CN102417249B - Method for treating nitrobenzene waste water - Google Patents
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- CN102417249B CN102417249B CN 201010294619 CN201010294619A CN102417249B CN 102417249 B CN102417249 B CN 102417249B CN 201010294619 CN201010294619 CN 201010294619 CN 201010294619 A CN201010294619 A CN 201010294619A CN 102417249 B CN102417249 B CN 102417249B
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Abstract
The invention relates to a method for treating nitrobenzene waste water. The method comprises steps of: step 1. according to a molar ratio, taking 50 parts of nitrobenzene waste water with a pH of 9-13 and adding 0.2-0.4 parts of sulfonating agent; step 2. adding 1-2 parts of ketone compound or acrylic acid compound into the nitrobenzene waste water for acetone sulfonation reaction; step 3. adding 2-4 parts of aldehyde compound or oxirane into nitrobenzene waste water for condensation polymerization; step 4. adding 450-950 parts of nitrobenzene waste water, continuing the condensation polymerization in step 3. for 0.5-1.0 h, thereby preparing a coal water slurry additive with an effective concentration of 0.5-1%. According to the method for treating nitrobenzene waste water of the invention, the coal water slurry additive is prepared in the waste water phase through solution polymerization, so as to avoid environmental pollution caused by discharge of nitrobenzene waste water and realize reuse of nitrobenzene waste water.
Description
Technical field
The present invention relates to the nitrobenzene waste water treatment process, is a kind of method for the treatment of of Nitrobenzene waste water specifically.
Background technology
Chemical industry is the traditional mainstay industry of China, and important industrial chemicals and the product of production are widely used in national defence, printing and dyeing, plastics, agricultural chemicals and medicine industry.Along with the fast development of national economy, the chemical industry of China has also entered high-speed development period.Equipment and state of the art obviously promote, and production technique and equipment are constantly updated and regenerated, and simultaneously, the chemical industry wastewater emission amount is also constantly soaring.Chemical industry develop the lasting deterioration that brings water surrounding rapidly.At present industrial area of concentration and northern part water-deficient area are with in Jiangsu and Zhejiang Provinces, Guangdong one, have generally improved the wastewater treatment emission standard, and the wastewater displacement of chemical enterprise is also strictly limited, and get water resources taxes, fee of sewage discharge and also begin significantly to promote.The raising of environmental requirement has made the energy-conservation expansion of some areas chemical enterprise be faced with serious threat.
On this basis, the economy that how to adopt the water treatment new technology constantly to promote recycling has become the focus that present most of chemical enterprise is paid close attention to.
The wastewater from chemical industry that chemical industry take the benzene chemical industry as representative produces is organism, dyestuff intermediate, auxiliary agent and the poisonous and hazardous compound of difficult degradation mostly.It is large to have the water yield, and the organic contamination substrate concentration is high, the characteristics such as kind is many, colourity is dark, alkalescence is large, complicated component, belongs to unmanageable trade effluent.Organic concentration height and difficult degradation in this class waste water at home and abroad there is no the treatment process of reasonable.
On the south to change company's nitrobenzene plant waste water be example, this waste water is by take acid benzene as raw material, and it is nitrated to adopt nitration mixture to be that nitrating agent carries out, and the nitrated acid crude product that obtains needs the alkali lye neutralization, and then washing and rectifying, separating-purifying obtains the oil of mirbane sterling.Collect at the waste water that the p-nitrophenyl crude product carries out producing in alkali lye neutralization, washing and the rectifying, behind the stripping, the waste water that effluxes from tower reactor is nitrobenzene waste water.This burst wastewater pH is 12, and colourity is up to more than 2000 times, COD
CrBe 500～5000.
The existing treatment process of this class waste water is mainly biochemistry and catalytic oxidation at present, has investment greatly, the shortcoming that cost is high, and be difficult to steady running and qualified discharge.
Coal water slurry is a kind of by about 60～70% pulverized coal particle, the coal-based liquid fuel that about 30～40% water and about 1～1.5% additive are prepared from through physical mixed.Have the same flowability of image-stone oil and stable, can adopt pumping, directly spray burning is easy to loading and unloading and storage, also can grow distance and carry and long-time preservation, and the fuel such as alternative oil, Sweet natural gas are directly used in Industrial Boiler, station boiler etc.Under the guarantee of the coal reserve of China's abundant, the coal water slurry as an alternative clear energy sources of the economy of oil, gas equal energy source has broad application prospects.
In the coal water slurry preparation, to add chemical additive, the Main Function of chemical additive is to change the surface properties of pulverized coal particle, pulverized coal particle can be disperseed in water, strengthen the electrostatic repulsion between pulverized coal particle, form spatial separation steric effect etc., do not form and reunite and precipitation, thereby make coal water slurry have good flowability and stable.Different according to effect, described chemical additive can be divided into dispersion agent, stablizer and auxiliary agent three classes.Wherein dispersion agent is most important additive, take tensio-active agent as main.
At present tensio-active agent commonly used has two kinds of anionic and non-ionic types during the preparation coal water slurry.Aniorfic surfactant belongs to low molecular weight electrolyte or macromole and accurate complex polyelectrolyte particle, comprise sulfonate, carboxylate salt and a small amount of phosphoric acid ester, what generally use is sulfonate, such as naphthalenesulfonate, sulfonated humic acid salt, sulfonated lignin and sulfonated petro-leum etc.Sulfonated lignin and sulfonated humic acid salt series are because of the low widespread use of its cost, but its coal subject range is narrow, and the pulping effect is bad.Nonionic surface active agent mainly contains polyoxyethylene series and polyoxy ethane series.Although the non-ionic type surface additive is effective, cost is high.
In recent years, prepare slurries additive agent with black liquid, or academic research and industrial applications that trade effluent prepares coal water slurry also have corresponding patent and bibliographical information, such as the modified lignin mahogany sulfonate dispersion agent of the coal water slurry and preparation method thereof (patent No.: 02135096.5, notification number: CN 1194802C), a kind of environment protection type coal water slurry and the method for making thereof (patent No.: 200810079340.2, notification number: CN 101440317A), utilize coal water slurry process to administer the method (patent No.: 01112295.1 of cotton pulp black liquor, notification number: CN 1313426A) etc., adopt such technical finesse waste water not only to reduce the cost of coal water slurry, and solved the impact of the exhaust emission environment of waste water.But also do not realize so far utilizing wastewater from chemical industry to prepare slurries additive agent.
Synthetic and the performance of documents 1(slurries additive agent sulphonated acetone formaldehyde polycondensates, Zhou Mingsong, Qiu Xueqing etc., fine chemistry industry, 2005, No.22(3): 185-188) reported the synthesis technique of slurries additive agent sulphonated acetone formaldehyde polycondensates in pure water, yet also be not implemented in now this base polymer of preparation in the wastewater from chemical industry.
Summary of the invention
For the defective that exists in the prior art, the object of the present invention is to provide a kind of method for the treatment of of Nitrobenzene waste water, by utilizing solution polymerization to prepare slurries additive agent at this useless aqueous phase, avoid the nitrobenzene waste water discharging to the environment produced pollution, realized the recycling of nitrobenzene waste water.
For reaching above purpose, the technical scheme that the present invention takes is:
A kind of method for the treatment of of Nitrobenzene waste water is characterized in that, may further comprise the steps:
Step 1, getting pH according to mol ratio is 50 parts of 9～13 nitrobenzene waste waters, in temperature is under 40～60 ℃ the condition, to add 0.2～0.4 part of sulphonating agent; 0.2～0.4 part of described sulphonating agent comprises the sulphonating agent that contains in the waste water;
Step 2 adds 1～2 part of ketone compounds or acrylic compounds in the nitrobenzene waste water and carries out the acetone sulfonation reaction, and the control temperature of reaction is 40～60 ℃, and the reaction times is 20～40min; 1～2 part of described ketone compounds comprises the ketone compounds that contains in the waste water;
Step 3 adds 2～4 parts in aldehyde compound or oxyethane in the nitrobenzene waste water and carries out polycondensation, and the control temperature of reaction is 75～90 ℃, and the reaction times is 1～2 hour; 2～4 parts in described aldehyde compound or oxyethane comprise aldehydes or the oxirane compound that contains in the waste water;
Step 4 adds 450～950 parts of nitrobenzene waste waters again, and the control temperature of reaction is 75～90 ℃, the polycondensation of continuation step 3 0.5～1.0 hour, make the slurries additive agent of effective concentration 0.5%～1%, described effective concentration needs the salt that contains in the deduction waste water by determination of solid content.
On the basis of technique scheme, further comprising the steps of:
Step 5, non-caking coal is obtained coal dust by ball mill or rod mill grinding, in the described coal dust median size less than the mass ratio of 75 μ m particles greater than 80%, the slurries additive agent that described coal dust and step 4 are obtained mixes by following mass percent, and stir defibrination with electric blender and obtain coal water slurry, coal dust: slurries additive agent=59～62%:41～38%.
On the basis of technique scheme, described sulphonating agent is one or more in following: S-WAT, Sodium Pyrosulfite and sodium bisulfite, to get above multiplely when making composite sulphonating agent when appointing, and proportioning is any.
On the basis of technique scheme, described ketone compounds is one or more in following: acetone, cyclohexanone analog compound, when to choose ketone compounds be multiple, proportioning was any.
On the basis of technique scheme, described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, when to choose aldehyde compound be multiple, proportioning was any.
The method for the treatment of of Nitrobenzene waste water of the present invention by utilizing solution polymerization to prepare slurries additive agent at this useless aqueous phase, has avoided the nitrobenzene waste water discharging to the environment produced pollution, realizes the recycling of nitrobenzene waste water.
Description of drawings
The present invention has following accompanying drawing:
Fig. 1 is embodiment 1 different molecular weight distribution curve,
Fig. 2 is embodiment 2 different molecular weight distribution curves,
Fig. 3 is embodiment 3 different molecular weight distribution curves,
Fig. 4 is the molecular weight distribution gel chromatography figure of slurries additive agent.
Embodiment
Below in conjunction with accompanying drawing the present invention is described in further detail.
On the south change the producing nitrobenzene of company waste water be example, contain large weight organic compounds in the nitrobenzene waste water of the present invention, its water quality characteristics is as follows:
| Wastewater source | Nitrobenzene |
| pH | |
| 10～13 | |
| COD(mg/L) | 500～5000 |
| Main organic composition | 2,4-dinitrophenol, 2, the 6-dinitrophenol |
For this type of nitrobenzene waste water, the present invention has provided a kind of method for the treatment of of Nitrobenzene waste water, may further comprise the steps:
Step 1, getting pH according to mol ratio is 50 parts of 9～13 nitrobenzene waste waters, in temperature is under 40～60 ℃ the condition, to add 0.2～0.4 part of sulphonating agent; 0.2～0.4 part of described sulphonating agent comprises the sulphonating agent that contains in the waste water;
Step 2 adds 1～2 part of ketone compounds or acrylic compounds in the nitrobenzene waste water and carries out the acetone sulfonation reaction, and the control temperature of reaction is 40～60 ℃, and the reaction times is 20～40min; 1～2 part of described ketone compounds comprises the ketone compounds that contains in the waste water;
Step 3 adds 2～4 parts in aldehyde compound or oxyethane in the nitrobenzene waste water and carries out polycondensation, and the control temperature of reaction is 75～90 ℃, and the reaction times is 1～2 hour; 2～4 parts in described aldehyde compound or oxyethane comprise aldehydes or the oxirane compound that contains in the waste water;
Step 4 adds 450～950 parts of nitrobenzene waste waters again, and the control temperature of reaction is 75～90 ℃, the polycondensation of continuation step 3 0.5～1.0 hour, make the slurries additive agent of effective concentration 0.5%～1%, described effective concentration needs the salt that contains in the deduction waste water by determination of solid content.
On the basis of technique scheme, further comprising the steps of:
Step 5, non-caking coal is obtained coal dust by ball mill or rod mill grinding, in the described coal dust median size less than the mass ratio of 75 μ m particles greater than 80%, the slurries additive agent that described coal dust and step 4 are obtained mixes by following mass percent, and stir defibrination with electric blender and obtain coal water slurry, coal dust: slurries additive agent=59～62%:41～38%.
On the basis of technique scheme, described sulphonating agent is one or more in following: S-WAT, Sodium Pyrosulfite and sodium bisulfite, to get above multiplely when making composite sulphonating agent when appointing, and proportioning is any.
On the basis of technique scheme, described ketone compounds is one or more in following: acetone, cyclohexanone analog compound, when to choose ketone compounds be multiple, proportioning was any.According to the letones of sulfonation and the characteristics of aldehyde radical reaction, the compound that contains similar group with acetone can both participate in reaction, as: acetone, cyclohexanone analog compound.
On the basis of technique scheme, described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, when to choose aldehyde compound be multiple, proportioning was any.The compound that contains similar group with formaldehyde can both participate in reaction, as: acetaldehyde, propionic aldehyde, oxalic dialdehyde, glutaraldehyde.
The present invention is directed to nitrobenzene waste water, prepare first slurries additive agent, again slurries additive agent and non-caking coal slurrying are obtained coal water slurry, optimized proportioning raw materials and reaction conditions, and utilize the active principle in the nitrobenzene waste water to participate in reaction, improve reaction efficiency.
The invention has the beneficial effects as follows:
The method for the treatment of of Nitrobenzene waste water of the present invention, utilize this waste water as solvent, utilize therein ketone and aldehydes to react to prepare slurries additive agent, efficiently solve on the one hand the discharging of this type of wastewater from chemical industry and administer a difficult problem, reduced the pollution of organic waste water to environment.Also reduce on the other hand the cost of coal water slurry, realized the purpose that turns waste into wealth, and reduced investment and the working cost of processing waste water, had obvious economic and social benefit.
By this invention formulation additives and non-caking coal are carried out with slurry, the additive that evidence should series has good dispersion and falls glutinous usefulness, and the slurry stability that makes is good.Because non-caking coal belongs to the coal of difficult slurrying, therefore measurable this additive is fit to the coal slurrying of different rank.
Compare with the report of documents 1, the present invention utilizes nitrobenzene waste water as solvent, adjusted different components (S-WAT in the polymerization process, formaldehyde, acetone) proportioning, and sulfonation temperature and temperature of reaction be optimized, and utilize that the reactive behavior of organic constituent makes it participate in polyreaction in the waste water, play the effect of utilization of waste material.
Preparation method's improvement difference is in the present invention and the documents 1:
1) the described waste water of the present invention's application is alkalescence, OH wherein
-Ion can be as initiator and the catalyzer of this polyreaction, and what contain has preferably stabilization take NaCl as main mineral compound, and the additive that documents 1 adopts clear water to make needs a certain amount of inorganic salt of composite adding as stablizer in actual production coal water slurry process again.Therefore, the present invention utilizes the OH in the waste water
-Ion and NaCl have improved on the one hand reaction efficiency the reaction times are shortened, and have saved on the other hand the step of composite inorganic salt stablizer in the preparation slurries additive agent process, and have saved cost;
2) proportioning of the sulphonating agent in the documents 1, acetone and formaldehyde and reaction conditions are improved and optimize, great changes have taken place for the optimum amount of various reaction reagents, wherein the amount of sulphonating agent obviously reduces, secondly in invention step 4, pass through to improve temperature, useful component and group in the waste water can be reacted by attend fully;
3) the described waste water used of the present invention contains higher concentration isoreactivity material and can participate in this polyreaction as reaction raw materials, and the adjustment that the molecular weight distribution of the composite slurries additive agent that obtains of reaction is can be with the variation of reaction mass consumption, reaction times and temperature of reaction regular is to adapt to the needs of Coal rank and pulping process.
It below is specific embodiment.
Embodiment 1
Get the 100mL nitrobenzene waste water, to wherein adding respectively the 4-9g S-WAT, dissolving post-heating to 40 ℃, add 10mL acetone, be warming up to 80 ℃ behind the reaction 30min, add 20mL formaldehyde solution, continue reaction 1h after the time, keep temperature to add 950 parts of nitrobenzene waste waters, the slurries additive agent of the effective concentration 0.5% that reaction made in 1 hour; Naturally cool to room temperature, its different molecular weight distribution curve as shown in Figure 1, molecular weight of product significantly reduces with the increase of sulphonating agent consumption.Wherein S-WAT is that the appearance of 4g descends owing to under-sulfonate causes the product wetting ability, forms faint yellow insolubles.
Non-caking coal is passed through ball mill grinding, obtain median size less than the mass percent of the particle of 75 μ m greater than 80% coal dust, the slurries additive agent that 5g S-WAT sulfonation reaction is obtained and non-caking coal coal dust according to mass ratio 38:62 preparation mixing after, stir with electric blender and to obtain coal water slurry in 10 minutes.When the additive capacity of this coal water slurry was 1.0%, slurrying concentration was 61%, and the slurrying of this coal water slurry is better mobile, placed 10 days, a small amount of bleed, soft precipitation.
Embodiment 2
Get the 100mL nitrobenzene waste water, to wherein adding respectively the 5g S-WAT, dissolving post-heating to 40 ℃, add 6-14mL acetone, be warming up to 80 ℃ behind the reaction 30min, add 20mL formaldehyde solution, continue reaction 1h after the time, keep temperature to add 950 parts of nitrobenzene waste waters, the slurries additive agent of the effective concentration 0.5% that reaction made in 1 hour; Naturally cool to room temperature, its different molecular weight distribution curve as shown in Figure 2, along with the increase of acetone consumption, molecular weight of product increases first, after reduce.Acetone consumption hour may be to cause molecular weight because sulfonation excessively causes, and initial reaction rate be lower; And when the acetone large usage quantity, speed of reaction is too fast, and large keto-aldehyde is than the reduction that causes easily the polymerization degree, so that molecular weight reduces.
Non-caking coal is passed through ball mill grinding, obtain median size less than the mass percent of the particle of 75 μ m greater than 80% coal dust, the slurries additive agent that 10ml acetone reaction is obtained and non-caking coal coal dust according to mass ratio 38:62 preparation mixing after, stir with electric blender and to obtain coal water slurry in 10 minutes.When the additive capacity of this coal water slurry was 1.0%, slurrying concentration was 61%, and the slurrying of this coal water slurry is better mobile, placed 10 days, a small amount of bleed, soft precipitation.
Embodiment 3
Get the 100mL nitrobenzene waste water, to wherein adding respectively the 5g S-WAT, dissolving post-heating to 40 ℃, add 10mL acetone, be warming up to 80 ℃ behind the reaction 30min, add 12-24mL formaldehyde solution, continue reaction 1h after the time, keep temperature to add 950 parts of nitrobenzene waste waters, the slurries additive agent of the effective concentration 0.5% that reaction made in 1 hour; Naturally cool to room temperature, its different molecular weight distribution curve as shown in Figure 3, along with the increase of formaldehyde consumption, molecular weight of product is distributed with considerable influence.
Non-caking coal is passed through ball mill grinding, obtain median size less than the mass percent of the particle of 75 μ m greater than 80% coal dust, the slurries additive agent that the 20ml formaldehyde reaction is obtained and non-caking coal coal dust according to mass ratio 38:62 preparation mixing after, stir with electric blender and to obtain coal water slurry in 10 minutes.When the additive capacity of this coal water slurry was 1.0%, slurrying concentration was 61%, and the slurrying of this coal water slurry is better mobile, placed 10 days, a small amount of bleed, soft precipitation.
Embodiment 4
Get the 100mL nitrobenzene waste water, to wherein adding the 5g S-WAT, adopt after the dissolving and be heated to 60 ℃ of reaction conditionss, add 10mL acetone, be warming up to 80 ℃ behind the reaction 30min, add 20mL formaldehyde solution, continue reaction 1h after the time, keep temperature to add 950 parts of nitrobenzene waste waters, the slurries additive agent of the effective concentration 0.5% that reaction made in 1 hour; Naturally cool to room temperature.Contents of Main Components in the solution is measured, in the waste water 2,4-dinitrophenol and 2, the content of 6-dinitrophenol is respectively 416,256mg/L, carries out polymerization and measure 2 later on again in waste water, 4-dinitrophenol content＜10mg/L, the content of 2,6-dinitrophenol is content＜20mg/L respectively, illustrates that most of dinitrophenol has all participated in reaction in reaction process.The molecular weight distribution of the slurries additive agent that 60 ℃ of sulfonation reactions make among the embodiment 4 as shown in Figure 4.Both most range of molecular weight distributions are 2000～50000.
Non-caking coal is passed through ball mill grinding, obtain median size less than the mass percent of the particle of 75 μ m greater than 80% coal dust, the slurries additive agent that 60 ℃ of sulfonation reactions are obtained and non-caking coal coal dust according to mass ratio 38:62 preparation mixing after, stir with electric blender and to obtain coal water slurry in 10 minutes.When the additive capacity of this coal water slurry was 1.0%, slurrying concentration was 62%, and the apparent viscosity of coal water slurry is 548mPas.The slurrying of this coal water slurry is better mobile, places 10 days, a small amount of bleed, soft precipitation.
Claims (5)
1. the method for a treatment of Nitrobenzene waste water is characterized in that, may further comprise the steps:
Step 1, getting pH according to mol ratio is 50 parts of 9～13 nitrobenzene waste waters, in temperature is under 40～60 ℃ the condition, to add 0.2～0.4 part of sulphonating agent; 0.2～0.4 part of described sulphonating agent comprises the sulphonating agent that contains in the waste water;
Step 2 adds 1～2 part of ketone compounds or acrylic compounds in the nitrobenzene waste water and carries out the acetone sulfonation reaction, and the control temperature of reaction is 40～60 ℃, and the reaction times is 20～40min; 1～2 part of described ketone compounds comprises the ketone compounds that contains in the waste water;
Step 3 adds 2～4 parts in aldehyde compound or oxyethane in the nitrobenzene waste water and carries out polycondensation, and the control temperature of reaction is 75～90 ℃, and the reaction times is 1～2 hour; 2～4 parts in described aldehyde compound or oxyethane comprise aldehydes or the oxirane compound that contains in the waste water;
Step 4 adds 450～950 parts of nitrobenzene waste waters again, and the control temperature of reaction is 75～90 ℃, the polycondensation of continuation step 3 0.5～1.0 hour, make the slurries additive agent of effective concentration 0.5%～1%, described effective concentration needs the salt that contains in the deduction waste water by determination of solid content.
2. the method for the treatment of of Nitrobenzene waste water as claimed in claim 1 is characterized in that, and is further comprising the steps of:
Step 5, non-caking coal is obtained coal dust by ball mill or rod mill grinding, in the described coal dust median size less than the mass ratio of 75 μ m particles greater than 80%, the slurries additive agent that described coal dust and step 4 are obtained mixes by following mass percent, and stir defibrination with electric blender and obtain coal water slurry, coal dust: slurries additive agent=59～62%:41～38%.
3. the method for the treatment of of Nitrobenzene waste water as claimed in claim 1 or 2, it is characterized in that: described sulphonating agent is one or more in following: S-WAT, Sodium Pyrosulfite and sodium bisulfite, get above multiplely when making composite sulphonating agent when appointing, proportioning is any.
4. the method for the treatment of of Nitrobenzene waste water as claimed in claim 1 or 2 is characterized in that: described ketone compounds is one or more in following: acetone, cyclohexanone analog compound, when to choose ketone compounds be multiple, proportioning was any.
5. the method for the treatment of of Nitrobenzene waste water as claimed in claim 1 or 2 is characterized in that: described aldehyde compound is one or more in following: formaldehyde, acetaldehyde, propionic aldehyde, oxalic dialdehyde and glutaraldehyde, when to choose aldehyde compound be multiple, proportioning was any.
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