CN103880211A - Process for resourceful treatment of high-salt wastewater containing magnesium - Google Patents

Process for resourceful treatment of high-salt wastewater containing magnesium Download PDF

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CN103880211A
CN103880211A CN201410096147.5A CN201410096147A CN103880211A CN 103880211 A CN103880211 A CN 103880211A CN 201410096147 A CN201410096147 A CN 201410096147A CN 103880211 A CN103880211 A CN 103880211A
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salt wastewater
salt
magnesium
magnesium oxide
treatment process
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CN103880211B (en
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徐万福
张现刚
刘成成
俞氽叶
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ZHEJIANG DIBANG CHEMICAL CO Ltd
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ZHEJIANG DIBANG CHEMICAL CO Ltd
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Abstract

The invention discloses a process for resourceful treatment of high-salt wastewater containing magnesium. The process comprises the following steps: (1) classifying and collecting high-salt mother liquor wastewater which has magnesium ions and is produced in a dye production process to carry out suction filtration and recycle a dye intermediate or a dye product; (2) adjusting pH value to be 3.0-6.0 and adding powder active carbon to carry out suction filtration; (3) adding sodium hydroxide till the pH value of the high-salt wastewater to be 10.0-11.0 and adding a flocculating agent to flocculate, settle and centrifugally separate; (4) converting magnesium hydroxide to light magnesium oxide through a self-control program in an industrial microwave oven under a heating condition, crushing and grinding the light magnesium oxide to prepare powder light magnesium oxide; (5) processing a clear liquor obtained in the step (3) by using a nanofiltration membrane to obtain a sodium salt solution and reuse the sodium salt solution in a production process. The intermediate high-salt mother liquor wastewater generated in the disperse dye production process is processed by a series of processes of removing COD, decolorizing, carrying out microwave treatment and membrane treatment, so that the waste liquid is recycled, thus realizing zero discharging of the wastewater.

Description

A kind of recycling treatment process containing magnesium high-salt wastewater
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
Since reform and opening-up along with the continuous sustained and rapid development of China's dyestuffs industries, dyestuff associated row had become one of mainstay industry for the Economic development of China already, simultaneously in order to adapt to the market specification of quality more and more higher to dye product, DYE PRODUCTION technique is constantly innovation thereupon also, and the difficulty of three wastes processing also increases thereupon.Particularly acid, alkali, inorganic salt etc. are as requisite raw material in dyestuffs industries, in various dye well intermediate production processes, nearly all to use the inorganic salt that inorganic salt and neutralization reaction produce, but in production process, inorganic salt do not enter product substantially, cause a large amount of inorganic salt to enter in waste liquor water, the difficulty that has not only increased enterprise's sewage disposal causes a large amount of wastings of resources simultaneously.Especially during " 12 ", along with constantly carrying out of national energy-saving reduction of discharging and cleaner production, the three wastes processing of dyestuffs industries is faced with stern challenge more, therefore how high salinity mother liquor waste water is carried out to effective processing and has become the new the difficult problem of environmental protection that dyestuff enterprise faces.
The high salt mother liquor waste water of at present domestic dye industry is administered thinking mainly based on direct evaporation concentration method, service water dilution method, biochemical treatment process, wet oxidation process, Fenton oxidation style, Ozonation etc.In evaporation concentration method, due to a large amount of steam of needs consumption, residual organic substances and inorganic salt become dangerous solid waste, can not thoroughly solve environmental issue; Service water dilution method need to consume a large amount of service waters, although can qualified discharge, do not meet the basic demand of energy-saving and emission-reduction, increase a large amount of effluent charge simultaneously; Biochemical treatment process is processed need to consume a large amount of service waters because salinity is higher, 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 remain in water, and cost of investment is larger, and equipment requirements is higher, cannot extensively popularize; Fenton oxidation style, Ozonation are substantially the same with wet oxidation process effect, can not solve equally the problem of salinity.Some producer adopts the combination of above two kinds of methods, has obtained certain effect.The patent documentation that for example publication number is CN103588307A discloses a kind of method of dye wastewater treatment using, comprises microorganism electrochemical coupled system is set, and microorganism electrochemical coupled system is by microbiological fuel cell and microorganism electrolysis cell coupling; Then the cathode compartment that pending waste water from dyestuff is packed into microorganism electrolysis cell is degraded.But the method needs complicated equipment, processing cost is higher.
In the face of increasingly serious environmental protection pressure, the discharge that how can effectively reduce three-waste pollution thing becomes current dye industry needs a great problem of solution badly.Dye industry need to change at present and is treated to main administration way with " end ", and in the links of production technique, constantly technical renovation, adjusts the product mix, and implements energy-saving and emission-reduction from source, controls and constantly reduces total emission volumn.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 approaching neutral middle height salt mother liquor waste water that contains magnesium chloride and sodium-chlor is prepared into the by product such as light magnesium oxide and sodium chloride solution, after clear liquid in centrifugal process being processed by membrane separation technique, can carry out recycling in production technique by direct reuse simultaneously, thereby reach the object of waste water reclaiming recycling and zero release.
Containing a recycling treatment process for magnesium high-salt wastewater, comprise the steps:
(1) collection and pre-treatment: what DYE PRODUCTION process was produced carries out categorised collection containing the high salt mother liquor waste water of magnesium ion, and carries out suction filtration pre-treatment respectively, dyestuff intermediate or dye product that recovery part runs off;
(2) decolouring is processed: in the pretreated high-salt wastewater of step (1) suction filtration, add acid, be adjusted to high-salt wastewater pH value 3.0~6.0, add Powdered Activated Carbon, and suction filtration after stirring, recycle after Powdered Activated Carbon regeneration;
(3) magnesium hydroxide separates: the high-salt wastewater that step (2) was processed adds continuously sodium hydroxide under agitation condition, until high-salt wastewater pH value stabilization is 10.0~11.0, add flocculation agent to carry out flocculating settling, after sedimentation, sediment enters centrifugation;
(4) prepare light magnesium oxide: centrifugal step (3) magnesium hydroxide obtaining is completed to magnesium hydroxide under automatic program Elevated Temperature Conditions in industrial microwave oven and be converted into light magnesium oxide, make powdery light magnesium oxide through pulverizing, grinding;
(5) film processing: the clear liquid that step (3) sedimentation and centrifugal treating are obtained adopts nanofiltration membrane treatment, obtaining mass percent through separating treatment is 20%~30% sodium salt solution, is back to the production technique of dyestuff or dyestuff intermediate as end water.
In step (1), what DYE PRODUCTION process was produced while carrying out categorised collection, generally carries out categorised collection according to dyestuff of the same race or dyestuff intermediate, so that the recycling of dyestuff and dyestuff intermediate containing the high salt mother liquor waste water of magnesium ion.In the high salt mother liquor waste water that collection obtains, the content of magnesium ion changes to some extent according to dye technology difference, all being suitable for method of the present invention processes, 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 is preferably and adopts magnesium oxide to prepare N as acid binding agent, the waste water producing in N-diethyl-3-acetylaminoaniline process containing the high salt mother liquor waste water of magnesium ion; Also can adopt other taking magnesium hydroxide, magnesium oxide, magnesiumcarbonate as the dyestuff of acid binding agent or mother liquid coming or the washing water etc. of dyestuff intermediate.
In step (2), the acid of employing can be hydrochloric acid, sulfuric acid etc.Waste Sulfuric Acid, the waste hydrochloric acid etc. that also can adopt preparation of dyestuff process to reclaim.Powdered Activated Carbon (English name: Powdered Activated Carbon, PAC), has good absorption property, and 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 showed, that, 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 determine 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 monitor by online pH meter, ensure that reaction end is pH value 10.0~11.0.After having reacted, add flocculation agent, flocculation agent can be selected PAM(polyacrylamide), as further preferably, described flocculation agent can be selected 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%.While experiment showed, the flocculation agent that adopts above-mentioned composition, better to the flocculating effect of magnesium hydroxide in high-salt wastewater.
In addition, in step (3), be to ensure flocculating effect, as preferably, add continuously stirring in flocculation agent process, after flocculation agent has added, then stir 15~30min, rotating speed control is 30r/min~45r/min, and then standing sedimentation 4~6h, and then carries out centrifugally operated.
In step (3), after having flocculated, generally adopt Horizontal sedimentation separating centrifuge to carry out detached job, for improving centrifugal treating efficiency and ensureing the clarity of clear liquid, as preferably, centrifuge speed is 2000~3500r/min; And it is 1.0~1.5t/h that separate unit whizzer is processed concentrated solution amount.The solid content of the magnesium hydroxide obtaining after centrifugation is 30%~45%.
In step (4), light magnesium oxide is the loose unformed powder of white lightweight, odorless, tasteless, nontoxic, the shared volume of light magnesium oxide is about three times of left and right of heavy-calcined magnesia, be worth relatively high, for obtaining the light magnesium oxide that quality is higher, the present invention adopt utilize industrial microwave oven process magnesium hydroxide.Experimental results show that, the control of temperature is larger to the quality influence of light magnesium oxide, 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.After having reacted, obtain light magnesium oxide, pulverizer is broken, grind that to obtain tap density be that 0.1~0.3g/mL, particle diameter are the light magnesium oxide that is not more than 2 μ m.The light magnesium oxide preparing can direct reuse to dyestuff or dyestuff intermediate preparation process, also can be used as production marketing, improve the benefit of enterprise.
Nanofiltration membrane is to allow solvent molecule or some low molecular weight solutes or ion sees through at a low price the functional semi-permeable membranes of one, to the desalination of monovalent anion salts solution lower than high price anion salt solution.In step (5), after adopting film to 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 processing: the clear liquid that step (3) sedimentation and centrifugal treating are obtained adopts nanofiltration membrane treatment, obtaining mass percent through separating treatment is 20%~30% sodium salt solution, is back to the production technique of dyestuff or dyestuff intermediate as end water.
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, waste liquid is carried out to recycling, turn waste into wealth, abandoned traditional evaporation concentration or advanced oxidation and processed method not thoroughly; In this technique, adopt energy-efficient microwave integration apparatus simultaneously, the magnesium hydroxide in waste water is made to light magnesium oxide, produce and greatly save production cost for intermediate; Simultaneously in addition by energy-efficient film processing, can direct reuse in production plant, realized waste water reclaiming processing intent, the while is also reduced the immense pressure that environmental protection of enterprise faces greatly.
Brief description of the drawings
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, after suction filtration, reclaim the dyestuff intermediate product in mother liquor, the clear liquid that suction filtration obtains is used sulfur waste acid for adjusting pH to 5.0~6.0, by adding 1% PAC of total processing 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 recycle after manipulation of regeneration, evenly add sheet alkali and constantly stir in color-less mother liquor by cage equipment, be 10.0~11.0 by online pH meter control terminal pH, under agitation condition, add continuously flocculation agent PAM(cationic polyacrylamide CP-7, 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 control is 30r/min, standing sedimentation 4h, the slurry magnesium hydroxide of precipitation separation after concentrated in bucket, (centrifugal speed is 2000r/min to pump into horizontal decanter centrifuge by spiral pump, it is 1.0t/h that separate unit whizzer is processed concentrated solution amount), it is 30% solid hydrogen magnesium oxide that separation obtains solid content, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, 480 DEG C of automatic control top temperatures, 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 the powder light magnesium oxide that is not more than 2 μ m, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtaining is by energy-efficient film processing (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 can be used as service water direct reuse in related production technique, greatly reduces this process operation cost.
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, after suction filtration, reclaim the dyestuff intermediate product in mother liquor, the clear liquid that suction filtration obtains is used sulfur waste acid for adjusting pH to 5.0~6.0, by adding 1.0% PAC of total processing 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 recycle after manipulation of regeneration, evenly add sheet alkali and constantly stir in color-less mother liquor by cage equipment, be 10.0~11.0 by online pH meter control terminal pH, under agitation condition, add continuously flocculation agent PAM(anion-polyacrylamide AP, 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 control is 40r/min, standing sedimentation 6h, the slurry magnesium hydroxide of precipitation separation after concentrated in bucket, (centrifugal speed is 2500r/min to pump into horizontal decanter centrifuge by spiral pump, it is 1.5t/h that separate unit whizzer is processed concentrated solution amount), it is 40% solid hydrogen magnesium oxide that separation obtains solid content, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, 490 DEG C of automatic control top temperatures, 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 the powder light magnesium oxide that is not more than 2 μ m, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtaining is by energy-efficient film processing (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 can be used as service water direct reuse in related production technique, greatly reduces this process operation cost.
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, after suction filtration, reclaim the dyestuff intermediate product in mother liquor, the clear liquid that suction filtration obtains is used sulfur waste acid for adjusting pH to 5.0~6.0, by adding 1% PAC of total processing 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 recycle after manipulation of regeneration, evenly add sheet alkali and constantly stir in color-less mother liquor by cage equipment, be 10.0~11.0 by online pH meter control terminal pH, under agitation condition, add continuously flocculation agent PAM(zwitter-ion polyacrylamide, 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 control is 45r/min, standing sedimentation 5h, the slurry magnesium hydroxide of precipitation separation after concentrated in bucket, (centrifugal speed is 3000r/min to pump into horizontal decanter centrifuge by spiral pump, it is 1.5t/h that separate unit whizzer is processed concentrated solution amount), it is 25% solid hydrogen magnesium oxide that separation obtains solid content, solid hydrogen magnesium oxide is by energy-efficient microwave integrated equipment for wastewater treatment, 470 DEG C of automatic control top temperatures, rate of heating is 10 DEG C/min, magnesium hydroxide is converted into after magnesium oxide becomes and pulverizes, it is 0.2g/mL for amassing density that grinding obtains particle diameter, be not more than the powder light magnesium oxide of 2 μ m, can direct reuse in original intermediate production technique.The centrifugal clear liquid obtaining is by energy-efficient film processing (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 can be used as service water direct reuse in related production technique, greatly reduces this process operation cost.
Test example 1:
According to national standard HG/T2573-2012, the by product light magnesium oxide product reclaiming in embodiment 1~3 is carried out to mass analysis, the results are shown in following table 1:
Table 1
From upper table 1, the by product sodium chloride solution and the light magnesium oxide that adopt processing method provided by the invention to obtain, meet enterprise completely industrial goods are used to basic index requirement, and membrane sepn clear liquid can be used 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, accomplish the processing intent of the utilization of high-salt wastewater complete resource with the zero release of dye technology generation.

Claims (10)

1. containing a recycling treatment process for magnesium high-salt wastewater, comprise the steps:
(1) collection and pre-treatment: what DYE PRODUCTION process was produced carries out categorised collection containing the high salt mother liquor waste water of magnesium ion, and carries out suction filtration pre-treatment respectively, dyestuff intermediate or dye product that recovery part runs off;
(2) decolouring is processed: in the pretreated high-salt wastewater of step (1) suction filtration, add acid, be adjusted to high-salt wastewater pH value 3.0~6.0, add Powdered Activated Carbon, and suction filtration after stirring, recycle after Powdered Activated Carbon regeneration;
(3) magnesium hydroxide separates: the high-salt wastewater that step (2) was processed adds continuously sodium hydroxide under agitation condition, until high-salt wastewater pH value is 10.0~11.0, adds flocculation agent to carry out flocculating settling, and after sedimentation, sediment enters centrifugation;
(4) prepare light magnesium oxide: centrifugal step (3) magnesium hydroxide obtaining is completed to magnesium hydroxide under automatic program Elevated Temperature Conditions in industrial microwave oven and be converted into light magnesium oxide, make powdery light magnesium oxide through pulverizing, grinding;
(5) film processing: the clear liquid that step (3) sedimentation and centrifugal treating are obtained adopts nanofiltration membrane treatment, obtaining mass percent through separating treatment is 20%~30% sodium salt solution, is back to the production technique of dyestuff or dyestuff intermediate as end water.
2. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, is characterized in that, in step (1), 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, is characterized in that, described flocculation agent is anion-polyacrylamide, cationic-type polyacrylamide, amphoteric ionic polyacrylamide.
4. according to the recycling treatment process containing magnesium high-salt wastewater described in claim 1 or 3, it 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, 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 (3), add continuously stirring in flocculation agent process, after flocculation agent has added, then stir 15~30min, rotating speed control is 30r/min~45r/min, and then standing sedimentation 4~6h, and then carry out centrifugally operated.
7. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, is characterized in that, in step (3), after having flocculated, adopts Horizontal sedimentation separating centrifuge to carry out detached job, and centrifuge speed is 2000~3500r/min; And it is 1.0~1.5t/h that separate unit whizzer is processed concentrated solution amount.
8. 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, intensification frequency is 10~15 DEG C/min.
9. 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 that reaction obtains is that 0.1~0.3g/mL, particle diameter are for being not more than 2 μ m.
10. the recycling treatment process containing magnesium high-salt wastewater according to claim 1, it is characterized in that, in step (1), described is to adopt magnesium oxide to prepare N as acid binding agent, the waste water producing in N-diethyl-3-acetylaminoaniline process containing the high salt mother liquor waste water of magnesium ion.
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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
CN111204780A (en) * 2020-01-09 2020-05-29 西安交通大学 Resource utilization process of salt mud in chlor-alkali industry
CN113401925A (en) * 2021-06-21 2021-09-17 宋纯 Method for removing organic impurities in waste sulfuric acid water in 2-ethyl anthraquinone production

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CN113401925A (en) * 2021-06-21 2021-09-17 宋纯 Method for removing organic impurities in waste sulfuric acid water in 2-ethyl anthraquinone production
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

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