CN101928088B - Method for treating reverse osmosis concentrated water of petrochemical enterprises - Google Patents

Method for treating reverse osmosis concentrated water of petrochemical enterprises Download PDF

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CN101928088B
CN101928088B CN2009100877811A CN200910087781A CN101928088B CN 101928088 B CN101928088 B CN 101928088B CN 2009100877811 A CN2009100877811 A CN 2009100877811A CN 200910087781 A CN200910087781 A CN 200910087781A CN 101928088 B CN101928088 B CN 101928088B
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water
nanofiltration
handled
reverse osmosis
reverse
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CN101928088A (en
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刘正
张新妙
彭海珠
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00Water conservation; Efficient water supply; Efficient water use
    • Y02A20/124Water desalination
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00Water conservation; Efficient water supply; Efficient water use
    • Y02A20/124Water desalination
    • Y02A20/131Reverse-osmosis

Abstract

The invention relates to a method for treating reverse osmosis concentrated water. Aiming at the water quality characteristic of the reverse osmosis concentrated water of petrochemical enterprises, treatment processes of nanofiltration, alkalinity adjustment, air flotation for magnesium removal, calcium removal, microfiltration, neutralization, reverse osmosis, multiple-effect evaporation and desiccation are adopted. Producing water obtained by treatment can return to a previous-level reverse osmosis system to be recycled; and residue obtained in the treatment process can be treated in a centralized mode. The method reduces the membrane pollution of the reverse osmosis, improves treatment efficiency, reduces overall operating cost and has obvious social benefit and economic benefit; and the recovery rate of water reaches about 95 percent.

Description

A kind of treatment process of reverse osmosis concentrated water of petrochemical enterprises
Technical field
The present invention relates to a kind of processing method of industrial waste water, especially relate to a kind of advanced treatment and reclamation method of reverse osmosis concentrated water of petrochemical enterprises.
Background technology
In recent years, along with the fast development of industries such as China's chemical industry, metallurgy, r-o-oneself substitution ion exchange is technological with electrodialysis desalination gradually, become the one preferred technique of waste water recycling process field.Reverse-osmosis treated can produce the dense water more than 30%, and salinity, the hardness of this strand reverse osmosis concentrated water are higher, directly discharges serious environment pollution, and causes the waste of water resources.
In order to make full use of water resources, reduce the influence of high salt, high hard waste water to environment, need effectively administer reverse osmosis concentrated water, thoroughly remove wherein salinity and hardness.Economical, remove salinity and hardness in the reverse osmosis concentrated water effectively, become the key issue of reverse osmosis technology in using.
Remove the hardness in the waste water, generally adopt physics and chemistry to remove hard method.At present, conventional water softening method has the softening and ion exchange method of lime, though these methods are widely used, all has some shortcomings.Lime softening method, limited to the removal of hardness ions, water outlet generally more than 20mg/L (with CaCO 3Meter), effluent quality is wayward; The ion exchange softening method needs frequent regeneration, consumes a large amount of regenerators, the regenerative wastewater contaminate environment of generation.
Nanofiltration is as a kind of pressure-driven membrane process between r-o-and ultrafiltration; Have that working pressure is low, concentrated water discharge is few, effluent quality is excellent, simple to operate, advantage such as level of automation is high, floor space is little; Overcome the shortcoming of lime softening method and ion exchange softening method, so the nf membrane tenderizer has very strong competitive power in removing hard technology.The working cost and the ion exchange method of nanofiltration are suitable, if add the wastewater treatment expense that IX produces, the working cost of nano filtering process is lower than ion exchange method, and it is economically viable therefore adopting nanofiltration tenderizer substitutional ion exchange tenderizer.
In the prior art, foreign patent US035278 has developed " (NF) → r-o-(SWRO) → MSF (MSF) is softened in nanofiltration " sea water desaltination novel process.Seawater has been removed the hardness more than 80% after the NF pre-treatment, TDS has descended about 40%; And removed all organic pollutants, thereby improved the recovery of SWRO, the concentrated seawater of SWRO process is handled via MSF again; Obtain fresh water, the recovery of whole process can be brought up to about 90%.It is obvious that this technology is used for the sea water desaltination treatment effect, and nanofiltration can effectively reduce the processing water yield of reverse osmosis seawater desalting as the pre-treatment of r-o-, improves the cycles of concentration of reverse osmosis system.
Summary of the invention
The water quality characteristics of, high salt hard to the reverse osmosis concentrated water of petrochemical enterprises height; The invention provides a kind of concentrated drying method; Improve the recovery utilization rate (the water recovery of whole process reaches about 95%) of water resources; Avoid the discharging of reverse osmosis concentrated water, and the salinity in the waste water is converted into solid-state, be convenient to ultimate disposal.
Treatment process of the present invention is achieved in that
A kind of treatment process of reverse osmosis concentrated water; The pH of said reverse osmosis concentrated water is 7.0~10.0, specific conductivity is that 3000~70001 μ S/cm, total hardness are that 1000~3000mg/L, COD are 20~200mg/L, and the treatment process of said reverse osmosis concentrated water may further comprise the steps successively:
(1) said reverse osmosis concentrated water being carried out nanofiltration handles; Said nanofiltration is handled and adopted the aperture is flat, tubular type or the rolling nf membrane of 0.001~0.003 μ m; The working pressure that said nanofiltration is handled is that 0.2~1.0MPa, service temperature are that 10~50 ℃, pH are 6~9, and the recovery of control nf membrane is 60~75%, permeation flux is 10~40L/m 2H;
(2) in the dense water of nanofiltration that said nanofiltration processing produces, add NaOH, regulating its pH is 10.0~11.5; Then, the dense water of said nanofiltration is carried out air supporting handle, it is hard to remove magnesium; Air pressure 0.2~0.4MPa, GWR that said air supporting is handled are 2~6: 1; Then, in the dense water of said nanofiltration, add Na 2CO 3, through post precipitation, carrying out solid-liquid separation, to remove calcium hard; Said Na 2CO 3Add-on be Na 2CO 3Generate CaCO with calcium ion reaction in the dense water of said nanofiltration 3Required Na 2CO 31.0~1.2 times of theoretical value;
(3) hard the dense water of nanofiltration after hard carries out the micro-filtration processing with calcium to demagging; Said micro-filtration is handled and adopted the aperture is flat, pocket type or the hollow fiber microfiltration membrane of 0.1~1.01 μ m; The working pressure that said micro-filtration is handled is that-0.02~0.20MPa, service temperature are that 10~50 ℃, pH are 9.0~11.5, and the permeation flux of microfiltration membrane is 40~100L/m 2H;
(4) in the product water that said micro-filtration is handled, add hydrochloric acid, regulating its pH is 6~9; Carry out reverse-osmosis treated then; Said reverse-osmosis treated adopts rolled membrane module; The operating pressure of said reverse-osmosis treated is that 1.8~4.0MPa, operating temperature are that 10~50 ℃, pH are 6~9, and membrane flux is 15~45L/m 2H, cycles of concentration are 3~5;
(5) the dense water that said reverse-osmosis treated is produced carries out multiple-effect evaporation to be handled; Said multiple-effect evaporation is handled and is adopted 2~4 to imitate cocurrent flow type or counterflow evaporator, and the temperature head between imitating and imitating is not less than 12 ℃; Then said multiple-effect evaporation is handled the dense salt debris that produces and carry out drying and other treatment;
The multiple-effect evaporation that the nanofiltration product water that step (1) produces, the reverse osmosis produced water that step (4) produces and step (5) produce produces water, directly or according to the water requirement handles the back reuse; The mummification slag that the micro-filtration slag that air supporting slag that step (2) produces and deliming slag, step (3) produce, step (5) produce is disposed as solid waste.
In the specific implementation, in step (1), said nanofiltration is handled and adopted the aperture is the rolling nf membrane of 0.002 μ m; The working pressure that said nanofiltration is handled is that 0.6~0.8MPa, service temperature are that 15~25 ℃, pH are 7.0~7.5; In step (2), the pH that regulates the dense water of said nanofiltration is 10.8~11.2; The air pressure that said air supporting is handled is that 0.3~0.4MPa, GWR are 3~5: 1; Said Na 2CO 3Add-on be Na 2CO 3Generate CaCO with calcium ion reaction in the dense water of said nanofiltration 3Required Na 2CO 31.0 times of theoretical value; In step (3), said micro-filtration is handled and adopted the aperture is the hollow fiber microfiltration membrane of 0.2 μ m; The working pressure that said micro-filtration is handled is-0.008~-0.015MPa, service temperature are that 15~25 ℃, pH are 10~11; In step (4), said reverse-osmosis treated adopts sea water desaltination series rolled membrane module; In the product water that said micro-filtration is handled, add hydrochloric acid, regulating its pH is 6.5~7.5; The operating pressure of said reverse-osmosis treated is that 2.0~2.5MPa, operating temperature are that 15~25 ℃, pH are 6.8~7.2; In step (5), said multiple-effect evaporation is handled and is adopted 3 to imitate cocurrent flow type or counterflow evaporator; Said drying and other treatment adopts nature to place mummification.
Utilize nf membrane to divalence, polyvalent ion (Ca 2+, Mg 2+, SO 4 2-) and the organic height of molecular weight between 200~1000 held back and to univalent ion (K +, Na +, Cl -) the low characteristic of holding back, can realize dense water softening, softening mainly is to remove incrustation ion (Ca in the reverse osmosis concentrated water 2+And Mg 2+), can not remove all inorganic salt in the dense water.Adopt method of the present invention, bivalent ions clearance is more than 83% in the reverse osmosis concentrated water, and the COD clearance is 35~95%, and the TDS clearance is 35~95%
The present invention is through alkali adjusting and hardness removing, and the magnesium in the dense water is removed to below the 10mg/L firmly, calcium is firmly almost all removed.Behind the alkali adjusting and hardness removing, the dense water turbidity of waste water raises, and possibly contain a certain amount of suspended solids, must remove turbidity and the SS in the water.Handle through micro-filtration, the calcium in the dense water is hard almost all to be removed with SS, and the product water turbidity is lower than 0.05NTU, and remaining magnesium is had certain removal effect firmly.
Through the dense water after alkali adjusting and hardness removing and the micro-filtration processing, the pH value is very high, is about about 10~11, for calcium, the magnesium scale that prevents not remove in the dense water, must carry out neutralizing treatment, reduces dense water pH value.Dense water after the neutralization, monovalent salt concentration are very high, and the hardness in the dense water is almost all got rid of, and this just greatly reduces the possibility of fouling, adopt reverse osmosis system that dense water is further concentrated, and remove the unit price salt in the dense water.What r-o-was selected for use is sea water desaltination series rolled membrane module, feed water by reverse osmosis SDI≤3.Ratio of desalinization reaches more than 95%, and the reverse osmosis concentration multiple is 3~5 times.
After the reverse osmosis system concentration, the salt concn in the dense water through adopting multiple-effect evaporation, with the further spissated while of dense water, realizes the reuse of vaporize water near supersaturation.The effect number of multiple-effect evaporation depends primarily on the temperature head that is evaporated between material maximum heating temperature and effect and the effect.Usually for electrolyte solution, adopt two to imitate or triple effect evaporation.
Adopt method of the present invention, after reverse osmosis concentrated water was handled through nanofiltration, nanofiltration was produced water and is returned the prime reverse osmosis system; After the dense water that nanofiltration produces is removed hardness; The entering reverse osmosis system concentrates, and the dense water that reverse osmosis concentration produces gets into multi-effect evaporation system, and the steam condensate of reverse osmosis produced water and multiple-effect evaporation can be back to production technique; High salt debris behind the multiple-effect evaporation obtains the salt slag through natural mummification, centrally disposes.Method of the present invention has realized " zero release " of reverse osmosis concentrated water basically, has remarkable social benefit and economic benefit.
The present invention adopts nanofiltration pre-treatment reverse osmosis concentrated water first; Greatly reducing the water yield of alkali adjusting and hardness removing step, is the alkali adjusting and hardness removing medicament with NaOH, and adopts air floating method to remove the magnesium in the dense water; Clearance to calcium, magnesium is high; Reduced the processing load of follow-up reverse osmosis concentrated compression system, the films such as fouling that reduced reverse osmosis membrane pollute, and have guaranteed long-term safety, the steady running of reverse osmosis membrane assembly.
Compare with seawater, waste water quality according to the invention is more complicated, except that having higher electricity leads; Also contain higher hardness and COD, compare, the present invention is directed to the reverse osmosis concentrated water of petrochemical enterprises water quality characteristics with " (NF) → r-o-(SWRO) → MSF (MSF) is softened in nanofiltration " desalination process; After the process nanofiltration is softening; Remove hardness through demagging, deliming, improve cycles of concentration to 3~5 times of reverse osmosis concentrated water, reduced the fouling of reverse osmosis membrane; Reduced the load of follow-up multiple-effect evaporation, and the water recovery of whole process is reached about 95%.
Description of drawings
Fig. 1 is a schematic flow sheet of the present invention.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is detailed further, protection scope of the present invention is not limited to following embodiment.
Embodiment 1~3
Certain reverse osmosis concentrated water of petrochemical enterprises, its electricity is led, TDS and always higher firmly, and contains a small amount of organism.The water quality and the analytical procedure of this dense water are seen table 1.
Table 1
Sequence number Project The dense water water quality of RO
1 pH 7.34
2 Electricity is led (μ S/cm) 5323
3 Colourity 69
4 Turbidity (NTU) 0.19
5 TDS(mg/L) 2820
6 Total alkalinity (CaCO 3)(mg/L) 591.2
7 Total hardness (CaCO 3)(mg/L) 1121.6
8 Solvable silicon (mg/L) 8.91
9 Total silicon (mg/L) 9.56
10 Ferrous (mg/L) <0.03
11 Total iron (mg/L) <0.03
12 Total phosphorus (mg/L) 11.19
13 COD cr(mg/L) 68
14 TOC(mg/L) 32.68
15 TN(mg/L) 32.14
16 K +(mg/L) 23.0
17 Na +(mg/L) 650.7
18 Ca 2+(mg/L) 306.8
19 Mg 2+(mg/L) 80.3
20 NH 4 +-N(mg/L) <0.2
21 F -(mg/L) 1.6
22 Cl -(mg/L) 704.6
23 NO 3 -(mg/L) 147.6
24 PO 4 3-(mg/L) 17.3
25 SO 4 2-(mg/L) 698.4
26 Petroleum-type (mg/L) 0.21
27 Mn 2+(mg/L) 0.054
1, add an amount of organic inhibitor agent (Hypersperse MDC220) at reverse osmosis concentrated water, behind the adjusting pH, the employing aperture is that the rolling nf membrane of 0.002 μ m is carried out the nanofiltration processing;
2, in the dense water of nanofiltration, add NaOH and regulate pH; Then, the dense water of nanofiltration is carried out air supporting handle, it is hard to remove magnesium, in the dense water of nanofiltration, adds Na 2CO 3, it is hard to remove calcium through precipitate and separate;
3, adopting the aperture is that the hollow fiber microfiltration membrane of the 0.2 μ m waste water after to alkali adjusting and hardness removing carries out micro-filtration and handles;
4, in micro-filtration product water, add hydrochloric acid, regulate its pH; Adopt sea water desaltination series rolled membrane module (Tao Shi SW30 sea water desaltination series rolled membrane module) to carry out reverse-osmosis treated then;
5, adopt 3 to imitate the cocurrent flow type vaporizer, the dense water that reverse-osmosis treated is produced carries out the multiple-effect evaporation processing, carries out nature then and places mummification.
The nanofiltration that said process produces is produced water, reverse osmosis produced water and multiple-effect evaporation and is produced water, the reverse osmosis system before getting back to, reuse after treatment; Air supporting slag that said process produces and deliming slag, micro-filtration slag, mummification slag centrally dispose as solid waste.
Embodiment 1~3 respectively handles unitary operational condition and sees table 2, and treatment effect sees 3.
Table 2
Each cell processing effect among table 3 embodiment

Claims (2)

1. the treatment process of a reverse osmosis concentrated water; The pH of said reverse osmosis concentrated water is 7.0~10.0, specific conductivity is that 3000~7000 μ S/cm, total hardness are that 1000~3000mg/L, COD are 20~200mg/L, and the treatment process of said reverse osmosis concentrated water may further comprise the steps successively:
(1) said reverse osmosis concentrated water being carried out nanofiltration handles; Said nanofiltration is handled and adopted the aperture is flat, tubular type or the rolling nf membrane of 0.001~0.003 μ m; The working pressure that said nanofiltration is handled is that 0.2~1.0MPa, service temperature are that 10~50 ℃, pH are 6~9, and the recovery of control nf membrane is 60~75%, permeation flux is 10~40L/m 2H;
(2) in the dense water of nanofiltration that said nanofiltration processing produces, add NaOH, regulating its pH is 10.0~11.5; Then, the dense water of said nanofiltration is carried out air supporting handle, it is hard to remove magnesium; The air pressure that said air supporting is handled is that 0.2~0.4MPa, GWR are 2~6: 1; Then, in the dense water of said nanofiltration, add Na 2CO 3, through post precipitation, carrying out solid-liquid separation, to remove calcium hard; Said Na 2CO 3Add-on be Na 2CO 3Generate CaCO with calcium ion reaction in the dense water of said nanofiltration 3Required Na 2CO 31.0~1.2 times of theoretical value;
(3) hard the dense water of nanofiltration after hard carries out the micro-filtration processing with calcium to demagging; Said micro-filtration is handled and adopted the aperture is flat, pocket type or the hollow fiber microfiltration membrane of 0.1~1.0 μ m; The working pressure that said micro-filtration is handled is that-0.02~0.20MPa, service temperature are that 10~50 ℃, pH are 9.0~11.5, and the permeation flux of microfiltration membrane is 40~100L/m 2H;
(4) in the product water that said micro-filtration is handled, add hydrochloric acid, regulating its pH is 6~9; Carry out reverse-osmosis treated then; Said reverse-osmosis treated adopts rolled membrane module; The operating pressure of said reverse-osmosis treated is that 1.8~4.0MPa, operating temperature are that 10~50 ℃, pH are 6~9, and membrane flux is 15~45L/m 2H, cycles of concentration are 3~5;
(5) the dense water that said reverse-osmosis treated is produced carries out multiple-effect evaporation to be handled; Said multiple-effect evaporation is handled and is adopted 2~4 to imitate cocurrent flow type or counterflow evaporator, and the temperature head between imitating and imitating is not less than 12 ℃; Then said multiple-effect evaporation is handled the dense salt debris that produces and carry out drying and other treatment;
Wherein, the multiple-effect evaporation that the nanofiltration product water that step (1) produces, the reverse osmosis produced water that step (4) produces and step (5) produce produces water, directly or according to the water requirement handles the back reuse; The mummification slag that the micro-filtration slag that air supporting slag that step (2) produces and deliming slag, step (3) produce, step (5) produce is disposed as solid waste.
2. treatment process according to claim 1 is characterized in that:
In step (1), said nanofiltration is handled and adopted the aperture is the rolling nf membrane of 0.002 μ m; The working pressure that said nanofiltration is handled is that 0.6~0.8MPa, service temperature are that 15~25 ℃, pH are 7.0~7.5;
In step (2), the pH that regulates the dense water of said nanofiltration is 10.8~11.2; The air pressure that said air supporting is handled is that 0.3~0.4MPa, GWR are 3~5: 1; Said Na 2CO 3Add-on be Na 2CO 3Generate CaCO with calcium ion reaction in the dense water of said nanofiltration 3Required Na 2CO 31.0 times of theoretical value;
In step (3), said micro-filtration is handled and adopted the aperture is the hollow fiber microfiltration membrane of 0.2 μ m; The working pressure that said micro-filtration is handled is-0.008~-0.015MPa, service temperature are that 15~25 ℃, pH are 10~11;
In step (4), said reverse-osmosis treated adopts sea water desaltination series rolled membrane module; In the product water that said micro-filtration is handled, add hydrochloric acid, regulating its pH is 6.5~7.5; The operating pressure of said reverse-osmosis treated is that 2.0~2.5MPa, operating temperature are that 15~25 ℃, pH are 6.8~7.2;
In step (5), said multiple-effect evaporation is handled and is adopted 3 to imitate cocurrent flow type or counterflow evaporator; Said drying and other treatment adopts nature to place mummification.
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CA2847882C (en) * 2011-09-09 2020-12-15 Sylvan Source, Inc. Industrial water purification and desalination
CN102627364A (en) * 2012-04-17 2012-08-08 南京丹恒科技有限公司 Process flow for recycling and treating reverse osmosis concentrated water
CN103663769A (en) * 2012-09-07 2014-03-26 中国石油化工股份有限公司 Method for desalting sewage by using membrane separation technology
CN102942279A (en) * 2012-10-12 2013-02-27 江苏华晖环保科技有限公司 Treatment method for circulating water sewerage and reverse osmosis concentrated water and equipment thereof
CN102897965A (en) * 2012-11-06 2013-01-30 南京南自科林系统工程有限公司 Method for treating water with high recovery rate by using membrane method
CN102936067A (en) * 2012-11-23 2013-02-20 天津凯铂能膜工程技术有限公司 Method for selectively removing calcium ions from concentrated water byproduct of sea water desalination process and other high-calcium-magnesium-content concentrated brines
CN104418451B (en) * 2013-08-20 2016-07-06 中国石油化工股份有限公司 A kind of processing method of reverse osmosis concentrated water
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