CN103880211B - A kind of recycling treatment process containing magnesium high-salt wastewater - Google Patents
A kind of recycling treatment process containing magnesium high-salt wastewater Download PDFInfo
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Abstract
The invention discloses a kind of recycling treatment process containing magnesium high-salt wastewater, comprising: what DYE PRODUCTION process produced by (1) contains the categorised collection of magnesium ion height salt mother liquor waste water, suction filtration, reclaims dyestuff intermediate or dye product; (2) be adjusted to pH value 3.0 ~ 6.0, add Powdered Activated Carbon, suction filtration; (3) add sodium hydroxide, paramount salt waste water ph is 10.0 ~ 11.0, adds flocculation agent, flocculating settling, centrifugation; (4) in industrial microwave oven, complete magnesium hydroxide under automatic program Elevated Temperature Conditions and be converted into light magnesium oxide, through pulverizing, grinding obtained powdery light magnesium oxide; (5) sodium salt solution that clear liquid step (3) obtained adopts nanofiltration membrane treatment to obtain is back to production technique.The present invention takes off COD, decolouring, microwave, a series of process of film process by the middle height salt mother liquor waste water warp produced in dispersed dye production process, carries out recycling, achieve wastewater zero discharge to waste liquid.
Description
Technical field
The invention belongs to water reuse field, specifically relate to a kind of recycling treatment process containing magnesium high-salt wastewater.
Background technology
Along with the continuous sustained and rapid development of China's dyestuffs industries since reform and opening-up, one of dyestuff associated row mainstay industry already having become the Economic development of China, simultaneously in order to adapt to the market specification of quality more and more higher to dye product, DYE PRODUCTION technique is also constantly reformed thereupon, and the difficulty of three-protection design also increases thereupon.Particularly acid, alkali, inorganic salt etc. are as raw material requisite in dyestuffs industries, the inorganic salt of inorganic salt and neutralization reaction generation nearly all will be used in various dye well intermediate production process, but inorganic salt do not enter product substantially in production process, a large amount of inorganic salt are caused to enter in waste liquor water, not only increase the difficulty of enterprise's sewage disposal, cause a large amount of wastings of resources simultaneously.Especially in " 12 " period, along with national energy-saving reduces discharging and constantly the carrying out of cleaner production, the three-protection design of dyestuffs industries is faced with stern challenge more, therefore how carries out effective process to high salinity mother liquor waste water and has become the new the difficult problem of environmental protection that dyestuff enterprise faces.
Dye industry height salt mother liquor waste water river harnessing ideas domestic is at present mainly based on direct evaporation concentration method, service water dilution method, biochemical treatment process, wet oxidation process, Fenton oxidation method, Ozonation etc.In evaporation concentration method, because needs consume a large amount of steam, residual organic substances and inorganic salt become dangerous solid waste, thoroughly can not solve environmental issue; Service water dilution method needs to consume a large amount of service water, although can qualified discharge, does not meet the basic demand of energy-saving and emission-reduction, increases a large amount of effluent charge simultaneously; Biochemical treatment process process needs because salinity is higher to consume a large amount of service water, otherwise high salinity causes biochemical system fluctuation of service, and can not ensure treatment effect; Wet oxidation process has good removal effect to high salt COD using hydrogen peroxide, air etc. as oxygenant under high-temperature and high-pressure conditions, and salinity does not almost change, and still remains in water, and cost of investment is comparatively large, and equipment requirements is higher, cannot extensively popularize; Fenton oxidation method, Ozonation are substantially the same with wet oxidation process effect, can not solve the problem of salinity equally.Some producer adopts the combination of above two kinds of methods, achieves certain effect.Such as publication number is a kind of method that patent document discloses dye wastewater treatment of CN103588307A, comprises and arranges microorganism electrochemical coupled system, and microorganism electrochemical coupled system is coupled with microorganism electrolysis cell by microbiological fuel cell; Then the cathode compartment pending waste water from dyestuff being loaded microorganism electrolysis cell is degraded.But the method needs complicated equipment, and processing cost is higher.
In the face of increasingly serious environmental protection pressure, the discharge that how effectively can reduce three-waste pollution thing becomes a great problem that current dye industry needs solution badly.Dye industry needs change to be treated to main administration way with " end " at present, and in the links of production technique, continuous technical renovation, adjusts the product mix, implement energy-saving and emission-reduction from source, controls and continuous emissions reduction total amount.Treatment technology is turned to recycling treatment direction simultaneously, finally make whole technique reach the target of cleaner production.
Summary of the invention
The invention provides a kind of recycling treatment process containing magnesium high-salt wastewater, by the close neutral middle height salt mother liquor waste water containing magnesium chloride and sodium-chlor is prepared into the by product such as light magnesium oxide and sodium chloride solution, simultaneously by the clear liquid in centrifugal process by recycling can be carried out in production technique by direct reuse after membrane separation technique process, thus reach waste water reclaiming recycling and the object of zero release.
Containing a recycling treatment process for magnesium high-salt wastewater, comprise the steps:
(1) collection and pre-treatment: what DYE PRODUCTION process produced carries out categorised collection containing magnesium ion height salt mother liquor waste water, and carries out suction filtration pre-treatment respectively, the dyestuff intermediate that recovery part runs off or dye product;
(2) desolventing technology: add acid in the pretreated high-salt wastewater of step (1) suction filtration, be adjusted to high-salt wastewater pH value 3.0 ~ 6.0, add Powdered Activated Carbon, and suction filtration after stirring, Powdered Activated Carbon regeneration Posterior circle utilizes;
(3) magnesium hydroxide is separated: the high-salt wastewater that step (2) processed is added sodium hydroxide under agitation continuously, be stabilized in till 10.0 ~ 11.0 until high-salt wastewater pH value, add flocculation agent and carry out flocculating settling, after sedimentation, sediment enters centrifugation;
(4) light magnesium oxide is prepared: centrifugal for step (3) magnesium hydroxide obtained is completed magnesium hydroxide under automatic program Elevated Temperature Conditions in industrial microwave oven and is converted into light magnesium oxide, through pulverizing, grinding obtained powdery light magnesium oxide;
(5) film process: the clear liquid that step (3) sedimentation and centrifugal treating obtained adopts nanofiltration membrane treatment, and obtaining mass percent through separating treatment is 20% ~ 30% sodium salt solution, as the production technique of end Water circulation in dyestuff or dyestuff intermediate.
In step (1), DYE PRODUCTION process is produced containing magnesium ion height salt mother liquor waste water carry out categorised collection time, generally carry out categorised collection according to dyestuff of the same race or dyestuff intermediate, so that the recycling of dyestuff and dyestuff intermediate.The content collecting magnesium ion in the high salt mother liquor waste water obtained changes to some extent according to dye technology difference, all be suitable for method of the present invention to process, as preferably, in described high salt mother liquor waste water, the mass percentage content of magnesium ion is 10 ~ 70%, more preferably 10 ~ 30%.
In step (1), described being preferably containing magnesium ion height salt mother liquor waste water adopts magnesium oxide to prepare N as acid binding agent, the waste water produced in N-diethyl-3-acetylaminoaniline process; Also other can be adopted with the mother liquid coming or washing water etc. of magnesium hydroxide, magnesium oxide, dyestuff that magnesiumcarbonate is acid binding agent or dyestuff intermediate.
In step (2), the acid of employing can be hydrochloric acid, sulfuric acid etc.Also Waste Sulfuric Acid, waste hydrochloric acid etc. that preparation of dyestuff process reclaims can be adopted.Powdered Activated Carbon (English name: Powdered ActivatedCarbon, PAC), have good absorption property, chemical stability is good, can strong alkali-acid resistance, can stand water logging, high temperature.Specific surface area, up to 1000 ~ 1500 meters squared per gram, belongs to porous hydrophobic adsorbent.Experiment proves, under the condition of slant acidity, the adsorptive power of Powdered Activated Carbon is better.As preferably, be adjusted to high-salt wastewater pH value 5.0 ~ 6.0.The add-on of Powdered Activated Carbon can be determined according to actual needs, and as preferably, in high-salt wastewater total mass, the add-on of described Powdered Activated Carbon is 0.8% ~ 1.2%.More preferably 1%.PAC materialization manipulation of regeneration can adopt prior art.
In step (3), add in sheet alkali (sodium hydroxide) process, generally monitored by online pH meter, ensure that reaction end is pH value 10.0 ~ 11.0.After having reacted, add flocculation agent, flocculation agent can select PAM(polyacrylamide), as further preferably, described flocculation agent can select anion-polyacrylamide APAM(molecular weight 1800 ~ 2,000 ten thousand), cationic-type polyacrylamide CPAM(molecular weight is 1,000 ten thousand), amphoteric ionic polyacrylamide Am-PAM.In high-salt wastewater, described flocculation agent generally adopts the form of the aqueous solution to add, and in flocculant aqueous solution, the mass percent concentration of flocculation agent is 0.1% ~ 0.2%; In the total mass of high-salt wastewater, the add-on of described flocculation agent is 0.1% ~ 2%, more preferably 0.1% ~ 0.5%.Experiment proves, when adopting the flocculation agent of above-mentioned composition, better to the flocculating effect of magnesium hydroxide in high-salt wastewater.
In addition, in step (3), be ensure flocculating effect, as preferably, add continuously stirring in flocculation agent process, after flocculation agent has added, then stir 15 ~ 30min, rotating speed controls as 30r/min ~ 45r/min, and then standing sedimentation 4 ~ 6h, and then carries out centrifugally operated.
In step (3), after having flocculated, the general Horizontal sedimentation separating centrifuge that adopts carries out detached job, and for improving centrifugal treating efficiency and ensureing the clarity of clear liquid, as preferably, centrifuge speed is 2000 ~ 3500r/min; And separate unit whizzer process concentrated solution amount is 1.0 ~ 1.5t/h.The solid content of the magnesium hydroxide obtained after centrifugation is 30% ~ 45%.
In step (4), light magnesium oxide is that white lightweight is loosened unformed powder, odorless, tasteless, nontoxic, volume shared by light magnesium oxide is about about three times of heavy-calcined magnesia, be worth relatively high, for obtaining the higher light magnesium oxide of quality, the present invention adopts and utilizes industrial microwave oven process magnesium hydroxide.Experiment proves, the quality influence of control to light magnesium oxide of temperature is larger, as preferably, in described industrial microwave oven, automatic program Elevated Temperature Conditions is: program automatic control top temperature is 470 ~ 490 DEG C, more preferably 480 DEG C, drying time 45min ~ 2h, takes program mode heating mode, and intensification frequency is 10 ~ 15 DEG C/min.Obtain light magnesium oxide after having reacted, pulverizer is broken, grinding obtains that tap density is 0.1 ~ 0.3g/mL, particle diameter is be not more than the light magnesium oxide of 2 μm.The light magnesium oxide prepared can direct reuse in dyestuff or dyestuff intermediate preparation process, also can as production marketing, improve the benefit of enterprise.
Nanofiltration membrane is the functional semi-permeable membranes of one allowing solvent molecule or some low molecular weight solutes or ion permeable at a low price, to the desalination of monovalent anion salts solution lower than high-valence anion salts solution.In step (5), after adopting film process, residual organism and other impurity are filtered, and what obtain is the sodium salt solution that purity is very high, is generally the aqueous solution of sodium-chlor.The aqueous solution of sodium-chlor does not almost affect preparation of dyestuff, so can do end water use by direct reuse.
Film process: the clear liquid that step (3) sedimentation and centrifugal treating obtained adopts nanofiltration membrane treatment, and obtaining mass percent through separating treatment is 20% ~ 30% sodium salt solution, as the production technique of end Water circulation in dyestuff or dyestuff intermediate.
Novel process treatment process of the present invention, its superiority is mainly reflected in: the present invention by the middle height salt mother liquor waste water that produces in dispersed dye production process through adjust pH, de-COD, decolouring series of preprocessing, recycling is carried out to waste liquid, turn waste into wealth, abandoned traditional evaporation concentration or advanced oxidation process method not thoroughly; Adopt energy-efficient microwave integration apparatus in this technique simultaneously, the magnesium hydroxide in waste water is made light magnesium oxide, produce for intermediate and greatly save production cost; Simultaneously in addition by energy-efficient film process, can direct reuse in production plant, achieve waste water reclaiming processing intent, simultaneously the also immense pressure that faces of reduction environmental protection of enterprise greatly.
Accompanying drawing explanation
Fig. 1 is the schema of the recycling treatment process containing magnesium high-salt wastewater of the present invention.
Embodiment
Embodiment 1:
Collect and produce N, the high salt mother liquor (mass percentage content of magnesium ion is about 10%) of N-diethyl-3-acetylaminoaniline, be continuously pumped into Suction filtration device, the dyestuff intermediate product in mother liquor is reclaimed after suction filtration, clear liquid sulfur waste acid for adjusting pH to 5.0 ~ 6.0 that suction filtration obtains, by adding total PAC processing 1% of water yield quality, continuously stirring 30min, static 4h, suction filtration obtains colourless middle height salt mother liquor, assay colourity is less than 5 times, saturated PAC carries out the utilization of manipulation of regeneration Posterior circle, in color-less mother liquor, evenly add sheet alkali by cage equipment and constantly stir, controlling terminal pH by online pH meter is 10.0 ~ 11.0, flocculation agent PAM(cationic polyacrylamide CP-7 is added continuously under agitation condition, Shanghai constant force material for water treatment company limited) aqueous solution, the mass percent concentration of the PAM aqueous solution is 0.2%, add-on is 2kg/t, continuously stirring 30min, rotating speed controls as 30r/min, standing sedimentation 4h, in bucket precipitation separation concentrate after slurry magnesium hydroxide, (centrifugal speed is 2000r/min to pump into horizontal decanter centrifuge by spiral pump, separate unit whizzer process concentrated solution amount is 1.0t/h), be separated and obtain the solid hydrogen magnesium oxide that solid content is 30%, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, automatic control top temperature 480 DEG C, rate of heating is 10 DEG C/min, magnesium hydroxide is converted into after magnesium oxide becomes and pulverizes, it is 0.1g/mL that grinding obtains long-pending density, particle diameter is be not more than the powder light magnesium oxide of 2 μm, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtained is by energy-efficient film process (adopting the HNF-8040 series rolling nanofiltration membrane of Jinan Hydranautics Science and Technology Ltd.), obtain 20% sodium chloride solution can direct reuse in saltouing or chilled brine technique, membrane sepn clear liquid as service water direct reuse in related production technique, can reduce this process operation cost greatly.
Embodiment 2:
Collect and produce N, the high salt mother liquor (mass percentage content of magnesium ion is about 15%) of N-diethyl-3-acetylaminoaniline, be continuously pumped into Suction filtration device, the dyestuff intermediate product in mother liquor is reclaimed after suction filtration, clear liquid sulfur waste acid for adjusting pH to 5.0 ~ 6.0 that suction filtration obtains, by adding total PAC processing 1.0% of water yield quality, continuously stirring 30min, static 4h, suction filtration obtains colourless middle height salt mother liquor, assay colourity is less than 5 times, saturated PAC carries out the utilization of manipulation of regeneration Posterior circle, in color-less mother liquor, evenly add sheet alkali by cage equipment and constantly stir, controlling terminal pH by online pH meter is 10.0 ~ 11.0, flocculation agent PAM(anion-polyacrylamide AP is added continuously under agitation condition, Shanghai constant force material for water treatment company limited) aqueous solution, the mass percent concentration of the PAM aqueous solution is 0.1%, add-on is 1kg/t, continuously stirring 30min, rotating speed controls as 40r/min, standing sedimentation 6h, in bucket precipitation separation concentrate after slurry magnesium hydroxide, (centrifugal speed is 2500r/min to pump into horizontal decanter centrifuge by spiral pump, separate unit whizzer process concentrated solution amount is 1.5t/h), be separated and obtain the solid hydrogen magnesium oxide that solid content is 40%, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, automatic control top temperature 490 DEG C, rate of heating is 15 DEG C/min, magnesium hydroxide is converted into after magnesium oxide becomes and pulverizes, it is 0.2g/mL that grinding obtains long-pending density, particle diameter is be not more than the powder light magnesium oxide of 2 μm, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtained is by energy-efficient film process (adopting the HNF-8040 series rolling nanofiltration membrane of Jinan Hydranautics Science and Technology Ltd.), obtain 30% sodium chloride solution can direct reuse in saltouing or chilled brine technique, membrane sepn clear liquid as service water direct reuse in related production technique, can reduce this process operation cost greatly.
Embodiment 3:
Collect and produce N, the high salt mother liquor (mass percentage content of magnesium ion is about 20%) of N-diethyl-3-acetylaminoaniline, be continuously pumped into Suction filtration device, the dyestuff intermediate product in mother liquor is reclaimed after suction filtration, clear liquid sulfur waste acid for adjusting pH to 5.0 ~ 6.0 that suction filtration obtains, by adding total PAC processing 1% of water yield quality, continuously stirring 30min, static 4h, suction filtration obtains colourless middle height salt mother liquor, assay colourity is less than 5 times, saturated PAC carries out the utilization of manipulation of regeneration Posterior circle, in color-less mother liquor, evenly add sheet alkali by cage equipment and constantly stir, controlling terminal pH by online pH meter is 10.0 ~ 11.0, flocculation agent PAM(zwitter-ion polyacrylamide is added continuously under agitation condition, Shanghai constant force material for water treatment company limited) aqueous solution, the mass percent of the PAM aqueous solution is 0.5%, add-on is 5kg/t, continuously stirring 30min, rotating speed controls as 45r/min, standing sedimentation 5h, in bucket precipitation separation concentrate after slurry magnesium hydroxide, (centrifugal speed is 3000r/min to pump into horizontal decanter centrifuge by spiral pump, separate unit whizzer process concentrated solution amount is 1.5t/h), be separated and obtain the solid hydrogen magnesium oxide that solid content is 25%, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, automatic control top temperature 470 DEG C, rate of heating is 10 DEG C/min, magnesium hydroxide is converted into after magnesium oxide becomes and pulverizes, it is 0.2g/mL that grinding obtains particle diameter for amassing density, be not more than the powder light magnesium oxide of 2 μm, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtained is by energy-efficient film process (adopting the HNF-8040 series rolling nanofiltration membrane of Jinan Hydranautics Science and Technology Ltd.), obtain 25% sodium chloride solution can direct reuse in saltouing or chilled brine technique, membrane sepn clear liquid as service water direct reuse in related production technique, can reduce this process operation cost greatly.
Test example 1:
According to national standard HG/T2573-2012, mass analysis is carried out to the by product light magnesium oxide product reclaimed in embodiment 1 ~ 3, the results are shown in following table 1:
Table 1
From upper table 1, the side product chlorinated sodium solution adopting processing method provided by the invention to obtain and light magnesium oxide, meet enterprise completely and basic index requirement is used to industrial goods, and membrane sepn clear liquid can as service water direct reuse in original production technique, meet the basic demand of cleaner production and recycling economy, also there is considerable economic benefit by producing light magnesium oxide simultaneously, accomplishing that the high-salt wastewater complete resource that dye technology produces utilizes the processing intent with zero release.
Claims (8)
1., containing a recycling treatment process for magnesium high-salt wastewater, it is characterized in that, comprise the steps:
(1) collection and pre-treatment: what DYE PRODUCTION process produced carries out categorised collection containing magnesium ion height salt mother liquor waste water, and carries out suction filtration pre-treatment respectively, the dyestuff intermediate that recovery part runs off or dye product;
In described high salt mother liquor waste water, the mass percentage content of magnesium ion is 10 ~ 30%;
(2) desolventing technology: add acid in the pretreated high-salt wastewater of step (1) suction filtration, be adjusted to high-salt wastewater pH value to 3.0 ~ 6.0, add Powdered Activated Carbon, and suction filtration after stirring, Powdered Activated Carbon regeneration Posterior circle utilizes;
(3) magnesium hydroxide is separated: the high-salt wastewater that step (2) processed is added sodium hydroxide under agitation continuously, until high-salt wastewater pH value is 10.0 ~ 11.0, add flocculation agent and carry out flocculating settling, after sedimentation, sediment enters centrifugation;
In step (3), add continuously stirring in flocculation agent process, after flocculation agent has added, then stir 15 ~ 30min, rotating speed controls as 30r/min ~ 45r/min, and then standing sedimentation 4 ~ 6h, and then carries out centrifugally operated;
In step (3), after having flocculated, adopt Horizontal sedimentation separating centrifuge to carry out detached job, centrifuge speed is 2000 ~ 3500r/min; And separate unit whizzer process concentrated solution amount is 1.0 ~ 1.5t/h;
(4) light magnesium oxide is prepared: centrifugal for step (3) magnesium hydroxide obtained is completed magnesium hydroxide under automatic program Elevated Temperature Conditions in industrial microwave oven and is converted into light magnesium oxide, through pulverizing, grinding obtained powdery light magnesium oxide;
(5) film process: clear liquid step (3) sedimentation and centrifugal treating obtained adopts nanofiltration membrane treatment, obtaining mass percent through separating treatment is 20% ~ 30% sodium salt solution, as the production technique of end Water circulation in dyestuff or dyestuff intermediate.
2. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, it is characterized in that, in step (2), in high-salt wastewater total mass, the add-on of described Powdered Activated Carbon is 0.8% ~ 1.2%.
3. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, it is characterized in that, described flocculation agent is anion-polyacrylamide, cationic-type polyacrylamide, amphoteric ionic polyacrylamide.
4. the recycling treatment process containing magnesium high-salt wastewater according to claim 1 or 3, is characterized in that, described flocculation agent adopts the form of the aqueous solution to add, and in flocculant aqueous solution, the mass percent concentration of flocculation agent is 0.1% ~ 0.2%.
5. the recycling treatment process containing magnesium high-salt wastewater according to claim 4, it is characterized in that, in the total mass of high-salt wastewater, the add-on of described flocculation agent is 0.1% ~ 2%.
6. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, it is characterized in that, in step (4), in described industrial microwave oven, automatic program Elevated Temperature Conditions is: program automatic control top temperature is 470 ~ 490 DEG C, drying time 45min ~ 2h, take program mode heating mode, temperature rise rate is 10 ~ 15 DEG C/min.
7. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, is characterized in that, in step (4), the tap density of the light magnesium oxide be obtained by reacting is 0.1 ~ 0.3g/mL, particle diameter is for being not more than 2 μm.
8. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, it is characterized in that, in step (1), described prepares N as acid binding agent, the waste water produced in N-diethyl-3-acetylaminoaniline process containing magnesium ion height salt mother liquor waste water for adopting magnesium oxide.
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| CN104261443A (en) * | 2014-09-25 | 2015-01-07 | 池州西恩新材料科技有限公司 | Process for calcium-method production of magnesium hydrate by using nanofiltration membrane |
| CN104909494A (en) * | 2015-06-01 | 2015-09-16 | 上海晶宇环境工程有限公司 | Process for impurity removal and purification of industrial high-concentration brine and special equipment of process |
| CN109621895A (en) * | 2018-12-21 | 2019-04-16 | 安徽汇泽通环境技术有限公司 | A method of Water phosphorus is removed using modified water plant charcoal |
| CN111204780B (en) * | 2020-01-09 | 2021-04-27 | 西安交通大学 | Resource utilization process of salt mud in chlor-alkali industry |
| CN113401925B (en) * | 2021-06-21 | 2022-07-01 | 宋纯 | Method for removing organic impurities in waste sulfuric acid water in 2-ethyl anthraquinone production |
| TWI782826B (en) * | 2021-12-17 | 2022-11-01 | 泰鋒染化工業股份有限公司 | Method for treating wastewater |
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| CN101214975A (en) * | 2008-01-21 | 2008-07-09 | 上海西恩化工设备有限公司 | Advanced treatment technique for brine |
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