CN108128877A - A kind of synthetic method for the water purification one agent that is demulsified - Google Patents
A kind of synthetic method for the water purification one agent that is demulsified Download PDFInfo
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- CN108128877A CN108128877A CN201711394387.3A CN201711394387A CN108128877A CN 108128877 A CN108128877 A CN 108128877A CN 201711394387 A CN201711394387 A CN 201711394387A CN 108128877 A CN108128877 A CN 108128877A
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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
- C02F1/68—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water
- C02F1/682—Treatment of water, waste water, or sewage by addition of specified substances, e.g. trace elements, for ameliorating potable water by addition of chemical compounds for dispersing an oily layer on water
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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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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- Chemical & Material Sciences (AREA)
- Water Supply & Treatment (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of synthetic methods for the water purification one agent that is demulsified.The synthetic method includes the following steps：Polyethers cationic intermediate with primary amine, tertiary amine is obtained by the reaction with Hydrin successively respectively first, both sexes demulsification water purification one agent then is obtained by the reaction in intermediate and carbon disulfide.Demulsification water purification one agent product purifying water effect obtained by synthetic method of the present invention is good, and the not viscous group of flco densification, water quality is limpid, is especially suitable for applying in polymer-bearing waste-water processing.
Description
Technical field
The present invention relates to sump oil water-treatment technology fields, and in particular to a kind of synthetic method for the water purification one agent that is demulsified.
Background technology
With the application to deepen continuously with tertiary oil recovery technology of oil field development, the moisture content of crude oil is gradually increasing, part
The composite water cut of crude oil is higher than more than 90%, but the processing containing polymer sewage from oil extraction generated in oil recovery process is always
It is a problem.Polymer monomer has the characteristics such as good dispersion, emulsification and absorption in itself so that oil-water emulsion aggravates, and takes
The amount increase of the suspended matters such as the shale of band, emulsion become complicated, stablize, and crude oil demulsification dehydration is difficult.In polymer-bearing waste-water processing
The equipment at different levels of flow by polymer be precipitated it is cementing influence, dirt is stifled serious, leads to equipment frequent clean, influences equipment processing effect
Fruit.Existing Water purification medicament cannot be fully met containing poly- production fluid processing requirement, and medicament dewatering time still needs to more than 30min, simultaneously
The compatibility of chemical agent and polymer is undesirable, and generation is intermolecular to interact, and polymer is caused to be precipitated, is mutually tied with greasy filth
Viscoplasticity jelly is gradually formed after conjunction.The viscoplasticity jelly recycles in systems, and process flow dirt is caused to block up seriously, cleaning
Difficulty is big, influences the treatment effect of whole flow process.So the medicament that exploitation novel process gathers drive oil extraction-generated waste water has become oil field
Stablize exploitation institute urgent problem to be solved.
Chinese patent application CN201510902507.0 discloses a kind of chemical treatment method of polymer-bearing waste-water.1) Xiang Hanju
Cationic water cleaning agent is added in sewage, and is uniformly mixed；2) non-ionic clear water is added in into step 1) treated sewage
Agent, and be uniformly mixed；3) to step 2), treated that sewage summarizes adds in weak cation type water cleaning agent, and be uniformly mixed, i.e., in fact
Now to the purification of the polymer-bearing waste-water." classification adds in, combined treatment " method that the invention provides realizes water cleaning agent function spy
The Optimized Matching of point and sewage property, but repeatedly dosing increases labour cost, needs to develop a kind of good integrated agent of effect.
Invention content
In view of in place of the shortcomings of the prior art, the present invention provides a kind of chemically and thermally stability is good, the scope of application
Extensively, medicament dosage is few, de-emulsification speed is fast, flco is fine and close, the conjunction of the demulsification water purification one agent of the easy non-secondary pollution of oil recovery
Into method.
The present invention is achieved by the following technical programs above-mentioned technical problem.
A kind of synthetic method for the water purification one agent that is demulsified of the present invention, comprises the technical steps that：
1) synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in metered primary amine and alcohol-aqueous solvent,
Wherein alcohol-water quality ratio is 1:1~1:1.5, account for the 25%~45% of overall reaction system quality；Stirring, is added dropwise poly- epoxy chloropropionate
Alkane, for control temperature at 30 DEG C -45 DEG C, primary amine is 1 with the molar ratio of reacting of Hydrin:0.5~1:0.7.Treat polycyclic oxygen
After chloropropane is added dropwise, 45 DEG C of -50 DEG C of heat preservation 1-2h are warming up to, measure grignard viscosity, viscosity was by 0.8 second~1.2 seconds；
Adding tertiary amine, the reaction was continued, and tertiary amine is 0.4 with the molar ratio of reacting of primary amine:1~0.65:1, reaction temperature is
100 DEG C -105 DEG C, reaction time 2-4h, obtain the transparent water-soluble products of rufous；
2) synthesis of demulsification water purification one agent
Cationic intermediate and deionized water, mass ratio 3.5 are added in reaction unit:1-6.5:1；It is slowly added dropwise
Carbon disulfide and lye, controlling reaction temperature are 0 DEG C -25 DEG C；The rate of addition of lye is controlled to be more than carbon disulfide, control reaction
The pH=8.5-12 of liquid；It is added dropwise and is warming up to 35 DEG C -45 DEG C, the reaction was continued 3-5h, cooling discharge obtains transparent salmon liquid
Body, wherein cationic intermediate and carbon disulfide reaction molar ratio are 1:2.0~1:3.5.
A kind of synthetic method for the water purification one agent that is demulsified of the present invention, has the characteristics that：(1) there is water-soluble quaternary ammonium salt
The special construction of cation and dithiocar-bamate anion, chemically and thermally stability is good, applicable pH range and temperature model
It encloses wide；(2) structure contains hydrophilic and oleophilic base, adds in containing the surface reactive material that oil-water interfaces can be substituted in poly- sump oil water, makes
Emulsion takes off steady realize and is demulsified；(3) special reticular structure forms the volume effect of sweeping of building bridge, and forms the flco of fine and close not viscoelastic, water
Matter is limpid；(4) can with anionic polymer compatible use and with cationic polymer compatible use, use scope is wide；
(5) anions and canons group has apparent synergistic effect in water treatment procedure.Advantage is compared with prior art：
The demulsifier one agent medicament dosage of synthetic method synthesis is few, de-emulsification speed is fast, flco is fine and close, not only improves oil removal efficiency, and
And be conducive to the recycling of sump oil, avoid the problem of traditional flocculant generates a large amount of mud, causes secondary pollution.
Specific embodiment
Technical solution of the present invention is further described below by embodiment.
Embodiment 1
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in diethylenetriamine (41.27g,
0.4mol) and methanol-water solvent (72g, methanol content 30%)；It opens and stirs, dropwise addition Hydrin (18.5g,
0.2mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, it is warming up to 50 DEG C of heat preservations
1.5h measures grignard viscosity, and viscosity was by 0.9 second.Add 33% trimethylamine (28.66g, 0.16mol), controlling reaction temperature
It it is 100 DEG C -105 DEG C, the reaction was continued 2h obtains the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 160g cationics
Body and 36g deionized waters；Carbon disulfide (60.8g, 0.8mol) and 40% sodium hydrate aqueous solution, control reaction is slowly added dropwise
Temperature is 0 DEG C -25 DEG C；The rate of addition of sodium hydrate aqueous solution is controlled to be more than carbon disulfide, controls the pH=9-11 of reaction solution；
It is added dropwise and is warming up to 30 DEG C, the reaction was continued 4h, cooling discharge obtains transparent salmon liquid 261g.
Embodiment 2
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in diethylenetriamine (41.27g,
0.4mol) and methanol-water solvent (72g, methanol content 30%)；It opens and stirs, dropwise addition Hydrin (18.5g,
0.2mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, it is warming up to 50 DEG C of heat preservations
1.5h measures grignard viscosity, and viscosity was by 00.9 second.33% trimethylamine (39g, 0.22mol) is added, controlling reaction temperature is
100 DEG C -105 DEG C, the reaction was continued 3h, obtain the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 170g cationics
Body and 36g deionized waters；Carbon disulfide (85g, 1.12mol) and 40% sodium hydrate aqueous solution, control reaction is slowly added dropwise
Temperature is 0 DEG C -25 DEG C；The rate of addition of sodium hydrate aqueous solution is controlled to be more than carbon disulfide, controls the pH=9-11 of reaction solution；
It is added dropwise and is warming up to 30 DEG C, the reaction was continued 4.5h, cooling discharge obtains transparent salmon liquid 331g.
Embodiment 3
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in triethylene tetramine (50.49g,
0.4mol) and methanol-water solvent (103.6g, methanol content 35%)；It opens and stirs, dropwise addition Hydrin (22.2g,
0.24mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, 50 DEG C of heat preservation 2h are warming up to,
Grignard viscosity is measured, viscosity was by 1.0 seconds.Add 33% trimethylamine (35.8g, 0.2mol), controlling reaction temperature 100
DEG C -105 DEG C, the reaction was continued 2.5h, obtain the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 212g cationics
Body and 34.5g deionized waters；Carbon disulfide (60.8g, 0.8mol) and 40% sodium hydrate aqueous solution is slowly added dropwise, control is anti-
It is 0 DEG C -25 DEG C to answer temperature；The rate of addition of sodium hydrate aqueous solution is controlled to be more than carbon disulfide, controls the pH=8- of reaction solution
12；It is added dropwise and is warming up to 35 DEG C, the reaction was continued 4h, cooling discharge obtains transparent salmon liquid 345g.
Embodiment 4
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in diethylenetriamine (41.27g,
0.4mol) and methanol-water solvent (110g, methanol content 35%)；It opens and stirs, dropwise addition Hydrin (32g,
0.35mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, it is warming up to 50 DEG C of heat preservations
1.5h measures grignard viscosity, and viscosity was by 0.9 second.Add 33% trimethylamine (39.41g, 0.2mol), controlling reaction temperature
It it is 100 DEG C -105 DEG C, the reaction was continued 2.5h obtains the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 222g cationics
Body and 55g deionized waters；Carbon disulfide (85.12g, 1.12mol) and 40% potassium hydroxide aqueous solution is slowly added dropwise, control is anti-
It is 0 DEG C -25 DEG C to answer temperature；The rate of addition of potassium hydroxide aqueous solution is controlled to be more than carbon disulfide, controls the pH=9- of reaction solution
11；It is added dropwise and is warming up to 40 DEG C, the reaction was continued 4h, cooling discharge obtains transparent salmon liquid 402g.
Embodiment 5
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in triethylene tetramine (50.49g,
0.4mol) and ethanol-water (95.37g, ethanol content 30%)；It opens and stirs, dropwise addition Hydrin (22.2g,
0.24mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, 50 DEG C of heat preservation 2h are warming up to,
Grignard viscosity is measured, viscosity was by 1.0 seconds.Triethylamine (20.24g, 0.2mol) is added, controlling reaction temperature is 100 DEG C -105
DEG C, the reaction was continued 3.5h obtains the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 188g cationics
Body and 31.78g deionized waters；Carbon disulfide (60.8g, 0.8mol) and 40% potassium hydroxide aqueous solution is slowly added dropwise, controls
Reaction temperature is 0 DEG C -25 DEG C；The rate of addition of potassium hydroxide aqueous solution is controlled to be more than carbon disulfide, controls the pH=of reaction solution
8-12；It is added dropwise and is warming up to 40 DEG C, the reaction was continued 4.5h, cooling discharge obtains transparent salmon liquid 318g.
Embodiment 6
Step 1：The synthesis of polyethers cationic intermediate
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask in add in diethylenetriamine (41.27g,
0.4mol) and methanol-water solvent (137g, methanol content 35%)；It opens and stirs, dropwise addition Hydrin (32.37g,
0.35mol), controlling reaction temperature is at 30 DEG C -45 DEG C；After Hydrin is added dropwise, it is warming up to 50 DEG C of heat preservations
1.5h measures grignard viscosity, and viscosity was by 0.9 second.Add 33% trimethylamine (28.66g, 0.16mol), controlling reaction temperature
It it is 100 DEG C -105 DEG C, the reaction was continued 2.5h obtains the transparent water-soluble products of rufous.
Step 2：The synthesis of demulsification water purification one agent
To with thermometer, reflux condenser, speed-adjustable stir four-hole boiling flask among metered 238g cationics
Body and 68g deionized waters；Carbon disulfide (85g, 1.12mol) and 40% sodium hydrate aqueous solution, control reaction is slowly added dropwise
Temperature is 0 DEG C -25 DEG C；The rate of addition of lye is controlled to be more than carbon disulfide, controls the pH=9-11 of reaction solution；Liter is added dropwise
Temperature is to 35 DEG C；The reaction was continued 4.5h, cooling discharge obtain transparent salmon liquid 451g.
Rp demulsification performance evaluation：
The demulsification water purification one agent of above-mentioned case synthesis is salmon liquid, miscible with water arbitrary proportion, and adds Fe2+From
Son compounding.To certain offshore oilfield oily waste water (oil content 19820ppm, turbidity>10000) it is handled, temperature is 60 DEG C, effect
Fruit is preferable, as a result see the table below.
The demulsification water purification one agent henchnmrk test result of table 1
Claims (4)
1. a kind of synthetic method for the water purification one agent that is demulsified, feature are, including：
1) synthesis of polyethers cationic intermediate
By metered primary amine and alcohol-aqueous solvent, wherein alcohol-water quality ratio is 1:1~1:1.5, account for overall reaction system
25wt%~45wt%；Hydrin is added dropwise in stirring, control temperature at 30 DEG C -45 DEG C, primary amine and Hydrin
It is 1 to react molar ratio:0.5~1:0.7；After Hydrin is added dropwise, 45 DEG C of -500 DEG C of heat preservation 1-2h are warming up to, are surveyed
Ding Geshi viscosity, viscosity was by 0.8 second~1.2 seconds；Adding tertiary amine, the reaction was continued, and tertiary amine is 0.4 with the molar ratio of reacting of primary amine:
1~0.65:1, reaction temperature is 10 DEG C -105 DEG C, reaction time 2-4h, obtains the transparent water-soluble products of rufous；
2) synthesis of demulsification water purification one agent
Cationic intermediate and deionized water, mass ratio 3.5 are added in reaction unit:1-6.5:1；Two sulphur are slowly added dropwise
Change carbon and lye, controlling reaction temperature is 0 DEG C -25 DEG C；The rate of addition of lye is controlled to be more than carbon disulfide, controls reaction solution
PH=8.5-12；It being added dropwise and is warming up to 35 DEG C -45 ° DEG C, the reaction was continued 3-5h, cooling discharge obtains transparent salmon liquid,
Wherein cationic intermediate and carbon disulfide reaction molar ratio is 1:2.0~1:3.5.
2. the synthetic method of demulsification water purification one agent according to claim 1, the primary amine is diethylenetriamine, three second
In alkene tetramine, tetraethylenepentamine, pentaethylene hexamine, six ethylene, seven amine, ten amine of seven ethylene, eight amine, eight ethylene, nine amine and nine ethylene
It is a kind of.
3. it is according to claim 1 demulsification water purification one agent synthetic method, the alcohols solvent for methanol, ethyl alcohol and
One kind in isopropanol.
4. it is according to claim 1 demulsification water purification one agent synthetic method, the tertiary amine for trimethylamine, triethylamine and
One kind in triethanolamine.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110872A (en) * | 2018-08-30 | 2019-01-01 | 赵晴晴 | A kind of oilfield sewage demulsification water purification agent and preparation process |
| CN114276549A (en) * | 2021-12-21 | 2022-04-05 | 中海石油(中国)有限公司 | Anionic high-surface-activity organosilicon water purifier and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109110872A (en) * | 2018-08-30 | 2019-01-01 | 赵晴晴 | A kind of oilfield sewage demulsification water purification agent and preparation process |
| CN114276549A (en) * | 2021-12-21 | 2022-04-05 | 中海石油(中国)有限公司 | Anionic high-surface-activity organosilicon water purifier and preparation method thereof |
| CN114276549B (en) * | 2021-12-21 | 2023-02-07 | 中海石油(中国)有限公司 | Anionic high-surface-activity organosilicon water purifier and preparation method thereof |
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