CN106495272B - A kind of binary combination flooding sewage water degreaser and preparation method thereof - Google Patents

A kind of binary combination flooding sewage water degreaser and preparation method thereof Download PDF

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CN106495272B
CN106495272B CN201611029355.9A CN201611029355A CN106495272B CN 106495272 B CN106495272 B CN 106495272B CN 201611029355 A CN201611029355 A CN 201611029355A CN 106495272 B CN106495272 B CN 106495272B
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degreaser
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formaldehyde
binary combination
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CN106495272A (en
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赵世芬
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Tianjin Shunchao Co., Ltd.
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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
    • C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
    • 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
    • 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)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Lubricants (AREA)
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Abstract

The invention belongs to disposing polluted water in oil technical fields, and in particular to a kind of binary combination flooding sewage water degreaser, the degreaser are to obtain Minnich alkali by condensation reaction by benzene methanamine, formaldehyde and cyclohexanone, then react acquisition with alkyl chloride again.Benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride molar ratio be 1:5~10:1.2~2:2.5~5, preferably 1:8:1.5:4.Degreaser of the invention, which has, prepares simple, adaptable, at low cost, oil removal rate up to 95% or more；And the oil recovery that separation generates does not influence subsequent crude oil dehydration, therefore, present invention is generally applicable in the oil removing process of binary combination flooding output water.

Description

A kind of binary combination flooding sewage water degreaser and preparation method thereof
Technical field
The present invention relates to a kind of degreasers for sewage treatment, and in particular to a kind of binary combination flooding sewage water degreaser and Preparation method.
Background technique
The most of late high water content period that all enters in east China major part oil field is widely used to improve oil recovery factor The tertiary oil recovery new technology of polymer flooding technique and binary combination flooding (polymer and surfactant).Binary combination flooding Tar productivity can be significantly improved, is had broad application prospects, but due to gathering in binary composite-driven produced water containing a large amount of Acrylamide and surfactant cause the viscosity of sewage to become larger, and Oil in Sewage Water bead diameter becomes smaller, and cause sewage emulsification tight Weight, processing difficulty are larger.
Conventional treatment process (natural subsidence-coagulant precipitation-filtering) is difficult to obtain binary composite-driven produced water at present It is effectively treated.Another method for removing oil field binary combination flooding output water Crude Oil is chemical method, that is, uses oil removing agent method. Degreaser is broadly divided into following two categories, and element of the first species's multiplicity, deoiling effect is good, but there is preparation process complexity, anti-salt property The shortcomings that difference, higher cost；Another kind of degreaser ingredient is single, and preparation method and technique are relatively simple, the requirement to water quality compared with It is low, but have the shortcomings that deoiling effect is poor.
Patent ZL201410254042.8 " a kind of composite flocculation deoiling agent for oily waste water treatment " uses sulfuric acid Aluminium, magnesium chloride, magnesium hydroxide, bentonite and polyacrylamide are combined, which has dosage few, and oil removal efficiency is high, The features such as preparation is simple, at low cost, but degreaser needs are used with corrosive magnesium hydroxide, the compound is to equipment With stronger corrosiveness.A large amount of magnesium ion and aluminium ion are used in the invention simultaneously, with polymerizeing in binary combination flooding Object or surfactant are easy to happen reaction, generate precipitating, it is difficult to apply in the processing of binary composite-driven produced water.
Summary of the invention
The present invention for currently available technology deficiency and a kind of binary combination flooding sewage water degreaser and its preparation side are provided Method, the degreaser have simple process, low in cost, adaptable, and the feature that deoiling effect is good.
The purpose of the present invention is to provide a kind of binary combination flooding sewage water degreaser, which is by benzene methanamine, formaldehyde Minnich alkali is obtained by condensation reaction with cyclohexanone, then reacts acquisition with alkyl chloride again, molecular formula is as follows:
Wherein R is C8~C12Linear paraffin, preferably R be C10Linear paraffin.
Further, the molar ratio of the benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride be 1:5~10:1.2~2:2.5~ 5, preferably 1:8:1.5:4.
It is another object of the present invention to provide a kind of preparation method of binary combination flooding sewage water degreaser, the preparation being somebody's turn to do Method specifically includes the following steps:
(1) the benzene first of above-mentioned molar ratio is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed Then etoh solvent is added in amine, the additional amount of ethyl alcohol is 10~20 times of benzene methanamine mole, 40 DEG C is warming up to, in stirring speed Rate is that 10~30min is stirred under 300~400rpm, and the cyclohexanone of aforementioned proportion is then added, and temperature rises to 60~70 DEG C, stirring Rate is 400~500rpm, is cooled to 30~35 DEG C after persistently stirring 20min, then with 15% salt acid for adjusting pH value to 2~ 5, obtain mixture A；
(2) it is put into constant pressure funnel after mixing the formaldehyde of above-mentioned molar ratio according to the molar ratio of 1:1 with ethyl alcohol, The temperature of mixture A is adjusted to 60~80 DEG C, the mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise to mixture A In, stir when being added dropwise, rate of addition is 2~3 drops/min, and stirring rate is 300~500rpm, after 3~5h of isothermal reaction oneself So being cooled to room temperature obtains solution B；
(3) for solution B in the case where stirring rate is 200~300rpm, temperature is adjusted to 40~50 DEG C, and above-mentioned molar ratio is added Alkyl chloride then heats to 80~100 DEG C, and stirring rate is adjusted to 300~400rpm, then constant temperature 1~7h of back flow reaction cools down The reaction was continued after to 50 DEG C 0.5~3h, obtains mixture C；
(4) mixture C is cooled to room temperature, be then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive Then formaldehyde places into drying in vacuum oven and for 24 hours, obtains degreaser of the invention.
The reaction equation is as follows:
A kind of binary combination flooding sewage water degreaser, as follows using technical process:
According to oil-containing situation in the binary combination flooding output sewage of oil field, degreaser of the invention is added into sewage, realizes Demulsification and water-oil separating are further processed after recycling petroleum substance for subsequent technique.The specific additional amount of degreaser is as follows:
(1) when oil-containing α >=500mg/L, degreaser, which is added, makes 50~100mg/L of mass concentration of degreaser in sewage；
When (2) 500 ﹥ oil-containing α >=200mg/L, degreaser, which is added, makes 20~50mg/ of mass concentration of degreaser in sewage L；
When (3) 200 ﹥ oil-containing α >=50mg/L, degreaser, which is added, makes 10~20mg/ of mass concentration of degreaser in sewage L；
(4) when oil-containing α < 50mg/L, degreaser, which is added, makes 0.1~10mg/L of mass concentration of degreaser in sewage.
The degreaser of binary combination flooding sewage provided by the invention, hydrophobic long-chain and polar aromatics and cycloalkane are one On a N atom, wherein lipophilic group can be adsorbed onto rapidly on the oil in sewage；The polarity of naphthenic base is lower, is easily formed micella, So additive amount is low；Positively charged ammonium ion is easy to be adsorbed onto the surface of greasy dirt, and at the interval of oxygen, nitrogen and nitrogen, nitrogen 2~3 noncoordinating atoms, the lone pair electrons of coordination atom enter the existing hydridization dsp unoccupied orbital in greasy dirt, form coordination Key, it is prone to which complexing, the flocculation for promoting greasy dirt increases, and then improves the effect to oilfield sewage oil removal treatment.
The present invention is had the following advantages and beneficial effects: compared with prior art
(1) raw material sources of degreaser of the invention are extensive, and synthesis technology is simple, and product is easily obtained and transports preservation；
(2) degreaser of the invention is adaptable, and dosage is few, can meet the needs of environmental protection and oil field development
(3) degreaser of the invention does not contain inorganic flocculation ingredient, and the flocculation ability of the ability that is demulsified and greasy dirt is stronger, point The dehydration of normal crude oil is had little effect from the oil recovery of generation；
(4) degreaser of the invention has the characteristics that oil removal efficiency is high, and the oil removal rate of binary composite-driven produced water is up to 95% More than, more existing medicament improves 45% or more, meets the pretreated requirement of oil removing of binary combination flooding oily wastewater.
Specific embodiment
The present invention is described in further detail below with reference to specific embodiment, and referring to data.It should be understood that these embodiments It is of the invention solely for the purpose of illustration, rather than limit the scope of the invention in any way.
Embodiment 1: degreaser G1And preparation method thereof
(1) degreaser G1Composition, component and molecular formula it is as follows:
Degreaser G1It is reacted by benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride according to molar ratio for 1:5:1.2:2.5 ratio It arrives, molecular formula is as follows:
Wherein R is C8Linear paraffin.
(2) degreaser G1The preparation method is as follows:
1. the benzene methanamine of 1mol is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed, then Solvent 10mol ethyl alcohol is added, is warming up to 40 DEG C, stirs 10min in the case where stirring rate is 300rpm, the ring of 1.2mol is then added Hexanone, temperature rise to 65 DEG C, stirring rate 400rpm, persistently stir 20min after be cooled to 30 DEG C, then with 15% hydrochloric acid PH value is adjusted to 2, obtains mixture A；
2. being put into constant pressure funnel after 5mol formaldehyde is mixed with 5mol ethyl alcohol, the temperature of mixture A is adjusted to 60 DEG C, the mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise in mixture A, is stirred when being added dropwise, rate of addition For 2 drops/min, room temperature is naturally cooling to after stirring rate 300rpm, isothermal reaction 3h and obtains solution B；
3. solution B is in the case where stirring rate is 200rpm, temperature is adjusted to 40 DEG C, and the alkyl chloride of 2.5mol is added, then rises For temperature to 80 DEG C, stirring rate is adjusted to 300rpm, constant temperature back flow reaction 1h, the reaction was continued after being then cooled to 50 DEG C 2h, is mixed Close object C；
4. mixture C is cooled to room temperature, it is then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive first Then aldehyde places into drying in vacuum oven and for 24 hours, obtains degreaser G of the invention1。
Embodiment 2: degreaser G2And preparation method thereof
(1) degreaser G2Composition, component and molecular formula it is as follows:
Degreaser G2It is reacted by benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride according to molar ratio for 1:6:1.8:3 ratio It arrives, molecular formula is as follows:
Wherein R is C9Linear paraffin.
(2) degreaser G2The preparation method is as follows:
1. the benzene methanamine of 1mol is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed, then Solvent 15mol ethyl alcohol is added, is warming up to 40 DEG C, stirs 15min in the case where stirring rate is 330rpm, the ring of 1.8mol is then added Hexanone, temperature rise to 62 DEG C, stirring rate 500rpm, persistently stir 20min after be cooled to 32 DEG C, then with 15% hydrochloric acid PH value is adjusted to 3, obtains mixture A；
2. being put into constant pressure funnel after 6mol formaldehyde is mixed with 6mol ethyl alcohol, the temperature of mixture A is adjusted to 70 DEG C, the mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise in mixture A, is stirred when being added dropwise, rate of addition For 2 drops/min, room temperature is naturally cooling to after stirring rate 350rpm, isothermal reaction 4h and obtains solution B；
3. solution B is in the case where stirring rate is 230rpm, temperature is adjusted to 48 DEG C, and the alkyl chloride of 3mol is added, then heats up To 85 DEG C, stirring rate is adjusted to 320rpm, constant temperature back flow reaction 2h, the reaction was continued after being then cooled to 50 DEG C 1h, is mixed Object C；
4. mixture C is cooled to room temperature, it is then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive first Then aldehyde places into drying in vacuum oven and for 24 hours, obtains degreaser G of the invention2。
Embodiment 3: degreaser G3And preparation method thereof
(1) degreaser G3Composition, component and molecular formula it is as follows:
Degreaser G3It is reacted by benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride according to molar ratio for 1:8:1.5:4 ratio It arrives, molecular formula is as follows:
Wherein R is C10Linear paraffin.
(2) degreaser G3The preparation method is as follows:
1. the benzene methanamine of 1mol is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed, then Solvent 18mol ethyl alcohol is added, is warming up to 40 DEG C, stirs 25min in the case where stirring rate is 370rpm, the ring of 1.5mol is then added Hexanone, temperature rise to 60 DEG C, stirring rate 450rpm, persistently stir 20min after be cooled to 33 DEG C, then with 15% hydrochloric acid PH value is adjusted to 4, obtains mixture A；
2. being put into constant pressure funnel after 8mol formaldehyde is mixed with 8mol ethyl alcohol, the temperature of mixture A is adjusted to 75 DEG C, the mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise in mixture A, is stirred when being added dropwise, rate of addition For 3 drops/min, room temperature is naturally cooling to after stirring rate 400rpm, isothermal reaction 4h and obtains solution B；
3. solution B is in the case where stirring rate is 280rpm, temperature is adjusted to 45 DEG C, and the alkyl chloride of 4mol is added, then heats up To 95 DEG C, stirring rate is adjusted to 350rpm, constant temperature back flow reaction 5h, the reaction was continued after being then cooled to 50 DEG C 0.5h, is mixed Close object C；
4. mixture C is cooled to room temperature, it is then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive first Then aldehyde places into drying in vacuum oven and for 24 hours, obtains degreaser G of the invention3。
Embodiment 4: degreaser G4And preparation method thereof
(1) degreaser G4Composition, component and molecular formula it is as follows:
Degreaser G4It reacts to obtain for 1:10:2:5 ratio according to molar ratio by benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride, Molecular formula is as follows:
Wherein R is C12Linear paraffin.
(2) degreaser G4The preparation method is as follows:
1. the benzene methanamine of 1mol is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed, then Solvent 20mol ethyl alcohol is added, is warming up to 40 DEG C, stirs 30min in the case where stirring rate is 400rpm, the hexamethylene of 2mol is then added Ketone, temperature rise to 70 DEG C, stirring rate 480rpm, persistently stir 20min after be cooled to 35 DEG C, then with 15% hydrochloric acid tune PH value is saved to 5, obtains mixture A；
2. be put into constant pressure funnel after 10mol formaldehyde is mixed with 10mol ethyl alcohol, adjust mixture A temperature to 80 DEG C, the mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise in mixture A, is stirred when being added dropwise, speed is added dropwise Degree is 3 drops/min, is naturally cooling to room temperature after stirring rate 500rpm, isothermal reaction 5h and obtains solution B；
3. solution B is in the case where stirring rate is 300rpm, temperature is adjusted to 50 DEG C, and the alkyl chloride of 5mol is added, then heats up To 100 DEG C, stirring rate is adjusted to 400rpm, constant temperature back flow reaction 7h, the reaction was continued after being then cooled to 50 DEG C 3h, is mixed Object C；
4. mixture C is cooled to room temperature, it is then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive first Then aldehyde places into drying in vacuum oven and for 24 hours, obtains degreaser G of the invention4。
5 degreaser G of embodiment1Field application
Multi-purpose station M2Water be binary combination flooding output water, test process scale be 100m3/ d, water oil content 628mg/L, sewage salinity 5685mg/L utilize degreaser G of the invention1To multi-purpose station M2Sewage carry out oil removal treatment, remove Finish G1Dosage be 5.6kg/d, the concentration for adding degreaser in sewage after degreaser is 56mg/L, and oil content drops after processing As low as 17.0mg/L, oil content reduces by 97.3%, reaches technique requirement.
6 degreaser G of embodiment2Field application
Multi-purpose station M5Water be binary combination flooding output water, test process scale be 50m3/ d, water oil content 355mg/ L, sewage salinity 3256mg/L utilize degreaser G of the invention2To multi-purpose station M5Sewage carry out oil removal treatment, degreaser G2 Dosage be 1.5kg/d, the concentration for adding degreaser in sewage after degreaser is 30.0mg/L, and oil content is reduced to after processing 10.65mg/L, oil content reduce by 97.0%, reach technique requirement.
7 degreaser G of embodiment3Field application
Multi-purpose station M25Water be binary combination flooding output water, test process scale be 80m3/ d, water oil content 925mg/L, sewage salinity 12560mg/L utilize degreaser G of the invention3To multi-purpose station M25Sewage carry out oil removal treatment, Degreaser G3Dosage be 6.4kg/d, the concentration for adding degreaser in sewage after degreaser is 80mg/L, oil content after processing It is reduced to 16.7mg/L, oil content reduces by 98.2%, reaches technique requirement.
8 degreaser G of embodiment4Field application
Multi-purpose station M12Water be binary combination flooding output water, test process scale be 60m3/ d, water oil content 128mg/L, sewage salinity 27650mg/L utilize degreaser G of the invention4To multi-purpose station M12Sewage carry out oil removal treatment, Degreaser G4Dosage be 0.9kg/d, the concentration for adding degreaser in sewage after degreaser is 15mg/L, oil content after processing It is reduced to 6.1mg/L, oil content reduces by 95.2%, reaches technique requirement.

Claims (4)

1. a kind of binary combination flooding sewage water degreaser, which is characterized in that its molecular formula is as follows:
Wherein, R C8~C13Straight-chain alkyl.
2. a kind of binary combination flooding sewage water degreaser according to claim 1, which is characterized in that the R is C10It is straight Chain alkylene.
3. the preparation method of binary combination flooding sewage water degreaser according to claim 1 or 2, which is characterized in that the preparation Method specifically includes the following steps:
(1) benzene methanamine is added in the three-necked flask that electric mixer, reflux condensing tube, thermometer are housed, solvent is then added Ethyl alcohol, the additional amount of ethyl alcohol are 10~20 times of benzene methanamine mole, are warming up to 40 DEG C, are 300~400rpm in stirring rate Then cyclohexanone is added in 10~30min of lower stirring, temperature rises to 60~70 DEG C, and stirring rate is 400~500rpm, is persistently stirred 30~35 DEG C are cooled to after mixing 20min, then obtains mixture A to 2~5 with 15% salt acid for adjusting pH value；
(2) it is put into constant pressure funnel after mixing formaldehyde according to 1: 1 molar ratio with ethyl alcohol, adjusts the temperature of mixture A The mixture of formaldehyde and ethyl alcohol in constant pressure funnel is added drop-wise in mixture A by degree to 60~80 DEG C, is stirred when being added dropwise It mixes, rate of addition is 2~3 drops/min, and stirring rate is 300~500rpm, is naturally cooling to room temperature after 3~5h of isothermal reaction and obtains To solution B；
(3) for solution B in the case where stirring rate is 200~300rpm, temperature is adjusted to 40~50 DEG C, and alkyl chloride is added, then heats up To 80~100 DEG C, stirring rate is adjusted to 300~400rpm, constant temperature 1~7h of back flow reaction, continues after being then cooled to 50 DEG C anti- 0.5~3h is answered, mixture C is obtained；
(4) mixture C being cooled to room temperature, be then transferred in round-bottomed flask, vacuum distillation removes solvent and excessive formaldehyde, Then it places into drying in vacuum oven and for 24 hours, obtains degreaser of the invention；
The benzene methanamine, formaldehyde, cyclohexanone and alkyl chloride molar ratio be 1: 5~10: 1.2~2: 2.5~5.
4. the preparation method of binary combination flooding sewage water degreaser according to claim 3, which is characterized in that the benzene first Amine, formaldehyde, cyclohexanone and alkyl chloride molar ratio be 1: 8: 1.5: 4.
CN201611029355.9A 2016-11-14 2016-11-14 A kind of binary combination flooding sewage water degreaser and preparation method thereof Active CN106495272B (en)

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