ozone is produced by ozonizer, and the after-odour oxygen content control in water is at 0.05-0.1mg/L.
9. the circulating water treatment method according to any one of claim 1-5, it is characterized in that hydrogen peroxide adds frequency is that every 2-4 days adds once, and adding concentration is 20mg/L.
10. circulating water treatment method according to claim 6, it is characterized in that hydrogen peroxide adds frequency is that every 2-4 days adds once, and adding concentration is 20mg/L.
11. circulating water treatment methods according to claim 7, it is characterized in that hydrogen peroxide adds frequency is that every 2-4 days adds once, and adding concentration is 20mg/L.
12. circulating water treatment methods according to claim 8, it is characterized in that hydrogen peroxide adds frequency is that every 2-4 days adds once, and adding concentration is 20mg/L.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1338433A (en) * | 2000-08-11 | 2002-03-06 | 中国石油化工股份有限公司 | Method for using treated sewage in circulating water system |
| CN1919752A (en) * | 2006-09-11 | 2007-02-28 | 北京瀚博英电力科技有限公司 | Environment-friendly type composite corrosion and scale inhibitor |
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| CN1338433A (en) * | 2000-08-11 | 2002-03-06 | 中国石油化工股份有限公司 | Method for using treated sewage in circulating water system |
| CN1919752A (en) * | 2006-09-11 | 2007-02-28 | 北京瀚博英电力科技有限公司 | Environment-friendly type composite corrosion and scale inhibitor |
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