CN114573160A - Treatment and recycling method of cold coke wastewater - Google Patents
Treatment and recycling method of cold coke wastewater Download PDFInfo
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Abstract
The invention provides a method for treating and recycling cold coke wastewater. The method comprises the following steps: A. the cold coke wastewater enters an oil separation unit to remove floating oil and large granular coke powder in the cold coke wastewater; B. the effluent after the oil removal treatment enters a reuse pretreatment unit to further remove petroleum and suspended matters; C. the effluent of the pretreatment unit passes through a cooling unit, and can be recycled as qualified coke cooling water after being cooled; D. and the effluent of the cooling unit enters a dual-waveband ultraviolet light catalysis unit for advanced treatment, so that the emission requirement of benzopyrene in water quality is met. The invention starts from the water-saving angle, and the coke cooling water is recycled through the combined process; on the basis of partial recycling, advanced treatment is carried out through dual-waveband ultraviolet light catalysis, and the requirements of standard-reaching discharge or circulating water replenishing and the like are met. The invention has simple processing process flow and low processing cost.
Description
Technical Field
The invention relates to the field of coking wastewater treatment, in particular to recycling and standard discharge treatment of cold coke wastewater.
Background
Delayed coking is one of the main processes for the current deep processing of heavy oil, and is often used for processing residual oil with high carbon-to-hydrogen ratio and high sulfur and nitrogen content, catalytic slurry oil and extra heavy crude oil. Therefore, the wastewater produced by the delayed coking unit is also one of the main pollution sources of the refinery. According to the process flow of the coking unit, the produced wastewater mainly comprises the following components: cold coke waste water, coke cutting waste water, condensation waste water and the like.
Wherein the cold coke wastewater accounts for a relatively large proportion in the coking wastewater; and after the coke is cooled by the coke tower, the temperature of the cold coke wastewater is about 80 ℃, and the cold coke wastewater contains a large amount of dirty oil, coke powder, polycyclic aromatic hydrocarbon compounds and the like. The oil, coke and temperature can be removed for recycling after follow-up oil removal, coke removal and temperature reduction. At present, the problem of coke powder blockage exists in the existing treatment process.
Patent 200410068149.X discloses a coke cooling sewage treatment method and device, which adopts equipment such as a hydrocyclone, a rotational flow type oil-water separator and the like to remove coke powder and separate oil from water. The method is complicated in equipment. Meanwhile, the problem of serious blockage exists, and the normal operation of the system is influenced.
Patent ZL02216056.6 discloses a closed treatment device for delayed coking coke cooling water, but practice proves that the device has the following disadvantages: the equipment investment is large, the system pressure drop is large, and the coke cooling water pump lift is required to be high; due to the existence of coke powder, the cyclone oil remover is easy to block; in addition, the oil-containing coke cooling water is easy to emulsify when being conveyed by a pump, so that the separation efficiency of a subsequent cyclone is low.
In addition, benzopyrene in the cold coke water is a strong carcinogen with the largest toxicity of polycyclic aromatic hydrocarbon compounds, strict requirements (less than or equal to 0.03 mu g/L) are provided for the emission limit in the emission standards GB 16171-2012 of coking chemical industry pollutants and the emission standards GB 31570-2015 of petroleum refining industry pollutants, the concentration of benzopyrene in the cold coke water is 0.5-180 mu g/L which is far higher than the emission standard limit, and the treatment difficulty is large.
Therefore, in order to realize the recycling of the cold coke water after the treatment or the use of the cold coke water as electric desalted water, circulating water and external drainage after the advanced treatment, a method for treating and recycling cold coke wastewater with low cost and good effect is urgently needed to be developed, the problems of blockage, low efficiency and the like in the prior art are solved, and the requirement of clean production of petrochemical industry is further met.
Disclosure of Invention
The invention aims to provide a method for treating and recycling cold coke wastewater. The method fully considers the characteristics of poor water solubility, easy dissolution in organic solvents and easy adsorption on suspended matters such as coke powder and the like of benzopyrene; the existing petroleum coke in a delayed coking workshop is used for preparing an adsorbent material for treating pollutants such as benzopyrene, petroleum and the like.
In order to achieve the purpose, in the oil removal stage, floating oil and large-particle coke powder in the cold coke water are removed, petroleum and benzopyrene pollutants are efficiently removed in a pretreatment unit by preferably utilizing a process of coupling petroleum coke-based adsorbent and flocculation, and the cooled cold coke water can be recycled; the invention carries out advanced treatment on the coke cooling water in a dual-waveband ultraviolet light catalysis stage, and can be used as circulating water, electric desalted water or external drainage and the like according to the water quality index of the effluent and the specific actual requirement.
The invention provides a method for treating and recycling cold coke wastewater, which comprises the following steps:
A. the cold coke water enters an oil separation unit to remove floating oil and large-particle coke powder in the cold coke wastewater;
B. the wastewater after oil removal enters a reuse pretreatment unit to further remove petroleum and suspended matters;
C. part of the effluent of the pretreatment unit passes through a cooling unit, and is cooled and recycled;
D. and the effluent of the other part of the cooling unit enters a dual-waveband ultraviolet light catalysis unit for advanced treatment, so that the emission requirement of benzopyrene in water quality is met, or the requirements of recycling circulating water and electric desalted water are met.
Furthermore, in the oil separation unit in the step A, an oil separation tank is adopted and is semi-sealed, the oil separation tank has oil removal and sludge discharge functions, and tail gas is provided with an alkali liquor absorption device; the retention time is 0.5-4 h, preferably 1-2 h; the floating oil and large granular coke powder are removed, and the temperature of the cold coke wastewater is also reduced.
Further, the recycling pretreatment unit in the step B can adopt one or more of air flotation, medicine-adding air flotation, flocculation and adsorption modes, preferably adopts an adsorption flocculation coupling mode for pretreatment, and can set 1-2 levels of adsorption flocculation treatment according to the properties of the cold coke wastewater.
The adsorbent used in the adsorption mode is an activated carbon adsorbent prepared from petroleum coke serving as a raw material, and the specific surface area of the adsorbent is 700-900 m2The total pore volume is 0.33-0.43 cm3Per g, wherein the volume of the micropore volume is 0.29-0.38 cm3The adsorbent is mainly microporous.
The adsorbent can be prepared by the following method: the method comprises the steps of taking petroleum coke as a raw material, taking an activating agent which is one or more of potassium hydroxide, sodium hydroxide, potassium carbonate and sodium carbonate, preferably taking KOH as the activating agent, grinding and screening the petroleum coke, then uniformly mixing the petroleum coke with the activating agent, carrying out an activation reaction under a nitrogen atmosphere, cooling, washing to be neutral, and drying to obtain the adsorbent, wherein the reaction temperature of the activation reaction is 750-850 ℃. The mass ratio of the petroleum coke to the activating agent is 1: 2-5, preferably 1: 2-3, and the petroleum coke grinding sieve is 50-100 meshes.
The dosage of the adsorbent is 50-100 mg/L, and the adsorbent is coupled with a flocculating agent for use.
Wherein, the flocculating agent used in the flocculation mode can be selected from at least one of aluminum chloride, polyaluminum chloride, ferric chloride, polyferric chloride, ferric sulfate, polyferric sulfate, aluminum sulfate and polyaluminum sulfate, and is preferably polyaluminum chloride; the coagulant aid is polyacrylamide.
Preferably, the dosage of the flocculant is 50-500 mg/L, and further preferably 100-200 mg/L; the dosage of the coagulant aid is 0-10 mg/L, and the preferred dosage is 2-5 mg/L.
The flocculation treatment mode can be used independently or coupled with an adsorbent, and is preferably an adsorption flocculation coupling treatment mode.
When the adsorption flocculation coupling treatment mode is selected, the dosage ratio of the adsorbent to the flocculant is 1: 2-5, preferably 1:3 to 4.
Further, the cooling unit of step C, the heat exchanger, may be specifically selected from one or more of an air-cooled heat exchanger, a shell-and-tube heat exchanger, a plate-fin heat exchanger, and a spiral plate heat exchanger.
According to the method, the temperature of the effluent of a part of pretreatment units is reduced to be less than or equal to 40 ℃, and the effluent can be recycled to the coke cooling water storage tank for coke cooling operation.
And D, further oxidizing the effluent of the other part of pretreatment units by a dual-waveband ultraviolet light catalysis unit to remove dissolved petroleum and benzopyrene and other organic matters, so that the effluent meets the water quality requirements of standard emission or circulating water and electric desalting reuse.
And D, arranging 1-3 levels of photocatalytic reactors in the dual-band ultraviolet catalytic unit in the step D, arranging dual-band ultraviolet lamps in each level, generating ultraviolet light with the wavelength of less than 200nm and 254nm, and adding an oxidant according to the treatment purpose. The oxidant can be one or more of hydrogen peroxide, sodium persulfate and ozone, and hydrogen peroxide is preferred; the dosage of the oxidant is 100-800 mg/L, and more preferably 350-550 mg/L.
On one hand, in the dual-waveband ultraviolet light catalysis unit, organic matters can be subjected to direct photolysis reaction by utilizing ultraviolet light of different wavebands; on the other hand, ultraviolet light irradiation water with the wavelength less than 200nm can generate homolytic reaction and photochemical ionization, and the generated hydroxyl free radicals can promote the degradation of organic matters; in addition, the organic matters can be degraded synergistically by the indirect photolysis generated by the added oxidant to generate additional free radicals.
The quality of the coke cooling water in the method of the invention is as follows: COD is 100-1300 mg/L, benzopyrene is 0.5-180 mu g/L, petroleum is 10-850 mg/L, turbidity is 100-2000 NTU, and conductivity is less than or equal to 1200 mu S/cm.
The invention starts from the water-saving and emission-reducing angle, and the coke cooling water meets the recycling requirement through a combined process; on the basis of recycling, advanced treatment is carried out through dual-waveband ultraviolet light catalysis, and the requirement of standard discharge or recycling of circulating water is met.
The invention has the advantages that:
(1) the treatment process flow is simple, the adsorption flocculation coupling process is preferably selected, pollutants such as suspended matters, petroleum and the like can be efficiently removed, the blockage of equipment such as a filter, a pump and the like is avoided, the continuous and stable normal operation of a coke cooling water circulation treatment system can be ensured, and the equipment maintenance cost is reduced;
(2) the method can use local materials, uses the petroleum coke on site to prepare the activated carbon adsorbent, fully utilizes the characteristic that benzopyrene, petroleum and the like are easy to adsorb suspended matters, and has low treatment cost;
(3) in the advanced treatment stage, the dual-waveband ultraviolet light catalysis method is adopted for advanced treatment, so that pollutants such as dissolved petroleum and benzopyrene can be efficiently oxidized and removed, the effluent meets the requirement of discharge or secondary reuse, and the purposes of water saving and emission reduction are achieved; meanwhile, the advanced treatment process does not produce secondary pollution, occupies small area and is easy to operate.
(4) The method can flexibly adjust the ratio of the water quantity of the cold coke wastewater recycling and the advanced treatment, not only can completely recycle the cold coke wastewater, but also can completely carry out the advanced treatment, and fully meets the field use requirement.
Drawings
FIG. 1 is a schematic view of a method for treating and recycling cold coke wastewater.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
Table 1 shows the water quality of the cold coke wastewater of a certain petrochemical plant.
TABLE 1 Coke cooling wastewater and discharge and circulating water make-up water quality index
Examples of preparation of adsorbents
Grinding and screening petroleum coke into 50-60 meshes, uniformly mixing the petroleum coke and KOH according to the mass ratio of 1:3, under the condition of nitrogen atmosphere, activating at 800 ℃ for 2h, cooling, washing with water to be neutral, and drying at 105 ℃ to obtain the activated carbon adsorbent. Adsorbent specific surface area 870m2Per g, pore volume of 0.41cm3Per g, pore volume of the micropores is 0.36cm3/g。
Example 1
Taking the cold coke wastewater 1 as a treatment object, setting the oil-separation retention time to be 2h, and allowing oil-separation effluent to enter a flocculation unit, wherein the PAC addition is 200mg/L and the PAM addition is 2 mg/L; after the supernatant passes through the air-cooled heat exchanger, the water quality analysis result is as follows: the petroleum is 15mg/L, the turbidity is 40NTU, the temperature is 35 ℃, and the requirement of recycling the cold coke water is met.
Example 2
Taking the cold coke wastewater 1 as a treatment object, setting the oil removal retention time to be 2h, enabling oil removal effluent to enter a flocculation unit, setting the PAC addition amount to be 200mg/L, the PAM addition amount to be 2mg/L, and setting the flocculation settling time to be 1 h; after the supernatant passes through the air-cooled heat exchanger, one part is recycled, the other part passes through the dual-waveband ultraviolet light catalysis unit, the light source intensity is 40W/L, the adding amount of hydrogen peroxide is 500mg/L, the reaction time is 2h, and the analysis result of the effluent quality is as follows: the petroleum is 0.5mg/L, the COD is 55mg/L, the turbidity is 6NTU, the temperature is 40 ℃, the benzopyrene concentration is 0.01 mu g/L, and the treated coke cooling water meets the requirements of standard discharge and circulating water replenishing.
Example 3
Taking the cold coke wastewater 1 as a treatment object, setting the oil removal retention time to be 2h, enabling oil removal effluent to enter a flocculation unit, adding 50mg/L of petroleum coke-based adsorbent, adding 150mg/L of PAC (polyaluminium chloride), adding 2mg/L of PAM (polyacrylamide), and flocculating and settling for 1 h; after the supernatant passes through the air-cooled heat exchanger, one part is recycled, the other part passes through the dual-waveband ultraviolet light catalysis unit, the light source intensity is 40W/L, the adding amount of hydrogen peroxide is 500mg/L, the reaction time is 2h, and the analysis result of the effluent quality is as follows: the petroleum is 0.3mg/L, the COD is 50mg/L, the turbidity is 5NTU, the temperature is 40 ℃, the benzopyrene concentration is lower than the detection limit (less than or equal to 0.004 mu g/L), and the treated coke cooling water meets the requirements of standard discharge and circulating water replenishing.
Example 4
Taking the cold coke wastewater 2 as a treatment object, setting the oil removal retention time to be 2h, enabling oil removal effluent to enter a flocculation unit, wherein the adding amount of petroleum coke-based adsorbent is 50mg/L, the adding amount of PAC is 150mg/L, the adding amount of PAM is 2mg/L, and the flocculation settling time is 1 h; after the supernatant passes through the air-cooled heat exchanger, one part is recycled, the other part passes through the dual-waveband ultraviolet light catalysis unit, the light source intensity is 40W/L, the adding amount of hydrogen peroxide is 500mg/L, the reaction time is 2h, and the analysis result of the effluent quality is as follows: the petroleum is 0.2mg/L, the COD is 45mg/L, the turbidity is 5NTU, the temperature is 40 ℃, the benzopyrene concentration is lower than the detection limit (less than or equal to 0.004 mu g/L), and the treated coke cooling water meets the requirement of reaching the standard and being discharged.
The method for treating and recycling the coke cooling water can effectively remove suspended matters such as floating oil, coke powder and the like, can keep the coke cooling water to be recycled for a long period, and can meet the requirement of standard external discharge or circulating water replenishing through dual-waveband ultraviolet light catalysis advanced treatment. Compared with the prior art, the method has the advantages of good treatment effect and simple process flow.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (16)
1. A method for treating and recycling cold coke wastewater comprises the following steps:
A. the cold coke water enters an oil separation unit to remove floating oil and large-particle coke powder in the cold coke wastewater;
B. the wastewater after oil removal enters a reuse pretreatment unit to further remove petroleum and suspended matters;
C. part of the effluent of the pretreatment unit passes through a cooling unit, and is cooled and recycled;
D. and the effluent of the other part of the cooling unit enters a double-waveband ultraviolet light catalysis unit for advanced treatment.
2. The method according to claim 1, wherein the oil separation unit of step A adopts a semi-sealed oil separation tank, and the tail gas is provided with a lye absorption device.
3. The method according to claim 1, wherein the recycling pretreatment unit of the step B adopts adsorption and/or flocculation treatment.
4. The method according to claim 3, wherein the adsorbent used in the adsorption mode is an activated carbon adsorbent prepared from petroleum coke.
5. The method according to claim 4, wherein the adsorbent has a specific surface area of 700 to 900m2The total pore volume is 0.33-0.43 cm3Per g, wherein the volume of the micropore volume is 0.29-0.38 cm3/g。
6. The method of claim 4, wherein the adsorbent is prepared by: the method comprises the steps of taking petroleum coke as a raw material, taking an activating agent as potassium hydroxide, grinding and screening the petroleum coke into 50-100 meshes, then uniformly mixing the petroleum coke with the activating agent, carrying out an activation reaction under a nitrogen atmosphere, cooling, washing to be neutral, and drying to obtain an adsorbent, wherein the reaction temperature of the activation reaction is 750-850 ℃, the reaction time is 1-3 h, and the mass ratio of the petroleum coke to the activating agent is 1:2 to 5.
7. A process according to any one of claims 4 to 6, wherein the adsorbent is used in an amount of 50 to 100 mg/L.
8. The method according to claim 3, wherein the flocculating agent used in the flocculation mode is selected from at least one of aluminum chloride, polyaluminum chloride, ferric chloride, polyferric chloride, ferric sulfate, polyferric sulfate, aluminum sulfate and polyaluminum sulfate.
9. The method according to claim 8, wherein the amount of the flocculant is 50 to 500 mg/L.
10. The method according to claim 3, wherein a coagulant aid polyacrylamide is further added, and the dosage of the coagulant aid is 0-10 mg/L.
11. The method according to claim 3, wherein, when the adsorption flocculation coupling treatment mode is selected, the dosage ratio of the adsorbent to the flocculating agent is 1:2 to 5.
12. The process of claim 1, wherein in the cooling unit of step C, the heat exchanger is selected from one or more of air-cooled heat exchangers, shell-and-tube heat exchangers, plate-fin heat exchangers, and spiral plate heat exchangers.
13. The method according to claim 1, wherein in the cooling unit of step C, a part of the effluent of the pretreatment unit is returned to the coke cooling operation after the temperature is reduced to be less than or equal to 40 ℃.
14. The method as claimed in claim 1, wherein the dual band uv light catalyzing unit of step D is provided with 1-3 stages of photocatalytic reactors, each stage being provided with a dual band uv lamp tube, generating uv light of less than 200nm and 254 nm.
15. The method according to claim 1, wherein in the step D, an oxidant is selectively added into the photocatalytic reactor, the oxidant is selected from one or more of hydrogen peroxide, sodium persulfate and ozone, and the adding amount of the oxidant is 100-800 mg/L.
16. The method according to claim 1, wherein the quality of the coke cooling water is as follows: COD is 100-1300 mg/L, benzopyrene is 0.5-180 mu g/L, petroleum is 10-850 mg/L, turbidity is 100-2000 NTU, and conductivity is less than or equal to 1200 mu S/cm.
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