CN103318984A - Method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite - Google Patents
Method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite Download PDFInfo
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Abstract
The invention relates to the field of industrial water treatment and in particular relates to a method for treating polymer flooding oil-extraction wastewater by employing organic modified sepiolite. The method comprises the following steps: 1) acid activation, namely adding a sepiolite raw material into a hydrochloric acid solution, mixing, stirring, filtering, washing, and drying to obtain sepiolite powder subjected to acid activation; 2) thermal activation, namely roasting and dehydrating the sepiolite powder subjected to acid activation, and cooling and grinding to obtain sepiolite powder subjected to thermal activation; 3) organic modification, namely adding the sepiolite powder subjected to thermal activation into an ethanol aqueous solution of cetyl trimethyl ammonium bromide, mixing, stirring, filtering, washing, drying and grinding to prepare the organic modified sepiolite powder; and 4) adsorption, namely regulating the pH value of the polymer flooding oil-extraction wastewater by using an acid, adding a water-soluble aluminum salt, adding the organic modified sepiolite powder obtained in the step 3) for adsorption, stirring or shaking, standing and settling. The sepiolite serves as a raw material and is low-price and readily available, the process for activation and modification of the sepiolite is simple, and the sepiolite is non-toxic and harmless, has an obvious adsorption effect, rapid in treatment and high in adsorption amount.
Description
Technical field
The present invention relates to the Treatment of Industrial Water field, particularly relate to the poly-waste water that contains of processing in the polymer flooding oil-extraction technology, come active adsorption partially hydrolyzed polyacrylamide (HPAM) wherein with this.
Background technology
Because China's oilfield exploitation steps into the middle and later periods, for improving oil recovery factor, improve the profit velocity ratio, production Crude Oil content is improved, begun extensively to adopt the polymer flooding oil-extraction technology, relatively inexpensive partially hydrolyzed polyacrylamide (HPAM) is widely used in oil recovery in this case.But the oil extraction waste water that contains partially hydrolyzed polyacrylamide that thereupon produces becomes the technical barrier of polymer flooding large scale application because intractability increases.Therefore, need to seek the method for a kind of middle partially hydrolyzed polyacrylamide (HPAM) that can effectively dispose of sewage.
Although partially hydrolyzed polyacrylamide does not have toxicity, yet the monomer acrylamide after its degraded is two class carcinogenic substances, can the peripheral nervous system of humans and animals be damaged.Simultaneously, the polymkeric substance in the entered environment can become the source of microbial nutrition material, promotes the accelerates multiplication of microorganism.
Contain a large amount of polymkeric substance HPAM in the polymer flooding oil-extraction wastewater, increased the viscosity of water, make water take oily ability and strengthen, greatly increased the stability of oily(waste)water, increased the difficulty that the polymer flooding oil-extraction purification of waste water is processed, reduced processing efficiency.Thereby be necessary the partially hydrolyzed polyacrylamide that contains in the poly-waste water is removed from water, improve the water quality of waste water, reduce the viscosity of water, be beneficial to the processing of follow-up pollutent.
At present, the processing that contains the HPAM oil extraction-generated waste water has been become a key difficult problem that affects field produces.Existing polymer flooding oil-extraction wastewater treatment technology mainly contains chemical degradation method, biological degradation method, chemical flocculation and absorption method.
Chemical degradation mainly contains oxidative degradation, photodegradation and photocatalytic degradation.Although it can be degraded to acrylamide monomer with HPAM, acrylamide monomer can cause secondary pollution to water resources, thereby has limited the range of application of chemical degradation method.
The biological method polymer-contained sewage mainly is to utilize microorganism to pass through the effect of its certain enzyme, take polyacrylamide as nutrition source, in its metabolism and growth process polyacrylamide is converted into small organic molecule and inorganics.But because biological degradation will be subject to the impact of the factors such as potential of hydrogen, temperature, salinity, oxygen, nutriment, thereby its application also is restricted.
Chemical flocculation uses flocculation agent to effects such as the voltage contracting of colloidal solid, static neutralization, absorption, and the structure of destruction colloid so that colloidal solid takes off surely, precipitates, is then swept congregation removal polymkeric substance by volume in water, higher to the clearance of polymkeric substance.It is larger that but the weak point of this method is dosing, and general chemical feeding quantity is identical with pending polymer concentration.
The problems such as there is deficiency more or less in actual applications in above these methods, and are many such as restricted condition, that cost is high, effect is bad, maintenance of the equipment is difficult.
Summary of the invention
The object of the present invention is to provide a kind of organically-modified sepiolite to process the method for polymer flooding oil-extraction waste water, the method adsorption effect is obvious, and adsorptive capacity is high.
For achieving the above object, the technical solution adopted in the present invention is that a kind of organically-modified sepiolite is processed the method for polymer flooding oil-extraction waste water, it is characterized in that it comprises the steps:
1) acid activation: it is the hydrochloric acid soln of 13wt%-15wt% that the sepiolite raw material is added concentration, mix and blend, and suction filtration, washing, oven dry obtain the acid activation sepiolite powder;
2) thermal activation: the roasting of acid activation sepiolite powder is anhydrated, and cooling, grinding obtain the sepiolite powder after the thermal activation;
3) organically-modified: as the sepiolite powder after the thermal activation to be added in the aqueous ethanolic solution of cetyl trimethylammonium bromide, wherein the mass ratio of the sepiolite powder after the thermal activation and cetyl trimethylammonium bromide is at 10-50:1, mix and blend, filtration, washing, oven dry, grinding make organically-modified sepiolite powder;
4) absorption: the pH value of driving oil extraction waste water with sour telomerized polymer is to 5-6, and adding water dissolvable aluminium salt makes Al
3+Concentration is 10mg/L-25mg/L, adds that the organically-modified sepiolite powder of gained adsorbs in the step 3) again, and the adsorption process temperature stirs or concussion, then standing sedimentation at 30 ℃ to 50 ℃.
In the embodiment of optimizing, process control is as follows:
Solid-to-liquid ratio in the step 1) (proportioning of sepiolite and hydrochloric acid soln) is 1g:8-25ml for 1:8-25g/ml(), churning time is 1h-3h.
Step 2) maturing temperature is 250 ℃-350 ℃ in, and roasting time is at 2h-8h, and grinding reaches 400 orders-800 order.
Solid-to-liquid ratio in the step 3) (proportioning of the sepiolite powder after the thermal activation and the aqueous ethanolic solution of cetyl trimethylammonium bromide) is 1g:8-25ml for 1:8-25g/ml(), churning time is 1h-3h, grinds to reach 600 orders-1000 order.
Water dissolvable aluminium salt is any one or the two kinds of mixing by any proportioning in Tai-Ace S 150 and the aluminum chloride in the step 4), solid-to-liquid ratio (proportioning of organically-modified sepiolite powder and polymer flooding oil-extraction waste water) is 1:300-600g/ml, the adsorption process temperature is 30 ℃-50 ℃, and stirring or concussion time are 1.5-3h.
In the embodiment of more optimizing, process control is as follows:
Step 2) maturing temperature is 300 ℃ in, grinds to reach 600 orders;
Mix 1.5h under the room temperature in the step 3), bake out temperature is 40 ℃, grinds to reach 800 orders;
Select Glacial acetic acid to regulate the pH value to 5-6 in the step 4), water dissolvable aluminium salt is selected Tai-Ace S 150, and the adsorption process temperature is 40 ℃, and the concussion time is 1.5h.
Sepiolite (Mg
8(H
2O)
4[Si
6O
15]
2(OH)
48H
2O) be the moisture magnesia silicate clay mineral of a kind of natural fiber shape, crystal structure model belongs to chain and stratiform transition type structure, be characterized in octahedra at two-layer tetrahedral si-o film therebetween one deck magnesia, the 3 D stereo skeleton structure that silicon-oxy tetrahedron and magnesia octahedron are interconnected to by common vertex, zeolite cavity and the space of running through total are arranged, specific surface area is large, has 900m
2The theoretical surface of/g is long-pending.And contain in a large number towards the Si-OH of outside group, organic compound had stronger avidity, can with gaseous state or liquid organic reaction agent direct effect, generate the humatite derivative.And in real market, the sepiolite price is cheap, and therefore the present invention selects sepiolite as raw material it to be carried out activation modification.
The acid activation of sepiolite can be removed on the one hand the carbonate impurity that is distributed in the sepiolite with Sample Purification on Single, removes impurity in its duct, increases its pore volume; On the other hand, the hydrogen ion in the acid replaces its interlayer calcium, magnesium, potassium and sodium ion, makes it have active hydrogen atom, generates new surface and improves its surface property, modifies its aperture and structure, increases micro-porosity, improves its absorption, purification and decoloring ability.Cross the structure that conference directly destroys sepiolite such as the concentration of tartaric acid, form at last silicate.Concentration is crossed and is hanged down then and can so that processing is not thorough, not reach activation effect.Therefore the present invention has adopted 13%-15% hydrochloric acid.
In the structure of sepiolite, there is triformed water, i.e. planar water, crystal water and hydroxy water.Water in the sepiolite crystalline structure can progressively lose in heat-processed.By high-temperature roasting, can effectively remove planar water in the crystalline structure (comprising the planar water in the planar water and duct between fiber), in clay, form new active face, make the Si-OH base change the Si-O tetrahedral structure into, thereby enlarged the passage in the crystal, and the structure screen work is constant, specific surface area increases, surfactivity improves, and adsorptive power strengthens.If treatment temp is too high, then not only to remove the planar water in the structure, and can remove crystal water and hydroxy water, thereby destroyed crystalline structure, experiment shows losing of crystal water and hydroxy water, and the absorption property of sepiolite is descended.Therefore the present invention has selected 250 ℃-300 ℃ temperature to carry out roasting.
Afrodite is for itself possessing absorption property because its unique multi-pore channel and microvoid structure make, and sepiolite forms thereby present electronegativity by the silica skeleton in addition, and this makes it particularly evident to cationic adsorptive power.The cats product grafting of positively charged is to the sepiolite the time, the charges of different polarity are inhaled mutually and are easy to realize, and make sepiolite be changed into the Activated Sepiolite that organises of positively charged by original electronegativity, thereby electronegative property material had powerful adsorption function.And because different hydrocarbon chains is introduced on the surface, improved the hydrophobic lipophilicity on surface, increased organic adhesive property.The present invention has selected cats product cetyl trimethylammonium bromide (CTAB) according to theory, as the organic modifiers that sepiolite is carried out modification.Cetyl trimethylammonium bromide (CTAB) can not only active adsorption in the sepiolite surface, and its moderate hydrocarbon chain length can not stop up the sepiolite duct, and can increase the viscosifying power to macromolecular material HPAM.
Being raise by low of temperature slowly dissociated the HPAM molecule, and long molecular chain is just submissive, viscosity diminishes, and HPAM more easily is adsorbed on the sorbent material, and adsorption rate at this moment is greater than its desorption rate, the amount of sorbent material absorption HPAM molecule is increased gradually, until reach running balance.When temperature is too high, can makes the increasing amount of its desorption rate greater than the increasing amount of adsorption rate, and the amount of sorbent material absorption HPAM molecule is reduced gradually, until new running balance.Through experiment, also when 40 ℃ of left and right sides, maximum value appears in the adsorptive capacity of sorbent material.Also just in time the temperature with oil extraction waste water is consistent for this, so the present invention processes oil extraction waste water, can save heating and the energy that consumes.After adsorption time had surpassed 1.5h, the adsorptive capacity of sorbent material remained unchanged substantially.
Because aluminum ion (Al
3+) HPAM is had throwing out, can so that the HPAM viscosity reduction, take off steady, assemble, so that macromole HPAM can not stop up sepiolite absorption duct, even the parcel sorbent material.Viscosity reduction, take off HPAM steady, after assembling, so that sorbent material is to its adsorption efficiency increase at double.And Al
3+Adding make more even that sorbent material disperses, settling velocity is faster.Adopt on this basis 800 purpose modified meerschaum powder sorbent materials, adsorb completely, the good separation effect is just arranged after leaving standstill 30min.
The invention has the beneficial effects as follows: adopting sepiolite is that starting material are cheap and easy to get, simple to its activating modification process, and nontoxic.In addition, present method consumption less but adsorption effect obviously and process rapidly, adsorptive capacity is high.For being in backland oil recovery base, can process on the spot, on the spot discharging, device requirement is few, and cost is low, quite is suitable for processing the polymkeric substance in the oil extraction waste water.
Embodiment
Embodiment 1:
Modified meerschaum powder preparation: get the 6g liuyang hunan and produce refining sepiolite powder, join 100ml, concentration is the hydrochloric acid soln of 15wt%, at 25 ℃ of lower mix and blend 1.5h; The vacuum pump suction filtration, washing, oven dry obtains the acid activation sepiolite powder; Acid activation sepiolite powder obtained in the previous step places retort furnace, and regulating temperature is 300 ℃, behind the roasting 4h, takes out cooling, grinds the sepiolite powder that reaches after 600 orders obtain thermal activation; Get the sepiolite powder 5g after the thermal activation obtained in the previous step, add the 0.3g cetyl trimethylammonium bromide, place together 100ml ethanol water (ethanol and water volume ratio 1:1) solution, 25 ℃ of lower mix and blend 1.5h, the vacuum pump suction filtration, distilled water and ethanol alternately wash repeatedly, then 40 ℃ of oven dry in the baking oven, and at last grinding reaches 800 orders and obtains organically-modified sepiolite powder.
The processing of polymer flooding oil-extraction waste water: getting 100mlHPAM concentration is the polymer flooding oil-extraction waste water of 100mg/l, and it is 5 that Glacial acetic acid is regulated the pH value, and the aqueous solution that adds Tai-Ace S 150 is regulated Al
3+Concentration is to 25mg/l, adds the organically-modified sepiolite powder of 0.0200g, with the solution temperature control at 40 ℃, vibration 1.5h,, leave standstill the 0.5h sedimentation.
The adsorption effect characterizing method: get supernatant liquor, use starch-cadmium iodide method, measure its absorbancy, and the concentration that obtains supernatant liquor according to concentration and the absorbancy typical curve of this HPAM solution; Then basis
{ q: adsorptive capacity (mg/g); C
0: HPAM starting point concentration (mg/L); C: HPAM concentration after the absorption; M: sorbent material dosage; V
0: wastewater volume } calculate the adsorptive capacity of sorbent material.
Absorption property: processing HPAM concentration is the polymer flooding oil-extraction waste water of 100mg/l, recording its average adsorptive capacity is 477mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 200mg/l, recording its average adsorptive capacity is 920.5mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 300mg/l, and recording its average adsorptive capacity is 1413.4mg/g.The method adsorption effect is obvious, adsorbs high.
Embodiment 2:
A kind of method of modified meerschaum adsorption of hydrolyzation polyacrylamide, it comprises the steps:
1) acid activation: it is the hydrochloric acid soln of 13wt% that the sepiolite raw material is added concentration, mix and blend, and suction filtration, washing, oven dry obtain the acid activation sepiolite powder; At 1:8g/ml, churning time is at 1h for solid-to-liquid ratio (proportioning of sepiolite and hydrochloric acid soln).
2) thermal activation: the roasting of acid activation sepiolite powder is anhydrated, and cooling, grinding obtain the sepiolite powder after the thermal activation; Maturing temperature is 250 ℃, and roasting time is at 2h, and grinding reaches 400 orders;
3) organically-modified: with in the aqueous ethanolic solution of the adding of the sepiolite powder after thermal activation cetyl trimethylammonium bromide (ethanol and water volume ratio 1:1), wherein the mass ratio of the sepiolite powder after the thermal activation and cetyl trimethylammonium bromide is at 10:1, mix and blend, filtration, washing, oven dry, grinding make organically-modified sepiolite powder; Solid-to-liquid ratio (proportioning of the sepiolite powder after the thermal activation and the aqueous ethanolic solution of cetyl trimethylammonium bromide) is at 1:8g/ml, and churning time 1h grinds and reaches 600 orders;
4) absorption: regulate the pH value to 5 that moisture solution polyacrylamide polymers is driven oil extraction waste water with acid, add water dissolvable aluminium salt and make Al
3+Concentration is 10mg/l, adds that the organically-modified sepiolite powder of gained adsorbs in the step 3) again, and the adsorption process temperature stirs or concussion, then standing sedimentation at 30 ℃.
Described water dissolvable aluminium salt is Tai-Ace S 150, and solid-to-liquid ratio (proportioning of organically-modified sepiolite powder and polymer flooding oil-extraction waste water) is 1:300g/ml, and the adsorption process temperature is at 30 ℃, and stirring or concussion time are 3h, standing sedimentation.
The adsorption effect characterizing method is with embodiment 1.Absorption property: processing HPAM concentration is the polymer flooding oil-extraction waste water of 100mg/l, recording its average adsorptive capacity is 483.6mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 200mg/l, recording its average adsorptive capacity is 948.3mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 300mg/l, and recording its average adsorptive capacity is 1446.5mg/g.The method adsorption effect is obvious, and adsorptive capacity is high.
Embodiment 3:
A kind of method of modified meerschaum adsorption of hydrolyzation polyacrylamide, it comprises the steps:
1) acid activation: it is the hydrochloric acid soln of 15wt% that the sepiolite raw material is added concentration, mix and blend, and suction filtration, washing, oven dry obtain the acid activation sepiolite powder; At 1:25g/ml, churning time is at 3h for solid-to-liquid ratio (proportioning of sepiolite and hydrochloric acid soln).
2) thermal activation: the roasting of acid activation sepiolite powder is anhydrated, and cooling, grinding obtain the sepiolite powder after the thermal activation; Maturing temperature is 350 ℃, and roasting time is at 8h, and grinding reaches 800 orders;
3) organically-modified: with in the aqueous ethanolic solution of the adding of the sepiolite powder after thermal activation cetyl trimethylammonium bromide (ethanol and water volume ratio 1:1), wherein the mass ratio of the sepiolite powder after the thermal activation and cetyl trimethylammonium bromide is at 50:1, mix and blend, filtration, washing, oven dry, grinding make organically-modified sepiolite powder;
Solid-to-liquid ratio (proportioning of the sepiolite powder after the thermal activation and the aqueous ethanolic solution of cetyl trimethylammonium bromide) is at 1:25g/ml, and churning time 3h grinds and reaches 1000 orders;
4) absorption: regulate the pH value to 6 that moisture solution polyacrylamide polymers is driven oil extraction waste water with acid, add water dissolvable aluminium salt and make Al
3+Concentration is 25mg/l, adds that the organically-modified sepiolite powder of gained adsorbs in the step 3) again, and the adsorption process temperature stirs or concussion, then standing sedimentation at 50 ℃.
The mixing (quality of Tai-Ace S 150 and aluminum chloride respectively accounts for 1/2) that described water dissolvable aluminium salt is Tai-Ace S 150 and aluminum chloride, solid-to-liquid ratio (proportioning of organically-modified sepiolite powder and polymer flooding oil-extraction waste water) is 1:600g/ml, the adsorption process temperature is at 50 ℃, and stirring or concussion time are 3h.
The adsorption effect characterizing method is with embodiment 1.Absorption property: processing HPAM concentration is the polymer flooding oil-extraction waste water of 100mg/l, recording its average adsorptive capacity is 462.2mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 200mg/l, recording its average adsorptive capacity is 853.3mg/g, processing HPAM concentration is the polymer flooding oil-extraction waste water of 300mg/l, and recording its average adsorptive capacity is 1286.3mg/g.The method adsorption effect is obvious, and adsorptive capacity is high.
Claims (8)
1. the method for an organically-modified sepiolite processing polymer flooding oil-extraction waste water is characterized in that it comprises the steps:
1) acid activation: it is the hydrochloric acid soln of 13wt%-15wt% that the sepiolite raw material is added concentration, mix and blend, and suction filtration, washing, oven dry obtain the acid activation sepiolite powder;
2) thermal activation: the roasting of acid activation sepiolite powder is anhydrated, and cooling, grinding obtain the sepiolite powder after the thermal activation;
3) organically-modified: as the sepiolite powder after the thermal activation to be added in the aqueous ethanolic solution of cetyl trimethylammonium bromide, wherein the mass ratio of the sepiolite powder after the thermal activation and cetyl trimethylammonium bromide is at 10-50:1, mix and blend, filtration, washing, oven dry, grinding make organically-modified sepiolite powder;
4) absorption: the pH value of driving oil extraction waste water with sour telomerized polymer is to 5-6, and adding water dissolvable aluminium salt makes Al
3+Concentration is 10mg/l-25mg/l, adds that the organically-modified sepiolite powder of gained adsorbs in the step 3) again, and the adsorption process temperature stirs or concussion, then standing sedimentation at 30 ℃ to 50 ℃.
2. a kind of organically-modified sepiolite according to claim 1 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that, solid-to-liquid ratio is 1:8-25g/ml in the step 1), and churning time is 1h-3h.
3. a kind of organically-modified sepiolite according to claim 1 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that step 2) in maturing temperature be 250 ℃-350 ℃, roasting time is 2h-8h, grinds to reach 400 orders-800 order.
4. a kind of organically-modified sepiolite according to claim 1 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that, solid-to-liquid ratio is 1:8-25g/ml in the step 3), and churning time is 1h-3h, grinds to reach 600 orders-1000 order.
5. a kind of organically-modified sepiolite according to claim 1 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that, water dissolvable aluminium salt is any one or the two kinds of mixing by any proportioning in Tai-Ace S 150 and the aluminum chloride in the step 4), the solid-to-liquid ratio of organically-modified sepiolite and polymer flooding oil-extraction waste water is 1:300-600g/ml, the adsorption process temperature is 30 ℃-50 ℃, and stirring or concussion time are 1.5-3h.
6. a kind of organically-modified sepiolite according to claim 3 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that step 2) in maturing temperature be 300 ℃, grind and reach 600 orders.
7. a kind of organically-modified sepiolite according to claim 4 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that, mixes 1.5h under the room temperature in the step 3), and bake out temperature is at 40 ℃, and grinding reaches 800 orders.
8. a kind of organically-modified sepiolite according to claim 5 is processed the method for polymer flooding oil-extraction waste water, it is characterized in that, select Glacial acetic acid to regulate the pH value to 5-6 in the step 4), water dissolvable aluminium salt is selected Tai-Ace S 150, the adsorption process temperature is 40 ℃, and the concussion time is 1.5h.
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