CN113292416A - Production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid - Google Patents
Production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid Download PDFInfo
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- CN113292416A CN113292416A CN202110624988.9A CN202110624988A CN113292416A CN 113292416 A CN113292416 A CN 113292416A CN 202110624988 A CN202110624988 A CN 202110624988A CN 113292416 A CN113292416 A CN 113292416A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention discloses a production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid. After the dihydroxy naphthalene waste liquid is pretreated by heating, flocculation, decoloration, filtration, Fenton oxidation and iron removal, the dihydroxy naphthalene waste liquid is reacted with industrial acetic acid and stone powder and filtered, and the product is mixed and reacted, and after secondary filtration, system pH adjustment, evaporation and concentration, carbon source liquid sodium acetate for sewage treatment is obtained. The method has the advantages of simple process, easy operation, low equipment investment, energy conservation and environmental protection, the obtained product meets the requirement of the carbon source liquid sodium acetate group standard (T/CSTE 0008-2020) for sewage treatment, the safety problem that the current carbon source of the sewage treatment plant uses methanol and is flammable and explosive is effectively solved, and the production cost is greatly reduced by changing waste into valuable.
Description
Technical Field
The invention relates to the field of wastewater treatment, in particular to a production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid.
Background
Dihydroxynaphthalene products such as 1, 6-dihydroxynaphthalene and 2, 7-dihydroxynaphthalene are widely used as naphthalene-series fine chemicals in the fields of high-end dyes, pharmaceutical intermediates, organic semiconductors, electronic materials, fibers, analytical reagents and the like. At present, the corresponding sodium naphthalene disulfonate is mainly used for producing the dihydroxynaphthalene product industrially by an alkali fusion acidification process, namely, the sodium naphthalene disulfonate reacts with flake caustic soda at high temperature to generate dihydroxynaphthalene sodium salt, then sulfuric acid acidification is carried out, filtration is carried out to obtain a crude dihydroxynaphthalene product, and then the crude product is refined and dried to obtain the high-purity dihydroxynaphthalene product. During the process of producing the crude dihydroxynaphthalene product by acidifying dihydroxynaphthalene sodium salt with sulfuric acid, a certain amount of waste liquid is generated, and main pollutants are naphthalene disulfonic acid, dihydroxynaphthalene, sulfuric acid, sodium sulfate and the like. The biochemical method is a method for converting organic pollutants in a dissolved state and a colloidal state in the wastewater into harmless substances by utilizing the metabolism of microorganisms so as to realize purification, has the advantages of economy, practicability, no secondary pollution and the like, and is widely applied to the treatment of industrial wastewater. However, the dihydroxynaphthalene waste liquid has high salt content, and organic matters have toxic action on microorganisms, so the dihydroxynaphthalene waste liquid is not beneficial to biochemical treatment. If the treatment can be carried out to realize the conversion of sodium sulfate in the sludge to prepare sodium acetate which is used as an external carbon source for sewage treatment and used for domesticating the denitrification sludge, the treatment can achieve two purposes, thus meeting the requirement of environmental protection and changing waste into valuable.
Disclosure of Invention
The invention aims to provide a production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid, which aims to solve the technical problems.
In order to achieve the purpose, the invention adopts the following technical scheme: a production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid comprises the following steps:
step 1, heating the dihydroxy naphthalene waste liquid to 25-60 ℃, adding activated carbon, decoloring and filtering, slowly adding a flocculating agent into the filtrate while stirring, continuously stirring in the adding process, standing to generate white precipitate, and filtering to obtain filtrate after the precipitate is completely precipitated;
step 2, filtering to obtain filtrate, heating to 25-60 ℃, stirring and adjusting the pH to 1-5;
step 3, adding ferrous sulfate for dissolution in Fenton oxidation, adding hydrogen peroxide every half an hour, and keeping the temperature of 25-60 ℃ and stirring for 1-4 hours after the hydrogen peroxide is added;
step 4, sampling and detecting a liquid phase after heat preservation is finished, adjusting the pH value to 7-10 by using calcium oxide or calcium hydroxide after organic impurities are completely oxidized, heating to 40-70 ℃, filtering to remove iron, adjusting the pH value of filtrate to 2-6 by using dilute sulfuric acid, decoloring and filtering by using activated carbon to obtain a pretreated solution A, and determining and calculating the content of sodium sulfate in the solution A;
step 5, adding metered industrial acetic acid into a reactor, adding water, stirring, slowly adding stoichiometric stone powder (calcium carbonate powder) at 25-60 ℃, stirring for 1-6 hours after adding, and filtering to obtain a filtrate B;
step 6, slowly adding the filtrate B into the treated solution A while stirring, continuously stirring for 1-4 hours after the addition is finished, detecting, and stopping stirring after the sodium sulfate completely reacts;
and 7, adjusting the pH of the system to 7.5-9 by using sodium carbonate or acetic acid, filtering to obtain gypsum (calcium sulfate dihydrate) and a sodium acetate solution, and heating and concentrating the filtrate to obtain a colorless transparent liquid with no pungent smell and sodium acetate content of more than or equal to 25%.
As a further scheme of the invention, the heating temperature of the dihydroxy naphthalene waste liquid in the step 1 is 45-50 ℃.
As a further scheme of the invention, in the step 1, the adding amount of the activated carbon is 1/240-1/60 of the quality of the dihydroxy waste liquid, and the adding amount of the flocculating agent is 1/120-1/35 of the quality of the dihydroxy waste liquid.
As a further scheme of the invention, the adding amount of the activated carbon in the step 1 is 1/80-1/60 of the quality of the dihydroxy waste liquid; the addition amount of the flocculating agent is 1/60-1/40 of the quality of the dihydroxy waste liquid.
In a further embodiment of the present invention, the flocculant is one or two of Polyacrylamide (PAM), polyaluminum chloride (PAC), polyaluminum sulfate (PAS), polyferric chloride (PFC), polyferric sulfate (PFS), and the like for water treatment.
As a further scheme of the invention, the amount of the ferrous sulfate catalyst added in the Fenton oxidation process is 1/600-1/200 of the mass of the dihydroxy waste liquid, and the amount of the hydrogen peroxide water added in three times every half hour is 1/600-1/150 of the mass of the dihydroxy waste liquid.
As a further scheme of the invention, the amount of the ferrous sulfate catalyst added in the Fenton oxidation process is 1/300-1/240 of the mass of the dihydroxy waste liquid, and the amount of the hydrogen peroxide water added in three times every half hour is 1/400-1/240 of the mass of the dihydroxy waste liquid.
As a further scheme of the invention, after the hydrogen peroxide is added in the step 3, the mixture is stirred and fully oxidized for 2 to 3 hours at the temperature of between 45 and 50 ℃.
As a further scheme of the invention, the reaction temperature of the industrial acetic acid and the stone powder in the step 5 is 25-40 ℃, and the filtrate B is obtained by stirring for 3-4 hours and filtering after the addition.
The invention has the beneficial effects that: (1) the production method and the process for preparing the sodium acetate by using the dihydroxy naphthalene waste liquid provided by the invention realize the purposes of circular and clean production, fundamentally reduce the environmental pollution of the dihydroxy naphthalene waste liquid and realize zero discharge of the liquid.
(2) The method and the process not only effectively solve the safety problem that the current carbon source of the sewage treatment plant uses methanol and is inflammable and explosive, but also realize the recycling of valuable resources to the maximum extent by changing waste into valuable, thereby greatly reducing the production cost.
(3) The method has the advantages of simple process, easy operation, low equipment investment, energy conservation and environmental protection, and is suitable for industrial production.
The sodium acetate obtained by the treatment and transformation of the method completely meets the requirements of carbon source liquid sodium acetate group standard (T/CSTE 0008-2020) for sewage treatment.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Heating 1200mL of crude dihydroxynaphthalene to 50 ℃, adding 8 g of activated carbon, decoloring and filtering, slowly adding 15 g of flocculant into the filtrate while stirring, continuously stirring in the adding process, standing for 3 hours to generate white precipitate, and filtering to obtain the filtrate after the precipitate is completely precipitated.
The filtrate was heated to 50 ℃ and stirred to adjust the pH to 3. 4 g of ferrous sulfate is added, 6mL of hydrogen peroxide is added every half an hour after dissolution, and 18mL of hydrogen peroxide is added in total. After the hydrogen peroxide is added, stirring for 3 hours at 50 ℃. And (3) sampling liquid phase detection after heat preservation is finished, adjusting the pH value to 8 by using calcium oxide or calcium hydroxide after organic impurities are completely oxidized, heating to 50 ℃, filtering to remove iron, adjusting the pH value to 3 by using dilute sulfuric acid, decoloring by using activated carbon, filtering to obtain a treated solution A, and measuring and calculating the content of sodium sulfate in the treated solution A. Adding metered industrial acetic acid into a reactor, adding water, stirring, slowly adding stoichiometric mountain flour (calcium carbonate powder) at 50 ℃, stirring for 3 hours after adding, and filtering to obtain filtrate B. And slowly adding the filtrate B into the treated solution A while stirring, continuously stirring for 3 hours after the addition is finished, detecting, and stopping stirring after the sodium sulfate completely reacts. Adjusting pH to 8.5 with sodium carbonate or acetic acid, filtering to obtain Gypsum Fibrosum (calcium sulfate dihydrate) and sodium acetate solution, heating and concentrating the filtrate to obtain colorless transparent liquid with no pungent odor and sodium acetate content of more than 25%.
And (3) detecting the obtained liquid, and loading the liquid into a barrel for later use, wherein the result of the detection reaches the requirement of the carbon source liquid sodium acetate group standard (T/CSTE 0008-2020) for sewage treatment. The product measurement results are shown in table 1.
TABLE 1 Properties and main indexes of sodium acetate solution for sewage treatment obtained by the present invention
Example 2
1300mL of the crude dihydroxynaphthalene product is heated to 50 ℃, 10 g of activated carbon is added, decolorization and filtration are carried out, 18 g of flocculating agent is slowly added into the filtrate while stirring, the stirring is continuously carried out during the addition, then the mixture is kept stand for 2 hours, white precipitate appears, and the filtrate is obtained after the precipitation is completed and filtration.
The filtrate was heated to 40 ℃ and stirred to adjust the pH to 4. Adding 4 g of ferrous sulfate, adding 5mL of hydrogen peroxide every half an hour after dissolving, and adding 15mL of hydrogen peroxide in total. After the hydrogen peroxide is added, stirring for 2 hours at 40 ℃. And (3) sampling liquid phase detection after heat preservation is finished, adjusting the pH value to 7.5 by using calcium oxide or calcium hydroxide after organic impurities are completely oxidized, heating to 40 ℃, filtering to remove iron, adjusting the pH value of the filtrate to 3 by using dilute sulfuric acid, decoloring by using activated carbon, filtering to obtain a treated solution A, and measuring and calculating the content of sodium sulfate in the treated solution A. Adding metered industrial acetic acid into a reactor, adding water, stirring, slowly adding stoichiometric mountain flour (calcium carbonate powder) at 50 ℃, stirring for 3 hours after adding, and filtering to obtain filtrate B. And slowly adding the filtrate B into the treated solution A while stirring, continuously stirring for 2 hours after the addition is finished, detecting, and stopping stirring after the sodium sulfate completely reacts. Adjusting pH to 8.0 with sodium carbonate or acetic acid, filtering to obtain Gypsum Fibrosum (calcium sulfate dihydrate) and sodium acetate solution, heating and concentrating the filtrate to obtain colorless transparent liquid with no pungent odor and sodium acetate content of more than 25%.
And (3) detecting the obtained liquid, and loading the liquid into a barrel for later use, wherein the result of the detection reaches the requirement of the carbon source liquid sodium acetate group standard (T/CSTE 0008-2020) for sewage treatment. The product measurement results are shown in table 2.
Table 2 Properties and Main indexes of sodium acetate solution for sewage treatment obtained by the invention
Example 3
2000mL of crude dihydroxynaphthalene product is heated to 40 ℃, 15 g of activated carbon is added, decolorization and filtration are carried out, 20 g of flocculating agent is slowly added into the filtrate while stirring, the stirring is continuously carried out during the addition, then the mixture is kept stand for 4 hours, white precipitate appears, and the filtrate is obtained after the precipitation is completed and filtration.
The filtrate was warmed to 35 ℃ and stirred to adjust the pH to 4.5. Adding 5 g of ferrous sulfate, adding 8mL of hydrogen peroxide every half an hour after dissolving, and adding 24mL of hydrogen peroxide in total. After the hydrogen peroxide is added, stirring for 3 hours at 50 ℃. And (3) sampling liquid phase detection after heat preservation is finished, adjusting the pH value to 8.5 by using calcium oxide or calcium hydroxide after organic impurities are completely oxidized, heating to 45 ℃, filtering to remove iron, adjusting the pH value of the filtrate to 2 by using dilute sulfuric acid, decoloring and filtering by using activated carbon to obtain a treated solution A, and measuring and calculating the content of sodium sulfate in the treated solution A. Adding metered industrial acetic acid into a reactor, adding water, stirring, slowly adding stoichiometric mountain flour (calcium carbonate powder) at 45 ℃, stirring for 4 hours after adding, and filtering to obtain filtrate B. And slowly adding the filtrate B into the treated solution A while stirring, continuously stirring for 3 hours after the addition is finished, detecting, and stopping stirring after the sodium sulfate completely reacts. Adjusting pH to 8.0 with sodium carbonate or acetic acid, filtering to obtain Gypsum Fibrosum (calcium sulfate dihydrate) and sodium acetate solution, heating and concentrating the filtrate to obtain colorless transparent liquid with no pungent odor and sodium acetate content of more than 25%. And (3) detecting the obtained liquid, and loading the liquid into a barrel for later use, wherein the result of the detection reaches the requirement of the carbon source liquid sodium acetate group standard (T/CSTE 0008-2020) for sewage treatment. The product measurement results are shown in table 3.
TABLE 3 Properties and main indexes of sodium acetate solution for sewage treatment obtained by the present invention
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (9)
1. A production method for preparing sodium acetate by utilizing dihydroxy naphthalene waste liquid is characterized by comprising the following steps:
step 1, heating the dihydroxy naphthalene waste liquid to 25-60 ℃, adding activated carbon, decoloring and filtering, slowly adding a flocculating agent into the filtrate while stirring, continuously stirring in the adding process, standing to generate white precipitate, and filtering to obtain filtrate after the precipitate is completely precipitated;
step 2, filtering to obtain filtrate, heating to 25-60 ℃, stirring and adjusting the pH to 1-5;
step 3, adding ferrous sulfate for dissolution in Fenton oxidation, adding hydrogen peroxide every half an hour, and keeping the temperature of 25-60 ℃ and stirring for 1-4 hours after the hydrogen peroxide is added;
step 4, sampling and detecting a liquid phase after heat preservation is finished, adjusting the pH value to 7-10 by using calcium oxide or calcium hydroxide after organic impurities are completely oxidized, heating to 40-70 ℃, filtering to remove iron, adjusting the pH value of filtrate to 2-6 by using dilute sulfuric acid, decoloring and filtering by using activated carbon to obtain a pretreated solution A, and determining and calculating the content of sodium sulfate in the solution A;
step 5, adding metered industrial acetic acid into a reactor, adding water, stirring, slowly adding stoichiometric stone powder (calcium carbonate powder) at 25-60 ℃, stirring for 1-6 hours after adding, and filtering to obtain a filtrate B;
step 6, slowly adding the filtrate B into the treated solution A while stirring, continuously stirring for 1-4 hours after the addition is finished, detecting, and stopping stirring after the sodium sulfate completely reacts;
and 7, adjusting the pH of the system to 7.5-9 by using sodium carbonate or acetic acid, filtering to obtain gypsum (calcium sulfate dihydrate) and a sodium acetate solution, and heating and concentrating the filtrate to obtain a colorless transparent liquid with no pungent smell and sodium acetate content of more than or equal to 25%.
2. The method for preparing sodium acetate from dihydroxynaphthalene waste liquid according to claim 1, wherein the heating temperature of the dihydroxynaphthalene waste liquid in the step 1 is 45-50 ℃.
3. The production method for preparing sodium acetate by using the dihydroxy naphthalene waste liquid as claimed in claim 1, wherein in step 1, the amount of the added activated carbon is 1/240-1/60 mass% of the dihydroxy waste liquid, and the amount of the added flocculant is 1/120-1/35 mass% of the dihydroxy waste liquid.
4. The method for preparing sodium acetate from dihydroxy naphthalene waste liquid as claimed in claim 3, wherein the amount of activated carbon added in step 1 is 1/80-1/60 mass% of dihydroxy waste liquid; the addition amount of the flocculating agent is 1/60-1/40 of the quality of the dihydroxy waste liquid.
5. The method for preparing sodium acetate from dihydroxy naphthalene waste liquid according to claim 1, wherein said flocculant is one or two of Polyacrylamide (PAM), polyaluminium chloride (PAC), polyaluminium sulfate (PAS), polyferric chloride (PFC), and polyferric sulfate (PFS) for water treatment.
6. The method for producing sodium acetate from dihydroxy naphthalene waste liquid as claimed in claim 1, wherein the amount of ferrous sulfate catalyst added during Fenton oxidation is 1/600-1/200 mass% of dihydroxy waste liquid, and the amount of dioxygen water added is 1/600-1/150 mass% of dihydroxy waste liquid every half an hour three times.
7. The method for producing sodium acetate from dihydroxy naphthalene waste liquid as claimed in claim 6, wherein the amount of ferrous sulfate catalyst added during Fenton oxidation is 1/300-1/240 mass% of dihydroxy waste liquid, and the amount of hydrogen peroxide added is 1/400-1/240 mass% of dihydroxy waste liquid every half an hour three times.
8. The production method for preparing sodium acetate by using the dihydroxy naphthalene waste liquid as claimed in claim 1, wherein hydrogen peroxide is added in step 3 and then stirred at 45-50 ℃ for sufficient oxidation for 2-3 hours.
9. The production method for preparing sodium acetate by using the dihydroxy naphthalene waste liquid as claimed in claim 1, wherein the reaction temperature of the industrial acetic acid and the stone powder in step 5 is 25-40 ℃, and after the reaction is completed, the industrial acetic acid and the stone powder are stirred for 3-4 hours and filtered to obtain filtrate B.
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Cited By (1)
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