CN112479423B - Wastewater treatment method for producing amino-containing phenolic compounds - Google Patents
Wastewater treatment method for producing amino-containing phenolic compounds Download PDFInfo
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- 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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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C02F2101/38—Organic compounds containing nitrogen
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- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
Abstract
The invention relates to a wastewater treatment technology, in particular to a separation treatment method of wastewater containing aminophenol compounds. Adjusting the pH value of the wastewater containing aminophenol compounds, controlling tar generated by neutralizing the wastewater, and realizing the treatment of waste residues in the wastewater by utilizing solid-liquid separation. By the method, the solid content of the waste residue can be increased from 30% to more than 80%, the separation efficiency is increased by 6 times, and the COD of the waste water can be reduced by about 10%.
Description
Technical Field
The invention relates to a wastewater treatment technology, in particular to a separation treatment method of wastewater containing aminophenol compounds.
Background
The aminophenol compound is an important intermediate for preparing dyes and medicines, and has high economic value. In the production process of the intermediate, more wastewater with high organic matter concentration, stable chemical structure and strong acidity can be generated. The intermediate wastewater is generally subjected to physical and chemical treatment by coagulation, oxidation, adsorption, and the like. However, the aminophenol compound wastewater has a high acid content, generally about 6% -10%, and strong acid can affect the treatment effect of a flocculant, an oxidant and the like on the wastewater, so before the wastewater is treated, the wastewater must be neutralized, then neutralized waste residues and tar generated by neutralization are separated from the wastewater, but because the neutralized waste residues and the tar are mixed together, the separation time is long, the solid content of filter residues is low, the filter residues are subjected to secondary treatment, and a more effective and quicker separation means is not available for separating the neutralized waste residues from the wastewater.
Nitro-compound is a representative variety of aminophenol compounds, is an acid dye and a medical intermediate, and the production process mainly comprises naphthol nitrosation, sulfonation and acidification transposition to obtain a 1,2,4-acid product; 5363 diazotizing and acidifying the acid 1,2,4 to obtain diazoxynaphthalenesulfonic acid product; the diazoxynaphthalene sulfonic acid is nitrified to obtain a nitrate product, and the wastewater generated in the production process has the typical characteristics of aminophenol compound wastewater.
The commonly used nitrate wastewater neutralization methods at present comprise the following steps:
1. neutralization of wastewater using sodium hydroxide
The sodium hydroxide is used for neutralizing the nitrate wastewater, and the advantage is that no solid inorganic substance residue is left. However, the sodium hydroxide is high in price and only suitable for neutralizing small-batch wastewater, so that the cost for treating large-batch wastewater is high, and the enterprise burden is large.
2. Neutralizing wastewater with sodium carbonate
The sodium carbonate is used for neutralizing the nitrate wastewater, and the advantage is that no solid inorganic substance residue is left. But the price is higher, and only be fit for small batch waste water neutralization use, the big waste water treatment cost of wholesale is high, and the enterprise bears a big burden.
3. Neutralization of wastewater using calcium oxide
The calcium oxide is used for neutralizing the nitrate wastewater, and has the advantages of low calcium oxide cost and low solid content of waste residues, and the industrial calcium oxide contains 10 percent of inorganic salt impurities mainly comprising silicon dioxide, and the impurities which do not react with acid are mixed with organic tar generated during the neutralization of the wastewater, so that dry-wet separation is needed, the separation effect is poor, and the solid content of the waste residues is low.
4. Neutralization of wastewater using magnesium oxide
The magnesium oxide is used for neutralizing the nitrate wastewater, the magnesium oxide has the advantage of low cost, and the industrial magnesium oxide contains 10-15% of inorganic salt impurities mainly comprising silicon dioxide, the impurities which do not react with acid are mixed with organic tar generated during the neutralization of wastewater, dry-wet separation is needed, the separation effect is poor, and the solid content of waste residue is low.
The above-mentioned treatment process is poor to carry out wet-dry separation effect, inefficiency to waste water and neutralization waste residue, and then an effectual separation technique is urgently needed.
Disclosure of Invention
The invention aims to provide a separation treatment method for waste water containing aminophenol compounds, which solves the problems of poor effect and low efficiency of dry-wet separation of waste water neutralization waste residues when using alkali or alkaline oxides to neutralize the aminophenol compound waste water.
In order to realize the purpose, the invention adopts the technical scheme that:
a process for treating the waste water containing aminophenol compounds includes regulating the pH value of the waste water, neutralizing the tar generated by waste water, and solid-liquid separation.
Further, the pH value of the wastewater containing the aminophenol compound is regulated in two stages, the process of generating tar during wastewater neutralization is controlled, solid-liquid separation is carried out when no tar is generated, waste residues are firstly separated out, then the pH value is continuously regulated to generate tar in the wastewater, and the tar is removed through the solid-liquid separation, so that the treatment of the waste liquid is realized.
Still further, an alkali or an alkaline oxide is added to the wastewater containing the aminophenol compound, the pH of the wastewater is adjusted to be in the range of 0.9 to 3.0 (preferably, pH = 2), solid-liquid separation is performed by using a dry-wet separation method, then the wastewater is collected and a soluble alkaline substance is added to the wastewater, the pH of the wastewater is adjusted to be in the range of 3.1 to 8.0 (preferably, pH = 7), the wastewater is neutralized to generate tar, and the tar is separated from the wastewater by using a dry-wet separation method, so that waste residues in the wastewater are removed.
The alkali or alkaline oxide is magnesium oxide, calcium carbonate, magnesium carbonate, calcium hydroxide, magnesium hydroxide, calcium bicarbonate or magnesium bicarbonate; magnesium oxide is preferred.
The soluble alkaline substance is sodium hydroxide or sodium carbonate.
The dry-wet separation mode is filtration or sedimentation.
The invention has the advantages that:
according to the method, the characteristic that organic tar is generated along with the change of the acid content when the aminophenol compound wastewater is neutralized is utilized, the time point of the generation of the organic tar when the aminophenol compound wastewater is neutralized is controlled, most of acid in the wastewater is neutralized by using alkali or alkaline oxide in the time period when the tar is not generated, and then neutralized waste residue which does not react with the acid and is insoluble in water is separated by a dry-wet separation means, so that the purposes of separating the neutralized waste residue and improving the treatment efficiency are achieved.
1. The alkali and the alkaline oxide used in the method for neutralizing the wastewater are low in price and good in economical efficiency, and the burden of an enterprise can be reduced.
2. The invention can control the time point of generating tar by neutralizing the aminophenol compound wastewater, so that the wastewater can be further treated controllably.
3. The treatment method of the invention utilizes the generation process of tar during neutralization, solid-liquid separation is carried out in two stages, thereby avoiding the mixing of the neutralized waste residue and the tar generated by neutralization, and the neutralized waste residue and the tar can be separated from the wastewater independently without secondary treatment.
4. The invention can increase the solid content of the waste residue from 30% to more than 80%, and the treatment efficiency can be improved by 6 times, thereby greatly reducing the working hours, improving the working efficiency and reducing the labor cost.
5. The invention can only use the dry-wet separation mode to separate the tar, thus reducing the COD of the wastewater and the subsequent treatment cost of the wastewater.
Detailed Description
For a better understanding of the present invention, the following examples are included to further illustrate the present invention, and the present invention is not limited to the following examples.
The method aims at neutralizing aminophenol compound wastewater by using alkali or alkaline oxide, efficiently separates neutralized inorganic waste residue from wastewater by controlling the time point of organic tar generation during the neutralization of the aminophenol compound wastewater, greatly improves the neutralization treatment efficiency and reduces the treatment cost, in particular to wastewater generated in the production process of nitrate.
Example 1
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 19.2kg of magnesium oxide (with main content of 85%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82 percent; and then 32.9kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 9.5%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 2
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 34.6kg of magnesium oxide (with main content of 85%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81 percent; then 6.6kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 3
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 38kg of magnesium oxide (with main content of 85%), and starting stirring; when pH =2.9 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.3 percent; then 6.6kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.7%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 4
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 15.6kg of magnesium oxide (with main content of 85%), and starting stirring; when pH =1 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.1%; then 26.8kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 5
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 28.1kg of magnesium oxide (with main content of 85%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 83.1 percent; then 5.4kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.7%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 6
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 30.9kg of magnesium oxide (with main content of 85%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.9 percent; then 0.54kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 10.4%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 7
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 25.4kg of calcium oxide (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 82.7%; then 32.9kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 11.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 8
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 45.7kg of calcium oxide (with main content of 90%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.5 percent; then 6.6kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.8%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 9
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 50.3kg of calcium oxide (with main content of 90%), and starting stirring; when pH =2.9 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.6 percent; then 0.7kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.5%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 10
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 20.6kg of calcium oxide (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81.9 percent; and then adding 26.8kg of sodium hydroxide (with 99% of main content) into the separated wastewater, starting stirring, detecting the pH value of the wastewater by using an acidimeter, generating tar in the wastewater when the pH value is =7 +/-0.5, separating the tar from the wastewater by using a sedimentation mode, measuring that the COD (chemical oxygen demand) of the wastewater is reduced by 10.4%, and then directly carrying out subsequent treatment on the separated wastewater.
Example 11
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 37.1kg of calcium oxide (with main content of 90%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.3 percent; then 5.4kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 12
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 40.9kg of calcium oxide (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 83.3 percent; then 0.54kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.3%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 13
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 45.4kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81.1 percent; then 32.9kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 14
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 81.6kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =2 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 82.5%; then 6.6kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.8%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 15
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 89.8kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 82.7%; then 0.7kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.1%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 16
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 36.8kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.4 percent; then 26.8kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.7%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 17
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 66.3kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81.7 percent; and then 5.4kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 10.3%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 18
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 73kg of calcium carbonate (with main content of 90%), and starting stirring; when the pH =2.9 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 83.1 percent; then 0.54kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 9.8%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 19
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 31.5kg of calcium hydroxide (with main content of 96%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81.1 percent; and then 32.9kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 11.3%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 20
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 56.6kg of calcium hydroxide (with main content of 96%), and starting stirring; when the pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.5 percent; then 6.6kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.1%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 21
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 62.3kg of calcium hydroxide (with main content of 96%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 83.3 percent; then 0.7kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 22
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 25.6kg of calcium hydroxide (with main content of 96%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.2 percent; then 26.8kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.6%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 23
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 46kg of calcium hydroxide (with main content of 96%), and starting stirring; when pH =2 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.1%; then 5.4kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, tar is generated in the wastewater when the pH is =7 +/-0.5, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 10.7%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 24
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 50.7kg of calcium hydroxide (with main content of 96%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 81.9 percent; then 0.54kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 9.9%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 25
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 24.9kg of magnesium hydroxide (with main content of 95%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 83.1%; then 32.9kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, tar is generated in the wastewater when the pH is =7 +/-0.5, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 10.5%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 26
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 44.9kg of magnesium hydroxide (with main content of 95%), and starting stirring; when the pH of the wastewater is detected to be =2 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 82.3%; then 6.6kg of sodium hydroxide (with 99% of main content) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the COD of the wastewater is measured to be reduced by 10.3%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 27
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 8%) into a reaction kettle, adding 49.3kg of magnesium hydroxide (with main content of 95%), and starting stirring; when the pH of the wastewater is detected to be =2.9 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 83.3 percent; then 0.7kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.2%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 28
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 19.6kg of magnesium hydroxide (with main content of 95%), and starting stirring; when the pH of the wastewater is detected to be =1 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 80.5 percent; then 26.8kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.9%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 29
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 35.3kg of magnesium hydroxide (with main content of 95%), and starting stirring; when the pH of the wastewater is detected to be =2 +/-0.1 by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is measured to be 82.4%; then 5.4kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 10.4%, and then the separated wastewater can be directly subjected to subsequent treatment.
Example 30
Taking waste water containing aminophenol compounds generated in the process of producing nitrate as a raw material, adding 1000kg of nitrate waste water (with acid content of 6.5%) into a reaction kettle, adding 38.8kg of magnesium hydroxide (with main content of 95%), and starting stirring; when pH =2.9 +/-0.1 of the wastewater is detected by using an acidimeter, no tar is generated in the wastewater, only the waste residue is neutralized, the wastewater and the neutralized waste residue are separated by using a filtering mode, and the solid content of the neutralized waste residue is 82.8%; then 0.54kg of sodium hydroxide (with the main content of 99%) is added into the separated wastewater, stirring is started, an acidimeter is used for detecting the pH value of the wastewater, when the pH value is =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated in a sedimentation mode, the measured COD (chemical oxygen demand) of the wastewater is reduced by 9.1%, and then the separated wastewater can be directly subjected to subsequent treatment.
Comparative example 1
Taking amino phenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 38.4kg of magnesium oxide (with main content of 85%), and stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the tar and the neutralized waste residue are mixed together, the waste residue and the wastewater are separated by using a filtering mode, the particle size of the tar is small, the rigidity is poor, a filtering medium is easy to block, the filtering medium needs to be replaced or cleaned for many times, the filtering time is 6 times that of the embodiment, the solid content of the filter residue is lower than 30%, and the neutralized waste residue and the tar are mixed together in the filter residue, so that secondary treatment is needed, and the cost and the working hour are increased.
Comparative example 2
Taking aminophenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 66kg of magnesium hydroxide (with main content of 99%), and stirring; when the pH value of the wastewater is detected by using an acidimeter, tar is generated in the wastewater when the pH is =7 +/-0.5, the tar and the wastewater are separated by using a sedimentation mode, the COD (chemical oxygen demand) of the wastewater can be reduced by 9.7%, but the industrial sodium hydroxide is expensive and cannot be used for neutralizing large-batch wastewater.
Comparative example 3
Taking amino phenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 88.3kg of sodium carbonate (with main content of 98%), and stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the tar and the wastewater are separated by using a sedimentation mode, the COD (chemical oxygen demand) of the wastewater can be reduced by 10.5%, but the industrial sodium carbonate is expensive and cannot be used for neutralizing the large-batch wastewater.
Comparative example 4
Taking amino phenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 50.8kg of calcium oxide (with main content of 90%), and stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the waste residue and the wastewater are separated by using a filtering mode, the particle size of the tar is small, the rigidity is poor, a filtering medium is easy to block, the filtering medium needs to be replaced or cleaned for many times, the filtering time is 6 times that of the embodiment, the solid content of the filter residue is lower than 30%, and the neutralized waste residue in the filter residue is mixed with the tar, so that the secondary treatment is needed, and the cost and the working hour are increased.
Comparative example 5
Taking amino phenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 90.7kg of calcium carbonate (with main content of 90%), and stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the tar and the neutralized waste residue are mixed together, the waste residue and the wastewater are separated by using a filtering mode, the particle size of the tar is small, the rigidity is poor, a filtering medium is easy to block, the filtering medium needs to be replaced or cleaned for many times, the filtering time is 6 times that of the embodiment, the solid content of the filter residue is lower than 30%, and the neutralized waste residue and the tar are mixed together in the filter residue, so that secondary treatment is needed, and the cost and the working hour are increased.
Comparative example 6
Taking aminophenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 62.9kg of calcium hydroxide (with main content of 96%), and starting stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the tar and the neutralized waste residue are mixed together, the waste residue and the wastewater are separated by using a filtering mode, the particle size of the tar is small, the rigidity is poor, a filtering medium is easy to block, the filtering medium needs to be replaced or cleaned for many times, the filtering time is 6 times that of the embodiment, the solid content of the filter residue is lower than 30%, and the neutralized waste residue and the tar are mixed together in the filter residue, so that secondary treatment is needed, and the cost and the working hour are increased.
Comparative example 7
Taking aminophenol compound-containing wastewater generated in the nitrate production process as a raw material, adding 1000kg of nitrate wastewater (with acid content of 8%) into a reaction kettle, adding 52.6kg of magnesium hydroxide (with main content of 90%), and starting stirring; the pH value of the wastewater is detected by using an acidimeter, when the pH =7 +/-0.5, tar is generated in the wastewater, the tar and the neutralized waste residue are mixed together, the waste residue and the wastewater are separated by using a filtering mode, the particle size of the tar is small, the rigidity is poor, a filtering medium is easy to block, the filtering medium needs to be replaced or cleaned for many times, the filtering time is 6 times that of the embodiment, the solid content of the filter residue is lower than 30%, and the neutralized waste residue and the tar are mixed together in the filter residue, so that secondary treatment is needed, and the cost and the working hour are increased.
The embodiment shows that the novel process technology used by the invention can effectively separate the waste water containing the aminophenol compound from the neutralized waste residue, has high treatment efficiency and low cost, and is economical and feasible.
Claims (4)
1. A method for treating wastewater generated in the production of aminophenol-containing compounds is characterized in that:
adding alkali or alkaline oxide into wastewater containing aminophenol compounds, adjusting the pH value of the wastewater to be within the range of 0.9-3.0, performing solid-liquid separation by using a dry-wet separation mode, then collecting the wastewater, adding soluble alkaline substances into the wastewater, adjusting the pH value of the wastewater to be within the range of 3.1-8.0, neutralizing the wastewater to generate tar, and then separating the tar from the wastewater by using the dry-wet separation mode, thereby removing waste residues in the wastewater.
2. The process of claim 1 wherein: the alkali or alkaline oxide is magnesium oxide, calcium hydroxide or magnesium hydroxide.
3. The process of claim 1 wherein: the soluble alkaline substance is sodium hydroxide or sodium carbonate.
4. The process of claim 1 wherein: the dry-wet separation mode is filtration or sedimentation.
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