CN1887729A - Method of purifying O-phenylenediamine sodium sulfide reducing waste water - Google Patents

Method of purifying O-phenylenediamine sodium sulfide reducing waste water Download PDF

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CN1887729A
CN1887729A CN 200610041069 CN200610041069A CN1887729A CN 1887729 A CN1887729 A CN 1887729A CN 200610041069 CN200610041069 CN 200610041069 CN 200610041069 A CN200610041069 A CN 200610041069A CN 1887729 A CN1887729 A CN 1887729A
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mother liquor
vacuum
sodium sulfide
phenylenediamine
purifying
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CN 200610041069
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CN100497189C (en
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赵志军
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Abstract

The present invention relates to new method of purifying o-phenylenediamine sodium sulfide reducing waste water. Unlike available sodium sulfide reducing waste water treating process, which results in secondary pollution, the method of the present invention treats o-phenylenediamine sodium sulfide reducing waste water through vacuum evaporation, eliminating sodium chloride, vacuum concentrating and other steps while obtaining sodium sulfite mixture. The present invention eliminates pollution caused by o-phenylenediamine radically.

Description

Novel method for purifying and treating o-phenylenediamine sodium sulfide reduction wastewater
The technical field is as follows:
the invention relates to a purification treatment technology of chemical wastewater, in particular to a novel method for purifying and treating o-phenylenediamine sodium sulfide reduction wastewater.
Background art:
o-phenylenediamine is a well-sold chemical product in the market at home and abroad, and is obtained by most of production plants by adopting a process method of reducing sodium sulfide. Because a large amount of high-concentration sodium sulfide reduction wastewater is generated in the production process of o-phenylenediamine, if no proper method is adopted for purification treatment and the wastewater is directly discharged, serious pollution is caused to the living environment of people. At present, manufacturers try to recover useful components in waste water by using o-phenylenediamine sodium sulfide reduction waste water as a treatment method for reproducing sodium thiosulfate, so that pollution is reduced. However, practice proves that the treatment method does not achieve the expected effect, because sulfur is required to be added for oxidation reaction in the process of producing the sodium thiosulfate product by using the wastewater, the power consumption and the coal consumption are high, the required amount of fresh water is extremely large in order to meet the process conditions, and a large amount of harmful sulfur dioxide gas, waste residues and wastewater generated cause secondary severe pollution. Therefore, the pollution problem cannot be solved, and the expanded production of the o-phenylenediamine is restricted to a certain extent. Therefore, in recent years, the technical personnel in the industry continuously strives to research the subject for seeking a new method for purifying and treating the o-phenylenediamine sodium sulfide reduction wastewater.
The invention content is as follows:
the invention provides a new method for purifying and treating o-phenylenediamine sodium sulfide reduction wastewater, which aims to fundamentally treat the o-phenylenediamine production wastewater, perfects a set of clean process for resource production by using the wastewater and thoroughly solves the pollution problem caused by the production of the o-phenylenediamine.
The technical solution of the invention is as follows:
the invention utilizes the effective components in the o-phenylenediamine sodium sulfide reduction wastewater (hereinafter referred to as mother liquor water) to formulate a specific process according to the principle of chemical reaction, and adopts the following steps to complete the whole wastewater treatment process and obtain useful materials. The method comprises the following steps:
firstly, evaporating mother liquor water in vacuum;
(II) removing sodium chloride contained in the mother liquor water;
and (III) concentrating the desalted mother liquor water in vacuum to obtain a material-sodium sulfite mixture.
The invention has the following positive effects:
the o-phenylenediamine sodium sulfide reduction wastewater is purified, so that the problem of serious pollution caused by the production of o-phenylenediamine is fundamentally solved;
the resource production is realized, other chemical materials are not needed to be added, and sodium sulfite and a mixture thereof produced by using the o-phenylenediamine sodium sulfide reduction wastewater are indispensable raw materials for manufacturing paper pulp by a sulfite method in the paper making industry;
the whole process of the invention is a clean production process, no secondary pollution is generated, and the pollution treatment effect is obviously better than that of the method for producing the sodium thiosulfate by using the mother liquor;
and fourthly, the method has the advantages of low investment, low energy consumption, simplicity and practicality, and easy popularization and utilization in the industry.
Description of the drawings:
the attached figure is a process flow block diagram of the invention
The specific implementation mode is as follows:
the basic chemical composition (in weight percentage) of the waste water-mother liquor water obtained in the production of o-phenylenediamine adopted by the invention is as follows:
sodium sulfide (Na)2S)2.5%-405%
3.6 to 9 percent of sodium hydroxide (NaoH)
Sodium thiosulfate (Na)2S2O3)17.5%~20%
8% -10% of sodium chloride (Nacl)
0.1 to 0.4 percent of other organic matters
The chemical reaction principle on which the present invention is based is the equation:
the final product of the reaction is a mixture of comprehensive reducing substances mainly comprising sodium sulfite, and the mixture can be used as a chemical raw material for manufacturing paper pulp in the paper industry.
The method steps of the invention are further described below with reference to the accompanying drawings:
filtering the mother liquor. Removing floating materials and the like in the mother liquor water, pumping the mother liquor water into the evaporator from a storage tank or a storage tank by using a pump, and enabling the mother liquor water to account for 40-60% of the total volume of the evaporator and not to exceed 60% of the total volume;
and (II) carrying out vacuum evaporation. When the concentration of the mother liquor in the container reaches 50-55 Baume degrees, the evaporation is stopped; in the evaporation process, cooling water is used for cooling steam through a condenser, condensed water with coffee color is collected and adsorbed by activated carbon, the adsorbed clean water is recycled as cooling water, and the adsorbed activated carbon can be used as boiler fuel to be incinerated into carbon residue.
And (III) removing sodium chloride contained in the mother liquor water. When desalting, the temperature of the mother liquor water is kept between 60 ℃ and 90 ℃ (the temperature is not more than 90 ℃), the mother liquor water is pumped into a salt precipitation tank, the temperature is kept continuously, after standing and precipitating for 2 to 2.5 hours, the bottom of the salt precipitation tank is opened, molten salt is discharged to a centrifugal machine, and the industrial salt is obtained by drying. Then collecting the mother liquor at the middle upper part of the salt precipitation tank and the mother liquor thrown out by a centrifugal machine.
(IV) concentrating in vacuum. Pumping the collected mother liquor into a vacuum scraper type concentration tank for concentration, stopping concentration when the vacuum degree reaches 80-85Kpa and the temperature of materials in the tank reaches 135-145 ℃, and discharging mixed materials taking sodium sulfite as a main body in the tank while the mixed materials are hot.
And (V) carrying out physical treatment on the materials, stacking the sodium sulfite mixture to a place which is cool, clean, dark and waterproof, keeping the stacking height of the materials to be not more than 30cm, cooling for 22-28 hours until the materials become hard black brown solid, cutting the materials into blocks, crushing the materials into granules or powder by a crusher, weighing and packaging to obtain the finished product.
The invention utilizes o-phenylenediamine waste water to produce sodium sulfite mixture with the content ratio as follows:
the product meets the requirements of chemical raw materials used for making pulp by papermaking.
Examples are now given:
4 tons of mother liquor water are treated, filtered and evaporated in vacuum, so that the amount of the mother liquor entering the evaporator accounts for 50 percent of the total capacity of the evaporator, the concentration of the mother liquor reaches 52 Baume degrees, and the evaporation is stopped. Keeping the temperature of the mother liquor at 60 ℃, pumping the mother liquor to a salt precipitation tank, standing for precipitation for 2 hours, opening a low valve of the salt precipitation tank, discharging molten salt, and performing spin-drying by using a centrifugal machine to obtain 300 kg of industrial salt. In the process, 2 tons of water are used for cooling steam, 2.4 tons of steam condensate water are collected and adsorbed by 10 kilograms of activated carbon, and the activated carbon can be used as boiler fuel for incineration and has no pollution. Pumping the mother liquor evaporated to 52 Baume degree and desalted into a vacuum scraper type reduced pressure concentration tank for concentration, wherein the vacuum degree is 80Kpa, the temperature of the material reaches 135 ℃, stopping concentration, discharging the material to a shady, shady and shady place without light and water, stacking the material to a height of 25cm (to prevent spontaneous combustion), and cooling for 24 hours to obtain 1 ton of solid sodium sulfite mixture. Then carrying out crushing treatment and finished product packaging of different specifications according to requirements. The finished product is tested, and the weight percentage content is as follows: sodium sulfite (Na)2SO3) 47% sodium thiosulfate (Na)2S2O3) 10.7% of sodium sulfide (Na)2S)25.2%。
In conclusion, no pollutant is discharged in the whole process of producing sodium sulfite by using the o-phenylenediamine sodium sulfide reduction wastewater resource, and the expected purpose is achieved.

Claims (7)

1. A new method for purifying and treating o-phenylenediamine sodium sulfide reduction wastewater is characterized in that: the method uses the o-phenylenediamine sodium sulfide reduction wastewater as mother liquor water for purification treatment, and obtains a mixture of sodium sulfite, sodium thiosulfate and sodium sulfide, and the method mainly comprises the following steps: firstly, evaporating mother liquor water in vacuum; secondly, removing the mother liquor water sodium chloride; and (III) concentrating the mother liquor water in vacuum.
2. The new method for purifying the o-phenylenediamine sodium sulfide reduction wastewater according to claim 1, wherein the method comprises the following steps: the step of filtering the mother liquor can be further included before the step of evaporating the mother liquor in vacuum; the step of concentrating the mother liquor water in vacuum also comprises a step of processing a concentrated material.
3. The new method for purifying the o-phenylenediamine sodium sulfide reduction wastewater according to claim 2, wherein the method comprises the following steps: and the concentrated material is treated by the steps of discharging the material subjected to vacuum reduced pressure concentration from a tank while the material is hot, stacking the material at a cool, clean, light-proof and water-proof position, wherein the stacking height is not more than 30cm, and cooling the material until the material becomes a solid.
4. The new method for purifying the o-phenylenediamine sodium sulfide reduction wastewater according to claim 1, wherein the method comprises the following steps: in the step of evaporating the mother liquor in vacuum, the amount of the mother liquor entering the evaporator accounts for 40-60% of the total capacity of the evaporator, and the evaporation is stopped when the evaporation concentration reaches 50-55 Baume degrees.
5. The novel method for purifying o-phenylenediamine sodium sulfide reduction wastewater according to claim 1 or 4, wherein the method comprises the following steps: in the step of evaporating the mother liquor in vacuum, the steam is cooled by water, and after the steam condensate water is gathered, the active carbon is used for adsorption treatment.
6. The new method for purifying the o-phenylenediamine sodium sulfide reduction wastewater according to claim 1, wherein the method comprises the following steps: in the step of removing the mother liquor water sodium chloride, the temperature of the mother liquor water is kept between 60 ℃ and 90 ℃, the mother liquor water is statically settled for 2 to 2.5 hours, and the obtained molten salt is dried by a centrifugal machine to obtain the finished product of industrial salt.
7. The new method for purifying the o-phenylenediamine sodium sulfide reduction wastewater according to claim 1, wherein the method comprises the following steps: the step of vacuum concentration of the mother liquor is carried out in a vacuum scraper type concentration tank, when the vacuum degree reaches 80-85Kpa and the temperature of materials in the tank reaches 135-145 ℃, the concentration is stopped, and a sodium sulfite mixture is discharged from the tank while the solution is hot.
CNB2006100410694A 2006-07-20 2006-07-20 Method of purifying O-phenylenediamine sodium sulfide reducing waste water Expired - Fee Related CN100497189C (en)

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CN100497189C CN100497189C (en) 2009-06-10

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200336B (en) * 2007-12-18 2010-12-08 赵志军 Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater
CN106746123A (en) * 2016-12-30 2017-05-31 黎炜杰 A kind of process for treating industrial waste water and system containing organic solvent
CN107867776A (en) * 2017-11-08 2018-04-03 江苏易简环保科技有限公司 A kind of method and technique by agricultural chemicals waste water recycling

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101200336B (en) * 2007-12-18 2010-12-08 赵志军 Process for zero-discharge treatment of o-phenylenediamine sodium sulfide reduction wastewater
CN106746123A (en) * 2016-12-30 2017-05-31 黎炜杰 A kind of process for treating industrial waste water and system containing organic solvent
CN107867776A (en) * 2017-11-08 2018-04-03 江苏易简环保科技有限公司 A kind of method and technique by agricultural chemicals waste water recycling

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