CN108585076A - Dithiocarbamates water purification agent and the preparation method and application thereof - Google Patents
Dithiocarbamates water purification agent and the preparation method and application thereof Download PDFInfo
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- CN108585076A CN108585076A CN201810485533.1A CN201810485533A CN108585076A CN 108585076 A CN108585076 A CN 108585076A CN 201810485533 A CN201810485533 A CN 201810485533A CN 108585076 A CN108585076 A CN 108585076A
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- water purification
- purification agent
- dithiocarbamates
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- carbon disulfide
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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
- C02F1/00—Treatment of water, waste water, or sewage
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of dithiocarbamates water purification agent, preparation method is：Epoxychloropropane is added into polyamines, 20 DEG C~50 DEG C are reacted 2 hours；The sodium hydroxide solution that mass concentration is 40%~50% is added, is cooled to 0 DEG C, the mixture of carbon disulfide and ethyl alcohol is added while stirring, continues to be stirred to react 4 hours；Be warming up to 50 DEG C, removal have neither part nor lot in the carbon disulfide of reaction to get.The present invention dithiocarbamates water purification agent, can be used for handling polymer-containing sewage in oil field, not with the polymer reaction in sewage, it is adding less, and the sludge generated is few, meets polymer-contained sewage under field condition, the effect of its rp demulsification is more preferable, and deoiling effect is more ideal.In application process, the oil and suspended matter in polymer-bearing waste-water can be removed in such a way that net is caught, processing speed is fast, and flocculate is close.In application process, it can go at different temperatures containing poly- oil and suspended matter except in sewage.
Description
Technical field
The present invention relates to a kind of dithiocarbamates water purification agents and preparation method thereof, and in handling polymer-containing sewage in oil field
Using belonging to Treatment of Industrial Water technical field.
Background technology
Oil field mining liquid produces a large amount of oil extraction-generated waste water after separation.It is reasonable development to carry out re-injection to oil field extracted water
With the right way using water resource, raising water circulation use rate the totality of water flooding is improved to keeping stratum energy
Economic benefit is of great significance.Currently, oil field produced water process mainly uses cationic polyacrylamide, poly-aluminium, Polyferric Sulfate class
Flocculant etc..Such flocculant handle it is non-contain poly- oilfield sewage when, have many advantages, such as throwing less developer, sinking speed is fast, so
And when it is applied to polymer-containing sewage in oil field processing, such flocculant not only carries out charge with particulate matter, oil droplet in sewage and gathers
Collection, while reacting with the polymer in sewage, cause dosage to greatly increase, increased production cost, and generates a large amount of
Polymer-containing oil sludge pollutes environment.In view of this, it is necessary to research and develop a kind of new non-ionic type water purification agent, make in its mechanism not
It reacts with the polymer in sewage, to reach the processing effect for effectively reducing dosage, significantly improving polymer-containing sewage in oil field
The advantageous effects such as sludge generation are greatly reduced in rate.
Invention content
For the above-mentioned prior art, to solve big dosage, generation sludge the problems such as, the present invention provides one kind two is thio
Amino water purification agent, and preparation method thereof and its application in handling polymer-containing sewage in oil field.The water purification agent of the present invention can be effective
Polymer-contained sewage reduces sludge quantity, can be widely applied to the land and marine processing containing poly- recovered water.
The present invention is achieved by the following technical solutions：
A kind of preparation method of dithiocarbamates water purification agent：The addition epoxychloropropane (as crosslinking agent) into polyamines, 20
DEG C~50 DEG C react 2 hours；It is slowly added to the sodium hydroxide solution (as catalyst) that mass concentration is 40%~50%, cooling
To 0 DEG C, the mixture of carbon disulfide and ethyl alcohol is added while stirring, continues to be stirred to react 4 hours；50 DEG C are warming up to, removal is not
The carbon disulfide of reaction is participated in get dithiocarbamates water purification agent, being weak yellow liquid (without further purification, can directly answer
With).
The polyamines, any one in ethylenediamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine or two
Kind or more, such as a kind of short chain polyamines and a kind of combination of long-chain polyamines, according to water quality situation and reaction process when concrete application
The middle size for generating floc sedimentation is selected.
The mole dosage of the epoxychloropropane is 0.3~0.7 times of polyamines total mole number.
The mole dosage of the sodium hydroxide is 1.5~2 times of polyamines total mole number.
The mole dosage of the carbon disulfide is 1.2~1.5 times of polyamines total mole number.
In the mixture of the carbon disulfide and ethyl alcohol, the volume ratio of carbon disulfide and ethyl alcohol is 1:2.
The dithiocarbamates water purification agent being prepared using the above method is nonionic water purification agent, can be used for handling oil
Field polymer-bearing waste-water, it is adding less not with the polymer reaction in sewage, and the sludge generated is few, meets under field condition
Manage polymer-bearing waste-water.In application process, the oil and suspended matter in polymer-bearing waste-water, processing speed can be removed in such a way that net is caught
Soon, flocculate is close.In application process, it can go at different temperatures containing poly- oil and suspended matter except in sewage.
The dithiocarbamates water purification agent of the present invention, the dithiocar-bamate type water purification agent phase with routine in the prior art
Than, strand is longer (being used as crosslinking agent by epoxychloropropane), and on strand dithiocarbamates distribution it is more, applying
To during disposing polluted water in oil, the effect of rp demulsification is more preferable, and deoiling effect is more ideal.
The various terms and phrase that the present invention uses are with well known to a person skilled in the art general senses.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated.However, the scope of the present invention is not limited to following realities
Apply example.One of skill in the art, can be to the present invention it is understood that under the premise of without departing substantially from the spirit and scope of the present invention
Carry out various change and modification.
Involved instrument, reagent, material etc., are existing in the prior art unless otherwise noted in following embodiments
Conventional instrument, reagent, material etc., can be obtained by regular commercial sources.Involved experimental method in following embodiments, inspection
Survey method etc. is unless otherwise noted existing routine experiment method in the prior art, detection method etc..
Embodiment 1 prepares dithiocarbamates water purification agent
Diethylenetriamine 20mL (0.186mol) is added into 500mL three-neck flasks, is slowly added to epoxychloropropane later
(as crosslinking agent) 0.06mol is gradually heated to 30 DEG C after adding, react 2 hours；It is 45% to be slowly added to mass concentration later
Sodium hydroxide solution (contain sodium hydroxide 0.30mol), stir evenly, and be gradually cooled to 0 DEG C, curing be added while stirring
The mixture (carbon disulfide 0.23mol, ethyl alcohol 27.5mL) of carbon and ethyl alcohol, continues to be stirred to react 4 hours；50 DEG C are warming up to, is gone
Except the carbon disulfide for having neither part nor lot in reaction, obtained faint yellow emulsion is dithiocarbamates water purification agent.
Embodiment 2 prepares dithiocarbamates water purification agent
Triethylene tetramine 20mL (0.134mol) is added into 500mL three-neck flasks, is slowly added to epoxychloropropane later
(as crosslinking agent) 0.067mol is heated to after adding and gradually 40 DEG C, reacts 2 hours；Being slowly added to mass concentration later is
40% sodium hydroxide solution (containing sodium hydroxide 0.25mol), stirs evenly, and be gradually cooled to 0 DEG C, two is added while stirring
The mixture (carbon disulfide 0.18mol, ethyl alcohol 22mL) of nitric sulfid and ethyl alcohol, continues to be stirred to react 4 hours；50 DEG C are warming up to,
Removal has neither part nor lot in the carbon disulfide of reaction, and obtained faint yellow emulsion is dithiocarbamates water purification agent.
Embodiment 3 prepares dithiocarbamates water purification agent
Triethylene tetramine 10mL (0.067mol) and diethylenetriamine 10mL is added into 500mL three-neck flasks
(0.093mol) is slowly added to epoxychloropropane (as crosslinking agent) 0.065mol later, is heated to after adding and gradually 40 DEG C,
Reaction 2 hours；It is slowly added to the sodium hydroxide solution (containing sodium hydroxide 0.28mol) that mass concentration is 50% later, stirring is equal
It is even, and it is gradually cooled to 0 DEG C, mixture (carbon disulfide 0.20mol, the ethyl alcohol of carbon disulfide and ethyl alcohol are added while stirring
24mL), continue to be stirred to react 4 hours；50 DEG C are warming up to, removal has neither part nor lot in the carbon disulfide of reaction, obtained faint yellow emulsus
Liquid is dithiocarbamates water purification agent.
The purifying water effect of 1 low concentration polymer-bearing waste-water of application examples
Taking the polymer-bearing waste-water of oil field oil recovery field 1L low polymers (30mg/L) concentration, oil content is 382mg/L in sewage,
Concentration of suspension is 273mg/L.In order to detect the different type water purification agent prepared by the present invention (respectively by 1,2 and 3 institute of embodiment
Prepare) effect, put into water purification agent in sewage, dosage is for 60mg, and reaction temperature is 40 DEG C, and the reaction time 1.5 is small
When.
It tests as a comparison, in same polymer-bearing waste-water, puts into the conventional compound water process of poly-aluminium+polyacrylamide
Agent, the wherein a concentration of 500mg/L of poly-aluminium, a concentration of 10mg/L of polyacrylamide, in same reaction temperature and reaction
Between under, test above two medicament purifying water effect.
As a result：After the water purification agent processing prepared by the present invention, according to water purification agent prepared by embodiment 1, after adding,
Oil content is reduced to 19mg/L, and the content of suspended matter is reduced to 17mg/L；According to water purification agent prepared by embodiment 2, after adding, contain
Oil mass is reduced to 14mg/L, and the content of suspended matter is reduced to 13mg/L；According to water purification agent prepared by embodiment 3, after adding, oil-containing
Amount is reduced to 21mg/L, and the content of suspended matter is reduced to 15mg/L；The requirement (being less than 30mg/L) of sewage disposal is reached.And it is right
Than in experiment, the oil content of the composite water disposal agent of conventional poly-aluminium and polyacrylamide is 59mg/L, and the content of suspended matter is
53mg/L, the not up to requirement of sewage disposal.
Generated sludge in processing procedure, front and back volume have significant changes：The water purification agent prepared according to embodiment 1
Treated sludge volume is 10.2mL, and treated that sludge volume is 9.8mL for the water purification agent prepared according to embodiment 2, according to
Water purification agent treated sludge volume prepared by embodiment 3 is 10.3mL；And in contrast test, treated, and sludge volume is about
43.2mL, its sludge content is 1/4 (volume) of conventional composite water disposal agent after the water purification agent processing that the present invention is developed.
In the sewage that the water purification agent processing of the present invention is completed, the concentration of polymer is held essentially constant, and is 29mg/L；And it is normal
It advises in the polymer-bearing waste-water after polymer treatment, polymer concentration is substantially reduced, and is 3mg/L.
It is fabulous that the above results illustrate that the water purification agent that the present invention is developed has the polymer-bearing waste-water of low copolymer concentration
Purifying water effect, and do not reduce the concentration of polymer in polymer-bearing waste-water, effectively save cost.
The treatment effect of 2 high concentration polymer-bearing waste-water of application examples
Take polymer-bearing waste-waters of the oil field oil recovery field 1L compared with high polymer concentration (200mg/L), oil content is in sewage
376mg/L, concentration of suspension 297mg/L.In order to detect the water purification agent prepared by the present invention (respectively by 1,2 and 3 institute of embodiment
Prepare) effect, put into water purification agent in sewage, dosage is 60mg, and reaction temperature is 40 DEG C, 1.5 hours reaction time.
It tests as a comparison, in same polymer-bearing waste-water, puts into the conventional compound water process of poly-aluminium+polyacrylamide
Agent, the wherein a concentration of 500mg/L of poly-aluminium, a concentration of 10mg/L of polyacrylamide, under same reaction temperature, in test
State the purifying water effect of two kinds of medicaments.
As a result：After the water purification agent processing prepared by the present invention, wherein according to water purification agent prepared by embodiment 1, add
Afterwards, oil content is reduced to 29mg/L, and the content of suspended matter is reduced to 35mg/L；According to water purification agent prepared by embodiment 2, add
Afterwards, oil content is reduced to 22mg/L, and the content of suspended matter is reduced to 29mg/L；According to water purification agent prepared by embodiment 3, add
Afterwards, oil content is reduced to 32mg/L, and the content of suspended matter is reduced to 32mg/L；The requirement for having reached sewage disposal (is less than
50mg/L).And in contrast test, the oil content of the composite water disposal agent of conventional poly-aluminium and polyacrylamide is 86mg/L, is hanged
The content of float is 68mg/L, the not up to requirement of sewage disposal.
Generated sludge in processing procedure, front and back volume have significant changes：The water purification agent prepared according to embodiment 1
Treated sludge volume is 11.2mL, and treated that sludge volume is 12.4mL for the water purification agent prepared according to embodiment 2, according to
Water purification agent treated sludge volume prepared by embodiment 3 is 13.3mL；And in contrast test, treated, and sludge volume is about
66.8mL, its sludge content is 1/6 (volume) of conventional composite water disposal agent after the water purification agent processing that the present invention is developed.
In the sewage that the water purification agent processing of the present invention is completed, the concentration of polymer is held essentially constant, and is 190mg/L；Often
It advises in the polymer-bearing waste-water after polymer treatment, polymer concentration is substantially reduced, and is 7mg/L.
The above results illustrate that the water purification agent that the present invention is developed also has pole for the polymer-bearing waste-water compared with high polymer concentration
Good purifying water effect, and the concentration of polymer in polymer-bearing waste-water is not reduced, effectively save cost.
Above-described embodiment is provided to those skilled in the art, how to implement and use to be advocated with full disclosure and description
Embodiment, rather than for limiting range disclosed herein.Obvious modification will to those skilled in the art
Within the scope of the appended claims.
Claims (10)
1. a kind of preparation method of dithiocarbamates water purification agent, it is characterised in that：It is added epoxychloropropane into polyamines, 20 DEG C~
50 DEG C are reacted 2 hours；The sodium hydroxide solution that mass concentration is 40%~50% is added, is cooled to 0 DEG C, two is added while stirring
The mixture of nitric sulfid and ethyl alcohol continues to be stirred to react 4 hours；50 DEG C are warming up to, removal has neither part nor lot in the carbon disulfide of reaction, i.e.,
Obtain dithiocarbamates water purification agent.
2. the preparation method of dithiocarbamates water purification agent according to claim 1, it is characterised in that：The polyamines, is selected from
In ethylenediamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine any one or it is two or more.
3. the preparation method of dithiocarbamates water purification agent according to claim 2, it is characterised in that：The polyamines is selected from two
Ethylene triamine, triethylene tetramine, or：The combination of diethylenetriamine and triethylene tetramine.
4. the preparation method of dithiocarbamates water purification agent according to claim 1, it is characterised in that：The epoxychloropropane
Mole dosage be 0.3~0.7 times of polyamines total mole number.
5. the preparation method of dithiocarbamates water purification agent according to claim 1, it is characterised in that：The sodium hydroxide
Mole dosage is 1.5~2 times of polyamines total mole number.
6. the preparation method of dithiocarbamates water purification agent according to claim 1, it is characterised in that：The carbon disulfide
Mole dosage is 1.2~1.5 times of polyamines total mole number.
7. the preparation method of dithiocarbamates water purification agent according to claim 1, it is characterised in that：The carbon disulfide and
In the mixture of ethyl alcohol, the volume ratio of carbon disulfide and ethyl alcohol is 1:2.
8. the preparation method of dithiocarbamates water purification agent according to any one of claims 1 to 7, it is characterised in that：Choosing
From one of following scheme：
Scheme one：Diethylenetriamine 20mL is added into 500mL three-neck flasks, is slowly added to epoxychloropropane 0.06mol later,
It is gradually heated to 30 DEG C after adding, reacts 2 hours；It is slowly added to the sodium hydroxide solution that mass concentration is 45% later, stirring
Uniformly, and it is gradually cooled to 0 DEG C, the mixture of carbon disulfide and ethyl alcohol is added while stirring, continues to be stirred to react 4 hours；It rises
For temperature to 50 DEG C, removal has neither part nor lot in the carbon disulfide of reaction, obtains dithiocarbamates water purification agent；
Scheme two：Triethylene tetramine 20mL is added into 500mL three-neck flasks, is slowly added to epoxychloropropane later
0.067mol is heated to after adding and gradually 40 DEG C, reacts 2 hours；It is slowly added to the hydroxide that mass concentration is 40% later
Sodium solution stirs evenly, and is gradually cooled to 0 DEG C, and the mixture of carbon disulfide and ethyl alcohol is added while stirring, and it is anti-to continue stirring
It answers 4 hours；50 DEG C are warming up to, removal has neither part nor lot in the carbon disulfide of reaction, obtains dithiocarbamates water purification agent；
Scheme three：Triethylene tetramine 10mL and diethylenetriamine 10mL is added into 500mL three-neck flasks, is slowly added to ring later
Oxygen chloropropane 0.065mol is heated to after adding and gradually 40 DEG C, reacts 2 hours；It is 50% to be slowly added to mass concentration later
Sodium hydroxide solution, stir evenly, and be gradually cooled to 0 DEG C, while stirring be added carbon disulfide and ethyl alcohol mixture, after
It is continuous to be stirred to react 4 hours；50 DEG C are warming up to, removal has neither part nor lot in the carbon disulfide of reaction, obtains dithiocarbamates water purification agent.
9. the dithiocarbamates water purification agent being prepared using the preparation method described in any one of claim 1~8.
10. application of the dithiocarbamates water purification agent in handling polymer-containing sewage in oil field described in claim 9.
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Cited By (3)
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| CN113526746A (en) * | 2021-08-25 | 2021-10-22 | 北京盖雅环境科技有限公司 | Method for removing sulfur ions in oil and gas field sewage |
| CN114989056A (en) * | 2022-05-31 | 2022-09-02 | 中海油天津化工研究设计院有限公司 | Polyalkyl polyamine nonionic water purifying agent and preparation method thereof |
| CN114989410A (en) * | 2022-05-13 | 2022-09-02 | 中海油(天津)油田化工有限公司 | Water clarifier for offshore oil field and preparation method thereof |
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