CN103588329A - Condensation mother liquid waste water pretreatment and resource system and method in compound neutralization reactor in disperse blue 56 production process - Google Patents
Condensation mother liquid waste water pretreatment and resource system and method in compound neutralization reactor in disperse blue 56 production process Download PDFInfo
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Abstract
The invention discloses condensation mother liquid waste water pretreatment and a resource system and a method in a compound neutralization reactor in a disperse blue 56 production process, which belongs to the waste water treatment field. The method comprises the following steps: highly basic condensation mother liquid waste water in the disperse blue 56 production process and a mixed acid solution (sulfuric acid and sulfamic acid) in the compound neutralization reactor are neutralized, three purposes of reducing the pH value of waste water, precipitating phenol and removing nitrite can be simultaneously realized; the neutralized waste water passes through a fixed bed adsorption column filled with adsorption resin, so that residual phenol in the waste water can absorb on the resin column. Resin after adsorption saturation is carried out with desorption and regeneration by using a NaOH solution and then the resin is repeatedly usable, and the desorption liquid passes through the processes of acidity adjusting and vacuum distillation of phenol to realize recycling of phenol. According to the condensation mother liquid waste water which is pretreated in the disperse blue 56 production process, CODCr value is decreased from about 55000mg/L to less than 500mg/L, the phenols substance concentration is decreased from about 19000mg/L to less than 20mg/L, the nitrite ion is decreased from 87000mg/L to less than 20mg/L; thereby the treatment and resource utilization of waste water can be effectively realized.
Description
Technical field
The present invention relates to Wastewater Pretreatment and resource utilization in a kind of disperse blue 56 production process, particularly a kind of condensed mother liquor Wastewater Pretreatment and recycling system and the method in compound neutralization reactor and disperse blue 56 production process.
Background technology
Disperse blue 56 (Disperse Blue56, No. CAS: 12217-79-7, be also called for short 56# orchid) and be a kind of important dyestuff, it can give off the dense strong basicity waste water containing phenol and Sodium Nitrite of a large amount of height, waste water COD in process of production
crbe about 55000mg/L, the about 1.9%(massfraction of phenol content), the about 8.7%(massfraction of nitrite ion content), pH>14, therefore this wastewater toxicity is large, biodegradability is poor, is difficult to subsequent disposal, if do not carry out effective improvement meeting, environment is not done great damage.Three technical barriers that exist in governance process of this waste water need to solve:
Therefore in needing in the strong basicity condensed mother liquor waste water treatment process in disperse blue 56 production process and the alkalescence of waste water, reclaim the phenol in waste water, and remove the nitrite ion in waste water.Completing above-mentioned target can effectively reduce wastewater toxicity, is convenient to the follow-up advanced treatment of waste water, brings obvious economic benefit to producer simultaneously.
Summary of the invention
1. the technical problem that will solve
For the waste water producing in disperse blue 56 production process, in governance process, there are three technical barriers, the object of this invention is to provide condensed mother liquor Wastewater Pretreatment and recycling system and method in a kind of compound neutralization reactor and disperse blue 56 production process, in and waste water alkalescence, remove waste water Nitrite ion and reclaim phenol in wastewater class material.
2. technical scheme
A kind of compound neutralization reactor, it is by outside water-in, vapor pipe is (for the nitrogen protoxide that guides reaction process to generate, nitrogen peroxide secondary contacts and is absorbed with alkaline waste water, also discharge nitrogen) simultaneously, inner inlet mouth, mixed acid solution injection port, throw out relief outlet (the phenol throw out producing for discharging neutralization precipitation), acid solution refluxing opening, stirring rake, condensate return pipe (is collected neutralization reaction, the heat that redox reaction process produces, intensification for resin desorption process), sloping plate deposition district (for phenol precipitation solid-liquid separation), the gas collection reflection centrum (nitrogen generating for collecting reaction process, nitrogen protoxide, nitrogen peroxide), outside water outlet, pH meter probe forms.Compound neutralization reactor inside is divided into reaction Ι district and two, П district of reaction conversion zone with dividing plate, and outside water-in lays respectively at the upper end of reacting Ι district and reaction П district with outside water outlet; Inner inlet mouth is positioned at the bottom of reactor NeiΙ district YuП district intersection; Mixed acid solution injection port, throw out relief outlet, acid solution refluxing opening are positioned at the bottom in reactor reaction П district; Stirring rake and condensate return pipe are positioned at the middle and lower part in reaction П district; Sloping plate deposition district is positioned at the top of condensate return pipe; Top, sloping plate deposition district is gas collection reflection centrum; Vapor pipe opening part is reaction Ι district and the gas collection reflection centrum position of reacting dividing plate between П district, and exhaust outlet is positioned at the bottom in reaction Ι district; Gas collection reflection centrum top is pH meter probe.
Compare with traditional neutralization reactor, compound neutralization reactor has following innovative point:
(1) there is oxidation restoring function, in reactor, not only carry out acid-base neutralisation reaction, also carry out redox reaction, remove nitrite ion;
(2) there is the sour gas of absorption function, in acid-base neutralisation reaction process, not only utilize in the mixed acid solution adding and waste water alkalescence, can also utilize the sour gas that waste water self alkalescence absorbs, neutralization generates, avoid the release of toxic gas;
(3) have solid-liquid separation function, the phenol precipitation that neutralization can be formed is separated from waste water.
Pre-treatment and the recycling system of the condensed mother liquor waste water in a kind of disperse blue 56 production process, its by sodium hydroxide solution storage tank, thionamic acid storage tank, vitriol oil storage tank, compound neutralization reactor (in and waste water alkalescence, precipitate a part of phenol, remove nitrite ion), resin absorbing column (reclaiming through the remaining phenol of compound neutralization reactor processed waste water for adsorbing), acid-base neutralisation solid-liquid separator form (for precipitating the phenol that reclaims desorption liquid and throw out); Structural relation between each composition is that compound neutralization reactor water outlet is connected with the water-in of resin absorbing column, its mixed acid solution injection port is connected with vitriol oil storage tank, thionamic acid storage tank respectively, and its throw out relief outlet, acid solution refluxing opening are connected with acid-base neutralisation solid-liquid separator respectively; Resin absorbing column desorption liquid injection port is connected with sodium hydroxide solution storage tank, and the desorption liquid outlet of resin absorbing column is connected with acid-base neutralisation solid-liquid separator.
This system advantage:
(1) utilize the vitriol oil in mixed acid solution in compound neutralization reactor in and strong basicity waste water, can directly reclaim phenol precipitation, and the NO and the NO that generate
2gas is absorbed by alkaline waste water, avoids being emitted in air working the mischief; Utilize thionamic acid in mixed acid solution that waste water Nitrite ion is reduced into nitrogen and discharge, remove nitrite ion, be convenient to water outlet and carry out subsequent disposal, and the sulfuric acid generating in reaction process can continue in and waste water alkalescence, save sour consumption;
(2) heat producing in acid-base neutralisation process is absorbed by the circulating condensing water in inside reactor prolong, and the resin column that is used for heating follow-up phase, to improve the desorption rate of resin, has been realized recovery and the utilization of heat;
(3) adopt resin adsorption method absorption Phenol for Waste Water class material, can effectively reduce waste water COD and phenol content, the resin adsorbing after saturated adopts thermokalite desorption and regeneration, realizes resin and reuses, and recyclable phenol after desorption liquid acid adjustment, realizes resource utilization target.
Pre-treatment and the method for resource of condensed mother liquor waste water in production process, its step comprises:
In step 1. and reduction: by the condensed mother liquor waste water in disperse blue 56 production process in compound neutralization reactor Ι district, with the mixed acid solution adjust pH of sulfuric acid and thionamic acid to 4-6, NO and the NO of N-process generation
2gas is most of in floating-upward process is absorbed (reaction formula 1-3) by alkaline waste water self, and thionamic acid react generation nitrogen (reaction formula 4) with nitrite ion, and nitrogen enters gas collection district through reflecting cone effect, by vapor pipe, by reactor П district, is discharged;
Concrete reaction equation is as follows:
2H
++NO
2 -+OH
-→HNO
2+H
2O （1）
2HNO
2→NO↑+NO
2↑+H
2O （2）
NO
2+NO+H
2O+2OH
-→2NO
2 -+2H
2O （3）
NH
2-SO
3H+NO
2 -→N
2↑+H
3O
++SO
4 2- （4）
Remaining a small amount of NO and NO
2gas enters gas collection district through reflection cone effect, after by escape pipe, enter compound neutralization reactor I district, again completely by alkaline waste water and absorption (reaction formula 3).The circulating condensing water that in reaction process, liberated heat is condensed in water return line absorbs, and the insulation jacket that heated water of condensation enters resin column guarantees desorption temperature.After waste water acid adjustment, part phenol forms Precipitation, through swash plate effect and waterpower backflow effect, deposits to reactor bottom, through peristaltic pump, is transported in acidifying solid-liquid separator.
3, beneficial effect:
(1) utilize compound neutralization reactor, add in nitration mixture and disperse blue 56 production process in strong basicity condensed mother liquor waste water, not only directly resource utilization reclaims the phenol of separating out in a large number and precipitates, the NO of its generation and NO
2gas can, by alkaline waste water absorption reaction in uphill process, both have been avoided NO and NO
2gas is emitted in air and works the mischief, and utilizes again acid NO
2in gas, with waste water alkalescence, save sour consumption;
(2) thionamic acid adding in nitration mixture is reduced into nitrogen discharge by waste water Nitrite ion, not only effectively remove nitrite ion, be convenient to water outlet and carry out subsequent disposal, and the sulfuric acid generating in reaction process can continue in and waste water alkalescence, save sour consumption;
(3) heat producing in acid-base neutralisation process is absorbed by the circulating condensing water in inside reactor prolong, and the resin column that is used for heating follow-up phase, to improve the desorption rate of resin, has been realized recovery and the utilization of heat, effectively saves the energy;
(4) adopt resin adsorption method absorption Phenol for Waste Water class material, can effectively reduce waste water COD and phenol content, the resin adsorbing after saturated adopts thermokalite desorption and regeneration, realizes resin and reuses, and recyclable phenol after desorption liquid acid adjustment, realizes resource utilization target.
Accompanying drawing explanation
Condensed mother liquor Wastewater Pretreatment and recycling system structure iron in a kind of disperse blue 56 production process of Fig. 1,1, sodium hydroxide solution storage tank, 2, thionamic acid storage tank, 3, vitriol oil storage tank, 4, compound neutralization reactor, 5, resin absorbing column, 6, acid-base neutralisation solid-liquid separator;
Fig. 2 resin absorbing column structural representation, 7, water-in, 7 ', desorption liquid injection port, 8, water outlet, 8 ', desorption liquid outlet, 16 ', water of condensation Link Port;
The compound neutralization reactor structural representation of Fig. 3,9, outside water-in, 10, vapor pipe, 11, inner inlet mouth, 12, mixed acid solution injection port, 13, throw out relief outlet, 14, acid solution refluxing opening, 15, stirring rake, 16, condensate return Guan，17, sloping plate deposition district, 18, gas collection reflection centrum, 19, outside water outlet, 20, pH meter probe;
Condensed mother liquor Wastewater Pretreatment and method of resource schema in a kind of disperse blue 56 production process of Fig. 4.
Embodiment
Further illustrate by the following examples the present invention.
Embodiment 1:
Strong basicity condensed mother liquor waste water COD in disperse blue 56 production process
crfor 54400mg/L, pH is greater than 14, and aldehydes matter concentration is 18900mg/L.
Wastewater treatment pilot test system as shown in Figure 1, comprise: sodium hydroxide solution storage tank 1, thionamic acid storage tank 2, vitriol oil storage tank 3, compound neutralization reactor 4, resin absorbing column 5, acid-base neutralisation solid-liquid separator 6, compound neutralization reactor water outlet is connected with a water-in of resin absorbing column, its mixed acid solution injection port is connected with vitriol oil storage tank, thionamic acid storage tank respectively, and its throw out relief outlet, acid solution refluxing opening are connected with acid-base neutralisation solid-liquid separator respectively; Two water-ins of resin absorbing column are connected with sodium hydroxide solution storage tank, compound neutralization reactor water outlet respectively, and one of them water outlet is connected with acid-base neutralisation solid-liquid separator.Resin absorbing column and compound neutralization reactor structure are as shown in accompanying drawing 2 and accompanying drawing 3, a kind of compound neutralization reactor, it is by outside water-in 9, vapor pipe 10, inner inlet mouth 11, mixed acid solution injection port 12, throw out relief outlet 13, acid solution refluxing opening 14, stirring rake 15, condensate return pipe 16, sloping plate deposition district 17, gas collection reflection centrum 18, outside water outlet 19, pH meter probe 20 forms, structural relation between each composition is that inside reactor is divided into two conversion zones with dividing plate, outside water-in lays respectively at reactor reaction Ι district with water outlet and reacts the top in П district, inner inlet mouth is positioned at the bottom of reactor reaction Ι district HeП district intersection, mixed acid solution injection port, throw out relief outlet, acid solution refluxing opening are positioned at bottom, reactor reaction П district, stirring rake and condensate return pipe are positioned at the middle and lower part in reactor reaction П district, sloping plate deposition district is positioned at the top of prolong, top, sloping plate deposition district is gas collection reflection centrum, vapor pipe opening part separates the gas collection reflection centrum position of plate for reacting Ι district and П, exhaust outlet is reaction bottom, Ι district, gas collection reflection centrum top is pH meter probe.Resin absorbing column structural representation, as Fig. 2, comprises water-in 7, desorption liquid injection port 7 ', water outlet 8, desorption liquid outlet 8 ', water of condensation Link Port 16 '.
The pre-treatment of the condensed mother liquor waste water in disperse blue 56 production process and resource utilization process as shown in Figure 4, the steps include:
1.1 by the strong basicity condensed mother liquor waste water in disperse blue 56 production process with flow velocity v
1=10L/min passes into compound neutralization reactor Ι district, sulfuric acid (mass concentration 95%, flow 0.2L/min) with thionamic acid solution (mass concentration 14.5%, flow 6.8L/min) mixed acid solution enters compound neutralization reactor by acid inlet tube, mechanical stirrer stir speed (S.S.) (120r/min), reaction is adjusted to water outlet (pH=4);
1.2 water outlets are with v
2the flow velocity of=10L/min enters and is filled with in 220L polystyrene-divinylbenzene superhigh cross-linking resin absorbing column, and the COD of the absorption water outlet of front 2200L is down to 424mg/L, and aldehydes matter concentration is down to 13.6mg/L.
1.3 use 80L NaOH(mass concentrations 8%) solution carries out desorption with the flow velocity of 2L/min to resin, 40 ℃ of desorption temperatures.
1.4 desorption liquids enter in acidifying solid-liquid separator, with sulfuric acid (95% mass concentration), adjust pH=6 to separate out precipitation, together with the precipitation in compound neutralization reactor in step 1.1, separate in the lump underpressure distillation (pressure :-0.075MPa, temperature: 60 ℃), be cooled to 25 ℃ of crystallisation by cooling.
After aforesaid method is processed, its Wastewater Pretreatment effect, as following table:
Embodiment 2:
Waste water quality is with embodiment 1, and Waste Water Treatment is similar to embodiment 1, and operation steps is as follows:
2.1 by the strong basicity condensed mother liquor waste water in disperse blue 56 production process with flow velocity v
1=20L/min passes into compound neutralization reactor Ι district; sulfuric acid (mass concentration 95%; flow 0.4L/min) with thionamic acid solution (mass concentration 14.5%; flow 14L/min) mixed acid solution enters compound neutralization reactor by acid inlet tube; mechanical stirrer stir speed (S.S.) (120r/min), reaction is adjusted to water outlet (pH=5);
2.2 water outlets are with v
2the flow velocity of=20L/min enters and is filled with in 220L polystyrene-divinylbenzene superhigh cross-linking resin absorbing column, and the COD of the absorption water outlet of front 1800L is down to 476mg/L, and aldehydes matter concentration is down to 18.5mg/L.
2.3 use 80L NaOH(mass concentrations 6%) solution carries out desorption with the flow velocity of 2L/min to resin, 50 ℃ of desorption temperatures.
2.4 desorption liquids enter in acidifying solid-liquid separator, with sulfuric acid (95% mass concentration), adjust pH=5 to separate out precipitation, together with the precipitation in compound neutralization reactor in step 1, separate in the lump underpressure distillation (pressure :-0.09MPa, temperature: 70 ℃), be cooled to 25 ℃ of crystallisation by cooling.
Wastewater Pretreatment effect is as follows:
Embodiment 3:
Waste water quality is with embodiment 1, and treatment system is similar with embodiment 1 to operation steps, but the resin of filling in process resin post changes macroporous polystyrene-divinylbenzene resin into.
3.1 by the strong basicity condensed mother liquor waste water in disperse blue 56 production process with flow velocity v
1=20L/min passes into compound neutralization reactor Ι district; sulfuric acid (mass concentration 95%; flow 0.4L/min) with thionamic acid solution (mass concentration 14.5%; flow 14L/min) mixed acid solution enters compound neutralization reactor by acid inlet tube; mechanical stirrer stir speed (S.S.) (120r/min), reaction is adjusted to water outlet (pH=6);
3.2 water outlets are with v
2the flow velocity of=20L/min enters and is filled with in 220L polystyrene-divinylbenzene superhigh cross-linking resin absorbing column, and the COD of the absorption water outlet of front 1800L is down to 476mg/L, and aldehydes matter concentration is down to 18.5mg/L.
3.3 use 80L NaOH(mass concentrations 4%) solution carries out desorption with the flow velocity of 2L/min to resin, 60 ℃ of desorption temperatures.
3.4 desorption liquids enter in acidifying solid-liquid separator, with sulfuric acid (95% mass concentration), adjust pH=4 to separate out precipitation, together with the precipitation in compound neutralization reactor in step 1, separate in the lump underpressure distillation (pressure :-0.1MPa, temperature: 80 ℃), be cooled to 25 ℃ of crystallisation by cooling.
Wastewater Pretreatment effect
Embodiment 4:
Waste water quality is with embodiment 1, and treatment system is similar with embodiment 1 to operation steps, but the resin of filling in resin column changes amido modified polystyrene-divinylbenzene superhigh cross-linking resin into, and other operational condition is constant, and its result of implementation is as follows.
Wastewater Pretreatment effect
Embodiment 5:
Step is with embodiment 1, but changes the concentration of sodium hydroxide solution in step 1.3 into 4%, and other operational condition is constant, and its result of implementation is as follows.
Wastewater Pretreatment effect
According to above-described embodiment, the present invention has following beneficial effect.
(1) can effectively remove the COD in the strong basicity condensed mother liquor waste water in disperse blue 56 production process, clearance is greater than 99%, water outlet COD<500mg/L;
(2) can effectively remove the nitrite ion in the strong basicity condensed mother liquor waste water in disperse blue 56 production process, clearance is greater than 99%, water outlet nitrite ion concentration <20mg/L;
(3) the strong basicity condensed mother liquor waste water alkalescence in can be effectively and in disperse blue 56 production process, water outlet pH=5-7;
(4) aldehydes matter in the strong basicity condensed mother liquor waste water in can efficient recovery disperse blue 56 production process, water outlet phenol concentration <20mg/L, the phenol rate of recovery is greater than 70%.
Claims (8)
1. a compound neutralization reactor, it is comprised of outside water-in (9), vapor pipe (10), inner inlet mouth (11), mixed acid solution injection port (12), throw out relief outlet (13), acid solution refluxing opening (14), stirring rake (15), condensate return pipe (16), sloping plate deposition district (17), gas collection reflection centrum (18), outside water outlet (19), pH meter probe (20); Compound neutralization reactor inside is divided into reaction Ι district, reaction two, П district conversion zone with dividing plate, and what outside water-in (9) and outside water outlet (19) laid respectively at reactor reacts Ι district and the top of reacting П district; Inner inlet mouth (11) is positioned at the dividing plate bottom in reactor reaction Ι district and П interval; Mixed acid solution injection port (12), throw out relief outlet (13), acid solution refluxing opening (14) are positioned at the bottom in reaction П district; Stirring rake (15) and condensate return pipe (16) are positioned at the middle and lower part in reaction П district; Sloping plate deposition district is positioned at the top of condensate return pipe; Top, sloping plate deposition district is gas collection reflection centrum; Gas collection reflection centrum top is pH meter probe.
2. compound neutralization reactor according to claim 1, is characterized in that, described vapor pipe, and its opening part is the gas collection reflection centrum position of two reaction zone dividing plates, exports the bottom into compound neutralization reactor reaction Ι district, inner inlet mouth (11) place.
3. pre-treatment and the recycling system of the condensed mother liquor waste water in disperse blue 56 production process, it is comprised of sodium hydroxide solution storage tank (1), thionamic acid storage tank (2), vitriol oil storage tank (3), compound neutralization reactor (4), resin absorbing column (5), acid-base neutralisation solid-liquid separator (6); The outside water outlet of compound neutralization reactor (4) is connected with resin absorbing column water-in, its mixed acid solution injection port be connected with vitriol oil storage tank (3), thionamic acid storage tank respectively (2), compound neutralization reactor (4) throw out relief outlet, acid solution refluxing opening are connected with acid-base neutralisation solid-liquid separator (6) respectively, the desorption liquid injection port of resin absorbing column (5) is connected with sodium hydroxide solution storage tank, and the desorption liquid outlet of resin absorbing column is connected with acid-base neutralisation solid-liquid separator (6).
4. pre-treatment and the method for resource of the condensed mother liquor waste water in disperse blue 56 production process, its step comprises:
In step 1 and waste water alkalescence, separate out phenol and remove nitrite anions: the condensed mother liquor waste water in disperse blue 56 production process and the mixed acid solution of sulfuric acid and thionamic acid pass into the compound neutralization reactor described in claim 1, neutralization reaction, is adjusted to water outlet pH value 4-6;
Step 2 absorption: the water outlet after step 1 is processed, by being filled with the resin absorbing column adsorption column of polymeric adsorbent, is attracted to the phenol in water on resin;
Step 3 resin desorption: the resin sodium hydroxide solution desorption after step 2 absorption is saturated;
Step 4 reclaims phenol: the desorption liquid of step 3 enters in acidifying solid-liquid separator, with sulfuric acid, adjust pH≤6 to separate out precipitation, together with the precipitation in compound neutralization reactor in step 1, separate in the lump, acid solution is back to compound neutralization reactor, and the precipitation of separating obtains crude product phenol through drying under reduced pressure.
5. according to method claimed in claim 4, it is characterized in that: in the reaction process of described step 1 add thionamic acid and equate with the molar weight of waste water Nitrite ion.
6. method according to claim 4, is characterized in that: the resin in step 2 is that skeleton is polymeric adsorbent or the amido modified polystyrene-divinylbenzene superhigh cross-linking resin of polystyrene-divinylbenzene.
7. method according to claim 4, is characterized in that: the desorbing agent in described step 3 is mass concentration 4～8%NaOH solution, and desorption temperature is 40～60 ℃.
8. method according to claim 4, drying under reduced pressure in described step 4, its pressure :-0.1～-0.075MPa, temperature: 60-80 ℃.
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