CN109095572A - Polysilicate aluminum ferric sulfate flocculant, preparation method and application - Google Patents
Polysilicate aluminum ferric sulfate flocculant, preparation method and application Download PDFInfo
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- CN109095572A CN109095572A CN201710476250.6A CN201710476250A CN109095572A CN 109095572 A CN109095572 A CN 109095572A CN 201710476250 A CN201710476250 A CN 201710476250A CN 109095572 A CN109095572 A CN 109095572A
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- sulfate
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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
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/08—Chemical Oxygen Demand [COD]; Biological Oxygen Demand [BOD]
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- Hydrology & Water Resources (AREA)
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- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of polysilicate aluminum ferric sulfate flocculants, preparation method and application, belong to oil gas field technical field of waste water purification.Polysilicate aluminum ferric sulfate flocculant is prepared by the following steps to obtain: 1) by the sodium metasilicate solution soluble in water for obtaining 0.2~0.5mol/L of concentration, adjusting solution ph is 2.1~5, and 10~30min of stirring polymerization, obtains polysilicon acid at room temperature；2) aluminum sulfate and ferrous sulfate are added according to molar ratio, (Al+Fe)/Si=0.5~2.2, Al/Fe=0.5~2.2,10~30min of stirring polymerization at room temperature, stand 20~28h of curing to get.The flocculant is exclusively used in oilfield drilling liquid waste processing, and flocculation sedimentation effect is good, and single dose adds and to add dosage small, and COD removal rate is high, and processed waste water COD index is lower than national emission standard.
Description
Technical field
The present invention relates to a kind of polysilicate aluminum ferric sulfate flocculants, also relate to the preparation method of the flocculant and answer
With belonging to oil gas field technical field of waste water purification.
Background technique
Rejected well drilling liquid is one of main pollution sources of oil and gas industry.With the fast development of petroleum industry, drilling fluid
Type is continuously increased, and the type of drilling fluid additive is also increasing, and composition is extremely complex, and COD index is up to thousands of millis
Gram per liter, outlet processing is up to standard extremely difficult.With continuing to increase for drilling fluid dosage, Discarded Drilling Materials liquid measure is also increasing.
Rejected well drilling liquid, well-drilling waste water are not handled or are dealt with improperly, can cause seriously to pollute to natural environment.According to statistics, each well
The mud amount of generation about 100~200m3, flatly 3000 to 4000m common oil/gas well is bored, rejected well drilling liquid is close after complete well
300m3.According to annual 150~220 mouthfuls of calculating of newly-increased drilling well, Discarded Drilling Materials liquid measure should not be underestimated, if without safe and harmlessization
Processing certainly will generate ecological environment and seriously affect, cause environmental pollution hidden danger.Rejected well drilling liquid is as industrial gas oil
Primary pollution source, it has also become the big technical problem of the one of oil gas field environmental protection.
Currently, common inorganic polymer flocculant is aluminium salt and molysite in wastewater treatment, as aluminium polychloride (PAC),
Bodied ferric sulfate (PFS), the two has their own advantages in flocculation treatment, but effect is owed in the well-drilling waste water of processes composition complexity
Good, not only dosage is big, costly, and waste water COD index is also difficult to up to standard.There is studies have shown that by inorganic flocculating agent and organic-flocculation
Agent be used in compounding can enhanced flocculation performance, reduce processing cost, but in practical applications reagent cost reduce it is not significant and more
Kind flocculant adds inconvenient benefit simultaneously, and enforcement difficulty increases.
Poly-aluminum-ferric-silicate-sulfate (PAFSS) can integrate the advantages of poly-aluminium, Polyferric Sulfate and polysilicon acid flocculant, while avoid wadding a quilt with cotton
Because using, remaining aluminum concentration is high, Polyferric Sulfate remnants coloration is big, polysilicon acid stability difference disadvantage after poly-aluminium for solidifying water outlet, in flocculation process
In simultaneously play charge neutrality, adsorption bridging and sedimentation screen catch effect etc., reach preferable treatment effect.Currently, " integrated wastewater row
Put standard " do not provide chlorinity index in waste water also, but chloride ion content is closely bound up with human lives, and chlorine ion concentration is excessively high
It will cause the bitter saline taste of drinking-water, corrosive pipeline and the salinization of soil, it is serious to be also detrimental to health.As society is to water process
The continuous improvement of quality requirement, limitation chloride ion concentration of emission have become inexorable trend, the application of flocculant containing chlorine such as PAC etc.
It will suffer exit, PAFSS can effectively avoid secondary pollution without pollution elements such as chlorine.
Poly-aluminum-ferric-silicate-sulfate synthesis technology is complicated, cumbersome in the prior art, and generated time is long, is unable to satisfy
The requirement that rejected well drilling liquid scene is quickly handled, and the existing processing for the PAFSS flocculant of coking wastewater to waste liquid of drilling
Less effective, it is therefore desirable to develop a kind of new PAFSS flocculant for being exclusively used in oilfield drilling liquid waste processing.
Summary of the invention
The object of the present invention is to provide a kind of polysilicate aluminum ferric sulfate flocculant for being exclusively used in oilfield drilling liquid waste processing,
Flocculating effect is good, and COD removal rate is high, and it is small to add dosage.
Meanwhile the present invention also provides a kind of preparation methods of polysilicate aluminum ferric sulfate flocculant.
Finally, the present invention provides a kind of application of polysilicate aluminum ferric sulfate flocculant again.
In order to achieve the goal above, the technical scheme adopted by the invention is that:
Polysilicate aluminum ferric sulfate flocculant is prepared by the following steps to obtain:
1) by the sodium metasilicate solution soluble in water for obtaining 0.2~0.5mol/L of concentration, adjusting solution ph is 2.1~5, room
The lower stirring 10~30min of polymerization of temperature, obtains polysilicon acid (PAS)；
2) aluminum sulfate and ferrous sulfate are added according to molar ratio, (Al+Fe)/Si=0.5~2.2, Al/Fe=0.5~
2.2,10~30min of stirring polymerization, stands 20~28h of curing, obtains polysilicate aluminum ferric sulfate (PAFSS) at room temperature.
Solution ph is adjusted in step 1) can be used sulfuric acid or sodium hydroxide solution, and adjustment speed first quick and back slow, such as uses
The sulfuric acid of volume fraction 20% quickly adjusts pH value to 6, then is slowly adjusted to pH 2~5, to avoid PAS when close to neutrallty condition
Quickly cohesion, sulfuric acid dosage are 8~15mL.
Step 1), 2) in sodium metasilicate, aluminum sulfate, ferrous sulfate be crystalline state.
Step 1), 2) the middle speed stirred is 80~300r/min.
The time of curing is stood preferably for 24 hours in step 2).
The preparation method of polysilicate aluminum ferric sulfate flocculant, steps are as follows:
1) by the sodium metasilicate solution soluble in water for obtaining 0.2~0.5mol/L of concentration, adjusting solution ph is 2.1~5, room
The lower stirring 10~30min of polymerization of temperature, obtains polysilicon acid (PAS)；
2) aluminum sulfate and ferrous sulfate are added according to molar ratio, (Al+Fe)/Si=0.5~2.2, Al/Fe=0.5~
2.2,10~30min of stirring polymerization, stands 20~28h of curing, obtains polysilicate aluminum ferric sulfate (PAFSS) at room temperature.
Solution ph is adjusted in step 1) can be used sulfuric acid or sodium hydroxide solution, and adjustment speed first quick and back slow, such as uses
The sulfuric acid of volume fraction 20% quickly adjusts pH value to 6, then is slowly adjusted to pH 2~5, to avoid PAS when close to neutrallty condition
Quickly cohesion, sulfuric acid dosage are 8~15mL.
Step 1), 2) in sodium metasilicate, aluminum sulfate, ferrous sulfate be crystalline state.
Step 1), 2) the middle speed stirred is 80~300r/min.
The time of curing is stood preferably for 24 hours in step 2).
The application of polysilicate aluminum ferric sulfate flocculant, specifically: waste water to be processed (with tap water) is first diluted to COD value
600~1100mg/L adds polysilicate aluminum ferric sulfate to 0.5~7g/L of final concentration, flocculation sedimentation.Waste liquid of drilling spy's needle
To rejected well drilling liquid Centrifugal Effluent Treatment, need to dilute 0~5 times with tap water before treatment according to the difference of water quality, make COD value between
Between 600~1100mg/L, polysilicate aluminum ferric sulfate flocculant is added to 0.5~7g/L of optimal use concentration.
Beneficial effects of the present invention:
Polysilicate aluminum ferric sulfate flocculant is exclusively used in oilfield drilling liquid waste processing in the present invention, and flocculation sedimentation effect is good,
Single dose adds and to add dosage small, and COD removal rate is high, and processed waste water COD index is lower than national emission standard.Polysilicate sulfuric acid
The form of ferro-aluminum crystal is in branch shape branch, and branch shape structure is made of numerous grid cells, forms large stretch of network on the whole
Structure, flocculant surface are in compact lamella accumulation shape, and molecular structure is close, which is conducive to adsorption bridging effect and precipitating
Net catches the performance of effect.
The preparation process of polysilicate aluminum ferric sulfate flocculant is simple in the present invention, easy to operate, synthesizes in 1 hour, and 24 is small
It can be used after Shi Chenhua, live rapid preparing, requirement can be met.
Detailed description of the invention
Fig. 1 is the microstructure phenogram that embodiment 2 prepares polysilicate aluminum ferric sulfate flocculant.
Specific embodiment
Only invention is further described in detail for following embodiments, but does not constitute any limitation of the invention.
Embodiment 1
The preparation step of polysilicate aluminum ferric sulfate flocculant is as follows in the present embodiment:
1) by the crystalline sodium disilicate solution soluble in water for obtaining concentration 0.2mol/L, the sulfuric acid using volume fraction 20% is fast
Velocity modulation section solution ph is to 6, then is slowly adjusted to 5, polymerize 10min at room temperature with the mixing speed of 80r/min, obtains polysilicon acid
(PAS)；
2) crystalline sulfuric acid aluminium is added in the solution of step 1) according to molar ratio and crystalline sulfuric acid is ferrous, makes rubbing for Al, Fe
The ratio of your quality sum and the molal weight of Si is that the ratio of the molal weight of 0.5, Al and the molal weight of Fe is 0.5, room
10min is polymerize with the mixing speed of 80r/min under temperature, then stands curing 28h, obtains polysilicate aluminum ferric sulfate (PAFSS).
Application of the polysilicate aluminum ferric sulfate flocculant in terms of oilfield drilling liquid waste processing, specifically: by Henan Oil Field
Secrete the contaminated product system waste drilling mud unstability water outlet of 160-1 well with tap water dilute 4 times to COD value be 1000mg/L, thereto
The polysilicate aluminum ferric sulfate of above-mentioned preparation is added to final concentration of 0.5g/L, the COD value drop of flocculation water outlet is measured after flocculation sedimentation
For 111.36mg/L ﹤ 150mg/L, reach secondary discharge standard in " integrated wastewater discharge standard " GB 8978-1996.
Embodiment 2
The preparation step of polysilicate aluminum ferric sulfate flocculant is as follows in the present embodiment:
1) by the crystalline sodium disilicate solution soluble in water for obtaining concentration 0.35mol/L, using the sulfuric acid of volume fraction 20%
Solution ph is quickly adjusted to 6, then is slowly adjusted to 3.5,20min is polymerize with the mixing speed of 180r/min at room temperature, is gathered
Silicic acid (PAS)；
2) crystalline sulfuric acid aluminium is added in the solution of step 1) according to molar ratio and crystalline sulfuric acid is ferrous, makes rubbing for Al, Fe
The ratio of your quality sum and the molal weight of Si is that the ratio of the molal weight of 1.25, Al and the molal weight of Fe is 1.25,
20min is polymerize with the mixing speed of 180r/min at room temperature, then stands curing for 24 hours, obtains polysilicate aluminum ferric sulfate (PAFSS).
Fig. 1 is the microstructure phenogram of polysilicate aluminum ferric sulfate, and A is the microstructure for amplifying 100 times in figure, and B is to put
Big 200 times of microstructure.It can be seen in fig. 1 that the form of polysilicate aluminum ferric sulfate is in branch shape branch, surface is compact
Lamella aggregation, illustrates that its molecular structure is close, and branch shape branch is conducive to play adsorption bridging effect and the sedimentation screen effect of catching.
It can be seen from figure 1b the whole branch shape structure of polysilicate aluminum ferric sulfate is made of numerous grid cells, and entirety forms greatly
The network structure of piece enhances the effect of catching of flocculated net.
Application of the polysilicate aluminum ferric sulfate flocculant in terms of oilfield drilling liquid waste processing, specifically: by Henan Oil Field
It is 860mg/L that 137-1 well polymeric system waste liquid of drilling unstability water outlet, which dilutes 3 times to COD value with tap water, is added thereto
The polysilicate aluminum ferric sulfate of preparation is stated to final concentration of 2g/L, the COD value that flocculation water outlet is measured after flocculation sedimentation is reduced to
84.28mg/L ﹤ 150mg/L reaches secondary discharge standard in " integrated wastewater discharge standard " GB 8978-1996.
Embodiment 3
The preparation step of polysilicate aluminum ferric sulfate flocculant is as follows in the present embodiment:
1) by the crystalline sodium disilicate solution soluble in water for obtaining concentration 0.5mol/L, the sulfuric acid using volume fraction 20% is fast
Velocity modulation section solution ph is to 6, then is slowly adjusted to 2.1, at room temperature with the mixing speed polyase 13 0min of 300r/min, obtains poly- silicon
Sour (PAS)；
2) crystalline sulfuric acid aluminium is added in the solution of step 1) according to molar ratio and crystalline sulfuric acid is ferrous, makes rubbing for Al, Fe
The ratio of your quality sum and the molal weight of Si is that the ratio of the molal weight of 2.2, Al and the molal weight of Fe is 2.2, room
With the mixing speed polyase 13 0min of 300r/min under temperature, then curing 20h is stood, obtains polysilicate aluminum ferric sulfate (PAFSS).
Application of the polysilicate aluminum ferric sulfate flocculant in terms of oilfield drilling liquid waste processing, specifically: by Henan Oil Field
Secreting 137-1 well contaminated product system waste drilling mud unstability water outlet to be diluted to COD value with tap water is 600mg/L, is added thereto
To final concentration of 2g/L, the COD value that flocculation water outlet is measured after flocculation sedimentation is reduced to the polysilicate aluminum ferric sulfate of above-mentioned preparation
66.2mg/L ﹤ 150mg/L reaches secondary discharge standard in " integrated wastewater discharge standard " GB 8978-1996.
Comparative example 1
The preparation step of poly silicate aluminium ferric flocculating agent is as follows in this comparative example:
1) waterglass is diluted with water to SiO2Mass content be 3% solution, with dilute sulfuric acid adjust solution ph be
2, curing 2 hours are stood, polymerization of silicic acid solution is obtained；
2) polymerization of silicic acid solution is mixed with aluminum sulfate and ferrum sulfuricum oxydatum solutum, makes the quality sum of Al and Fe in mixed solution
Mass ratio with Si is that the mass ratio of 2:1, Al and Fe are 2:1, is quickly stirred evenly, and curing is stood.But this method is simultaneously
Stable poly silicate aluminium ferric flocculating agent is not obtained, therefore can not carry out subsequent floc test.
Comparative example 2
The preparation step of poly silicate aluminium ferric flocculating agent is as follows in this comparative example:
1) waterglass is diluted with water to SiO2Mass content be 3% solution, with dilute sulfuric acid adjust solution ph be
2, curing 2 hours are stood, polymerization of silicic acid solution is obtained；
2) polymerization of silicic acid solution is mixed with aluminum sulfate and ferrum sulfuricum oxydatum solutum, makes the sum of mole of Al and Fe in mixed solution
The ratio between mole with Si is that the ratio between mole of 2:1, Al and Fe are 2:1, is quickly stirred evenly, and curing is stood.But this method is still
Stable poly silicate aluminium ferric flocculating agent is not obtained, therefore can not carry out subsequent floc test yet.
Test example
1, Henan Oil Field secretes the flocculation treatment of 160-1 well contaminated product system waste drilling mud unstability water outlet
Raw water sample COD value 4150mg/L, COD value 1000mg/L after tap water dilutes 4 times select low molecule inorganic flocculating agent
Ferrous sulfate, iron chloride, aluminium chloride, aluminum sulfate and macromolecule inorganic flocculating agent aluminium polychloride (PAC), bodied ferric sulfate
(PFS), polyaluminum ferric chloride (PAFC), polymeric aluminum sulfate iron (PAFS) and embodiment 1 prepare polysilicate aluminum ferric sulfate
(PAFSS), it is added into after dilution respectively in water sample according to adding concentration in the following table 1, compares the flocculating effect of each flocculant, table
Listed in 1 PAC, PFS, PAFSS, iron chloride, aluminium chloride, aluminum sulfate and PAFC add concentration and water outlet COD value, it is not ugly
The flocculating effect of PAC, PFS is not good enough compared with PAFSS out, and the flocculating effect of ferrous sulfate, PAFS are poor, substantially not stratified, does not survey
Its data.
The flocculating effect of table 1 PAC, PFS and PAFSS compare
2, the flocculation treatment of Henan Oil Field 137-1 well polymeric system waste liquid of drilling unstability water outlet
Raw water sample COD value 2650mg/L, COD value 860mg/L after tap water dilutes 3 times select macromolecule inorganic flocculating agent
Aluminium polychloride (PAC) and embodiment 2 prepare polysilicate aluminum ferric sulfate (PAFSS), according to adding concentration in the following table 1 respectively for it
It is added after diluting in water sample, compares the flocculating effect of both flocculants, test result see the table below 2.
The flocculating effect of table 2 PAC, PAFSS compare
From table 2, it is not difficult to find out that, the flocculating effect of PAC is not good enough compared with PAFSS.
3, Henan Oil Field secretes the flocculation treatment of 137-1 well contaminated product system waste drilling mud unstability water outlet
Raw water sample COD value 2650mg/L, COD value 600mg/L after tap water dilution select the polymerization of macromolecule inorganic flocculating agent
Aluminium chloride (PAC) and embodiment 3 prepare polysilicate aluminum ferric sulfate (PAFSS), are added into respectively according to concentration is added in the following table 1
After dilution in water sample, the flocculating effect of both flocculants is compared, test result see the table below 3.
The flocculating effect of table 3 PAC, PAFSS compare
From table 3, it is not difficult to find out that, the flocculating effect of PAC is not good enough compared with PAFSS.
Claims (7)
1. polysilicate aluminum ferric sulfate flocculant, it is characterised in that: be prepared by the following steps to obtain:
1) by the sodium metasilicate solution soluble in water for obtaining 0.2~0.5mol/L of concentration, adjusting solution ph is 2.1~5, at room temperature
Stirring 10~30min of polymerization, obtains polysilicon acid；
2) aluminum sulfate and ferrous sulfate, (Al+Fe)/Si=0.5~2.2, Al/Fe=0.5~2.2, room is added according to molar ratio
Temperature 10~30min of lower stirring polymerization, stand 20~28h of curing to get.
2. flocculant according to claim 1, it is characterised in that: step 1), 2) in sodium metasilicate, aluminum sulfate, ferrous sulfate
It is crystalline state.
3. flocculant according to claim 1, it is characterised in that: step 1), 2) the middle speed stirred is 80~300r/
min。
4. the preparation method of polysilicate aluminum ferric sulfate flocculant, it is characterised in that: steps are as follows:
1) by the sodium metasilicate solution soluble in water for obtaining 0.2~0.5mol/L of concentration, adjusting solution ph is 2.1~5, at room temperature
Stirring 10~30min of polymerization, obtains polysilicon acid；
2) aluminum sulfate and ferrous sulfate, (Al+Fe)/Si=0.5~2.2, Al/Fe=0.5~2.2, room is added according to molar ratio
Temperature 10~30min of lower stirring polymerization, stand 20~28h of curing to get.
5. the preparation method according to claim 4, it is characterised in that: step 1), 2) in sodium metasilicate, aluminum sulfate, sulfuric acid it is sub-
Iron is crystalline state.
6. the preparation method according to claim 4, it is characterised in that: step 1), 2) the middle speed stirred is 80~300r/
min。
7. the application of polysilicate aluminum ferric sulfate flocculant as described in any one of claims 1 to 3, it is characterised in that: will be wait locate
Wastewater dilution is managed to 600~1100mg/L of COD value, adds polysilicate aluminum ferric sulfate to 0.5~7g/L of final concentration, flocculation sedimentation
?.
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| CN110374529A (en) * | 2019-06-25 | 2019-10-25 | 四川广阳环保科技有限公司 | A kind of recovery and treatment method of well drilling detritus and products thereof and application |
| CN112079590A (en) * | 2020-09-28 | 2020-12-15 | 武汉聚信创为科技有限公司 | Anti-mud agent and use method thereof |
| CN112875821A (en) * | 2020-06-11 | 2021-06-01 | 江苏中电创新环境科技有限公司 | Composite coagulant and preparation method and application thereof |
| CN113102124A (en) * | 2020-01-11 | 2021-07-13 | 中石化石油工程技术服务有限公司 | Synthetic base drilling fluid recycling method |
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| CN115259278A (en) * | 2022-07-30 | 2022-11-01 | 深圳市鼎深科技有限公司 | Preparation method of special treating agent for high-oil-content sewage |
| CN115612553A (en) * | 2022-10-31 | 2023-01-17 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
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| CN110374529A (en) * | 2019-06-25 | 2019-10-25 | 四川广阳环保科技有限公司 | A kind of recovery and treatment method of well drilling detritus and products thereof and application |
| CN113102124A (en) * | 2020-01-11 | 2021-07-13 | 中石化石油工程技术服务有限公司 | Synthetic base drilling fluid recycling method |
| CN112875821A (en) * | 2020-06-11 | 2021-06-01 | 江苏中电创新环境科技有限公司 | Composite coagulant and preparation method and application thereof |
| CN112079590A (en) * | 2020-09-28 | 2020-12-15 | 武汉聚信创为科技有限公司 | Anti-mud agent and use method thereof |
| CN113354045A (en) * | 2021-05-18 | 2021-09-07 | 中国石油大学(北京) | Polysilicate aluminum ferric flocculant and preparation method and application thereof |
| CN115259278A (en) * | 2022-07-30 | 2022-11-01 | 深圳市鼎深科技有限公司 | Preparation method of special treating agent for high-oil-content sewage |
| CN115612553A (en) * | 2022-10-31 | 2023-01-17 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
| CN115612553B (en) * | 2022-10-31 | 2024-04-05 | 上海中器环保科技有限公司 | Process for recovering biodiesel from crude glycerol |
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Application publication date: 20181228 |