CN108017233B - Method for treating sewage of forestry chemical enterprises - Google Patents

Method for treating sewage of forestry chemical enterprises Download PDF

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CN108017233B
CN108017233B CN201711328607.2A CN201711328607A CN108017233B CN 108017233 B CN108017233 B CN 108017233B CN 201711328607 A CN201711328607 A CN 201711328607A CN 108017233 B CN108017233 B CN 108017233B
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water
treated water
tank
oil
sewage
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CN108017233A (en
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黎月清
张陆春
祝军
郭超仁
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Guangdong Hualin Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/24Treatment of water, waste water, or sewage by flotation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/40Devices for separating or removing fatty or oily substances or similar floating material
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F3/00Biological treatment of water, waste water, or sewage
    • C02F3/30Aerobic and anaerobic processes

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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physical Water Treatments (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The invention provides a method for treating sewage of forestry chemical enterprises, which comprises the following steps: (1) filtering; (2) oil-water separation; (3) demulsifying; (4) oil removal and sedimentation; (5) carrying out irradiation treatment; (6) electrolyzing by an iron-carbon micro-electrolysis device; (7) neutralizing and settling; (8) back pressure filtration; (9) squeezing and filtering; (10) the pre-aeration tank, the wastewater adjusting tank, the anaerobic reaction tank, the acidification hydrolysis tank, the aerobic reaction tank, the deep sedimentation tank, the coagulation air flotation tank and the membrane filtering device are used for processing to obtain qualified water reaching the discharge standard. The invention can effectively treat the sewage of forest chemical enterprises, can reach the discharge standard after the sewage is treated, and can be recycled, thereby realizing zero discharge of the sewage.

Description

Method for treating sewage of forestry chemical enterprises
Technical Field
The invention belongs to the field of forestry chemical industry, and particularly relates to a method for treating sewage of forestry chemical enterprises.
Background
The rosin chemical industry is the backbone industry of the forest chemical industry in China and is one of the products with the largest yield in the forest chemical products, and the utilization of rosin resources is established on the basis of the resin collection of living pine trees. As a renewable resource, the rosin chemical industry is an effective way to efficiently utilize forest resources. The rosin has excellent performances of corrosion resistance, moisture resistance, insulation, adhesion, emulsification, softening and the like, and is widely applied to various fields of national economy.
China is the first major country of world rosin production and plays a significant role in the world rosin market. In 2013, the yield of rosin in China is about 80 ten thousand tons, the annual yield accounts for about 38 percent of the total world yield, and the export yield accounts for about 50 percent of the total world rosin trade amount. However, the rosin processing process generates a large amount of waste water, and the waste water is characterized by high organic matter content, and the main components are organic matters such as oils, resin acids, tannins, alcohols, esters and the like, so that the waste water has poor biodegradability and is difficult to treat. In addition, because a large amount of oxalic acid is added in the process of extracting rosin, the wastewater is acidic, and the difficulty of wastewater treatment is increased. Therefore, the rosin sewage is difficult to reach the national discharge standard by adopting the conventional coagulation and sedimentation treatment, and becomes one of high-concentration organic wastewater which is difficult to treat.
At present, most of sewage treatment of domestic rosin and deep processing enterprises thereof is simple physical separation, simple neutralization reaction treatment, settlement and coagulation, filtration and clarification treatment, and the sewage treatment is not thorough; even if some sewage is biochemically treated, the sewage is difficult to treat due to too many impurities and high oil content caused by low process level, high operation cost and the like, and the sewage is incompletely and incompletely treated due to insufficient bacterial content; during biochemical treatment, bacteria can be starved or saturated, and sewage treatment is not complete; the sewage is not filtered well, so that a large amount of suspended matters exist in the sewage, and the sewage cannot be recycled as cooling water. After treatment, the quality of the effluent can not reach the first-level discharge standard specified in national integrated wastewater discharge Standard GB8978-1996 and local integrated wastewater discharge Standard DB4426-2001 in Guangdong province, and the effluent can not be used as water for greening, road cleaning, rosin maintenance and the like; some treated water is easy to produce scaling due to high salt content and more impurities, and thus the treated water cannot be used as cooling water of a condenser. The sewage treatment is incomplete due to various reasons, only a small part of substances are recycled, and the zero emission is achieved.
The Guangdong province is a national key production and scientific research area which uses the pine resin as the raw material for processing and deep processing, has a great position in China, and the annual rosin and the deep processing products thereof are more than 50 million tons, the annual value is 70-100 million yuan, and more than 60 percent of the rosin and the deep processing products thereof in China are exported in the Guangdong province. The fields of rosin and turpentine related to the forest chemical products and deep processing of the rosin and the turpentine are the main prop industrial industries of Guangdong province, and forest chemical enterprises which are processed and produced by taking the turpentine as a raw material in provinces are mainly distributed in Zhaoqing, Yunfao, Yangjiang, Maoyang, Qingyuan, Shaoguan and other mountain cities and counties; even developed bead triangle cities have turpentine and its deep processed product manufacturing enterprises and major downstream industries, such as: the chemical industries such as adhesives, printing ink, coatings, spices and the like are developed; through technical research and development and technical innovation, the core competitiveness of products is improved, the value of the products is improved, the income of farmers is increased, the farmers and enterprises are guided to wastefully plant pine forests, the development of upstream forestry industries is promoted, and a great industrial chain is formed.
Zhaoqing area is a famous rosin processing and production base in Guangdong and even China, and Zhaoqing has rosin and deep processing and production enterprises thereof in every county, city and region, which are the biggest forest product producing and selling areas in China, and a lot of new forest technologies, new products and new standards are born in the country. The sealed county is the country of Chinese turpentine, and the Hualin company in the sealed county is a comprehensive forest chemical enterprise with the most complete deep processing varieties of rosin and turpentine and the largest production scale; is one of the largest comprehensive forestry product production enterprises in China; is the biggest rosin production and food-grade rosin resin production enterprise in China; is the first region in China where the rosin resin emulsion is produced; the seal is also the biggest disproportionated rosin production and export area in China. Deqing is the main production area of turpentine oil deep processing and spices, and also has enterprises for rosin production and rosin resin production; in high and new areas, large industrial-grade rosin resin production enterprises exist, Guangning mainly produces ink resin, and integrates the production of rosin, turpentine and disproportionated rosin; ding lake also has rosin resin production, and has the biggest rosin barrel production enterprise.
Along with the development of society, the requirement on environment protection work is more and more emphasized, the deep treatment of sewage, even the realization of zero emission, is a great trend, is the requirement of social development, and the research and development of a new process for sewage treatment has wide market space. The successful project research is beneficial to the conversion of environmental protection technology of companies, the cyclic utilization of the sewage of enterprises after treatment is facilitated, and the zero discharge of the sewage is realized. Therefore, a method for effectively treating the sewage of the forest chemical industry enterprises needs to be developed.
Chinese patent with application number CN201210246171.3 discloses a waste water treatment process for rosin production, which comprises the following steps: the wastewater enters a primary slag sedimentation tank to precipitate coarse slag in the wastewater; the wastewater after the coarse slag is precipitated flows through a coal slag channel, and fine slag and partial organic matters are filtered; the wastewater enters an active carbon treatment tank, and organic matters or harmful substances in the wastewater are precipitated and adsorbed to obtain supernatant; enabling the supernatant to enter an acid-base reaction tank, adding lime to alkalize the supernatant, stirring simultaneously, and controlling the pH value of the supernatant to be 6-9 to obtain clear water; the clean water flows through the fine sand filtering channel to filter fine slag, and water meeting the discharge standard is obtained. The actual treatment effect of the patent is not good, and the effluent quality is not good.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a method for treating the sewage of the forestry chemical enterprises, which can effectively treat the sewage of the forestry chemical enterprises, can reach the discharge standard after the sewage is treated, and can be recycled, thereby realizing zero discharge of the sewage.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a method for treating the sewage of the forestry chemical industry enterprises comprises the following steps:
(1) filtering the forest chemical industry enterprise sewage through a primary filter and a secondary filter in sequence to obtain treated water I, wherein the mesh number of a screen of the primary filter is smaller than that of a screen of the secondary filter;
(2) separating the treated water I into an oil phase I and a water phase I through an oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, and stirring for 2 hours to obtain treated water II;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, and conveying the stainless steel disc into an irradiation chamber provided with an electron accelerator for irradiation treatment to obtain treated water III;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the treated water IV into a neutralization sedimentation tank containing alkali liquor for neutralization sedimentation to obtain treated water V;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) and treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water meeting the discharge standard.
Further, in the step (1), the waste water of the forest chemical industry enterprise is waste water of a rosin plant, waste water of a rosin resin plant, waste water of an ink resin plant, waste water of a disproportionated rosin plant, or waste water of a terpene resin plant.
Furthermore, in the step (1) of the invention, the mesh number of the screen of the first filter is 30-60 meshes, and the mesh number of the screen of the second filter is 100-120 meshes.
Further, in the step (2) of the present invention, the oil-water separator is a multi-stage oil-water separator.
Furthermore, in the step (3) of the invention, the ratio of the demulsifier to the first water phase is 0.1-0.4 g/L.
Further, in the step (3), the demulsifier is prepared by mixing an AR type demulsifier and an amino acid ionic liquid in a mass ratio of 5:1, and the preparation step of the amino acid ionic liquid is as follows:
mixing 1-butyl-3-methylimidazole and bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, evaporating under reduced pressure to remove distilled water to obtain an amino acid ionic liquid
Further, in the step (5) of the present invention, the thickness of the second aqueous phase in the stainless steel plate is 4mm, the energy of the electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy.
Further, in the step (7) of the present invention, the alkali solution is a calcium hydroxide solution.
The working principle of the invention is as follows:
forest chemical enterprise sewage at first passes through primary filter and secondary filter, and big impurity passes through primary filter filtering separation, and little impurity passes through secondary filter filtering separation, and the impurity that the filtration obtained can be gone into the bag packing while filtering, convenient operation. The sewage of the forest chemical enterprises contains oil, the oil-water separation of the sewage is relatively easy after the impurity separation, the oil-water separation of the sewage after the impurity separation is clean after the sewage is separated by the multistage oil-water separator, but the oil contained in the sewage is still partially emulsified, so that the oil contained in the sewage is separated out by the demulsifier, and then the separation of the oil, the water and the impurity is realized by the oil separation sedimentation tank, the impurity sedimentation and the waste oil recovery are realized. Then the sewage is electrolyzed by an iron-carbon micro-electrolysis device, the electrolysis method has high efficiency and easy operation for treating the wastewater, and has good decolorization effect, and the removal rates of COD, SS and chroma respectively reach 70 percent, 80 percent and 60 percent. The sewage enters a neutralization sedimentation tank containing alkali liquor after being electrolyzed, the alkali liquor and acidic substances in the sewage are subjected to neutralization reaction to generate salt, the discharged water is conveyed to a boiler to be used as dust removal water, the dust removal water passes through a back pressure filter to remove coal ash and ash slag, and the impurities are further removed by impurity squeezing and filtering after the discharged water is discharged. Therefore, through a series of measures such as filtering, oil-water separation, neutralization reaction, sedimentation and the like, organic matters, oils and chemicals in the sewage become less, and the sewage is beneficial to entering the next biochemical treatment process. The sewage after the treatment sequentially passes through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device, and after the series of treatment, the sewage reaches the GB18920-2002 standard, can be reused for plant oil tank spray cooling water, turpentine maintenance, production workshop equipment cooling circulation water, road equipment site cleaning and the like, and sludge obtained by separating water can be used as an organic fertilizer after being treated.
Compared with the prior art, the invention has the following beneficial effects:
1) the system effluent treated by the invention reaches the first-level standard in the fourth table of GB8978-1996 Integrated wastewater discharge Standard and the first-level discharge standard specified in the local Integrated wastewater discharge Standard DB4426-2001 in Guangdong province, and the treated wastewater can be directly recycled and is mainly used for flower and plant spraying, road cleaning, turpentine maintenance, condenser recycling water and the like, so that zero discharge of wastewater is realized.
2) The demulsifier in the step (3) of the invention is formed by mixing the AR type demulsifier and the amino acid ionic liquid, the amino acid ionic liquid has the effects of dissolving and destroying the oil in the sewage, the phase separation process is accelerated, the amino acid ionic liquid and the AR type demulsifier generate a synergistic effect, the demulsification effect is effectively improved, the oil in the sewage is further favorably removed, in addition, the amino acid ionic liquid has good biodegradability and very low toxicity, and the quality of the effluent water cannot be influenced.
3) The irradiation operation in the step (5) of the invention can lead the organic matters and microorganisms in the sewage to be irradiated and degraded into micromolecules, which is beneficial to improving the treatment effect of the subsequent electrolytic treatment, thereby thoroughly removing the organic matters and the microorganisms in the sewage.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Treating the forest chemical industry enterprise sewage according to the following steps:
(1) sequentially filtering the forest chemical industry enterprise sewage through a primary filter with a screen mesh of 30-60 meshes and a secondary filter with a screen mesh of 100-120 meshes to obtain treated water I;
(2) separating the treated water I into an oil phase I and a water phase I through a multi-stage oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, stirring for 2 hours to obtain treated water II, wherein the ratio of the demulsifying agent to the water phase I is 0.1g/L, the demulsifying agent is formed by mixing an AR type demulsifying agent and amino acid ionic liquid in a mass ratio of 5:1, and the preparation method of the amino acid ionic liquid comprises the following steps: mixing 1-butyl-3-methylimidazole with bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, and evaporating under reduced pressure to remove distilled water to obtain an amino acid ionic liquid;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, controlling the thickness of the water phase II to be 4mm, conveying the stainless steel disc into an irradiation workshop provided with an electron accelerator for irradiation treatment to obtain treated water III, wherein the energy of the electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the fourth treated water into a neutralization sedimentation tank containing a calcium hydroxide solution for neutralization sedimentation to obtain fifth treated water;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) and treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water meeting the discharge standard.
Example 2
Treating the forest chemical industry enterprise sewage according to the following steps:
(1) sequentially filtering the forest chemical industry enterprise sewage through a primary filter with a screen mesh of 30-60 meshes and a secondary filter with a screen mesh of 100-120 meshes to obtain treated water I;
(2) separating the treated water I into an oil phase I and a water phase I through a multi-stage oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, stirring for 2 hours to obtain treated water II, wherein the ratio of the demulsifying agent to the water phase I is 0.3g/L, the demulsifying agent is formed by mixing an AR type demulsifying agent and amino acid ionic liquid in a mass ratio of 5:1, and the preparation method of the amino acid ionic liquid comprises the following steps: mixing 1-butyl-3-methylimidazole with bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, and evaporating under reduced pressure to remove distilled water to obtain an amino acid ionic liquid;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, controlling the thickness of the water phase II to be 4mm, conveying the stainless steel disc into an irradiation workshop provided with an electron accelerator for irradiation treatment to obtain treated water III, wherein the energy of the electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the fourth treated water into a neutralization sedimentation tank containing a calcium hydroxide solution for neutralization sedimentation to obtain fifth treated water;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) and treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water which reaches the emission standard.
Example 3
Treating the forest chemical industry enterprise sewage according to the following steps:
(1) sequentially filtering the forest chemical industry enterprise sewage through a primary filter with a screen mesh of 30-60 meshes and a secondary filter with a screen mesh of 100-120 meshes to obtain treated water I;
(2) separating the treated water I into an oil phase I and a water phase I through a multi-stage oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, stirring for 2 hours to obtain treated water II, wherein the ratio of the demulsifying agent to the water phase I is 0.4g/L, the demulsifying agent is formed by mixing an AR type demulsifying agent and amino acid ionic liquid in a mass ratio of 5:1, and the preparation method of the amino acid ionic liquid comprises the following steps: mixing 1-butyl-3-methylimidazole with bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, and evaporating under reduced pressure to remove distilled water to obtain an amino acid ionic liquid;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, controlling the thickness of the water phase II to be 4mm, conveying the stainless steel disc into an irradiation workshop provided with an electron accelerator for irradiation treatment to obtain treated water III, wherein the energy of the electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the fourth treated water into a neutralization sedimentation tank containing a calcium hydroxide solution for neutralization sedimentation to obtain fifth treated water;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) and treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water which reaches the emission standard.
Example 4
Treating the forest chemical industry enterprise sewage according to the following steps:
(1) sequentially filtering the forest chemical industry enterprise sewage through a primary filter with a screen mesh of 30-60 meshes and a secondary filter with a screen mesh of 100-120 meshes to obtain treated water I;
(2) separating the treated water I into an oil phase I and a water phase I through a multi-stage oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, stirring for 2 hours to obtain treated water II, wherein the ratio of the demulsifying agent to the water phase I is 0.2g/L, the demulsifying agent is formed by mixing an AR type demulsifying agent and amino acid ionic liquid in a mass ratio of 5:1, and the preparation method of the amino acid ionic liquid comprises the following steps: mixing 1-butyl-3-methylimidazole with bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, and evaporating under reduced pressure to remove distilled water to obtain an amino acid ionic liquid;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, controlling the thickness of the water phase II to be 4mm, conveying the stainless steel disc into an irradiation workshop provided with an electron accelerator for irradiation treatment to obtain treated water III, wherein the energy of the electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the fourth treated water into a neutralization sedimentation tank containing a calcium hydroxide solution for neutralization sedimentation to obtain fifth treated water;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) and treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water which reaches the emission standard.
Comparative example 1
The difference from the example 2 is that the amino acid ionic liquid is not contained in the demulsifier, and other steps are the same as the example 2.
Comparative example 2
The difference from example 2 is that step (5) of irradiation treatment was not included, and the other steps are the same as example 2.
Comparative example 3
Unlike example 2, the step (7) of the neutralization sedimentation treatment was not included, and the other steps were the same as example 2.
The waste water of the forest chemical industry in examples 1 to 4 and comparative examples 1 to 3 was rosin plant waste water, rosin resin plant waste water, ink resin plant waste water, disproportionated rosin plant waste water, or terpene resin plant waste water.
Comparative example
The comparison example is the Chinese patent with the application number of CN201210246171.3
The first experimental example: pH value test of effluent
The test results are shown in table 1:
PH
example 1 7.5
Example 2 7.0
Example 3 8.2
Example 4 6.4
Comparative example 1 7.8
Comparative example 2 8.3
Contrast experimentExample 3 12.1
Comparative example 8.1
TABLE 1
As can be seen from Table 1, the effluent of inventive examples 1-4 had a pH substantially less than the control and all achieved the discharge standard (pH range 6-9). The partial steps of comparative examples 1-3 are different from example 2, wherein the pH values of the effluent of comparative example 1 and comparative example 2 are almost the same as those of examples 1-4, which shows that the amino acid ionic liquid in the emulsifier used in the invention and the step of irradiation treatment have no substantial influence on the pH value of the effluent; the effluent from comparative example 3 had a significantly higher pH than the effluent from examples 1-4, indicating that the neutralization and sedimentation treatment step of the present invention effectively lowered the pH of the effluent.
Experiment example two: CODcr test of effluent
The test results are shown in table 2:
CODcr(mg/l)
example 1 42
Example 2 36
Example 3 40
Example 4 44
Comparative example 1 66
Comparative example 2 87
Comparative example 3 41
Comparative example 96
TABLE 2
As can be seen from Table 2, the effluent waters of examples 1-4 of the present invention all had CODcr values significantly less than the control and all reached the discharge standard (CODcr value ≦ 90mg/l), with the effluent water of example 2 having the lowest CODcr value. The steps of comparative examples 1-3 are different from those of example 2, wherein the CODcr value of the effluent of comparative example 1 is slightly increased, which shows that the amino acid ionic liquid in the emulsifier used in the invention has a certain reducing effect on organic matters in the sewage; the CODcr value of the effluent of comparative example 2 is greatly increased, which shows that the irradiation treatment step of the invention can well reduce the organic matters in the sewage; the CODcr value of the effluent of comparative example 3 is comparable to examples 1-4, demonstrating that the neutralization settling treatment step of the present invention has substantially no effect on the CODcr value of the effluent.
Experiment example three: BOD of the effluent5Testing
The test results are shown in table 3:
BOD5(mg/l)
example 1 12
Example 2 8
Example 3 10
Example 4 13
Comparative example 1 11
Comparative example 2 37
Comparative example 3 9
Comparative example 44
TABLE 3
As can be seen from Table 3, the BOD of the effluent of examples 1-4 of the present invention5The values are all obviously smaller than those of the control example and all reach the discharge standard (BOD)5Value ≤ 20mg/l), wherein the effluent of example 2 has a BOD5The value is minimal. Comparative examples 1-3 differ from example 2 in part of the procedure, in that comparative example 2 gives the effluent BOD5The value is increased a lot, which shows that the step of irradiation treatment of the invention can well reduce the microorganisms in the sewage; BOD of effluent of comparative examples 1, 35The values are comparable to those of examples 1 to 4, said thatThe amino acid ionic liquid in the emulsifier of the invention and the step of neutralization sedimentation treatment on BOD of the effluent5The values have substantially no effect.
Experimental example four: SS test of effluent
The test results are shown in table 4:
SS(mg/l)
example 1 29
Example 2 27
Example 3 30
Example 4 32
Comparative example 1 31
Comparative example 2 45
Comparative example 3 28
Comparative example 85
TABLE 4
As can be seen from Table 4, the SS values of the effluent of examples 1-4 of the present invention are all significantly lower than those of the comparative examples, and all reach the emission standard (SS value is less than or equal to 70mg/l), wherein the SS value of the effluent of example 2 is the smallest. The steps of comparative examples 1-3 are different from those of example 2, wherein the SS value of the effluent of comparative example 2 is slightly increased, which shows that the irradiation treatment step of the invention can effectively reduce suspended matters in the sewage; the SS values of the effluent of comparative examples 1 and 3 are almost the same as those of examples 1 to 4, which shows that the amino acid ionic liquid in the emulsifier of the present invention and the step of the neutralization and sedimentation treatment have substantially no influence on the SS values of the effluent.
Experimental example five: oil value test of effluent
The test results are shown in table 5:
oils (mg/l)
Example 1 2.5
Example 2 2.2
Example 3 2.6
Example 4 2.8
Comparative example 1 4.7
Comparative example 2 3.9
Comparative example 3 2.7
Comparative example 8.3
TABLE 5
As can be seen from Table 5, the effluent of examples 1-4 of the present invention all had significantly lower oil values than the control and all reached the emission standards (oil values ≤ 5mg/l), with the effluent of example 2 having the lowest oil value. The steps of comparative examples 1-3 are different from those of example 2, wherein the oil value of the effluent of comparative example 2 is slightly increased, which shows that the step of irradiation treatment according to the invention has a certain reduction effect on the oil in the wastewater; the oil value of the effluent of comparative example 1 is greatly increased, which shows that the amino acid ionic liquid in the emulsifier used in the invention is beneficial to greatly reducing the oil in the sewage; the oil value of the effluent of comparative example 3 is comparable to examples 1-4, indicating that the neutralization and sedimentation treatment step of the present invention has substantially no effect on the oil value of the effluent.
Experimental example six: color test of effluent
The test results are shown in table 6:
chroma (double)
Example 1 32
Example 2 30
Example 3 33
Example 4 36
Comparative example 1 34
Comparative example 2 49
Comparative example 3 34
Comparative example 77
TABLE 6
As can be seen from Table 6, the effluent of examples 1-4 of the present invention all had significantly smaller chroma values than the control and all reached the discharge standard (chroma value ≤ 50 times), wherein the effluent of example 2 had the smallest chroma value. The steps of comparative examples 1-3 are different from those of example 2, wherein the colorimetric value of the effluent of comparative example 2 is increased to a certain extent, which shows that the step of irradiation treatment of the invention can effectively reduce the colorimetric value of the sewage; the colorimetric values of the effluent of comparative examples 1 and 3 are almost the same as those of examples 1 to 4, which shows that the amino acid ionic liquid in the emulsifier of the present invention and the step of the neutralization and sedimentation treatment have no substantial influence on the colorimetric values of the effluent.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (7)

1. A method for treating the sewage of the forestry chemical enterprises is characterized by comprising the following steps: the method comprises the following steps:
(1) filtering the forest chemical industry enterprise sewage through a primary filter and a secondary filter in sequence to obtain treated water I, wherein the mesh number of a screen of the primary filter is smaller than that of a screen of the secondary filter;
(2) separating the treated water I into an oil phase I and a water phase I through an oil-water separator;
(3) adding the water phase I into a demulsifying separator containing a demulsifying agent, and stirring for 2 hours to obtain treated water II;
(4) settling and separating the treated water II into an oil phase II, a water phase II and impurities through an oil separation settling pond, recovering the oil phase II and discarding the impurities;
(5) placing the water phase II in a stainless steel disc, and conveying the stainless steel disc into an irradiation chamber provided with an electron accelerator for irradiation treatment to obtain treated water III;
(6) carrying out electrolytic treatment on the treated water tee joint by an iron-carbon micro-electrolysis device to obtain treated water IV;
(7) adding the treated water IV into a neutralization sedimentation tank containing alkali liquor for neutralization sedimentation to obtain treated water V;
(8) conveying the treated water V to a boiler to obtain water for dust removal, and filtering the water for dust removal through a back pressure filter to remove coal ash and ash residues to obtain treated water VI;
(9) filtering the treated water six through a squeezing filter to remove impurities to obtain treated water seven;
(10) treating the treated water seven sequentially through a pre-aeration tank, a wastewater adjusting tank, an anaerobic reaction tank, an acidification hydrolysis tank, an aerobic reaction tank, a deep sedimentation tank, a coagulation air flotation tank and a membrane filtration device to obtain qualified water meeting the discharge standard;
in the step (3), the demulsifier is formed by mixing an AR type demulsifier and an amino acid ionic liquid in a mass ratio of 5:1, and the preparation step of the amino acid ionic liquid is as follows:
mixing 1-butyl-3-methylimidazole and bromoethane in a mass ratio of 1:3, stirring and reacting for 2 hours at 50 ℃, cooling to room temperature to obtain a first reactant, extracting residual bromoethane in the first reactant with ethyl acetate, drying in vacuum at 80 ℃ to constant weight to obtain an intermediate product, adding the intermediate product into water, uniformly mixing to obtain a mixed solution, passing the mixed solution through strong-base anion exchange resin to obtain a hydroxide intermediate product, mixing the hydroxide intermediate product with alanine in an equal molar ratio, adding distilled water, heating and stirring until the alanine is completely dissolved, stirring and reacting for 3 hours at 50 ℃ to obtain a second reactant, evaporating the second reactant under reduced pressure to remove unreacted raw materials, washing with distilled water to be neutral, and evaporating under reduced pressure to remove distilled water to obtain the amino acid ionic liquid.
2. The forest chemical industry enterprise sewage treatment method according to claim 1, wherein the method comprises the following steps: in the step (1), the forest chemical industry enterprise sewage is rosin plant wastewater, rosin resin plant wastewater, printing ink resin plant wastewater, disproportionated rosin plant wastewater or terpene resin plant wastewater.
3. The forest chemical industry enterprise sewage treatment method according to claim 2, wherein the method comprises the following steps: in the step (1), the mesh number of the screen of the first-stage filter is 30-60 meshes, and the mesh number of the screen of the second-stage filter is 100-120 meshes.
4. The forest chemical industry enterprise sewage treatment method according to claim 3, wherein the method comprises the following steps: in the step (2), the oil-water separator is a multistage oil-water separator.
5. The forest chemical industry enterprise sewage treatment method according to claim 4, wherein the method comprises the following steps: in the step (3), the ratio of the demulsifying agent to the water phase I is 0.1-0.4 g/L.
6. The forest chemical industry enterprise sewage treatment method according to claim 5, wherein the method comprises the following steps: in the step (5), the thickness of the water phase II in the stainless steel disc is 4mm, the energy of an electron accelerator is 10MeV, the power is 100kW, and the irradiation dose is 15 kGy.
7. The forest chemical industry enterprise sewage treatment method according to claim 6, wherein the method comprises the following steps: in the step (7), the alkali liquor is calcium hydroxide solution.
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CN101792239A (en) * 2010-03-31 2010-08-04 成都蜀光石油化学有限公司 Method for treatment of waste emulsion
CN106673300A (en) * 2016-12-16 2017-05-17 三达膜科技(厦门)有限公司 Treatment method for wastewater of forestry chemical industry

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CN101792239A (en) * 2010-03-31 2010-08-04 成都蜀光石油化学有限公司 Method for treatment of waste emulsion
CN106673300A (en) * 2016-12-16 2017-05-17 三达膜科技(厦门)有限公司 Treatment method for wastewater of forestry chemical industry

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Denomination of invention: A Method for Treating Wastewater from Forestry and Chemical Enterprises

Effective date of registration: 20231107

Granted publication date: 20200519

Pledgee: Guangdong Fengkai Rural Commercial Bank Co.,Ltd. Pingfeng Branch

Pledgor: GUANGDONG HUALIN CHEMICAL Co.,Ltd.

Registration number: Y2023980064468