CN110420482B - Composite flocculant for treating oil sand mine tailings and method for treating mature fine tailings - Google Patents
Composite flocculant for treating oil sand mine tailings and method for treating mature fine tailings Download PDFInfo
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- CN110420482B CN110420482B CN201910748708.8A CN201910748708A CN110420482B CN 110420482 B CN110420482 B CN 110420482B CN 201910748708 A CN201910748708 A CN 201910748708A CN 110420482 B CN110420482 B CN 110420482B
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- B01D21/01—Separation of suspended solid particles from liquids by sedimentation using flocculating agents
Abstract
The invention provides a composite flocculant for treating oil sand mine tailings and a method for treating mature fine tailings, wherein the flocculant comprises the following components: 30-70% of polyacrylamide; 5-30% of poly dimethyl diallyl ammonium chloride; 2-20% of a calcium-containing substance, wherein the calcium-containing substance is one or more of calcium carbonate and calcium oxide; 1-20% of an adsorbent, wherein the adsorbent is one or more of diatomite and activated carbon. The composite flocculant has high settling speed; after solid-liquid separation, the supernatant is clear, the content of suspended matters is low, and the turbidity is small; the floc formed after flocculation is compact, and the solid content of the bottom mud is high; the temperature adaptability is strong. The composite flocculant has good solubility, can be directly added with dry powder by matching with a proper dosing device, saves a flocculant dissolving device and reduces the investment. The invention can be used for treating mature fine tailings; and the method can also be used for secondary dehydration of the bottom mud, and after the bottom mud is added, the capillary suction time is short, the yield stress is moderate, and the dehydration rate is high.
Description
Technical Field
The invention belongs to the technical field of tailing treatment, and particularly relates to a composite flocculant for treating oil sand tailings and a method for treating cured fine tailings.
Background
Oil sands refer to deposited sands rich in natural bitumen, also known as "tar sands". In essence, oil sands are a natural mixture consisting of bitumen, sand, mineral-rich clay, and water. The oil sand components and the content thereof are different in each region; typical oil sands compositions, in mass fractions, are: the asphalt content is 3-20%, the inorganic substance accounts for 80-85%, and the balance is 3-6% of water. The oil sand ore can be extracted and further extracted and separated to obtain the synthetic crude oil. Oil sand bitumen oil having high density, high viscosity, high hydrocarbon ratio and high metal content can be extracted from the oil sand. In large-scale industrial production, the oil sand is usually mined and refined by hot alkaline water extraction, and the extraction rate is 1m per mining3Will produce 1.5m of asphalt3The tailings of (2).
The main components of the oil sand tailings are water, clay, sand and residual asphalt. The tailings are usually discharged into a tailing dam to realize solid-liquid separation, so that water is recycled. Coarse sand particles settle out rapidly from the slurry, while fine particles form a stable dispersion in suspension, which after about one or two years forms a slurry with a solids content of about 30%, known as mature fine placer. After this, the settling becomes slower and slower, and the tailings remain in this circulation state for typically decades or even centuries. Mature fine placer is a byproduct of oil sand mining and is a mixture of bitumen, sandy soil, fine sand, fine clay particles and industrial wastewater. The waste water contains a large amount of organic and inorganic components, and due to the characteristics of large volume, poor consolidation capability, poor water release capability and the like, the waste water causes serious damage to the environment, and the waste water has attracted great attention to the economy and the environment of people due to the consumption of water, the pollution of the atmosphere and the land, the imbalance of soil and the like.
Scholars at home and abroad carry out a great deal of research on the treatment of mature fine tailings to find a method for dewatering the mature fine tailings to the maximum extent, thereby achieving the purpose of shortening the reclamation time of the tailings. Wherein, flocculation is a method for rapidly and effectively realizing solid-liquid separation; the suspended particles in water or liquid are made to agglomerate or form floc, so as to speed up the coagulation of particles and separate solid from liquid. Flocculants are mainly positively (negatively) charged groups that come into close proximity with the difficult-to-separate particles or grains that are negatively (positively) charged in water, lowering their potential and leaving them in an unstable state, and using their polymeric nature, concentrate and separate these grains by physical or chemical means.
The flocculating agent is added when the mature fine tailings are treated, and the following effects are mainly achieved: 1) neutralizing the charge of the colloidal particles, destabilizing the stable particles, thereby aggregating together, enlarging the particles, and settling down; 2) the bridging function can be realized among the single particles, so that the original small particles form larger micelles and are settled; 3) while reducing suspended matters, can also remove heavy metals, organic matters and the like in water. The current common method treats mature fine sand tailings by using polyacrylamide as a flocculating agent. However, when the existing flocculating agent is used for treatment, the sedimentation rate is slow, and after flocculation, the supernatant has a lot of suspended matters and large turbidity, the water content of the bottom mud is high, and the treatment effect needs to be improved.
Disclosure of Invention
In view of the above, the application provides a composite flocculant for treating oil sand mine tailings and a method for treating mature fine tailings.
The invention provides a composite flocculant for treating oil sand mine tailings, which comprises the following components in percentage by mass:
30-70% of polyacrylamide;
5-30% of poly dimethyl diallyl ammonium chloride;
2-20% of a calcium-containing substance, wherein the calcium-containing substance is one or more of calcium carbonate and calcium oxide;
1-20% of an adsorbent, wherein the adsorbent is one or more of diatomite and activated carbon.
Preferably, the polyacrylamide has a viscosity average molecular weight of 800 to 1200 ten thousand.
Preferably, the composite flocculant comprises 5-15% of calcium-containing substances, and the calcium-containing substances are calcium carbonate or calcium oxide.
Preferably, the composite flocculant comprises the following components in percentage by mass:
30-70% of polyacrylamide;
5-30% of poly dimethyl diallyl ammonium chloride;
2-20% of a calcium-containing substance;
0.5-19% of diatomite;
0.5-1% of activated carbon.
Preferably, the diatomite is modified diatomite modified by organic matters, and the surface of the diatomite is charged.
Preferably, the composite flocculant is solid particles in appearance, and the density at 20 ℃ is 0.7-0.8 g/cm3And the pH value of the 0.5% aqueous solution is 7-8.
The invention provides a method for treating mature fine tailings, which comprises the following steps:
adding a flocculating agent into the aged fine tailings, and then carrying out solid-liquid separation to obtain a supernatant and bottom mud;
the flocculant is a composite flocculant as described hereinbefore.
Preferably, the flocculant is directly added in a dry powder form, and the adding amount is 100-400 g/ton dry weight ratio.
Preferably, the flocculating agent is added in the form of a solution with the concentration of 200-500 ppm.
Preferably, the processing method further comprises: and adding the flocculating agent into the obtained bottom mud to obtain a secondary dewatered substance.
Compared with the prior art, the invention provides a composite flocculant for treating oil sand mine tailings, which mainly comprises two organic polymer flocculating substances of polyacrylamide and poly dimethyl diallyl ammonium chloride, and an inorganic calcium-containing substance and an adsorbent are used as coagulation aiding substances for compounding. In the invention, the molecular weight of the poly dimethyl diallyl ammonium chloride is smaller than that of polyacrylamide, and the poly dimethyl diallyl ammonium chloride has good coagulation effect on fine particle substances in tailings; the polyacrylamide has large molecular weight generally, can play a role of bridging, further coagulates the formed micelle into larger floc, and the combination of the polyacrylamide and the larger floc can adapt to a tailing system with wider particle size distribution. The composite flocculant of the invention has rapid reaction and high sedimentation speed; after solid-liquid separation, the supernatant is clear, the content of suspended matters is low, and the turbidity is small; the floc formed after flocculation is compact, and the solid content of the bottom mud is high; the temperature adaptability is strong, especially low temperature.
In addition, the composite flocculant has better solubility, can be directly added with dry powder by matching with a proper dosing device, saves a flocculant dissolving device and reduces the investment. The composite flocculant can be used for treating mature fine tailings and the like; and the method can also be used for secondary dehydration of the bottom mud, and after the bottom mud is added, the capillary suction time is short, the yield stress is moderate, and the dehydration rate is high.
Drawings
Fig. 1 is a graph of the particle size distribution of mature fine tailings in some embodiments of the present invention;
FIG. 2 is a settling curve using a composite flocculant in example 2 of the present invention;
FIG. 3 is a graph showing the sedimentation curve of polyacrylamide used in example 2 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a composite flocculant for treating oil sand mine tailings, which comprises the following components in percentage by mass:
30-70% of polyacrylamide;
5-30% of poly dimethyl diallyl ammonium chloride;
2-20% of a calcium-containing substance, wherein the calcium-containing substance is one or more of calcium carbonate and calcium oxide;
1-20% of an adsorbent, wherein the adsorbent is one or more of diatomite and activated carbon.
The composite flocculant provided by the invention is mainly used for treating mature oil sand fine tailings, can quickly realize solid-liquid separation of the mature oil sand fine tailings, effectively removes suspended matters, COD (chemical oxygen demand) and asphalt in supernatant, reduces turbidity and improves the solid content of bottom mud.
According to the mass percentage, the composite flocculant provided by the invention comprises 30-70% of Polyacrylamide (PAM), and the content of the PAM is preferably 40-65%. And the composite flocculant comprises 5-30% of poly dimethyl diallyl ammonium chloride (PDADMAC). In the examples of the present invention, the viscosity average molecular weight of the polyacrylamide is 800 to 1200 ten thousand (generally referred to in the art as the relative molecular weight, room temperature). The ionicity of the polyacrylamide is determined according to different tailing sample screens, and the anionic and/or nonionic types are commonly used for oil sands. The relative molecular weight of the poly dimethyl diallyl ammonium chloride is 30-60 ten thousand, and the dissolving time is 5-10 min.
In the invention, the molecular weight of the poly dimethyl diallyl ammonium chloride is smaller than that of polyacrylamide, and the poly dimethyl diallyl ammonium chloride has good coagulation effect on fine particle substances in tailings; the polyacrylamide has large molecular weight generally, can play a role of bridging, further coagulates the formed micelle into larger floc, and the combination of the polyacrylamide and the larger floc can adapt to a tailing system with wider particle size distribution.
In addition, the solubility of the poly dimethyl diallyl ammonium chloride is very good, and the poly dimethyl diallyl ammonium chloride is compounded with polyacrylamide for use, so that the defect of long dissolution time of the polyacrylamide can be overcome; and the dry powder can be directly added by matching with a proper dosing device, a flocculating agent dissolving device is omitted, and the investment is reduced.
The invention is a composite flocculant compounded by the two organic polymer flocculating substances and the inorganic coagulation aiding substance; and it includes 2-20% calcium-containing substance and 1-20% adsorbent. Wherein the calcium-containing substance is one or more of calcium carbonate and calcium oxide, and is preferably calcium carbonate. The adsorbent is one or more of diatomite and activated carbon and mainly plays a role in adsorption.
In the embodiment of the invention, the composite flocculant preferably comprises 5-15% of calcium-containing substances; the calcium-containing substance can be calcium carbonate or calcium oxide. Calcium carbonate is preferably used in the present invention, and functions thereof are as follows: the surface adsorption and coagulation aiding are adopted to assist PAM and PDADMAC to generate a flocculation effect. The examples of the present invention generally employ calcium carbonate or calcium oxide, although magnesium salts may have some other particular uses, but are not suitable for use in the system of the present invention.
Preferably, the composite flocculant comprises the following main components in percentage by weight: 30-70% of polyacrylamide; 5-30% of poly dimethyl diallyl ammonium chloride; 2-20% of calcium carbonate; 0.5-19% of diatomite; 0.5-1% of activated carbon.
The diatomite is preferably modified diatomite modified by organic matters, and the content of the diatomite is preferably 5-19%; the adsorption performance of the diatomite after organic modification is enhanced compared with the prior diatomite, the surface of the diatomite is charged, and the diatomite has a better removing effect on suspended matters in tailings. In particular, the modified diatomite particlesThe degree is 70 to 90 micrometers, for example, about 75 micrometers; SiO 22The content of (A) is 65-75%, and the bulk density is 0.40g/cm3Left and right. The activated carbon is preferably coconut shell activated carbon, and the particle size can be 0.5-2 mm.
According to the embodiment of the invention, the compound flocculant can be prepared by adopting various commercially available component raw materials and adopting a mixer through conventional operations such as mixing, drying and the like; the appearance of the product is gray solid particles, and the effective content is more than or equal to 88 percent. The effective content is the mass content of solids (solid content for short, wherein the dry powder raw materials of polyacrylamide and poly dimethyl diallyl ammonium chloride both contain water). The density (20 ℃) of the composite flocculant is generally 0.7-0.8 g/cm3(ii) a The pH value of the 0.5 wt% aqueous solution is 7-8.
The composite flocculant is mainly used for treating the oil sand mature fine tailings, can quickly realize solid-liquid separation of the mature oil sand fine tailings, effectively remove suspended matters, COD (chemical oxygen demand) and asphalt in supernatant, reduce turbidity, improve the solid content of bottom mud, and is convenient to use and low in cost.
Correspondingly, the embodiment of the invention provides a method for treating mature fine tailings, which comprises the following steps: adding a flocculating agent into the aged fine tailings, and then carrying out solid-liquid separation to obtain a supernatant and bottom mud; the flocculant is a composite flocculant as described hereinbefore.
The main components of the oil sand tailings are water, clay, sand and residual asphalt. When the tailings are discharged into a tailings dam, coarse sand particles are rapidly separated from the slurry by sedimentation, while fine particles form stable dispersions in the suspension, which dispersions, after a period of time, form a gelatinous slurry with a solids content of about 30% by weight, which is called mature oil sand fine sand, mature fine tailings for short. In the examples of the present invention, the properties of the mature fine tailings can be seen in table 1 and fig. 1, and fig. 1 is a particle size distribution diagram of the mature fine tailings of the examples of the present invention.
TABLE 1 Properties of mature fine tailings in some examples of the invention
In the embodiment of the invention, the composite flocculant is adopted to treat mature fine tailings, a certain amount of the flocculant is added into the mature fine tailings, and after flocculation is carried out for a certain time, solid-liquid separation is carried out to respectively obtain supernatant and bottom mud. In some embodiments of the invention, the composite flocculant is directly added in a dry powder form, a dissolving device is not needed for dissolving the flocculant, and the input can be reduced; the addition amount can be 100-400 g/ton dry weight ratio, such as 250g/ton dry weight ratio and 300g/ton dry weight ratio. Here, the dosage is the ratio of the dry amount of flocculant (grams) to the dry amount of tailings sample (tons). In other embodiments of the invention, the composite flocculant is added in the form of a solution with the concentration of 200-500 ppm.
In addition, the retention time of the flocculant in the embodiment of the invention can be more than 2 hours, and the treatment temperature is generally normal temperature; the solid-liquid separation can be realized by adopting a separation mode commonly used in the field.
The prior art can not use the same medicament to carry out secondary dehydration on the settled bottom mud, and corresponding dissolving equipment is required to be added when one medicament is added, thereby increasing the input cost. The processing method according to the embodiment of the present invention preferably further includes: and adding the flocculating agent into the obtained bottom mud to obtain a secondary dewatered substance.
The composite flocculant can also be used for secondary dehydration of the bottom mud, and after the composite flocculant is added into the bottom mud, the capillary suction time is short, the yield stress is moderate, the dehydration rate is high, and the investment cost is further reduced.
For further understanding of the present application, the composite flocculant for treating oil sands tailings and the treatment method of mature fine tailings provided herein are specifically described below with reference to examples. It should be understood, however, that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention, which is defined by the following examples.
Meanwhile, various raw material reagents and equipment referred to in the specification of the present application are commercially available and can be used as they are without further description.
In the following examples, the tailings samples are commercially available mature fine tailings, the properties of which are shown in table 1 and fig. 1; the particle size of the modified diatomite is about 75 mu m; SiO 22The content of (A) is 65-75%, and the bulk density is 0.40g/cm3Left and right. The activated carbon is coconut shell activated carbon, and the granularity is 0.5-2 mm.
Example 1
The composite flocculant is prepared by mixing 50% of polyacrylamide (with the viscosity average molecular weight of 1000 ten thousand and the ionic degree of 30%), 30% of polydimethyldiallylammonium chloride (with the relative molecular weight of 50 ten thousand), 10% of calcium carbonate, 9.5% of modified diatomite and 0.5% of activated carbon.
The flocculating agent is gray solid particles in appearance, the effective content is more than or equal to 88 percent, and the density (20 ℃) is 0.7-0.8 g/cm3And the pH value of the 0.5% aqueous solution is 7-8.
Example 2
After shaking the tailing sample thoroughly, 1000g was weighed and placed in a 1L beaker. The sample was stirred with a stirrer at 350rpm for 3 minutes, then the speed was reduced to 160rpm and 0.05% of the aqueous flocculant solution prepared in example 1 was added.
Once the flocculant solution is added, timing is started, the time for adding the flocculant is 1min, and stirring is continued for 1min after the addition is finished. The stirrer was turned off and the flocculated tailing sample was transferred to a 1L graduated paper graduated cylinder. The timekeeping was started quickly and the sedimentation height versus time sedimentation curve was recorded.
Meanwhile, a sedimentation experiment is carried out by adding the composite flocculant and the single polyacrylamide with different dosage. Referring to FIGS. 2 and 3, FIG. 2 shows the settling curves of the composite flocculant of the present invention, and the dosage is 100g/ton, 200g/ton, 300g/ton and 400 g/ton. FIG. 3 shows the sedimentation curves of polyacrylamide at doses of 200g/ton, 300g/ton and 400g/ton, respectively. Comparing fig. 1 and fig. 2, it can be seen on the sedimentation curve that 100g/ton of polyacrylamide alone hardly sedimented and thus no sedimentation curve was obtained, whereas with 100g/ton of the composite flocculant, the sample solids sedimented significantly; the sedimentation velocity of the tailing samples treated by the composite flocculant is obviously higher than that of the tailing samples treated by PAM alone when the dosage is 200g/ton, 300g/ton and 400 g/ton. Using 300g/ton of the composite flocculant, sedimentation was almost complete within 2 seconds.
The results after treatment are shown in table 2, and it can be seen from table 2 that compared with polyacrylamide, the composite flocculant provided by the invention has the advantages of high settling speed, clear supernatant after solid-liquid separation, small turbidity, high solid content of bottom mud and better treatment effect.
TABLE 2 results of the flocculated samples
Example 3
65% of polyacrylamide (with viscosity average molecular weight of 1000 ten thousand and ionic degree of 30%), 5% of polydimethyldiallylammonium chloride (with relative molecular weight of 50 ten thousand), 10% of calcium carbonate, 19% of modified diatomite and 1% of activated carbon are mixed to prepare the composite flocculant.
The flocculating agent is gray solid particles in appearance, the effective content is more than or equal to 88 percent, and the density (20 ℃) is 0.7-0.8 g/cm3And the pH value of the 0.5% aqueous solution is 7-8.
Example 4
The bottom sludge produced after the first stage flocculation of example 2 was dewatered a second time using the flocculant prepared in example 3. The method specifically comprises the following steps:
after settling for 2h in the first stage flocculation, the supernatant was decanted and the bottom sludge was placed in a beaker as a sample for the second stage dehydration. The sediment sample was stirred at 200rpm for 1min, followed by the addition of 0.2% of the flocculant solution and the start of the timekeeping. The adding time of the flocculating agent is 1min, and the stirring is continued for 1min after the adding is finished. The stirrer was turned off and the flocculated sample was quickly transferred to a 1L graduated cylinder.
Meanwhile, the dehydration effects of the composite flocculant and the single polyacrylamide with different dosage are compared.
The dewatering effect is measured by dewatering rate, yield stress and capillary suction time:
dehydration rate: (water content of the bottom mud before dehydration-water content of the bottom mud after adding flocculant to dehydrate)/water content of the bottom mud before dehydration is multiplied by 100%;
yield stress: measuring with Brookfield RVDV-3T viscometer, and testing with paddle rotor at 0.5rpm to obtain yield stress of the sample at 25 deg.C;
capillary Suction Time (CST): the samples were tested using a TRITON ELECTRONICS LIMITED TYPE 304M capillary suction timekeeper to obtain capillary suction time, which is used to reflect the sample's ability to dewater.
The specific results are shown in Table 3, and it can be seen from Table 3 that the addition of 100g/ton dry weight ratio of the flocculant can achieve good dewatering effect, while the addition of polyacrylamide requires 250g/ton dry weight ratio to achieve the effect, which is still inferior to the present application.
TABLE 3 results of dewatering of the bottom sludge with flocculant
According to the embodiments, the composite flocculant provided by the invention has the advantages of rapid reaction and high settling speed; after solid-liquid separation, the supernatant is clear, the content of suspended matters is low, and the turbidity is small; the floc formed after flocculation is compact, and the solid content of the bottom mud is high; the temperature adaptability is strong, especially low temperature. In addition, the composite flocculant has better solubility, can be directly added with dry powder by matching with a proper dosing device, saves a flocculant dissolving device and reduces the investment. The composite flocculant can be used for treating mature fine tailings and the like; and the method can also be used for secondary dehydration of the bottom mud, and after the bottom mud is added, the capillary suction time is short, the yield stress is moderate, and the dehydration rate is high.
The above description is only a preferred embodiment of the present invention, and it should be noted that various modifications to these embodiments can be implemented by those skilled in the art without departing from the technical principle of the present invention, and these modifications should be construed as the scope of the present invention.
Claims (9)
1. The composite flocculant for treating the oil sand mine tailings is characterized by being solid particles in appearance and comprising the following components in percentage by mass:
30-70% of polyacrylamide;
5-30% of poly dimethyl diallyl ammonium chloride;
2-20% of a calcium-containing substance, wherein the calcium-containing substance is one or more of calcium carbonate and calcium oxide;
1-20% of an adsorbent, wherein the adsorbent is one or more of diatomite and activated carbon;
the molecular weight of the poly dimethyl diallyl ammonium chloride is smaller than that of polyacrylamide, and the viscosity-average molecular weight of the polyacrylamide is 800-1200 ten thousand; the relative molecular weight of the polydimethyldiallylammonium chloride is 30-60 ten thousand.
2. The composite flocculant according to claim 1, wherein the composite flocculant comprises 5-15% of a calcium-containing substance, and the calcium-containing substance is calcium carbonate or calcium oxide.
3. The composite flocculant according to claim 1, characterized by comprising the following components in percentage by mass:
30-70% of polyacrylamide;
5-30% of poly dimethyl diallyl ammonium chloride;
2-20% of a calcium-containing substance;
0.5-19% of diatomite;
0.5-1% of activated carbon.
4. The composite flocculant of claim 3, wherein the diatomaceous earth is modified with an organic substance, and the surface of the diatomaceous earth is charged.
5. The composite flocculant according to any one of claims 1 to 4, wherein the density of the composite flocculant at 20 ℃ is 0.7 to 0.8g/cm3And the pH value of the 0.5% aqueous solution is 7-8.
6. A treatment method of mature fine tailings comprises the following steps:
adding a flocculating agent into the aged fine tailings, and then carrying out solid-liquid separation to obtain a supernatant and bottom mud;
the flocculant is the composite flocculant of any one of claims 1 to 5.
7. The treatment method according to claim 6, wherein the flocculating agent is directly added in a dry powder form, and the adding amount is 100-400 g/ton dry weight ratio.
8. The treatment method according to claim 6, wherein the flocculant is added in the form of a solution having a concentration of 200 to 500 ppm.
9. The process of any one of claims 6 to 8, further comprising: and adding the flocculating agent into the obtained bottom mud to obtain a secondary dewatered substance.
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| CN104356294A (en) * | 2014-11-14 | 2015-02-18 | 天津大港油田滨港集团博弘石油化工有限公司 | Polyacrylamide flocculant and preparation method thereof |
| CN107442293A (en) * | 2017-08-31 | 2017-12-08 | 中国矿业大学 | Grey method drops in a kind of superfine granule ub-bituminous coal selective flocculation reverse flotation |
| CN107840424A (en) * | 2017-11-04 | 2018-03-27 | 南京银茂铅锌矿业有限公司 | A kind of method of the efficient separate-recycling of lead-zinc metallogenic belt beneficiation wastewater |
| CN108033533A (en) * | 2017-12-27 | 2018-05-15 | 山东诺尔生物科技有限公司 | A kind of thin tailing flucculation process of oil-sand |
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