CN108299593A - A kind of method of preparation and use of ammonium hydroxide detersive - Google Patents

A kind of method of preparation and use of ammonium hydroxide detersive Download PDF

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Publication number
CN108299593A
CN108299593A CN201711416257.5A CN201711416257A CN108299593A CN 108299593 A CN108299593 A CN 108299593A CN 201711416257 A CN201711416257 A CN 201711416257A CN 108299593 A CN108299593 A CN 108299593A
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China
Prior art keywords
tar
detersive
ammonia water
ammonia
ammonium hydroxide
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Pending
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CN201711416257.5A
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Chinese (zh)
Inventor
马凯
程晓婷
李洪社
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Weihai Xiang Ze New Mstar Technology Ltd
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Weihai Xiang Ze New Mstar Technology Ltd
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Priority to CN201711416257.5A priority Critical patent/CN108299593A/en
Publication of CN108299593A publication Critical patent/CN108299593A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/52Amides or imides
    • C08F220/54Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
    • C08F220/56Acrylamide; Methacrylamide
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D17/00Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02Separation of non-miscible liquids
    • B01D17/04Breaking emulsions
    • 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
    • C02F1/54Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
    • C02F1/56Macromolecular compounds

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)

Abstract

The present invention provides a kind of method of preparation and use of coking ammonia water detersive, and the structural formula of the ammonium hydroxide detersive is:

Description

A kind of method of preparation and use of ammonium hydroxide detersive
Technical field
The present invention relates to chemical industry water treatment field, more particularly to a kind of preparation method of coking cycle ammonium hydroxide detersive and make Use method.Background:
1. coke-oven plant uses coal damping STD technologies, the moisture of as-fired coal is reduced and controlled by indirectly heat.Its effect It is coke and the increase of chemical products yield, the raising of coke-stove gas incidence, the gas using quantity reduction of coke oven heating, remained ammonia Amount is reduced.But after coal humidity control device comes into operation, the coal dust entrainment in coal gas obviously increases;If coke oven is using high simultaneously Ammonium hydroxide Anthracite coal is pressed, pressure is higher, and ammonia atomization spray effect is better, and the negative pressure for collecting air flue generation is also bigger, waste coal The dust of gas entrainment is also more serious.Coal dust, coke powder have certain compatibility to grease, cause tar and ammonium hydroxide further newborn Change, it is difficult to sedimentation separation.Cause suspended matter in ammonium hydroxide and tar content rising, cyclic ammonia water spray nozzle clogging, air blower leading Become smaller to adjustable range, transverse pipe initial cooler coal dust tar sticks the deposition of object and naphthalene crystal, cause primary cooler resistance it is high, Ammonia still process column plate and heat exchanger block, and influence coke oven, cold, ammonia still process the normal production of drum.
2, due to tar and ammonium hydroxide difference of specific gravity, on the surface, oil floats on the surface, but due to oxidation, The organic acidic material that a part contains carboxyl (- COOH) can be generated in oil-water mixture, substance of this kind has with the hydroxyl (- OH) in water Affinity interaction is in spherical, is commonly called as Water-In-Oil or oil-in-water, forms stable emulsion, cause cyclic ammonia water oil-water separation Difference, oil content, suspension content and turbidity are very high in cyclic ammonia water.Simultaneously because using coal debugging technique, tar ash content is big, glutinous Degree is high, is easy to bond and formed the tar slag of some bulks after cyclic ammonia water cooling, influences tar quality.In order to break Above-mentioned emulsification system accelerates the separation of tar and ammonium hydroxide, and most efficient method is to accelerate water-oil separating using chemical method at present. The oil content in ammonium hydroxide can be not only reduced in this way while can also reduce the moisture content in tar, and it is stifled to reduce equipment Plug and shortening technological process, save steam and maintenance of equipment expense.
3, the presently used tar ammonia release agent in coke-oven plant can accelerate the separating rate of tar and ammonium hydroxide, significantly reduce burnt Moisture content in oil, but to this emulsifying can be stablized using coal humidifying technology cyclic ammonia water coke powder entrainment height or other The solution (acid tar oil, leakage mother liquor, desulfurization workshop section waste liquid, solid ammonium-salt, crude benzol waste water of ammonium sulfate workshop section etc.) of state imports clarification In the case of slot, ammonium hydroxide and tar relatively difficulty separate.
Invention content
1. the object of the present invention is to provide a kind of preparation and application of coking ammonia water detersive, coordinate nonionic polyoxyalkylene The tar slag reduced while assisting being demulsified in cyclic ammonia water suspended matter, coke powder and tar is added in tar ammonia release agent.
2. to achieve the above object, a kind of coking ammonia water detersive of the invention has following structural formula:
3. high cationic charge density has both certain flocculation ability on the detersive strand, oily packet can be quickly neutralized The negative electrical charge on water/oil-in-water surface layer, compression double electric layer make oil droplets potential reduce, and Distance Shortened between particle makes absorption oil droplet Macromolecular chain interlink, wind and achieve the purpose that De-emulsification flocculent.
4. to achieve the above object, a kind of preparation method of coking ammonia water detersive of the present invention uses following synthetic route
A kind of coking ammonia water detersive, which is characterized in that including following synthesis step:Equipped with thermometer, constant pressure titration Pipe, blender three-necked flask in sequentially add deionized water, EDETATE SODIUM, acrylamide (AM), 60% dimethyl diene Propyl ammonium chloride solution (DMDAAC).Keep bath temperature at 25 DEG C, opening stirring makes material be uniformly mixed, and is adjusted with HCL molten The pH of liquid is 3.5~3.8.Logical nitrogen purges deoxygenation 30min, and redox initiator is added, and during which controls Redox Initiator The speed of agent is added dropwise in 30min.Low temperature causes polymerization 6h at 25 DEG C, reaches expected viscosity and molecular weight, followed by It is continuous to be warming up to 65 DEG C of further aging 2h, add stabilizer after aging and remaining water continue stirring 30min can be obtained it is transparent Gum polymers.
The molar ratio of comonomer AM and DMDAAC described in 5. are 1:0.2~0.4 and the total solid content of monomer maintain 20%.
6. redox initiator used in is ammonium persulfate and sodium hydrogensulfite.
7. stabilizer used in is oxalic acid.
8. to achieve the goals above, a kind of application method of coking ammonia water detersive of the present invention uses following scheme:
9. tar ammonia is added with the adding consistency of 1~3ppm according to cyclic ammonia water amount in the coking ammonia water detersive to mix It closes in object.
10. the coking ammonia water detersive is continuously added to mechanizeding ammonia clarifying groove inlet by dosing metering pump Tar ammonia mixing line on.
Specific implementation mode
The molar ratio of adjustment AM and DMDAAC obtains the polymer of different ions degree and intrinsic viscosity, and design parameter is listed in table 1:
Influences of the table 1AM with DM amount ratios to polymerizeing
The different cationic degree high-efficiency ammonia-water detersives of anthology invention table 1 coordinate the tar ammonia release agent reference oil of my company Content is according to the survey of determination method for oil content and national standard GB11914-89 CODs in national standard SYT 0530-93 oilfield sewages Determine method, specific experiment condition and the results are shown in Table 2.
2 experiment condition of table and result
The tar ammonia release agent of ammonium hydroxide detersive cooperation our company can solve tar ammonia in coal humidifying technology Difficult problem is detached, also has certain booster action to the removal of COD while reducing cyclic ammonia water oil-containing, is recycled reducing The obstruction of ammonia spray nozzle, pipe-line equipment deposition, increases the system tar rate of recovery, reduces the blocking and steaming of follow-up ammonia steaming system column plate There is certain positive effect in terms of the purified treatment difficulty of ammonia waste water.

Claims (7)

1. a kind of coking ammonia water detersive, which is characterized in that its structural formula is:
2. a kind of coking ammonia water detersive, which is characterized in that including following synthesis step:Equipped with thermometer, constant pressure buret, Deionized water, EDETATE SODIUM, acrylamide are sequentially added in the three-necked flask of blender(AM), 60% dimethyl diallyl Ammonium chloride solution(DMDAAC);Keep bath temperature at 25 DEG C, opening stirring makes material be uniformly mixed, and solution is adjusted with HCL PH is 3.5 ~ 3.8;Logical nitrogen purges deoxygenation 30min, and redox initiator is added, and during which controls the speed of redox initiator Degree is added dropwise in 30min;Low temperature causes polymerization 6h at 25 DEG C, reaches expected viscosity and molecular weight, is further continued for heating up To 65 DEG C of further aging 2h, stabilizer is added after aging and remaining water continues stirring 30min and can be obtained transparent glue Polymer.
3. synthetic method according to claim 2, which is characterized in that the molar ratio of the comonomer AM and DMDAAC 1:0.2 ~ 0.4 and the total solid content of monomer maintain 20%.
4. synthetic method according to claim 2, which is characterized in that redox initiator used be ammonium persulfate and Sodium hydrogensulfite.
5. synthetic method according to claim 2, which is characterized in that stabilizer used is oxalic acid.
6. a kind of application method of coking ammonia water detersive according to claim 1, which is characterized in that by the coking ammonia Water detersive is added with the adding consistency of 1 ~ 3ppm in tar ammonia mixture according to cyclic ammonia water amount.
7. a kind of application method of coking ammonia water detersive according to claim 6, which is characterized in that by the coking ammonia Water detersive is continuously added to by dosing metering pump in the tar ammonia mixing line of mechanizeding ammonia clarifying groove inlet.
CN201711416257.5A 2017-12-25 2017-12-25 A kind of method of preparation and use of ammonium hydroxide detersive Pending CN108299593A (en)

Priority Applications (1)

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CN201711416257.5A CN108299593A (en) 2017-12-25 2017-12-25 A kind of method of preparation and use of ammonium hydroxide detersive

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Application Number Priority Date Filing Date Title
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Publications (1)

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CN108299593A true CN108299593A (en) 2018-07-20

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102504851A (en) * 2011-11-03 2012-06-20 河南中鸿集团煤化有限公司 Equipment and process for producing light tar by controlling the QI (Quality Index) value of tar
CN103772600A (en) * 2012-10-18 2014-05-07 西安交大京盛科技发展有限公司 PDA preparation method
CN104356294A (en) * 2014-11-14 2015-02-18 天津大港油田滨港集团博弘石油化工有限公司 Polyacrylamide flocculant and preparation method thereof
CN106495241A (en) * 2016-10-25 2017-03-15 四川鸿康科技股份有限公司 A kind of coking chemical waste water displacement of reservoir oil demulsifier and its preparation technology and purposes

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102504851A (en) * 2011-11-03 2012-06-20 河南中鸿集团煤化有限公司 Equipment and process for producing light tar by controlling the QI (Quality Index) value of tar
CN103772600A (en) * 2012-10-18 2014-05-07 西安交大京盛科技发展有限公司 PDA preparation method
CN104356294A (en) * 2014-11-14 2015-02-18 天津大港油田滨港集团博弘石油化工有限公司 Polyacrylamide flocculant and preparation method thereof
CN106495241A (en) * 2016-10-25 2017-03-15 四川鸿康科技股份有限公司 A kind of coking chemical waste water displacement of reservoir oil demulsifier and its preparation technology and purposes

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Application publication date: 20180720

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