WO2015123825A1 - Purification assistant for coal chemical industry production, and uses thereof in coal chemical industry production - Google Patents
Purification assistant for coal chemical industry production, and uses thereof in coal chemical industry production Download PDFInfo
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- WO2015123825A1 WO2015123825A1 PCT/CN2014/072252 CN2014072252W WO2015123825A1 WO 2015123825 A1 WO2015123825 A1 WO 2015123825A1 CN 2014072252 W CN2014072252 W CN 2014072252W WO 2015123825 A1 WO2015123825 A1 WO 2015123825A1
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- WO
- WIPO (PCT)
- Prior art keywords
- purification
- coal tar
- coal
- water
- aid
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G33/00—Dewatering or demulsification of hydrocarbon oils
- C10G33/04—Dewatering or demulsification of hydrocarbon oils with chemical means
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/02—Removal of water
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/30—Physical properties of feedstocks or products
- C10G2300/302—Viscosity
Definitions
- the present invention relates to the field of coal chemical production, and in particular to a purification aid for coal chemical production and its application in coal chemical production.
- BACKGROUND OF THE INVENTION In the coal chemical production industry, the degree of separation of coal tar suspended in ammonia water and phenol water is an important indicator of concern in the production of gasification plants and coking plant chemical production plants. If the separation of coal tar in ammonia or phenol water is not good, it will not only affect the production of coal tar in the liquid product separation system, but also affect the recovery system of ammonia water and phenol water, resulting in fouling of the tray in the recovery system, increasing the cleaning. The maintenance cost of the trays makes the production impossible, and the production cost is increased.
- a purification aid for coal chemical production which comprises 90 to 99 parts of oleylamine polyoxyethylene ether and 1 to 5 parts of aliphatic amine by weight. . Further, in parts by weight, 94 to 99 parts of oleyl polyoxyethylene ether and 1 to 3 parts of fatty amine are included. Further, 99 parts of oleyl polyoxyethylene ether and 1 part of a fatty amine are included in parts by weight.
- the fatty amine is selected from one or more of a fatty primary amine, a secondary fatty amine, a fatty tertiary amine, and a fatty polyamine, preferably a primary fatty amine.
- the oleylamine polyoxyethylene ether is oleylamine polyoxyethylene ether 5EO ⁇ 20EO. According to another aspect of the present invention, there is provided the use of any of the above-described purification aids for coal chemical production in coal chemical production. Further, a purification aid is added to the suction port of the circulating water pump of the recycling cycle system in the coal chemical production. Further, a purifying aid is added to the recycling system by using a high-pressure metering pump at the suction port of the circulating water pump.
- a purification aid is added to the recycling cycle system in the coal chemical production by successively increasing the addition manner.
- the successive incremental addition manners include: Sl, adding a purification aid consuming 1 ⁇ 3 ppm of circulating water in the recycling circulation system to the recycling cycle system for 10 to 15 days; S2, adding to the recycling cycle to the recycling cycle The purification agent with a circulating water volume of 3 ⁇ 5ppm in the system is kept for 25 ⁇ 30 days; and S3, the purification auxiliary agent which accounts for 5 ⁇ 10ppm of circulating water in the recycling system is added to the recycling system until the circulating water in the recycling system The coal tar content has dropped to 20% to 30%.
- the purification auxiliary consisting of oleylamine polyoxyethylene ether and fatty amine provided by the invention is added to the recycling circulation system of the coal chemical production process to purify the circulating water, because the purification auxiliary can The small liquid bead of the dispersed phase of the emulsion is aggregated to form a large droplet, and finally the oil and water in the circulating water are separated into two phases to thereby purify the object. Therefore, the purification auxiliary can effectively remove the coal chemical production process.
- the coal tar and coal dust contained in ammonia water, phenol water and waste gas are high-efficiency products that can reduce the viscosity of coal tar and reduce the moisture content of oil. The specific effects are as follows:
- FIG. 1 is a schematic flow chart of an ammonia water recovery cycle system in a coal chemical production process according to an exemplary embodiment of the present invention.
- the specific lung type needs to be described that the features in the embodiments and the embodiments in the present application can be combined with each other without conflict.
- the invention will be described in detail below with reference to the embodiments.
- the invention provides a purification aid for coal chemical production, which comprises 90-98 parts of oleylamine polyoxyethylene ether and 1 to 5 parts by weight. Fatty amine.
- the purification auxiliary consisting of oleylamine polyoxyethylene ether and fatty amine provided by the invention is added to the recycling cycle system of the coal chemical production process to purify the circulating water, since the purification auxiliary agent can disperse the dispersed phase of the emulsion
- the coal tar and coal dust contained in it are high-efficiency products that can reduce the viscosity of coal tar and reduce the moisture content of oil. The specific effects are as follows:
- the frequency of cleaning the system improves the processing effect of the equipment, prolongs the service life of the equipment, so that the production will not be reduced due to maintenance and maintenance equipment, ensuring the maximum economic benefits of the enterprise, and ensuring the safe production of each workshop; 5) Reduce the COD and phenol content in the gasification wastewater, and have a positive effect on maintaining COD stability, while the odor is also significantly reduced, bringing great environmental benefits; at the same time cleaning the waste gas, reducing the load of the waste gas purification system It is beneficial to improve the quality of the end products; 6) avoiding the fouling of each tray in the coal production system, saving steam consumption; reducing the deposition of coal tar on the production system and improving the heat transfer of each system The effect ensures continuity of production at the optimum design value.
- the purification aid comprises 98 parts oleyl polyoxyethylene ether and 1 to 3 parts of a fatty amine in parts by weight.
- the purification aid comprises 98 parts oleyl polyoxyethylene ether and 1 part fatty amine in parts by weight.
- the oleylamine polyoxyethylene ether has excellent emulsification, dispersion, solubilization, antistatic, lubrication and corrosion inhibition capabilities, and also has a certain bactericidal ability.
- the present invention employs a fatty amine added to oleylamine polyoxyethylene ether because the fatty amine can lower the surface tension of water, increase the solubility of organic compounds, and on the other hand act as a solvent.
- the fatty amine used in the present invention refers to a large class of organic amine compounds having a carbon chain length in the range of C 8 to C 12 .
- the fatty amine is selected from the group consisting of primary aliphatic amines and secondary fatty amines.
- One or more of a fatty tertiary amine and a fatty polyamine are preferably primary fatty amines.
- the type of fatty primary amine, fatty secondary amine and fatty tertiary amine depends on the number of hydrogen atoms in the amine which are substituted by thiol groups. It is preferred to use primary aliphatic amines mainly considering the addition of fatty primary amines to ethylene oxime.
- the oleylamine polyoxyethylene ether used in the present invention is also a nonionic surfactant-polyether-amine polycondensation, and a good synergy between the primary aliphatic amine and the oleylamine polyoxyethylene ether.
- the role of the use of fatty secondary amines has the commonalities and advantages of other fatty secondary amines, fatty tertiary amines and fatty polyamines.
- the invention combines oleylamine polyoxyethylene ether with fatty amine in a certain ratio to obtain a purification auxiliary agent with better functions of demulsification, dispersion, viscosity reduction, dehydration and flocculation, and the purification auxiliary agent Applied to the recycling system of coal chemical production, coal tar in ammonia water or phenol water can be separated well, and the moisture content in the separated coal tar is the lowest.
- the purification aid is used for demulsification purification of ammonia or phenol water in coal chemical production, the demulsification temperature is generally above 70 °C.
- the oleylamine polyoxyethylene ether may be a commercially available product, or may be synthesized by a conventional method using oleylamine and epoxy oxime as a raw material, and in view of demulsification and dispersion effect, it is preferably used in a purity of 95% to 99%.
- Oil amine is used as a raw material for synthetic oleylamine polyoxyethylene ether.
- the present invention uses oleylamine polyoxyethylene ether 5EO ⁇ 20EO mixed with a fatty amine, and applies the purification aid obtained after mixing to the coal chemical production, which can more effectively remove the coal chemical production process. Coal tar and coal dust contained in ammonia water, phenol water and waste gas.
- the purification aid obtained by the technical scheme of the invention has the following characteristics: deep amber to pale yellow liquid, odorless, flash point ⁇ 90.5 °C and pour point ⁇ -12.3 ° C, at standard atmospheric pressure and 15.6 ° C, The ratio of the specific gravity of the purification aid to water is 0.95 0.99, and the viscosity is 1045 to 1067 Pa*S. According to another aspect of the present invention, there is provided the use of any of the above-described purification aids for coal chemical production in coal chemical production.
- the purification aid can be added to any system in the coal chemical production as needed, in order to better remove the coal tar and coal dust in the ammonia water and the phenol water, preferably, the circulating water pump suction in the recovery circulation system in the coal chemical production Add a purification aid to the mouth.
- a purification aid is added to the recovery cycle system by using a high-pressure metering pump at the suction port of the circulating water pump.
- the invention adds the purification aid to the circulating water (ammonia or phenol water) recovery circulation system by using a high-pressure metering pump in the circulating water (ammonia or phenol water) pump suction port, and firstly ensures the continuity of the purification auxiliary addition, so that The coal tar removal is more thorough.
- the high-pressure metering pump is used to continuously pump the purification auxiliaries, which is beneficial to the enterprise to continuously recover the continuously produced coal tar and has higher recovery efficiency.
- the purification aid has a good cleaning effect on the scale deposited in the recycling cycle system, in order to avoid various clogging phenomena caused by rapid cleaning after the addition of the purification aid, it is preferred to adopt a successive incremental addition method to the coal.
- a purification aid is added to the recycling system in the chemical production. By slowly and incrementally adding purification aids at the beginning, the amount of purification aid is gradually increased while analyzing the test data and ensuring that the individual heat exchangers and trays are not clogged.
- the purification aid provided by the invention is applied to the ammonia water or phenol water recovery circulation system in the coal chemical production process, thereby improving the separation degree of coal tar and coal dust in the ammonia water or the phenol water, and effectively solving the ammonia and phenol recovery system.
- the problem of blockage of the trays prolongs the maintenance period and service life of the equipment, and has the advantages of low production cost, low energy consumption and high production safety factor.
- the incrementally increasing adding manner comprises: Sl, adding a purification auxiliary agent that accounts for 1-3 ppm of circulating water in the recycling cycle system to the recycling cycle system for 10 to 15 days; S2, adding to the recycling system for recycling The purification agent with circulating water volume of 3 ⁇ 5ppm in the circulation system is kept for 25 ⁇ 30 days; and S3, the purification auxiliary agent which accounts for 5 ⁇ 10ppm of circulating water in the recycling system is added to the recycling system until the circulating water in the recycling system The coal tar content in the plant has dropped to 20% to 30%.
- the purification agent prepared by the invention has better separation and impurity removal effects according to the following experiments.
- Example 10 In the production process of the gas plant of Zhongmei Longhua Harbin Coal Chemical Co., Ltd., the phenol water was purified by adding the purification aid in the first embodiment of the present invention to the recovery cycle system. The specific process is as follows: The crude gas from the gas plant exits the gas outlet and passes through the circulating water pump to enter the phenol water recovery cycle system of high temperature phenol water spray. In the phenol water recycling phenol water recycling cycle system, the high-pressure metering pump is used to add the purification assistant to the phenol water recovery circulation system in a manner of increasing the amount of addition at the suction port of the circulating water pump.
- the specific addition method is as follows: First, the recovery method is as follows: Adding 3 ppm of phenolic water circulation purification agent to the recycling system for 15 days; secondly, adding 5 ppm of phenolic water circulation purification agent to the recycling system for 30 days; A purification aid which accounts for 10 ppm of phenol water circulation in the circulation system is added to the recovery cycle system until the coal tar content in the phenol water circulating water volume in the recovery cycle system is reduced to 20%.
- the phenol water added to the purification aid passes through the heat exchanger (remaining heat recovery) --- - casing heat exchanger --- tube heat exchanger -- flash tank -- -- - - coal Tar phenol water separator ----heat exchanger --- -- light oil separator --- -- buffer tank --- --- oil water filter (also known as dual media filter) --...large Storage tanks...-light oil separators...air flotation devices...large buffer tanks...-deacidification towers...-heat exchangers...deamination towers...-heat exchangers...extraction...heat exchangers...distilled water Tower... - - Biochemical treatment.
- Example 11 The operation steps and methods were the same as those in Example 10 except that the purification aid prepared in Example 3 was used in Example 11, and the content of the purification assistant added was different, as follows: In the production process of the gas generating plant of Harbin Coal Chemical Co., Ltd., the phenol water is purified by adding the purification aid in the third embodiment of the present invention to the recycling cycle system.
- the specific process is as follows: The crude gas from the gas plant exits the gas outlet and passes through the circulating water pump into the phenol water recovery cycle system of high-temperature phenol water spray. In the phenol water recovery cycle system of high-temperature phenol water spray, the inhalation of the circulating water pump The high-pressure metering pump is used to add the purification aid to the phenol water recovery cycle system in increments of the added amount.
- the specific addition method is as follows:
- the phenol water added to the purification aid passes through the heat exchanger (remaining heat recovery) --- - casing heat exchanger --- tube heat exchanger -- flash tank -- -- - - coal Tar phenol water separator ----heat exchanger --- -- light oil separator --- -- buffer tank --- --- oil water filter (also known as dual media filter) --...large Storage tanks...-light oil separators...air flotation devices...large buffer tanks...-deacidification towers...-heat exchangers...deamination towers...-heat exchangers...extraction...heat exchangers...distilled water Tower... - - Biochemical treatment.
- the conventional oil and fat titration method is used to detect the coal tar content in the phenol water of the coal tar phenol water separator, the oil water filter and the distilled water tower, respectively, wherein the conventional oil and fat titration method is used for the initial coal.
- the coal tar content in the phenol water of the tar phenol water separator, the oil-water filter and the distilled water tower were measured at 2.0 g/L, 1.5 g/L and 3 g/L, respectively, and the maintenance period of the whole set of equipment was 6 months.
- Example 12 The following uses the purification aid of the present invention to carry out on-line purification treatment of the ammonia water recovery cycle in the coal chemical production process, as follows: In the production process of the chemical production recycling workshop of Wuhai Taihe Coal Coking Group Co., Ltd., the present invention will be The purification aid in the embodiment 1 is added to the ammonia water recovery cycle system, wherein FIG.
- 1 is a flow chart of the equipment of the ammonia water recovery cycle system, where 1 represents the primary cooler, 2 represents the gas-liquid separator, 3 represents the waste gas, and 4 represents The remaining ammonia water tank, 5 represents the circulating water pump, 6 represents the ammonia water storage tank, 7 represents the coal tar ammonia water separation large tank, 8 represents the coal tar intermediate tank, and 9 represents the purification aid addition point.
- the ammonia water is circulated between the coal tar ammonia water separation tank 7, the ammonia water tank 6, the circulating water pump 5, the waste gas 3, and the gas-liquid separator 2 to recover and separate the ammonia water and the coal tar contained therein.
- the separated coal tar enters the coal tar intermediate tank 8, and the separated ammonia water enters the remaining ammonia water tank 4.
- the purifying aid is added by the metering pump in a stepwise increment manner at the point of addition of the purifying aid at the suction port of the circulating water pump, and the specific adding manner is as follows: Sl, adding to the recycling loop system at the point of addition of the purifying aid 9
- S2 adding to the recycling loop system at the point of addition of the purifying aid 9
- the purification auxiliaries which account for 3ppm of ammonia circulation in the recycling system are kept for 15 days;
- S2 the purification auxiliaries which account for 5ppm of ammonia circulation in the recovery circulatory system are added to the ammonia circulation system for 30 days;
- S3 to the recycling system
- the ammonia water contains a large amount of suspended solids and coal tar.
- the color of the ammonia water is turbid.
- the color of the ammonia water is transparent pale orange (ammonia color), and the test contains almost no coal. Tar, ammonia is more pure.
- the coal tar finally separated in the first embodiment was tested, and it was found that the separated coal tar moisture content was reduced from 4% to 5% in the prior art without adding a purification aid to 0.6 to 1.0%.
- the purifying agent of the invention can quickly separate the coal tar from the ammonia water in only 60 days, and the separated coal tar has a water content of only 1.6%, which is as high as 85% compared with the prior art.
- the purification aid of the invention has better demulsification and dehydration effects on coal tar in ammonia water, and has high dehydration speed and high efficiency.
- the separated waste gas was detected by a gas chromatograph, and it was found that the waste gas became purer than before. Before the purification aid of the present invention is used, when the electric coal tar is deactivated for half an hour, a large amount of coal tar will flow out in the electric coal tar, and flow to the sulfur tank, when the purification aid of the invention is used.
- Packing benzene tower is an important chemical equipment for recovering crude benzene from waste gas.
- the coal gas in the coal chemical production is not pure, and the coal tar and naphthalene in the waste gas block the filler seriously. , resulting in increased resistance of equipment, up to 1800Pa, making crude benzene production only 15 tons / day, seriously affecting the recovery of crude benzene, causing serious economic losses.
- the purification aid After the purification aid is used, the coal tar content in the waste gas is significantly reduced, and the waste gas is relatively pure, so that the plugged coal tar and naphthalene accumulated on the original packed benzene tower are effectively cleaned, the equipment resistance is reduced to 1000 Pa, and This resistance is maintained at all times and crude benzene production is increased to 19-20 tons/day. It can be seen that the use of the purification aid of the invention greatly reduces the frequency of cleaning the benzene washing tower, reduces the labor intensity of the worker, increases the recovery amount of the crude benzene, and has considerable economic benefits. The cleaning aid of the invention also plays a large role in the cleaning of the pipeline.
- the gas collecting pipe located above the coke oven is often prevented from being sprayed by the coal tar and coal tar slag blocking nozzle.
- the effect is that the artificial clearing nozzle is needed every 3 ⁇ 5 days.
- the frequency of still cleaning is greatly reduced, and the phenomenon that the nozzle is blocked and cannot be sprayed does not occur, and the gate valves and valves are not Manually repaired due to blockage of coal tar and coal tar slag, the separated coal tar slag also became looser and less lustrous, indicating a significant reduction in oil content.
- the purification aid of the present invention Before the purification aid of the present invention is used, a certain amount of coal tar is excluded periodically (for example, every week) under the ammonia distillation tower, and the ammonia distillation tower is treated for 60 days by adding a purification aid, and it is not necessary to exclude coal tar.
- the COD chemical oxygen absorption
- the COD of the wastewater is 200 mg/L, and after purification treatment, the COD of the wastewater is controlled between 100 and 150 mg/L, which is reduced by nearly 25%. 50%.
- the use of the purification aid of the invention not only reduces the moisture content in the coal tar, but also increases the coal tar yield: before the purification aid of the invention is used, the coal tar recovery ratio is 0.033, and the purification aid of the invention is used for 60 days.
- the coal tar recovery ratio is increased to 0.0342.
- the coal tar output of 2,000 tons per month the coal tar has a moisture content of 4% and the average moisture content of coal tar is 0.9%. (The monthly output of coal tar has not changed)
- the average moisture content of coal tar decreased by 3.1%.
- the decrease of coal tar moisture content in the case of constant coal tar production means an increase in coal tar production.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113604263A (en) * | 2021-08-24 | 2021-11-05 | 周晓宇 | Method for preparing coal briquette from coking waste residues |
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US20070111903A1 (en) * | 2005-11-17 | 2007-05-17 | General Electric Company | Separatory and emulsion breaking processes |
CN102249383A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Compound degreasing agent for removing tar oil from residual ammonia water of coked wastewater |
CN102839007A (en) * | 2011-06-24 | 2012-12-26 | 上海宝钢化工有限公司 | Demulsification, neutralization and dehydration method of acidic emulsified tar |
CN103801114A (en) * | 2014-02-19 | 2014-05-21 | 张征北 | Purification assistant for coal chemical industry production and application thereof in coal chemical industry production |
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2014
- 2014-02-19 WO PCT/CN2014/072252 patent/WO2015123825A1/en active Application Filing
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US4729832A (en) * | 1986-04-21 | 1988-03-08 | Kerr-Mcgee Chemical Corporation | Method for removal of coal tar based contaminants from waste waters |
US20070111903A1 (en) * | 2005-11-17 | 2007-05-17 | General Electric Company | Separatory and emulsion breaking processes |
CN102249383A (en) * | 2011-05-06 | 2011-11-23 | 清华大学 | Compound degreasing agent for removing tar oil from residual ammonia water of coked wastewater |
CN102839007A (en) * | 2011-06-24 | 2012-12-26 | 上海宝钢化工有限公司 | Demulsification, neutralization and dehydration method of acidic emulsified tar |
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