CN107445330B - Low-cost MTO alkaline washing waste alkali liquid zero-emission treatment process - Google Patents

Low-cost MTO alkaline washing waste alkali liquid zero-emission treatment process Download PDF

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CN107445330B
CN107445330B CN201610377730.2A CN201610377730A CN107445330B CN 107445330 B CN107445330 B CN 107445330B CN 201610377730 A CN201610377730 A CN 201610377730A CN 107445330 B CN107445330 B CN 107445330B
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alkali liquor
oil
waste
waste alkali
washing
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CN107445330A (en
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段波
潘珂
陈海
王振维
赵百仁
雷正香
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Sinopec Engineering Inc
Sinopec Engineering Group Co Ltd
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Sinopec Engineering Group Co Ltd
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/96—Regeneration, reactivation or recycling of reactants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/30—Alkali metal compounds
    • B01D2251/304—Alkali metal compounds of sodium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/60—Inorganic bases or salts
    • B01D2251/604—Hydroxides
    • 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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • 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
    • 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
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

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  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Biomedical Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Sustainable Development (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Hydrology & Water Resources (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Physical Water Treatments (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The invention provides a low-cost MTO alkaline washing waste alkali liquor zero-emission treatment process, which comprises the following steps: (1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil, preliminarily removing oil carried in the waste alkali liquor, and then carrying out reduced pressure treatment; (2) standing the storage tank: preliminarily removing oils and waste alkali liquor after pressure reduction treatment, standing in a storage tank, and further removing floating oil after oil and water are layered; (3) removing carbonate: adding a carbonate precipitator into the waste alkali liquor after standing for deoiling for precipitation reaction, and removing the precipitate in the waste alkali liquor after standing for layering; (4) alkali liquor regeneration: and adding sodium hydroxide into the waste alkali liquor from which the carbonate is removed to regenerate the alkali liquor. Through the treatment process, sodium hydroxide can be recycled, zero discharge of waste alkali liquor treatment is realized, the use amount of the alkali liquor is greatly reduced, and the environmental protection pressure is reduced.

Description

Low-cost MTO alkaline washing waste alkali liquid zero-emission treatment process
Technical Field
The invention relates to the field of petrochemical wastewater treatment, and particularly relates to a low-cost MTO alkaline washing waste lye zero-discharge treatment process.
Background
The product gas of the MTO device contains CO2When the acid gas is equal, the technological process requires the CO in the product gas to be removed2Is removed to 10-6(VOL) below. At present, an alkaline washing tower is widely adopted to remove CO by a method of washing product gas by NaOH solution2. In the washing processThe acid gas and NaOH are chemically reacted to remove the acid gas and generate waste lye.
Unlike the waste lye generated by an ethylene plant, the MTO waste lye does not contain sulfur, but contains organic oxides such as dimethyl ether, methanol and the like. The existence of organic matters can cause the COD of the waste alkali liquor to be very high, and in the subsequent treatment process, the organic oxides are difficult to degrade by adopting the traditional biochemical sewage treatment, thereby bringing great environmental protection pressure to the operation of the device. If the organic matters in the waste alkali liquor can be removed to reduce COD, the waste alkali liquor can be directly neutralized and then sent to a sewage plant of a whole plant for treatment.
At present, the treatment method of domestic waste lye (slag) mainly comprises four major methods, namely an incineration method, a neutralization method, an oxidation method and a biological treatment method.
The incineration method belongs to a direct treatment method, and organic substances are made to generate CO at high temperature and normal pressure2And H2Conversion of O, NaOH to Na2CO3The sulphate and carbonate remain dissolved in the treated waste stream. The method is a feasible processing method and is simple to operate. The disadvantages are high energy consumption and high operation cost; meanwhile, sodium carbonate formed by combustion can seriously corrode refractory materials in the furnace at high temperature, and is easy to scale in quenching equipment and pipelines. The method needs to establish a whole set of complex flue gas treatment process to meet the standard emission requirement of flue gas. Therefore, the use of incineration is limited.
Neutralization method for neutralizing CO by concentrated sulfuric acid2The neutralization method is representative. The sulfuric acid consumption in the concentrated sulfuric acid neutralization method is high, the economic cost is high, and the corrosion to equipment is serious. CO 22The neutralization process requires stable CO2The gas source is not easy to provide in general petrochemical plants.
Oxidation processes include wet oxidation (WAO) and catalytic wet oxidation (CWAO); the MTO waste alkali liquor does not contain sulfur, so WAO and CWAO are not applicable when the MTO waste alkali liquor is treated.
The biological treatment method is represented by a QBR (quick Bioreactor) high concentration wastewater treatment technique and a Korean SK bio-augmentation technique, and is a bio-oxidation technique. The biological treatment process inevitably has the defects of long flow, large occupied area, low treatment efficiency, higher operation cost (needing to supplement strains periodically) and the like, and limits the application of a biological method to a certain extent. Meanwhile, a certain amount of sludge is generated by using a biological method, and the treatment of the sludge is increasingly limited.
In conclusion, for MTO waste lye, various treatment methods at present have the problems of inapplicability, large investment, high operating cost, low efficiency and the like.
Disclosure of Invention
The invention aims to provide a low-cost MTO alkaline washing waste alkali liquor zero-emission treatment process, aiming at the characteristics of no sulfur in MTO waste alkali liquor, high organic matter content and the like, the waste alkali liquor is regenerated while the organic matter content in the MTO waste alkali liquor is reduced at high efficiency and low cost, and is continuously used for an alkaline tower to remove acid gas, so that the high-efficiency zero-emission treatment and the cyclic utilization of the MTO waste alkali liquor are realized.
In order to achieve the aim, the invention provides a low-cost MTO alkaline washing waste lye zero-emission treatment process, which comprises the following steps:
(1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil to primarily remove oil carried in the waste alkali liquor; carrying out pressure reduction treatment on the waste alkali liquor after oil washing to reduce the pressure to 0.15 MPaG-torch pressure;
(2) standing the storage tank: preliminarily removing oils and waste alkali liquor after pressure reduction treatment, standing in a storage tank, and further removing floating oil after oil and water are layered;
(3) removing carbonate: adding a carbonate precipitator into the waste alkali liquor after standing for deoiling for precipitation reaction, and removing the precipitate in the waste alkali liquor after standing for layering;
(4) alkali liquor regeneration: and adding sodium hydroxide into the waste alkali liquor from which the carbonate is removed to regenerate the alkali liquor.
In the step (1), the oil washing is to inject washing oil into the waste alkali liquor, the oil in the waste alkali liquor is primarily dissolved into the washing oil by utilizing the different solubility of the washing oil and the waste alkali liquor to the oil in the waste alkali liquor, and the washing oil and the waste alkali liquor are separated by standing and layering, so that the purpose of deoiling the waste alkali liquor is achieved. According to the treatment process provided by the invention, preferably, in the step (1), the wash oil is benzene-containing gasoline.
The pressure of the waste alkali liquor from the alkaline tower is about 0.5-1.8MPaG, and according to the treatment process provided by the invention, preferably, in the step (1), the pressure of the oil-washed waste alkali liquor is reduced to 0.08 MPaG-torch pressure (about 0.05 MPaG). The pressure is reduced, the solubility of the hydrocarbon in the waste alkali liquor is reduced, the dissolved gaseous hydrocarbon can be removed, and a small amount of organic oxide can be extracted. After oil washing and degassing, the organic content in the waste alkali solution can be reduced from about 6000-10000mg/l to about 2000-4500 mg/l.
In the step (2), the waste alkali liquor needs to be kept still in the storage tank for enough time to separate oil from water so as to remove free oil. In addition to consideration of the standing residence time of oil-water separation, it is also necessary to consider the fluctuation of the operation load of the MTO main unit and the buffering time for the overhaul of the waste lye treatment apparatus. According to the treatment process provided by the invention, preferably, in the step (2), the retention time of the waste lye in the storage tank is 5-10 days, and more preferably 6-8 days.
In order to make small oil particles in the waste lye sufficiently coalesce into larger oil drops to ensure the oil removing effect, according to the treatment process provided by the invention, preferably, in the step (2), the waste lye is further removed with free oil through a coalescer after oil-water separation in the storage tank.
In the step (3), inorganic matters in the waste alkali liquor after standing treatment only contain NaOH and Na basically2CO3The carbonate precipitant is added to remove carbonate and increase the concentration of NaOH. In step (3), preferably, the carbonate precipitating agent is selected from calcium oxide and/or calcium hydroxide. According to Na2CO3The concentration determines the amount of calcium oxide or calcium hydroxide, sodium carbonate reacts with calcium hydroxide to generate sodium hydroxide and calcium carbonate precipitate, and the carbonate removal rate can reach over 99 percent. The reaction equation is:
Na2CO3+Ca(OH)2→2NaOH+CaCO3↓。
in the step (4), inorganic matters in the waste alkali liquor without the carbonate only contain NaOH, and trace amount of other inorganic matters does not influence the use of the regenerated alkali liquor. At the moment, solid sodium hydroxide or fresh sodium hydroxide solution with certain concentration is added into the waste alkali liquor, and the concentration of the sodium hydroxide in the regenerated waste alkali liquor is controlled to be consistent with the concentration required by the alkaline washing tower. The concentration of sodium hydroxide needed in the alkaline tower is 5-15 wt%, and the generated regenerated sodium hydroxide solution can be continuously used for the upstream alkaline tower to realize recycling.
Because the waste lye treated by the process can be recycled, even a small amount of organic oxide is contained in the waste lye, the yellow oil in the alkaline washing tower can be generated, but because the materials are recycled, the accumulated organic oxide with certain concentration can be removed by oil washing in the step (1), the content balance of the organic oxide is finally realized, and the yellow oil is continuously discharged due to the recycling of the lye.
The technical scheme of the invention has the following beneficial effects:
1. after the treatment by the process, the sodium hydroxide can be recycled, so that the zero emission of the waste alkali liquor treatment is realized, the use amount of the alkali liquor is greatly reduced, and the environmental protection pressure is reduced;
2. the invention can realize that fresh alkali liquor is added without an alkaline washing unit of an MTO device, does not need related equipment facilities, and reduces investment and occupied land;
3. the auxiliary conditions used by the method are common washing oil, steam, nitrogen and the like, and are easily obtained by a common factory;
4. the process operating conditions are mild, the equipment is made of carbon steel or stainless steel, and the cost is low;
5. calcium carbonate generated by the waste alkali liquor is solid waste, and the treatment is relatively easy;
6. the acid-base neutralization process is not needed, and the use of dangerous chemicals of sulfuric acid and the corrosion of equipment are avoided.
Drawings
FIG. 1 shows a flow chart of a treatment process for zero emission of low-cost MTO alkaline washing waste lye.
The numbers in the figures illustrate the following:
1-oil washing and degassing; 2-standing the storage tank; 3-carbonate removal; 4-regeneration of alkali liquor.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While the preferred embodiments of the present invention are shown in the drawings, it should be understood that the present invention may be embodied in various forms and should not be limited to the embodiments set forth herein.
Example 1
A strand of waste lye discharged from the bottom of the MTO alkaline washing tower, wherein: COD is 8000mg/l, Na2CO3The concentration was 7.6 wt%, the NaOH concentration was 1.6 wt%, the free oil content was 250mg/l, the methanol concentration was 0.03 mol%, and the dimethyl ether concentration was 0.01 mol%.
The processing flow chart shown in fig. 1 is adopted, and the processing steps are as follows:
(1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil according to different solubilities, and separating the washing oil from the waste alkali liquor by standing and layering to preliminarily remove oil carried in the waste alkali liquor; carrying out reduced pressure treatment on the waste alkali liquor after oil washing to reduce the pressure from 1.4MPaG to 0.05 MPaG; after oil washing and degassing, the oil content and the dissolved organic matter content in the waste alkali liquor are reduced to about 4000 mg/l;
(2) standing the storage tank: standing the preliminarily removed oil and the decompressed waste alkali liquor in a storage tank for 6 days; after the oil and water are layered, further removing floating oil by oil skimming;
(3) removing carbonate: according to Na2CO3The concentration of the sodium hydroxide is increased to 6 wt%, and the removal rate of carbonate can reach more than 99%;
(4) alkali liquor regeneration: adding 20 wt% of fresh sodium hydroxide solution into the waste alkali liquor without carbonate to regenerate the alkali liquor, and controlling the concentration of the sodium hydroxide in the regenerated waste alkali liquor to be consistent with the concentration of 10 wt% required by the alkaline washing tower.
Through the process treatment, even if organic oxides are contained in the waste alkali liquor, the grease in the alkaline washing tower can be generated, but because of material circulation, the accumulated organic oxides with certain concentration can be removed through oil washing in the step (1), the content balance of the organic oxides is finally realized, and the grease is continuously discharged due to alkali liquor circulation. Can realize the recycling of the alkali liquor.
Example 2
A strand of waste lye discharged from the bottom of the MTO alkaline washing tower, wherein: COD was 15000mg/l, Na2CO3The concentration was 6.7 wt%, the NaOH concentration was 1.5 wt%, the free oil was 1000mg/l, the methanol concentration was 0.04 mol%, and the dimethyl ether concentration was 0.02 mol%.
The processing flow chart shown in fig. 1 is adopted, and the processing steps are as follows:
(1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil according to different solubilities, and separating the washing oil from the waste alkali liquor by standing and layering to preliminarily remove oil carried in the waste alkali liquor; carrying out reduced pressure treatment on the waste alkali liquor after oil washing to reduce the pressure from 1.3MPaG to 0.05 MPaG; after oil washing and degassing, the oil content and the dissolved organic matter content in the waste alkali liquor are reduced to about 4000 mg/l;
(2) standing the storage tank: standing the preliminarily removed oil and the decompressed waste alkali liquor in a storage tank for 8 days; removing floating oil by skimming after oil and water are layered;
(3) removing carbonate: according to Na2CO3The concentration of the sodium hydroxide is increased to 5 wt%, and the removal rate of carbonate can reach more than 99%;
(4) alkali liquor regeneration: adding 20 wt% of fresh sodium hydroxide solution into the waste alkali liquor without carbonate to regenerate the alkali liquor, and controlling the concentration of the sodium hydroxide in the regenerated waste alkali liquor to be consistent with the concentration of 10 wt% required by the alkaline washing tower.
Through the process treatment, even if organic oxides are contained in the waste alkali liquor, the grease in the alkaline washing tower can be generated, but because of material circulation, the accumulated organic oxides with certain concentration can be removed through oil washing in the step (1), the content balance of the organic oxides is finally realized, and the grease is continuously discharged due to alkali liquor circulation. Can realize the recycling of the alkali liquor.
Example 3
A strand of waste lye discharged from the bottom of the MTO alkaline washing tower, wherein: COD is 8000mg/l, Na2CO3The concentration was 7.6 wt%, the NaOH concentration was 1.6 wt%, the free oil content was 250mg/l, the methanol concentration was 0.03 mol%, and the dimethyl ether concentration was 0.01 mol%.
The processing flow chart shown in fig. 1 is adopted, and the processing steps are as follows:
(1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil according to different solubilities, and separating the washing oil from the waste alkali liquor by standing and layering to preliminarily remove oil carried in the waste alkali liquor; carrying out reduced pressure treatment on the waste alkali liquor after oil washing to reduce the pressure from 1.4MPaG to 0.1 MPaG; after oil washing and degassing, the oil content and the dissolved organic matter content in the waste alkali liquor are reduced to about 5000 mg/l;
(2) standing the storage tank: standing the preliminarily removed oil and the decompressed waste alkali liquor in a storage tank for 6 days; removing floating oil by skimming after oil and water are layered;
(3) removing carbonate: according to Na2CO3The concentration of the sodium hydroxide is increased to 5 wt%, and the removal rate of carbonate can reach more than 99%;
(4) alkali liquor regeneration: adding 20 wt% of fresh sodium hydroxide solution into the waste alkali liquor without carbonate to regenerate the alkali liquor, and controlling the concentration of the sodium hydroxide in the regenerated waste alkali liquor to be consistent with the concentration of 10 wt% required by the alkaline washing tower.
Comparative example 1
A strand of waste lye discharged from the bottom of the MTO alkaline washing tower, wherein: COD is 8000mg/l, Na2CO3The concentration was 7.6 wt%, the NaOH concentration was 1.6 wt%, the free oil content was 250mg/l, the methanol concentration was 0.03 mol%, and the dimethyl ether concentration was 0.01 mol%.
The processing flow chart shown in fig. 1 is adopted, and the processing steps are as follows:
(1) degassing: carrying out decompression treatment on the waste alkali liquor to reduce the pressure from 1.4MPaG to 0.05 MPaG; the oil content and the dissolved organic matter content in the waste alkali liquor are reduced to about 7000mg/l after degassing;
(2) standing the storage tank: standing the decompressed waste alkali liquor in a storage tank for 6 days; removing floating oil by skimming after oil and water are layered;
(3) removing carbonate: according to Na2CO3The concentration of the sodium hydroxide is increased to 6 wt%, and the removal rate of carbonate can reach more than 99%;
(4) alkali liquor regeneration: adding 20 wt% of fresh sodium hydroxide solution into the waste alkali liquor without carbonate to regenerate the alkali liquor, and controlling the concentration of the sodium hydroxide in the regenerated waste alkali liquor to be consistent with the concentration of 10 wt% required by the alkaline washing tower.
The spent lye of comparative example 1 was treated according to the treatment process of example 1 except that no oil wash step was used. After treatment, the organic matter content is removed to below 7000mg/l, and the concentration of sodium hydroxide in the waste alkali liquor can reach the concentration of 10 wt% required by the alkaline washing tower. However, without the oil washing step, organic oxides contained in the waste lye can be accumulated, and simultaneously, a large amount of butter can be generated in the alkali washing tower, and the organic matters and the butter cannot be discharged out of the system. Therefore, the recycling of the alkali liquor cannot be realized, and zero emission cannot be achieved.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.

Claims (6)

1. A low-cost MTO alkaline washing waste alkali liquid zero-emission treatment process is characterized by comprising the following steps:
(1) oil washing and degassing: washing MTO waste alkali liquor by using washing oil to primarily remove oil carried in the waste alkali liquor; carrying out reduced pressure treatment on the oil-washed waste alkali liquor to reduce the pressure to 0.15 MPaG-0.05 MPaG; the wash oil is benzene-containing gasoline;
(2) standing the storage tank: preliminarily removing oils and waste alkali liquor after pressure reduction treatment, standing in a storage tank, and further removing floating oil after oil and water are layered;
(3) removing carbonate: adding a carbonate precipitator into the waste alkali liquor after standing for degreasing to perform precipitation reaction, so that the concentration of sodium hydroxide is increased to 5-6 wt%, and removing the precipitate in the waste alkali liquor after standing for layering;
(4) alkali liquor regeneration: and adding sodium hydroxide into the waste alkali liquor from which the carbonate is removed to regenerate the alkali liquor.
2. The low-cost zero-emission treatment process of MTO alkaline washing waste lye as claimed in claim 1, wherein in the step (1), the waste lye after oil washing is subjected to pressure reduction treatment to reduce the pressure to 0.08MPaG to 0.05 MPaG.
3. The low-cost zero emission treatment process of MTO caustic wash spent lye of claim 1, wherein in step (2) the spent lye is further freed from oils by a coalescer after separation of the oil from the water in the storage tank.
4. The low-cost zero-emission treatment process of MTO alkaline washing waste lye as claimed in claim 1, wherein in the step (2), the retention and standing time of the waste lye in the storage tank is 5-10 days.
5. The low-cost zero-emission treatment process of MTO alkaline washing waste lye as claimed in claim 4, wherein in the step (2), the retention and standing time of the waste lye in the storage tank is 6-8 days.
6. The low-cost zero emission treatment process of MTO alkaline washing spent lye as claimed in any one of the claims 1 to 5 wherein in step (3) the carbonate precipitating agent is selected from calcium oxide and/or calcium hydroxide.
CN201610377730.2A 2016-05-31 2016-05-31 Low-cost MTO alkaline washing waste alkali liquid zero-emission treatment process Active CN107445330B (en)

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