CN105481225A - Oil-containing scum dehydration method - Google Patents

Oil-containing scum dehydration method Download PDF

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Publication number
CN105481225A
CN105481225A CN201410528968.1A CN201410528968A CN105481225A CN 105481225 A CN105481225 A CN 105481225A CN 201410528968 A CN201410528968 A CN 201410528968A CN 105481225 A CN105481225 A CN 105481225A
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China
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oil
dehydration
scum
reverse
phase emulsifier
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CN201410528968.1A
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张传明
苟社全
张红宇
常文之
赵双霞
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China Petroleum and Chemical Corp
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China Petroleum and Chemical Corp
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Abstract

The invention relates to the field of environmental engineering, and relates to an oil-containing scum dehydration method. The method comprises the following steps: (1) a pH regulation agent is added into the scum, and the mixture is well mixed with a speed of 200-500r/min, such that scum pH is regulated to 7-14, and a coagulation conditioning reaction is carried out; (2) a reverse demulsifier is added into the scum, such that a demulsification reaction is carried out; (3) a high-molecular flocculating agent is added into the scum, such that a flocculation dehydration reaction is carried out; and (4) the scum is allowed to stand and is subjected to natural sedimentation. The oil-containing scum dehydration method provided by the invention has the advantages of simple process and low secondary pollution. After dehydration, scum viscosity is low. The dehydration efficiency is high, and a dehydration rate can reach 40-65%. The cost is low, and no special equipment is needed. Investment and operation cost are low, and the method is suitable for popularization and application. The amount of scum produced by a sewage treatment plant is high, and the scum is difficult to treat. With the method, the above problems are effectively solved. The method is suitable for the dehydration of oil-containing scum produced in a floatation treatment process of oil-containing sewage from oil refining enterprises.

Description

Oil-containing dross dehydration method
Technical field
The invention belongs to field of environment engineering, be specifically related to a kind of oil-containing dross dehydration method.
Background technology
The oil removal treatment of current domestic oil refining enterprises oily(waste)water generally adopts oil removal, one-level flotation and secondary floatation technique.Oil-containing dross is in the treating processes of oily(waste)water, a kind of end waste that air flotation cell produces.Air supporting is a kind of effective solid-liquid separating method, is combined process that is gas-solid adsorption and solid-liquid separation.It is by pressure air-dissolving tank by air dissolves in water in state of saturation, when water passes into flotation cell, pressure declines suddenly, the air dissolved in water discharges countless microbubble, bubble and waste water Midst density are adhered to close to the solid of water or liquid particle, form the air float body that density is less than water, and carry out solid-liquid or liquid-liquid separation at the effect float downward of buoyancy to the water surface.Various electronegative suspended particle (comprising oil in water emulsion, free elaioleucite), forms flocculation group by adding flocculation agent (being generally polymerize aluminum chloride, bodied ferric sulfate).In air supporting process, micro-bubble adheres to mutually with flocculation group, produces Float upward function form " water-gas-solid " three-phase mixed system because density is less than water, and make it be that the pollutent of suspended state is separated from water, namely the product of separation becomes oil-containing dross.
Oil-containing dross is the flocculation group of various particle, water and bubble formation, and in semi-solid state, viscosity is large, poor fluidity.Its main component is various chemical agent, various tensio-active agent, flocculation agent, oil in water emulsion, dispersed oil, mink cell focus composition, fine sand and a large amount of secondary clay mineral, various coagulation of materials together, emulsification flocculation is serious, its settling property extreme difference, dewater very difficult, and its water ratio is high, generally between 90% ~ 99%.
Scum treatment method conventional both at home and abroad at present utilizes delayed coking unit to mix refining.Mixing smelting method, to mainly contain two kinds: one be that scum silica frost is made coke drum quenching oil; Two is utilize coke drum waste heat to carry out gasification separation to scum silica frost.Second method is entered from coke drum rising pouring by scum silica frost in high temperature coke process of cooling, as little feedwater cooling down high-temperature coke; Utilize the high-temperature residual heat of coke by oil ingredient heating evaporation olifiant gas wherein, escape into contact cooling system from tower top; Solid impurity is then adsorbed on coke layer on the surface, and enters Jiao Chi with high pressure decoking process and become coke product, thus realizes the object of airtight environmental protection treatment scum silica frost.Adopt this method not only to save scum silica frost processing costs, the oil content in scum silica frost effectively can also be recycled, and increase the output of coke, therefore, this treatment process adopt by most refinery.
Along with the increase year by year of refinery crude runs, and crude quality is tending towards in poor quality, heaviness, and the inorganics in sewage, organism class substances content significantly increase, and the scum silica frost amount that air flotation cell produces also increases year by year.Simultaneously, the scum silica frost amount that coker processes every year is certain, and some scum silica frost like this cannot process, and outward transport process not only can produce secondary pollution but also likely occur pollution transportation phenomenon; And scum silica frost enters coking process, become sour water after wherein contained moisture is vaporized, in follow-up double tower stripping treating processes, need to consume a certain amount of low-pressure steam, therefore, scum silica frost is moisture more, and the quantity of steam of consumption is larger, and energy consumption is higher.So, under scum silica frost has the prerequisite of good fluidity, minimizing processed to be carried out to scum silica frost.
The existing method for dross dehydration is divided into physical method and chemical process.Physical method normally carries out centrifugal, press filtration or cold-heat treatment to scum silica frost, and require higher to treatment facility, operation energy consumption is high, and processing cost is expensive.Chemical process mainly adds medicament and carries out processed, and used treatment agent function is relatively single: the demulsification had is good, but flocculating effect is poor; Some flocculating effects are good, but settling velocity is slow, and the meeting also had causes secondary pollution; What have is effective, but cost intensive.
Chinese patent CN98110574.2 discloses a kind of method of lyophilization process scum silica frost, and the method running cost is higher, is difficult to apply.Chinese patent CN02117444.X disclose a kind of first add naphtenic acid after to alkalize the treatment process of last filter-press dehydration, the method filter-press dehydration poor effect.Chinese patent CN101367600A discloses a kind of additive for sludge dewatering, wherein additive comprise weight ratio be mud admittedly containing the quaternary ammonium salt cationic surfactant of 1.42-2.07% of thing, weight ratio be mud admittedly containing the flocculation agent of the 4.92-10.18% of thing, weight ratio be mud admittedly containing the auxiliary agent of the 5-10% of thing, auxiliary agent is the substratum after edible mushroom is plucked.Medicament mainly tensio-active agent, flocculation agent and the inorganic salts auxiliary agent adopted, additive amount of medicament is comparatively large and have more inorganics, ash content can be made to increase, calorific value decline.
Summary of the invention
The object of this invention is to provide a kind of oil-containing dross dehydration method, technological process is simple, and secondary pollution is little, and the scum silica frost viscosity after dehydration is low, and dewatering efficiency is high; With low cost, without the need to specific installation, investment and process cost low, be easy to apply; It is large that effective solution sewage work produces scum silica frost amount, is difficult to the difficult problem processed.
A kind of oil-containing dross dehydration method of the present invention, step is as follows:
(1) in scum silica frost, add pH adjusting agent to stir with 200-500r/min, scum silica frost is adjusted to pH=7 ~ 14, carry out coagulation opsonic reaction;
(2) continue to add reverse-phase emulsifier in scum silica frost, carry out breakdown of emulsion reaction;
(3) in scum silica frost, add polymeric flocculant, carry out flocculation dewatering reaction;
(4) natural subsidence is left standstill.
PH adjusting agent is one or more mixtures in sodium hydroxide, calcium oxide, calcium hydroxide or potassium hydroxide.Preferred sodium hydroxide.
Described pH value controls between 7 ~ 14.Preferable ph is between 8 ~ 11.
The add-on of reverse-phase emulsifier is 5 ~ 100mg/L, preferably 20 ~ 50mg/L; The add-on of described polymeric flocculant is 1 ~ 100mg/L, preferably 5 ~ 30mg/L.
Described reverse-phase emulsifier is polycation quaternary reverse-phase emulsifier.
Described polycation quaternary reverse-phase emulsifier is monomer by epoxy chloropropane and dimethylamine, reacts an obtained class epichlorohydrin-dimethylamine polymkeric substance (EPI-DMA) with organic amine linking agent.
Described organic amine linking agent is one or more mixtures in methylamine, ethamine, hexanediamine, Tetramethyl Ethylene Diamine, n-Butyl Amine 99 or amino dodecane.Preferred hexanediamine and n-Butyl Amine 99.
Polycation quaternary reverse-phase emulsifier preparation method is: the water-bath four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed being placed in 45 ~ 55 DEG C, add dimethylamine, slowly epoxy chloropropane is dripped by constant pressure funnel, organic amine linking agent is added after dropwising, then 75 ~ 85 DEG C are warming up to, isothermal reaction 6 ~ 10h, obtain synthetic product, synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier; Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and linking agent is 1:1 ~ 2:0.01 ~ 0.1.
Polymeric flocculant is macromolecule cation polyacrylamide.
The molecular weight of macromolecule cation polyacrylamide is 600 ~ 2,000 ten thousand, and cationic degree is between 10% ~ 35%.The molecular weight of macromolecule cation polyacrylamide preferably 8,000,000 ~ 1,600 ten thousand, cationic degree preferably 15% ~ 35%.Polymeric flocculant more preferably molecular weight is 1,400 ten thousand, and cationic degree is the polyacrylamide of 25%.
Cationic polyacrylamide is deployed into the solution of 0.1% ~ 0.3% mass concentration before using.
Compared with prior art, the present invention has following beneficial effect:
Oil-containing dross dehydration method of the present invention, technological process is simple, secondary pollution is little, and the scum silica frost viscosity after dehydration is low, and dewatering efficiency is high, dehydration rate can reach 40% ~ 65%, with low cost, without the need to specific installation, investment and process cost low, be easy to apply, it is large that effective solution sewage work produces scum silica frost amount, is difficult to the difficult problem processed.Be adapted to the method that oil refining enterprise's oily(waste)water carries out the oil-containing dross dehydration produced in flotation treating processes.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 50 DEG C, adds dimethylamine, slowly drip epoxy chloropropane by constant pressure funnel, hexanediamine is added after dropwising, then be warming up to 75 DEG C, isothermal reaction 6h, obtains synthetic product.Synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 1.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and hexanediamine is 1:1.5:0.05.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, under agitation condition, with sodium hydroxide, pH is adjusted to 10, then adds the reverse-phase emulsifier A of 25mg/L 1with the cationic polyacrylamide of 15mg/L, added cationic polyacrylamide molecular weight is 1,400 ten thousand, and cationic degree is 25%.After stirring, through natural subsidence, dehydration rate reaches 64.1%.
Cationic polyacrylamide is deployed into the solution of 0.1% mass concentration before using.
Embodiment 2
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 45 DEG C, adds dimethylamine, slowly drip epoxy chloropropane by constant pressure funnel, n-Butyl Amine 99 is added after dropwising, then be warming up to 85 DEG C, isothermal reaction 7h, obtains synthetic product.Synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 2.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and n-Butyl Amine 99 is 1:1.4:0.06.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with sodium hydroxide, pH is adjusted to 11, and stirs with the speed of 200r/min, then adds the reverse-phase emulsifier A of 35mg/L 2with the cationic polyacrylamide of 10mg/L.Added cationic polyacrylamide molecular weight is 1,200 ten thousand, and cationic degree is 20%.After stirring, through natural subsidence, dehydration rate reaches 60.5%.
Cationic polyacrylamide is deployed into the solution of 0.3% mass concentration before using.
Embodiment 3
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 45 DEG C, adds dimethylamine, slowly drip epoxy chloropropane by constant pressure funnel, amino dodecane is added after dropwising, then be warming up to 80 DEG C, isothermal reaction 8h, obtains synthetic product.Synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 3.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and amino dodecane is 1:1.4:0.04.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with potassium hydroxide, pH is adjusted to 9, and stirs with the speed of 300r/min, then adds the reverse-phase emulsifier A of 20mg/L 3with the cationic polyacrylamide of 30mg/L.Added cationic polyacrylamide molecular weight is 1,600 ten thousand, and cationic degree is 15%.After stirring, through natural subsidence, dehydration rate reaches 56.3%.
Cationic polyacrylamide is deployed into the solution of 0.2% mass concentration before using.
Embodiment 4
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 50 DEG C, adds dimethylamine, slowly drip epoxy chloropropane by constant pressure funnel, ethamine is added after dropwising, then be warming up to 80 DEG C, isothermal reaction 8h, obtains synthetic product.Synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 4.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and ethamine is 1:1.3:0.07.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, under agitation condition, with calcium oxide, pH is adjusted to 8, then adds the reverse-phase emulsifier A of 5mg/L 4with the cationic polyacrylamide of 80mg/L.Added cationic polyacrylamide molecular weight is 8,000,000, and cationic degree is 10%.After stirring, through natural subsidence, dehydration rate reaches 42.1%.
Cationic polyacrylamide is deployed into the solution of 0.3% mass concentration before using.
Embodiment 5
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 55 DEG C, adds dimethylamine, slowly drip epoxy chloropropane by constant pressure funnel, methylamine is added after dropwising, then be warming up to 80 DEG C, isothermal reaction 7h, obtains synthetic product.Synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 5.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and methylamine is 1:1.6:0.02.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with calcium hydroxide, pH is adjusted to 12, and stirs with the speed of 400r/min, then adds the reverse-phase emulsifier A of 50mg/L 5with the cationic polyacrylamide of 100mg/L.Added cationic polyacrylamide molecular weight is 2,000 ten thousand, and cationic degree is 35%.After stirring, through natural subsidence, dehydration rate reaches 50.4%.
Cationic polyacrylamide is deployed into the solution of 0.1% mass concentration before using.
Embodiment 6
The four-hole boiling flask that agitator, thermometer, reflux condensing tube and constant pressure funnel are housed is placed in the water-bath of 50 DEG C, add dimethylamine, slowly epoxy chloropropane is dripped by constant pressure funnel, Tetramethyl Ethylene Diamine is added after dropwising, then be warming up to 75 DEG C, isothermal reaction 6h, obtains synthetic product, synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier A 6.Wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and Tetramethyl Ethylene Diamine is 1:2:0.1.
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with calcium oxide, pH is adjusted to 14, and stirs with the speed of 400r/min, then adds the reverse-phase emulsifier A of 100mg/L 6with the cationic polyacrylamide of 50mg/L.Added cationic polyacrylamide molecular weight is 8,000,000, and cationic degree is 15%.After stirring, through natural subsidence, dehydration rate reaches 46.8%.
Cationic polyacrylamide is deployed into the solution of 0.3% mass concentration before using.
Embodiment 7
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with sodium hydroxide, pH is adjusted to 7, and stirs with the speed of 500r/min, then adds the polycation quaternary reverse-phase emulsifier A in the embodiment 1 of 5mg/L 1with the cationic polyacrylamide of 30mg/L.Added cationic polyacrylamide molecular weight is 1,000 ten thousand, and cationic degree is 18%.After stirring, through natural subsidence, dehydration rate reaches 44.7%.
Cationic polyacrylamide is deployed into the solution of 0.2% mass concentration before using.
Embodiment 8
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, with potassium hydroxide, pH is adjusted to 11, and stirs with the speed of 400r/min, then add in 20mg/L embodiment 1 polycation quaternary reverse-phase emulsifier A 2with the cationic polyacrylamide of 20mg/L.Added cationic polyacrylamide molecular weight is 1,300 ten thousand, and cationic degree is 30%.After stirring, through natural subsidence, dehydration rate reaches 55.6%.
Cationic polyacrylamide is deployed into the solution of 0.3% mass concentration before using.
Embodiment 9
Oil-containing dross dehydration method, step is as follows:
Certain refinery's water ratio is 95.2% scum silica frost, under agitation condition, with calcium hydroxide, pH is adjusted to 9, and stirs with the speed of 400r/min, then add in 80mg/L embodiment 1 polycation quaternary reverse-phase emulsifier A 3with the cationic polyacrylamide of 3mg/L.Added cationic polyacrylamide molecular weight is 6,000,000, and cationic degree is 10%.After stirring, through natural subsidence, dehydration rate reaches 43.8%.
Cationic polyacrylamide is deployed into the solution of 0.1% mass concentration before using.

Claims (10)

1. an oil-containing dross dehydration method, is characterized in that, preparation process is as follows:
(1) in scum silica frost, add pH adjusting agent to stir with 200 ~ 500r/min, carry out coagulation opsonic reaction;
(2) continue to add reverse-phase emulsifier in scum silica frost, carry out breakdown of emulsion reaction;
(3) in scum silica frost, add polymeric flocculant, carry out flocculation dewatering reaction;
(4) natural subsidence is left standstill.
2. oil-containing dross dehydration method according to claim 1, is characterized in that, pH adjusting agent is one or more mixtures in sodium hydroxide, calcium oxide, calcium hydroxide or potassium hydroxide.
3. oil-containing dross dehydration method according to claim 1, is characterized in that, the add-on of reverse-phase emulsifier is 5 ~ 100mg/L; The add-on of described polymeric flocculant is 1 ~ 100mg/L.
4. oil-containing dross dehydration method according to claim 1, is characterized in that, in step (1), scum silica frost is adjusted to pH=7 ~ 14.
5. oil-containing dross dehydration method according to claim 1, is characterized in that, described reverse-phase emulsifier is polycation quaternary reverse-phase emulsifier.
6. oil-containing dross dehydration method according to claim 5, it is characterized in that, described polycation quaternary reverse-phase emulsifier is monomer by epoxy chloropropane and dimethylamine, reacts an obtained class epichlorohydrin-dimethylamine polymkeric substance with organic amine linking agent.
7. oil-containing dross dehydration method according to claim 6, is characterized in that, described organic amine linking agent is one or more mixtures in methylamine, ethamine, hexanediamine, Tetramethyl Ethylene Diamine, n-Butyl Amine 99 or amino dodecane.
8. oil-containing dross dehydration method according to claim 6, it is characterized in that, polycation quaternary reverse-phase emulsifier preparation method is: agitator will be housed, thermometer, the four-hole boiling flask of reflux condensing tube and constant pressure funnel is placed in the water-bath of 45 ~ 55 DEG C, add dimethylamine, slowly epoxy chloropropane is dripped by constant pressure funnel, organic amine linking agent is added after dropwising, then 75 ~ 85 DEG C are warming up to, isothermal reaction 6 ~ 10h, obtain synthetic product, synthetic product is through dehydrated alcohol purification and vacuum-drying obtains thick liquid, i.e. polycation quaternary reverse-phase emulsifier, wherein, the ratio of the amount of substance of epoxy chloropropane, dimethylamine and linking agent is 1:1 ~ 2:0.01 ~ 0.1.
9. oil-containing dross dehydration method according to claim 1, is characterized in that, polymeric flocculant is macromolecule cation polyacrylamide.
10. oil-containing dross dehydration method according to claim 9, is characterized in that, the molecular weight of macromolecule cation polyacrylamide is 600 ~ 2,000 ten thousand, and cationic degree is between 10% ~ 35%.
CN201410528968.1A 2014-10-09 2014-10-09 Oil-containing scum dehydration method Pending CN105481225A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106007096A (en) * 2016-07-15 2016-10-12 嘉兴通惠环保科技有限公司 Pretreatment technology for textile machine cleaning high-oil-content waste liquor
CN106673401A (en) * 2016-12-30 2017-05-17 北京普利科林环境科技有限公司 Method for dewatering oily scum in petrochemical industry
CN108130122A (en) * 2017-12-12 2018-06-08 中海油天津化工研究设计院有限公司 A kind of more quaternary amine reverse-phase emulsifiers and preparation method thereof
CN109608018A (en) * 2018-12-05 2019-04-12 东莞理工学院 A kind of oily sludge recycling method for innocent treatment
CN112225432A (en) * 2020-10-10 2021-01-15 中国石油大学(北京) Method and device for separating scum and sludge water in oil refining sewage field

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CN102198969A (en) * 2010-03-22 2011-09-28 天津大港油田科远石油工程有限责任公司 Oil-removing compound and its preparation method
CN103922438A (en) * 2013-01-14 2014-07-16 中国地质大学(北京) Preparation of super heavy oil wastewater reverse-phase demulsifier, and demulsification process method

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CN1955122A (en) * 2005-10-26 2007-05-02 中国石油化工股份有限公司 Method for treating oil-containing waste water
JP2009106898A (en) * 2007-10-31 2009-05-21 Kurita Water Ind Ltd Method and apparatus for treating water
CN102198969A (en) * 2010-03-22 2011-09-28 天津大港油田科远石油工程有限责任公司 Oil-removing compound and its preparation method
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106007096A (en) * 2016-07-15 2016-10-12 嘉兴通惠环保科技有限公司 Pretreatment technology for textile machine cleaning high-oil-content waste liquor
CN106673401A (en) * 2016-12-30 2017-05-17 北京普利科林环境科技有限公司 Method for dewatering oily scum in petrochemical industry
CN108130122A (en) * 2017-12-12 2018-06-08 中海油天津化工研究设计院有限公司 A kind of more quaternary amine reverse-phase emulsifiers and preparation method thereof
CN108130122B (en) * 2017-12-12 2020-08-21 中海油天津化工研究设计院有限公司 Multi-quaternary ammonium salt reverse demulsifier and preparation method thereof
CN109608018A (en) * 2018-12-05 2019-04-12 东莞理工学院 A kind of oily sludge recycling method for innocent treatment
CN112225432A (en) * 2020-10-10 2021-01-15 中国石油大学(北京) Method and device for separating scum and sludge water in oil refining sewage field

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