CN104529010A - Pretreatment method for step-by-step demulsification and flocculation of DMTO catalyst centrifugal mother liquid through integrated internal-circulation reactor - Google Patents
Pretreatment method for step-by-step demulsification and flocculation of DMTO catalyst centrifugal mother liquid through integrated internal-circulation reactor Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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Abstract
The invention discloses a pretreatment method for step-by-step demulsification and flocculation of DMTO catalyst centrifugal mother liquid through an integrated internal-circulation reactor and relates to industrial sewage pretreatment methods. The pretreatment method aims to solve the technical problems that when an existing demulsification method is used for treating the DMTO catalyst centrifugal mother liquid, existing aluminium phosphate gel, sarciniform silicon aluminium phosphate gel (Al2O3-P2O5-SiO2-H2O) and other colloids are not dissolved out thoroughly, and in the flocculation treatment process, reaction re-dissolution happens, phosphate and aluminium gel is regenerated again, and the subsequent treatment process is disturbed. An integrated internal-circulation reactor system is composed of a reaction tank, a variable speed blender, a settling pond, an outflow water relay pond and an internal circulation backflow system. After the centrifugal mother liquid is treated step by step according to the order of pre-demulsification, demulsification, primary flocculation and secondary flocculation, COD is lowered by 70-90 percent, the sludge density index SDI15 of hydrocolloids is lower than four, and advanced treatment of recycling units is benefited. The method can be applied to pretreatment of other industrial sewage.
Description
Technical field
The present invention relates to technical field of waste water processing, be specifically related to a kind of integration-inner circulation reactor that utilizes and the pretreatment process of breakdown of emulsion and flocculation is carried out step by step to DMTO catalyzer centrifuge mother liquor.
Background technology
DMTO (preparing light olefins from methanol, Methanol to Olefins) is the gordian technique replacing the basic chemical raw materials such as oil production ethene, propylene with coal.The throughput of low-carbon alkene is the mark of a national oil chemical industry development and economic development level.As important petroleum chemicals, ethene and the propylene in the past main oil that relies on are produced.Along with the day by day minimizing of crude oil reserve, " replace oil with coal " produces low-carbon alkene, is the important channel realizing China's energy substitution strategy, ensure national energy security, cultivate novel industrial chain.Methyl alcohol is produced by coal based synthetic gas, alkene is obtained again by methyl alcohol, the intermediate that DMTO technology utilizes this Coal Chemical Industry of methyl alcohol important, achieves the coal leap that this grows out of nothing through preparing low carbon olefinic hydrocarbon with methanol, for China's " replace oil with coal " development strategy opens a new way.DMTO catalyzer is one of key factor realizing above-mentioned technique, plays very important effect to the selectivity of low-carbon alkene, transformation efficiency and yield.
Current Problems existing, be often produce 1 ton of DMTO catalyzer, can produce the brine waste of roughly 4 tons ~ 4.5 tons, this part brine waste solid content, between 8% ~ 10%, is referred to as mother liquor.An a part of not good liquor, also can become mother liquor after reuse for some time in addition.Because the content of phosphorus in mother liquor and aluminium is very high, add in mother liquor also containing pencil aluminium silicophosphate gel (Al
2o
3-P
2o
5-SiO
2-H
2o) and the colloid such as phosphaljel, the environment protection treating of mother liquor is made to seem very difficult.For many years, DMTO catalyst technology provider and enterprise take the multiple control measures about mother liquor, and also once for the environment protection treating of mother liquor has dropped into a large amount of funds, but problem is not solved all the time thoroughly.Along with the continuous increase of the DMTO catalyzer market requirement, mother liquor administers this environmental issue, has become the bottleneck of restriction enterprise development.
DMTO catalyzer centrifuge mother liquor---the mixed solution of not good liquor when being high slat-containing wastewater and the molecular sieve washing of Catalyst Production technological process discharge, not only solid content is high, in mother liquor also containing some amount, independent be the pencil aluminium silicophosphate gel (Al of suspended substance mutually
2o
3-P
2o
5-SiO
2-H
2o) and the colloid such as phosphaljel, stable emulsification system is constituted.DMTO Catalyst Production enterprise once utilized pencil aluminium silicophosphate gel can in the feature of stripping under sour environment, adopt acidization: in mother liquor, add sulfuric acid, as the method that centrifuge mother liquor " breakdown of emulsion " processes, but due to leachable excessive concentration, all the time there is leachable can not natural subsidence, leachable is difficult to dehydration, and the stripping of aluminium silicophosphate gel is thorough, and acidization process water outlet adopts further and again to form again emulsion and diluting water amount excessive problem during flocculation treatment.
Summary of the invention
The present invention to solve adopt acidization to DMTO catalyzer centrifuge mother liquor carry out leachable when " breakdown of emulsion " processes be difficult to dehydration, the stripping of pencil aluminium silicophosphate gel thoroughly and flocculation treatment time occur that reaction is returned molten, be concatenated to form the problem of phosphorus, alumina gel interference subsequent processes, and provide a kind of integration-inner circulation reactor that utilizes to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor.
Integration-inner circulation reactor system: integration-inner circulation reactor system is made up of reaction tank, variable-speed agitator, settling tank, water outlet relaying pond and inner circulating reflux system;
Integration-inner circulation reactor system is pressed: the sequential series that pre-breakdown of emulsion section, breakdown of emulsion section, one-level flocculation and secondary are wadded a quilt with cotton runs step by step; Being pre-breakdown of emulsion reactor A in pre-breakdown of emulsion section, is breakdown of emulsion reactor B in breakdown of emulsion section, is one-level flocculation reactor C in one-level flocculation section, is secondary flocculation reactor D in secondary flocculation section;
Wherein, water inlet A/the B/C/D of integration-inner circulation reactor is arranged on the bottom of reaction tank side, the water-in of pre-breakdown of emulsion reactor A is centrifuge mother liquor fluid inlet, feed liquor under meter A is arranged on the front portion of water inlet A, variable-speed agitator A/B/C/D is arranged on the inside of reaction tank A/B/C/D, dosing mouth A/B/C/D is arranged on the top of water inlet A/B/C/D, reaction tank overflows the top that mouth of a river A/B/C/D is arranged on reaction tank side, pH observing and controlling probe A/B/C/D is arranged on the below that reaction tank overflows mouth of a river A/B/C/D, settling tank inside arranges water inlet training wall A/B/C/D, settling tank bottom arranges precipitating sludge bucket A/B/C/D, sludge from sedimentation tank mouth A/B/C/D is arranged on sludge bucket lowermost end, settling tank overflow water outlet enters water outlet relaying pond A/B/C/D by effluent weir A/B/C/D, inner circulating reflux water out A/B/C/D is arranged on the bottom of side, relaying pond and is connected with inner circulating reflux system A/B/C/D, reactor overflow water outlet A/B/C/D is arranged on the top of side, relaying pond,
By pipe connecting, the overflow water outlet A of pre-breakdown of emulsion reactor is communicated with the water-in D of secondary flocculation reactor with the mouth of a river C that overflows of one-level flocculation reactor with the water-in C of one-level flocculation reactor with the water inlet B of breakdown of emulsion reactor, the overflow water outlet B of breakdown of emulsion reactor.
The present invention utilizes integration-inner circulation reactor to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, specifically carries out according to the following steps:
One, by the unit time treatment capacity of centrifuge mother liquor by design, the reaction tank of pre-breakdown of emulsion reactor is injected continuously through pre-breakdown of emulsion reactor water inlet A, and to centrifuge mother liquor thin up by a certain percentage, add pre-breakdown of emulsion medicament in proportion by dosing mouth A simultaneously, stirring reaction for some time, the pH value in pre-breakdown of emulsion reaction tank is made to reach and remain between 5.5 ~ 6.5, then pre-breakdown of emulsion settling tank is entered through overflow water outlet A, supernatant liquor after precipitate and separate overflows mill weir A by settling tank and enters water outlet relaying pond A and store, the clear liquid stored in the A of relaying pond, by pre-breakdown of emulsion section inner circulating reflux system flowback to pre-breakdown of emulsion reaction tank, progressively substitute tap water to dilute centrifuge mother liquor, until when the pre-breakdown of emulsion section precipitation supernatant liquor of backflow can substitute the tap water of dilution centrifuge mother liquor completely, pre-breakdown of emulsion reactor water outlet relaying pond overflow water outlet A starts water outlet.
Two, when above-mentioned pre-breakdown of emulsion section relaying pond overflow water outlet A starts water outlet, continue to inject centrifuge mother liquor to pre-breakdown of emulsion reactor, then pre-breakdown of emulsion reactor for treatment water outlet enters breakdown of emulsion reactor water inlet B by communicating pipe gravity flow, unlatching breakdown of emulsion reacts, add breakdown of emulsion medicament in proportion by dosing mouth B simultaneously, stirring reaction for some time, pH value in breakdown of emulsion reaction tank is reached and remains between 1.0 ~ 2.0, then breakdown of emulsion settling tank is entered through overflow water outlet B, supernatant liquor after gravitational settling is separated overflows mill weir B by settling tank and enters water outlet relaying pond B, then a part is intake to the dilution of breakdown of emulsion reaction tank through breakdown of emulsion section inner circulating reflux system flowback, a part is then the water outlet of breakdown of emulsion reactor.
Three, the water outlet of above-mentioned breakdown of emulsion section reactor overflow water outlet B, through communicating pipe, one-level flocculation tank C is entered continuously by one-level flocculation reactor water-in C, open one-level flocculation reactor, add certain density aqua calcis in proportion by dosing mouth C simultaneously, stirring reaction for some time, pH value is reached and remains between 4.5 ~ 5.5, then one-level flocculation sedimentation tank is entered through overflowing mouth of a river C, supernatant liquor after gravitational settling is separated overflows mill weir C by settling tank and enters water outlet relaying pond C, a part is intake to the dilution of one-level flocculation tank through one-level flocculation section inner circulating reflux system flowback, a part is then the water outlet of one-level flocculation reactor.
Four, the water outlet of above-mentioned one-level flocculation section reactor, secondary flocculation tank is entered continuously by secondary flocculation reactor water-in D with communicating pipe, open secondary flocculation reactor, add finite concentration aqua calcis in proportion by dosing mouth D simultaneously, stirring reaction for some time, pH value is reached and remains between 8.0 ~ 9.0, then secondary flocculation sedimentation tank is entered through overflowing mouth of a river D, supernatant liquor after gravitational settling is separated overflows mill weir D by settling tank and enters water outlet relaying pond D, a part is intake to the dilution of secondary flocculation tank through secondary flocculation section inner circulating reflux system flowback, a part then starts overflow water outlet for secondary flocculation reactor overflows mouth of a river D, complete utilization integration-inner circulation reactor carries out breakdown of emulsion and flocculation step by step pretreatment process to DMTO catalyzer centrifuge mother liquor,
Wherein, the pre-emulsion splitter added in step one is bodied ferric sulfate, and the emulsion splitter added in step 2 is the quality obtained after adopting sulfuric acid dissolution crystalline sulfuric acid magnesium is the Adlerika of 0.5% ~ 5.0% than concentration;
The aqua calcis added in step 3 and step 4, adds certain proportion water by calcium oxide and obtains;
The invention has the beneficial effects as follows: the present invention utilizes integration-inner circulation reactor to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, adopt the mode of two-part breakdown of emulsion and two-stage flocculation series operation, carry out processing step by step, continuously to DMTO centrifuge mother liquor, make the colloid in mother liquor in acid condition stripping and the reaction process of flocculating in the basic conditions separately carry out, fundamentally eliminate colloid indissoluble thing and react and return molten prerequisite; The present invention adopts independent backflow and the method with phegma dilution water inlet at each section further, while guarantee each section of sufficient reacting, saving dosage, save a large amount of diluting waters; The present invention selects inorganic macromolecule flocculant poly ferric sulfate as pre-emulsion splitter, make colloid stripping in mother liquor thorough with the use of crystalline sulfuric acid magnesium, and not containing objectionable impuritiess such as aluminium, chlorine and heavy metal ion in two kinds of medicaments, in reaction, also the aqueous phase of non-iron-ion and magnesium ion shifts; The present invention selects calcium hydroxide as flocculation agent, in obtaining and the major ingredient of flocculation be that calcareous mineral substance composition is beneficial to recovery.
Utilization integration-inner circulation reactor system that the present invention adopts, can run by sectional intermittent, also the form of connecting can be taked to run step by step, continuously by the order of pre-breakdown of emulsion section, breakdown of emulsion section, one-level flocculation section and secondary flocculation section;
Breakdown of emulsion reactor of the present invention, one-level flocculation reactor and the water inlet B of secondary flocculation reactor, the level attitude of C, D, respectively lower than the overflow water outlet A of pre-breakdown of emulsion reactor, breakdown of emulsion reactor and one-level flocculation reactor, the level attitude of B, C, make each reactor production water flow into next stage reactor step by step under gravity, reduce power consumption.
The present invention combines other treatment process, can realize wastewater reusing treatment.
Accompanying drawing explanation
Fig. 1 is integration-inner circulation reactor system schematic, in figure, 1 is reactor water inlet A/B/C/D, 2 is feed water flow gauge, 3 is variable-speed agitator A/B/C/D, 4 is dosing mouth A/B/C/D, 5 overflow mouth of a river A/B/C/D for reaction tank, 6 is pH meter A/B/C/D, 7 is training wall A/B/C/D, 8 is precipitating sludge bucket A/B/C/D, 9 is mud discharging mouth A/B/C/D, 10 overflow mill weir A/B/C/D for settling tank, 11 is inner circulating reflux water out A/B/C/D, 12 is relaying pond water outlet A/B/C/D, 13 is reaction tank A/B/C/D, 14 is settling tank A/B/C/D, 15 is relaying pond A/B/C/D, 16 is inner circulating reflux system A/B/C/D,
Fig. 2 is pre-breakdown of emulsion section, breakdown of emulsion section, one-level flocculation section and secondary flocculation section reactor assembly A/B/C/D series connection schematic diagram.
Embodiment
Embodiment one: present embodiment utilizes integration-inner circulation reactor to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, be realized by the sequential series of pre-breakdown of emulsion reactor A, breakdown of emulsion reactor B, one-level flocculation reactor C and secondary flocculation reactor D, the mode run step by step by integration-inner circulation reactor device A/B/C/D, specifically carry out according to the following steps:
One, first, by DMTO catalyzer centrifuge mother liquor thin up in proportion, centrifuge mother liquor: tap water=1: (3 ~ 5);
Two, by the unit time treatment capacity of the centrifuge mother liquor after dilution by design, through feed liquor under meter A2, pre-breakdown of emulsion reactor water inlet A 1 injects pre-breakdown of emulsion reaction tank A13 continuously, open the reaction of pre-breakdown of emulsion, add pre-breakdown of emulsion medicament in proportion by dosing mouth A4 simultaneously, stirring reaction 5 ~ 10min, pH value is reached and remains between 5.5 ~ 6.5, then pre-breakdown of emulsion settling tank A14 is entered through overflowing mouth of a river A5, pre-breakdown of emulsion settling tank hydraulic detention time is 30 ~ 60min, supernatant liquor after precipitate and separate overflows mill weir A10 by settling tank and enters water outlet relaying pond A15, the clear liquid stored in water outlet relaying pond A15, by inner circulating reflux system A16 be back to pre-breakdown of emulsion reaction tank A13 progressively substitute tap water centrifuge mother liquor is diluted, when quantity of reflux reaches more than 5 times of centrifuge mother liquor liquid inlet volume, the pre-breakdown of emulsion section precipitation supernatant liquor of backflow substitutes the tap water of dilution centrifuge mother liquor completely, pre-breakdown of emulsion reactor overflow water outlet A 12 starts overflow water outlet.
Three, after above-mentioned pre-breakdown of emulsion reactor overflow water outlet A 12 starts overflow water outlet, continue to inject centrifuge mother liquor to pre-breakdown of emulsion reactor water inlet A 1, pre-breakdown of emulsion section process water outlet is then through being entered the reaction tank B13 of breakdown of emulsion reactor communicating pipe continuously by breakdown of emulsion reactor water inlet B 1, unlatching breakdown of emulsion reacts, add breakdown of emulsion medicament in proportion by dosing mouth B4 simultaneously, stirring reaction 15 ~ 30min, pH value is reached and remains between 1.0 ~ 2.0, then breakdown of emulsion settling tank B14 is entered through overflowing mouth of a river B5, breakdown of emulsion settling tank hydraulic detention time is 60 ~ 120min, supernatant liquor after precipitate and separate, overflow mill weir B10 by settling tank and enter water outlet relaying pond B15, the clear liquid stored in water outlet relaying pond B15, breakdown of emulsion reaction tank B13 is back to by breakdown of emulsion section inner circulating reflux system B16, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, breakdown of emulsion reactor overflow water outlet B 12 starts overflow water outlet.
Four, the overflow water outlet of above-mentioned breakdown of emulsion reactor overflow water outlet B 12, through to be entered the reaction tank C13 of one-level flocculation reactor communicating pipe continuously by one-level flocculation reactor water-in C1, open one-level flocculation reaction, add certain density aqua calcis in proportion by dosing mouth C4 simultaneously, stirring reaction 15 ~ 30min, pH value is reached and remains between 4.5 ~ 5.5, then one-level flocculation sedimentation tank C14 is entered through overflowing mouth of a river C5, one-level flocculation sedimentation tank hydraulic detention time is 90 ~ 120min, supernatant liquor after precipitate and separate overflows mill weir C10 by settling tank and enters water outlet relaying pond C15, the clear liquid stored in water outlet relaying pond C15, one-level flocculation tank C13 is back to by one-level flocculation section inner circulating reflux system C16, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, one-level flocculation reactor overflows mouth of a river C12 and starts overflow water outlet.
Five, above-mentioned one-level flocculation reactor overflows the overflow water outlet of mouth of a river C12, through to be entered the reaction tank D13 of secondary flocculation reactor communicating pipe continuously by secondary flocculation reactor water-in D1, open secondary flocculation reaction, throw certain density hydro-oxidation calcium solution in proportion by dosing mouth D4 simultaneously, stirring reaction 30 ~ 60min, pH value is reached and remains between 8.0 ~ 9.0, then secondary flocculation sedimentation tank D14 is entered through overflowing mouth of a river D5, secondary flocculation sedimentation tank hydraulic detention time is 120 ~ 180min, supernatant liquor after precipitate and separate overflows mill weir D10 by settling tank and enters water outlet relaying pond D15, the clear liquid stored in water outlet relaying pond D15, by secondary flocculation section inner circulating reflux system flowback to secondary flocculation tank D13, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, secondary flocculation reactor overflows mouth of a river D and starts overflow water outlet, complete utilization integration-inner circulation reactor carries out breakdown of emulsion and flocculation step by step pretreatment process to DMTO catalyzer centrifuge mother liquor.
Embodiment two: this embodiment and embodiment one unlike the level attitude of: pre-breakdown of emulsion reactor water outlet A 12 higher than the level attitude 20cm of breakdown of emulsion reactor water outlet B 12, the level attitude of breakdown of emulsion reactor water outlet B 12 higher than the level attitude of the level attitude 20cm of one-level flocculation reactor water outlet C12, one-level flocculation reactor water outlet C12 higher than the level attitude 20cm of secondary flocculation reactor water outlet D12.Other is identical with embodiment one.
Embodiment three: this embodiment and embodiment one or two unlike: first pre-breakdown of emulsion reaction tank A13 and settling tank A14 is full of water, and with pre-emulsion splitter, the pH value in A13, A14 is adjusted between 6 ~ 6.5; Equally, also breakdown of emulsion reaction tank B13 settling tank B14 is full of water, with emulsion splitter, the pH value in B13, B14 is adjusted between 1.5 ~ 2.0 in advance, also one-level flocculation tank C13, settling tank C14 and secondary flocculation tank D13, settling tank D14 are full of water, and between with aqua calcis the pH value in C13, C14 and D13, D14 being adjusted to 4.5 ~ 5.0 respectively in advance and between 8.5 ~ 9.0, then inject centrifuge mother liquor by centrifuge mother liquor fluid inlet A1 to pre-breakdown of emulsion reaction tank A13.Other is identical with embodiment one or two.
Beneficial effect of the present invention is verified by following embodiment:
Embodiment one:
The present embodiment utilizes integration-inner circulation reactor to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, is to be realized according to the sequential series of pre-breakdown of emulsion reactor A, breakdown of emulsion reactor B, one-level flocculation reactor C and secondary flocculation reactor D, the mode run step by step by integration-inner circulation reactor device A/B/C/D.Specifically carry out according to the following steps:
One, first, by DMTO catalyzer centrifuge mother liquor thin up in proportion, centrifuge mother liquor: tap water=1: 3;
Two, by the unit time treatment capacity of the centrifuge mother liquor after dilution by design, through feed liquor under meter A2, pre-breakdown of emulsion reaction tank A13 is injected continuously by pre-breakdown of emulsion reactor water inlet A 1, open the reaction of pre-breakdown of emulsion, add pre-breakdown of emulsion medicament in proportion by dosing mouth A4 simultaneously, stirring reaction 5min, pH value is reached and remains between 5.5 ~ 6.5, then pre-breakdown of emulsion settling tank A14 is entered through overflowing mouth of a river A5, pre-breakdown of emulsion settling tank hydraulic detention time is 30min, supernatant liquor after precipitate and separate overflows mill weir A10 by settling tank and enters water outlet relaying pond A15, the clear liquid stored in water outlet relaying pond A15, by pre-breakdown of emulsion section inner circulating reflux system A16 be back to pre-breakdown of emulsion reaction tank A13 progressively substitute tap water centrifuge mother liquor is diluted, when quantity of reflux reaches 5 times of centrifuge mother liquor liquid inlet volume, the pre-breakdown of emulsion section precipitation supernatant liquor of backflow substitutes the tap water of dilution centrifuge mother liquor completely, pre-breakdown of emulsion reactor overflow water outlet A 12 starts overflow water outlet.
Three, after above-mentioned pre-breakdown of emulsion reactor overflow water outlet A 12 starts overflow water outlet, continue to inject centrifuge mother liquor to pre-breakdown of emulsion reactor water inlet A 1, pre-breakdown of emulsion section process water outlet then enters breakdown of emulsion reaction tank B13 through communicating pipe by breakdown of emulsion reactor water inlet B 1 continuously, unlatching breakdown of emulsion reacts, add breakdown of emulsion medicament in proportion by dosing mouth B4 simultaneously, stirring reaction 30min, pH value is reached and remains between 1.0 ~ 2.0, then breakdown of emulsion settling tank B14 is entered through overflowing mouth of a river B5, breakdown of emulsion settling tank hydraulic detention time is 120min, supernatant liquor after precipitate and separate overflows mill weir B10 by settling tank and enters water outlet relaying pond B15, the clear liquid stored in water outlet relaying pond B15, breakdown of emulsion reaction tank B13 is back to by breakdown of emulsion section inner circulating reflux system B16, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, breakdown of emulsion reactor overflow water outlet B 12 starts overflow water outlet.
Four, the overflow water outlet of above-mentioned breakdown of emulsion reactor overflow water outlet B 12, one-level flocculation tank C13 is entered continuously by one-level flocculation reactor water-in C1 through communicating pipe, open one-level flocculation reaction, add certain density aqua calcis in proportion by dosing mouth C4 simultaneously, stirring reaction 30min, pH value is reached and remains between 4.5 ~ 5.5, then one-level flocculation sedimentation tank C14 is entered through overflowing mouth of a river C5, one-level flocculation sedimentation tank hydraulic detention time is 90min, supernatant liquor after precipitate and separate overflows mill weir C10 by settling tank and enters water outlet relaying pond C15, the clear liquid stored in water outlet relaying pond C15, one-level flocculation tank is back to by one-level flocculation section inner circulating reflux system C16, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, one-level flocculation reactor overflows mouth of a river C12 and starts overflow water outlet.
Five, the overflow water outlet of above-mentioned one-level flocculation section reactor overflow water outlet C12, through to be entered the reaction tank D13 of secondary flocculation reactor communicating pipe continuously by secondary flocculation reactor water-in D1, open secondary flocculation reaction, throw certain density hydro-oxidation calcium solution in proportion by dosing mouth D4 simultaneously, stirring reaction 30 ~ 60min, pH value is reached and remains between 8.5 ~ 9.0, then secondary flocculation sediment district D14 is entered through overflowing mouth of a river D5, secondary flocculation sediment district hydraulic detention time is 120min, supernatant liquor after precipitate and separate overflows mill weir D10 by settling tank and enters water outlet relaying pond D15, the clear liquid stored in water outlet relaying pond D15, by secondary flocculation section inner circulating reflux system flowback to secondary flocculation tank D13, when quantity of reflux reaches 5 ~ 15 times of centrifuge mother liquor liquid inlet volume, secondary flocculation reactor overflows mouth of a river D and starts overflow water outlet, then collect, obtain the water outlet of secondary flocculation reactor.
The present embodiment secondary flocculation water outlet clear appearance, transparent, pH value 7.5 ~ 9.0, water-borne glue body alluvial density index SDI
15be 3.8, after one-level ultra-filtration membrane (UF) filters, water-borne glue body alluvial density index SDI
15drop to less than 2.5, for further advanced treatment and reclamation is had laid a good foundation.
Claims (6)
1. utilize integration-inner circulation reactor to carry out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that the method is flocculated by two-part breakdown of emulsion and two-stage to form, two-part breakdown of emulsion is by pre-breakdown of emulsion section, breakdown of emulsion section forms, two-stage flocculation is flocculated by one-level, secondary flocculation composition, integration-inner circulation reactor system is by reaction tank (13), settling tank (14), water outlet relaying pond (15) and inner circulating reflux system (16) composition, integration-inner circulation reactor is pre-breakdown of emulsion reactor A in pre-breakdown of emulsion section, be breakdown of emulsion reactor B in breakdown of emulsion section, one-level flocculation section be one-level flocculation reactor C, secondary flocculation section be secondary flocculation reactor D.
2. utilization integration-inner circulation reactor according to claim 1 carries out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that the method is carried out according to the following steps:
(1) centrifuge mother liquor is injected the reaction tank A (13) of pre-breakdown of emulsion reactor, add pre-breakdown of emulsion medicament in proportion by dosing mouth A (4) simultaneously, stirring reaction 5 ~ 10min, pH value is reached and remains between 5.5 ~ 6.5, then pre-breakdown of emulsion settling tank A (14) is entered through overflow water outlet A (5), supernatant liquor after precipitate and separate overflows mill weir A (10) by settling tank and enters water outlet relaying pond A (15), and a part of clear liquid is back to reaction tank A (13) by pre-breakdown of emulsion section internal circulation system A (16);
(2) through communicating pipe, gravity flow enters the reaction tank B (13) of breakdown of emulsion reactor in pre-breakdown of emulsion reactor water outlet, unlatching breakdown of emulsion reacts, add breakdown of emulsion medicament in proportion by dosing mouth B (4) simultaneously, stirring reaction 15 ~ 30min, pH value is reached and remains between 1.0 ~ 2.0, then breakdown of emulsion settling tank B (14) is entered through overflow water outlet B (5), supernatant liquor after precipitate and separate overflows mill weir B (10) by settling tank and enters water outlet relaying pond B (15), part clear liquid is back to breakdown of emulsion reaction tank B (13) by breakdown of emulsion section inner circulating reflux system B (16),
(3) through communicating pipe, gravity flow enters the reaction tank C (13) of one-level flocculation reactor to the water outlet of breakdown of emulsion section reactor, open one-level flocculation reaction, add certain density aqua calcis in proportion by dosing mouth C (4) simultaneously, stirring reaction 15 ~ 30min, pH value is reached and remains between 4.5 ~ 5.5, then one-level flocculation sedimentation tank C (14) is entered through overflowing mouth of a river C (5), supernatant liquor after precipitate and separate overflows mill weir C (10) by settling tank and enters water outlet relaying pond C (15), part clear liquid is back to one-level flocculation tank C (13) by one-level flocculation section inner circulating reflux system C (16),
(3) one-level flocculation section reactor water outlet, through communicating pipe, gravity flow enters the reaction tank D (13) of secondary flocculation reactor, open secondary flocculation reaction, add certain density hydro-oxidation calcium solution in proportion by dosing mouth D (4) simultaneously, stirring reaction 30 ~ 60min, pH value is reached and remains between 8.0 ~ 9.0, then secondary flocculation sedimentation tank D (14) is entered through overflowing mouth of a river D (5), supernatant liquor after precipitate and separate overflows mill weir D (10) by settling tank and enters water outlet relaying pond D (15), part clear liquid is back to one-level flocculation tank C (13) by one-level flocculation section inner circulating reflux system C (16).The water outlet of secondary flocculation treatment, collects in relaying pond D (15), completes and utilizes reaction-precipitation integral reactor to carry out the pretreatment process of two-part breakdown of emulsion and two-stage flocculation step by step to DMTO catalyzer centrifuge mother liquor.
3. the utilization integration-inner circulation reactor according to claim 1,2 carries out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that described step by step to the method that DMTO centrifuge mother liquor processes, be: pre-breakdown of emulsion section carries out pre-breakdown of emulsion process to centrifuge mother liquor, breakdown of emulsion section does further process to pre-breakdown of emulsion process water outlet, one-level flocculation section does flocculation treatment to breakdown of emulsion process water outlet, and secondary flocculation section does further process to one-level flocculation section process water outlet.
4. the utilization integration-inner circulation reactor according to claim 1,2,3 carries out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that described step one, two, three and step 4 carry out inner circulating reflux respectively.Wherein, the reflux ratio of step one is 5: 1, and the reflux ratio of step 2, step 3 and step 4 is (5 ~ 15): 1.
5. the utilization integration-inner circulation reactor according to claim 1,2,3 carries out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that described pre-breakdown of emulsion medicament is bodied ferric sulfate, described emulsion splitter adopts concentration be the quality obtained after 15% ~ 60% sulfuric acid dissolution crystalline sulfuric acid magnesium to be the Adlerika of 0.5% ~ 5% than concentration, and described aqua calcis adds certain proportion water by calcium oxide and obtains.
6. the utilization integration-inner circulation reactor according to claim 1,2,3,4 and 5 carries out the pretreatment process of breakdown of emulsion and flocculation step by step to DMTO catalyzer centrifuge mother liquor, it is characterized in that the hydraulic detention time in described pre-breakdown of emulsion settling tank A (14) is 30 minutes, hydraulic detention time in described breakdown of emulsion settling tank B (14) is 90 ~ 120 minutes, hydraulic detention time in described one-level flocculation sedimentation tank C (14) is 90 minutes, and the hydraulic detention time in described secondary flocculation sedimentation tank D (14) is 90 ~ 120 minutes.
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