CN108285215A - A kind of natural gas waste water method for removing hydrargyrum - Google Patents
A kind of natural gas waste water method for removing hydrargyrum Download PDFInfo
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- CN108285215A CN108285215A CN201710897269.8A CN201710897269A CN108285215A CN 108285215 A CN108285215 A CN 108285215A CN 201710897269 A CN201710897269 A CN 201710897269A CN 108285215 A CN108285215 A CN 108285215A
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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
-
- 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
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- 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
- C02F11/00—Treatment of sludge; Devices therefor
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F11/00—Treatment of sludge; Devices therefor
- C02F11/002—Sludge treatment using liquids immiscible with water
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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)
- Inorganic Chemistry (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Removal Of Specific Substances (AREA)
Abstract
The present invention relates to a kind of natural gas waste water method for removing hydrargyrum, step includes：S1, mercury agent for capturing is added into water to be reacted with the ion mercury compound dissolved in hydrocarbon fluid, forms the sediment of mercury compound not soluble in water；S2, the mercury compound of precipitation is separated from water by filter press；S3, it will be extracted with organophosphorous extractant after the filter cake of press filtration Acid leaching, then be stripped out high-purity mercury salt；S4, water is removed into the distillation of mercury salt aqueous solution, obtains mercury salt crystal.Mercury contaminants effectively can be reduced to discharge index level by the present invention, and the mercury of removing is extracted and is purified.
Description
Technical field
The present invention relates to a kind of method for treating waste liquid, especially a kind of natural gas waste water method for removing hydrargyrum.
Background technology
Mercury is a kind of argenteous liquid metals, and volatility is very big under room temperature, and aerial saturated concentration is up to 3.52
~29.5mg/m3.Since mercury has some special physics, chemical properties, so being widely applied to chemical industry and petrochemistry
The industrial departments such as industry, pharmacy, paper pulp papermaking, electric appliance and electronic instrument.China actually produces mercury quantity about 1100t every year, with mercury total amount
For 1100~1500t.So extensive to use, the annual whole world mercury in environment that scatters and disappears is about 1.5 × 104~3.0 × 104T,
Environment is polluted with " exhaust gas, waste residue, waste water " three kinds of approach.
Mercury and mercuric compounds are all noxious materials, can invade human body by all means, the main maincenter god for influencing people
Through mostly slow poisoning under normal circumstances.Its toxicity is accumulation, and wherein inorganic mercury mainly accumulates in internal organ, Shao Liangji
Gather in the other parts of brains, skin and human body.
The harm problem of mercury is recognized by people already, and has developed a variety of physics, chemistry and the processing side of microorganism
Method.However, the use scope due to mercury is extensive, also type is various for mercurous pollutant, and each is required for using different works
Skill can be handled preferably.Processing mercury-containing wastes need to expend a large amount of energy and resource more, and processing cost is high and is difficult to
Reach the effect of processing.
In world certain areas, the natural gas and crude oil of production contain a large amount of mercury, and presenting in an amount at least sufficient to keeps its processing problematic.
For example, the hydro carbons condensate of the natural gas derivatives produced from Southeast Asia certain areas may contain the mercury for having more than 1000ppbw, and
The crude oil of Argentinian certain areas is often containing the mercury for having more than 2000ppbw.The water quality of the waste water generated from natural gas and oil well
The mercury of high concentration may also be contained.
Mercury can exist in several forms, including ion, element, particle and organic matter.For example, crude oil may contain element
Mercury is simultaneously aoxidized, to generate water soluble salt (Hg+, Hg2+) and complex compound.In addition, anaerobic bacteria can be by granular suspension
Mercury is converted into water-soluble organic form, to which the transfer between two kinds of vehicle substances easily occur.
There are problems that of mercury can cause two kinds.First, mercury may corrode the gold in process equipment by forming mercury alloy
Belong to；The article as made of aluminium and aluminium alloy, such as the ice chest in Cryo Equipment, such as in petrochemical equipment and natural gas treatment plant
Ethylene separator.Mercury can also reduce the service life of catalyst.
Currently, few technologies remove mercury from waste water and industrial water.It can be used for handling the primary commercial skill of mercury in water
Art includes several commercially available one of precipitating reagents of addition, typically sulfide polymer, with the ionic mercury of precipitation dissolving and is led to
It crosses gas or air flotation removes, but it cannot remove all mercury substances that may be present, including insoluble granule shape mercuration closes
Object, element mercury, organic mercury are mainly monomethyl and dimethylmercury.
Handle water in mercury and and other heavy metals scheme such as United States Patent (USP) text US4814091A, US5667694A,
US6165366A and US7029202B2.In US4814091A pre-flock then it is pH adjusted after use sulfide precipitation, then flocculation and
Diafiltration.Organic clay adsorbent is used in US5667694, adsorbs the metal in water.Hypochlorous acid oxidization is used in US6165366A
Mercury reuses activated carbon adsorption filtering.It first uses lignin derivative to be formed with mercury or other metals in US7029202B2 to coordinate
Object uses flocculant to form flocculate, is then isolated and is precipitated as sludge later.However, these methods do not show foot
The mercury in waste water stream to be removed to the level for meeting environment protection emission index, and all there is the secondary pollution of the mercury containing high concentration
Object does not extract mercury, could not fundamentally prevent mercury pollution.
Invention content
Technical problem to be solved by the invention is to provide one kind from water (such as oil and gas exploitation waste water, production plus
Work water, process water) in remove the treatment technology of the removal of mercury, either ion, element, granular or organic, Dou Nengyou
Mercury contaminants are reduced to discharge index level by effect ground, and the mercury of removing is extracted and is purified.
The present invention solves technical solution used by above-mentioned technical problem：
A kind of natural gas waste water method for removing hydrargyrum, step include：
S1, mercury agent for capturing is added into water to be reacted with the ion mercury compound dissolved in hydrocarbon fluid, is formed not soluble in water
Mercury compound sediment；
S2, the mercury compound of precipitation is separated from water by filter press；
S3, it will be extracted with organophosphorous extractant after the filter cake of press filtration Acid leaching, then be stripped out high-purity mercury salt；
S4, water is removed into the distillation of mercury salt aqueous solution, obtains mercury salt crystal.
Further, the mercury agent for capturing includes and reacts to form mercury not soluble in water with the mercury compound dissolved in hydrocarbon fluid
Sulfide.
Preferably, the mercury agent for capturing include alkali metal sulphide, alkali metals polysulfide, alkaline earth sulfide,
It is one or more in alkaline earth metal polysulfides.
Further, the mercury agent for capturing includes thiazole, dialkyl dithiophosphoric acid or its salt, dialkyl group monothio phosphoric acid
Or its salt, dialkyl dithio hypophosphorous acid or its salt, dialkyl group monothio hypophosphorous acid or its salt, alkali metal thiocarbamic acid
One kind or more in salt, alkali metal dithiocar-bamate, alkali metal xanthate, alkali metal trithiocarbonic acid salt compound
Kind.
Preferably, the mercury agent for capturing includes water-soluble polymeric dithiocar-bamate, in the hydrocarbon fluid, mercury is not
Less than 100ppmw (concentration of mercury is indicated by ppbw in background technology and embodiment, and whether the PLSCONFM order of magnitude is problematic),
The water-soluble polymeric dithiocar-bamate of addition is not less than 200ppmw.
Further, the pH ranges in the step S1 are maintained at 3-9.
Preferably, the temperature range in the step S1 is maintained at 10-50 DEG C.
Further, flocculant is added when forming sediment in the step S1.
Preferably, the flocculant addition is less than 25ppmw (whether PLSCONFM 25ppm is quality).
Preferably, the organic phosphine extractant is the dialkyl phosphate or dialkyl hypophosphorous acid, dioxane of C4~C18
Base monothio hypophosphorous acid, dialkyl dithio hypophosphorous acid, trialkyl phosphates, one kind in trialkyl thiophosphate or more
Kind.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, following embodiment be explanation of the invention and
The invention is not limited in following embodiments.
Embodiment 1：
The ratio and percentage illustrated in the present embodiment is by weight.The water solubility that mercurous flow passes through pipeline and injection
The flow of mercury agent for capturing meets hybrid concurrency life reaction so that the ionic mercury of dissolving is precipitated out from solution.Then, the stream
Into filter press, solid not soluble in water is detached.Water substantially free of mercury substance after separation is left by pipeline, and can be with
Other post-processing steps, such as biological treatment are carried out to reduce its COD, can be discharged into environment after up to standard.It is press-filtered out and
Filter cake pass through Acid leaching, such as hydrochloric acid, using one of press filtration by sludge filtration, filtered sludge be substantially free of mercury or
It, can be as common fixed-end forces within discharge index.It leaches the mercury acid solution and extracts mercury by organic phosphine extractant,
Extract liquor forms mercury salt aqueous solution through back extraction, and mercury salt aqueous solution mercury salt after water removal is gone in distillation crystallizes, and reaches purification extraction mercury
Purpose.Raffinate acid solution and organophosphor extract liquor return to front-end-of-line recycling, form non-secondary pollution, and mercury purification is available
Purpose.
The mercury minimizing technology is suitable for all aqueous fluids containing mercury, including mercury-containing waste water and process water.As described above, this
Kind of flow is usually related with the exploitation of mercurous hydrocarbons, production and refining and by the mixed flow of these hydrocarbons.This contains
Mercury water may be generated close to production area, if not going the removal of mercury before transportation, may be produced in farther processor place
It is raw.This method proves processing containing the up to mercury-containing waste water of 10000ppb by testing；Result can reach after handling after tested
Within discharge index 50ppb.
According to the method for originally going the removal of mercury, initial step is the soluble mercury compound first by the ionic species in mercurous water
It is converted into insoluble mercury compound, then to be removed by physical method.For this purpose, in this step, mercury agent for capturing and dissolving
Mercury cation (be usually Hg2+) haptoreaction in flow.It can be added in flow by will simply capture agent solution
And mixed, to ensure that coming into full contact in entire water body is reacted to realize with all mercury.Although mercury agent for capturing and water
The mixing of stream can by such as flocculation stirring tank, or the tower with filler, adverse current mixer or other can be uniformly distributed
Device in entire mercurous flow, but these devices are not necessary conditions, because between agent for capturing and the mercury substance of dissolving
Be swift in response generation.It is sufficient in general, will capture agent solution with normal flow and be added in flow, but good to ensure to realize
Mixing, these capture agent solution addition point and may be mounted in such as high turbulent region of the suction inlet of pump, to make agent for capturing
It reacts between the ionic mercury of dissolving.When flocculant is added together with mercury agent for capturing, it has to be noted that ensure compatibility.Example
Such as, if using anion catching agent and cationic flocculant, at least 30 seconds mixed intervals should be provided between injection point,
To avoid reacting to each other between product, the effect for being unfavorable for the removal of mercury is caused.
Mercury agent for capturing includes that the sulfide to form insoluble mercuric sulphide sediment is reacted with the mercury ion of dissolving in the present invention.
Preferred class sulfide agent for capturing includes the water-soluble sulfides such as hydrogen sulfide, and the alkali metal sulphides such as vulcanized sodium and alkali metal are more
Sulfide, alkaline earth sulfide, alkaline earth metal polysulfides are based on its economy and commerciality.Also precipitation sulfide can be used
The other materials of the mercury of form includes thiazole, dialkyl dithiophosphoric acid or its salt, dialkyl group monothio phosphoric acid or its salt, dioxane
Base dithiophosphlic acid or its salt, dialkyl group monothio hypophosphorous acid or its salt, alkali metal thiocarbamate, two sulphur of alkali metal
For carbaminate, alkali metal xanthate and alkali metal trithiocarbonate such as trithiocarbonic acid sodium (Na2CS3)。
In order to meet the needs of the metal agent for capturing smaller to toxicity and also form big quick capture flocculate, efficiently
Metal-chelating polymers can be used as mercury agent for capturing.Such water solubility agent for capturing such as dialkyl dithio sodium hypophosphite,
The medicament can be efficiently used in the method, reduce the discharge risk of mercury itself or toxicity inorganic agent.In view of their energy
Enough there is high selective capture mercury, and in the ability of subsequent organophosphor extraction and back extraction desorption, the method for the present invention
It is preferable to use this agent for capturing, but flocculant can also be added.In containing the up to water of 10000ppb mercury, it has been found that make
It is enough to remove a large amount of mercury with the water-soluble dialkyl dithio sodium hypophosphite of up to 30ppm amounts.
Mercury agent for capturing usually uses under weak acid, neutrality or weak basic condition, and pH=8 is more typical state, although
The removal of mercury can be also gone under relatively low and higher pH value condition, but the mole of selected agent for capturing should be at least equal to preferred
Slightly it is in excess in the amount of mercury ion to be removed.However, should avoid using a large amount of excessive agent for capturing such as vulcanized sodium, because it can
The water-soluble vulcanization mercury complex for the removal for inhibiting mercury can be formed.In addition, excessive this sulfide and other agent for capturing may
Can be more than discharge index, and since these certain agent for capturing itself may be toxic, it is therefore necessary to which attention ensures them not
It is present in the water of discharge.Without using another reason for excessive precipitating reagent being residual quantity will be adsorbed on canvas press cloth.
For this reason, an order of magnitude of mercury content or more is not to be exceeded in the optimum amount of agent for capturing.Capture the temperature in step
It can be suitably in the range of 10-50 DEG C.The mean residence time that mercury captures in step answers long enough, so that reaction can lead to
Liquid progress is crossed, and catch is made to be formed completely, usual 10 to 20 minutes.
Pass through mercury and such as sulfide, polysulfide, mercaptan, thiocarbonate, thio organic phosphonium salt, thiocarbamate
Reaction with the agent for capturing such as xanthates and the metal complex sediment that is formed are typically do not allow free settling or filtering tiny
The form of solid, therefore being easy to blocking even can be by most of filtration system.Generally preferably addition flocculant, even if so as to
When using preferred polymeric dithiocarbamates precipitating reagent, this can also be removed effectively in subsequent press filtration step
A little suspended solids.In addition, in hydrocarbonaceous or suspended solid the water of high concentration, need that flocculant is added to help to remove these dirts
Object is contaminated, and avoids the mutual unfavorable effect with mercury agent for capturing.Flocculant can be organic or inorganic or both combination,
And can be polymerization, it is anion or cationic, aluminium polychloride and iron chloride are can be generally divided into, organic wadding is polymerize
Solidifying agent includes polyacrylamide, diallyldimethylammonium chloride (DADMAC) polymer, DADMAC- polyacrylamides and polycyclic
Oxygen chloropropane amine (EPI-DMA) polyamines.These coagulating agents and flocculant are usually added to the water before press filtration processing, they can be with
Continue on for the method for the present invention to promote the separation for the mercury compound being precipitated.In general, according to the property of flocculant, addition is high
When reach about 50ppm, in most cases, be sufficient less than 25ppm, such as 10ppm.
After addition agent for capturing and flocculant, the flow and sediment of insoluble mercury compound are sent to filter press and go
It removes.Press filtration step is used to concentrate the mercury in water, and removes other heavy metal metals in water, including lead, cadmium, nickel and copper.Pressure
Mercury content can reach environment protection emission index 50ppb or less in water after filter.
Mercurous filter cake is taken out after the short time filters and to form filter cake, is put into acid and leaches, such as hydrochloric acid by filter press.
Leaching time is generally 20 to 30 minutes in acid, and leaching temperature is at 20 to 50 DEG C.Acid solution is leached using mistake after a press filtration
Screening is mercurous up to standard, and when common useless processing, filtering acid solution further arrive organic phosphine extraction tank and carries out Extraction of Mercury, formed organic phase with
Water phase is layered, and organic phosphine extractant may be used not water-miscible organic solvent and be diluted, such as kerosene.Extraction time 30 minutes,
20~40 DEG C of temperature.By extraction, raffinate returns to Acid leaching process, and extract liquor further arrives the back extraction that back extraction slot carries out mercury
It takes, is stripped using strong acid, form high concentration mercury salt aqueous solution, process continues to participate in extraction before the organic phase after back extraction is gone
It takes, mercury salt aqueous solution further obtains mercury salt crystal salt after water is removed in distillation.Distilled water is not mercurous.70~100 DEG C of vapo(u)rizing temperature is i.e.
Can, mercury salt purity can reach 95% or more.
In order to confirm the validity of the method for the present invention, by simulating petroleum gas mercury-containing waste water, the removal of mercury in seven weeks has been done
Experiment.The mercury ion (mercury chloride) of the mercury content of 5000ppb is added in the waste water containing 0.1% crude oil, and 100ppb is added
Mercury metal, the organic mercury (dimethylmercury) of 100ppb.By using the method for the present invention, tested by seven weeks, in mercury agent for capturing
Under optimum chemical dosage addition rate, final process water mercury content goes mercury removal efficiency to be maintained at 99.9% all within 50ppb.And
The total recycling of 96% in filter residue is purified to 95% or more.
Furthermore, it is necessary to illustrate, the specific embodiment described in this specification, the shape of parts and components is named
Title etc. can be different.The equivalent or simple change that all structure, feature and principles according to described in inventional idea of the present invention are done, is wrapped
It includes in the protection domain of patent of the present invention.Those skilled in the art can be to described specific implementation
Example is done various modifications or additions or is substituted by a similar method, without departing from structure of the invention or surmounts this
Range as defined in the claims, is within the scope of protection of the invention.
Claims (10)
1. a kind of natural gas waste water method for removing hydrargyrum, step include：
S1, mercury agent for capturing is added into water to be reacted with the ion mercury compound dissolved in hydrocarbon fluid, forms mercury not soluble in water
The sediment of compound；
S2, the mercury compound of precipitation is separated from water by filter press；
S3, it will be extracted with organophosphorous extractant after the filter cake of press filtration Acid leaching, then be stripped out high-purity mercury salt；
S4, water is removed into the distillation of mercury salt aqueous solution, obtains mercury salt crystal.
2. natural gas waste water method for removing hydrargyrum according to claim 1, it is characterised in that：The mercury agent for capturing includes and hydrocarbon stream
The mercury compound dissolved in body reacts the sulfide to form mercury not soluble in water.
3. natural gas waste water method for removing hydrargyrum according to claim 2, it is characterised in that：The mercury agent for capturing includes alkali metal
It is one or more in sulfide, alkali metals polysulfide, alkaline earth sulfide, alkaline earth metal polysulfides.
4. natural gas waste water method for removing hydrargyrum according to claim 1, it is characterised in that：The mercury agent for capturing include thiazole,
Dialkyl dithiophosphoric acid or its salt, dialkyl group monothio phosphoric acid or its salt, dialkyl dithio hypophosphorous acid or its salt, dialkyl group
Monothio hypophosphorous acid or its salt, alkali metal thiocarbamate, alkali metal dithiocar-bamate, alkali metal xanthic acid
It is one or more in salt, alkali metal trithiocarbonic acid salt compound.
5. natural gas waste water method for removing hydrargyrum according to claim 4, it is characterised in that：The mercury agent for capturing includes water solubility
Polymeric dithiocarbamates, mercury is not less than 100ppbw, the water-soluble polymeric dithiocarbamates first of addition in the hydrocarbon fluid
Hydrochlorate is not less than 200ppmw.
6. natural gas waste water method for removing hydrargyrum according to claim 1, it is characterised in that：PH ranges in the step S1 are protected
It holds in 3-9.
7. natural gas waste water method for removing hydrargyrum according to claim 6, it is characterised in that：Temperature range in the step S1
It is maintained at 10-50 DEG C.
8. natural gas waste water method for removing hydrargyrum according to claim 6, it is characterised in that：Sediment is formed in the step S1
When flocculant is added.
9. natural gas waste water method for removing hydrargyrum according to claim 8, it is characterised in that：The flocculant addition is less than
25ppmw。
10. natural gas waste water method for removing hydrargyrum according to claim 1, it is characterised in that：The organic phosphine extractant is C4
The dialkyl phosphate or dialkyl hypophosphorous acid of~C18, dialkyl group monothio hypophosphorous acid, dialkyl dithio hypophosphorous acid, three
It is one or more in alkyl phosphate, trialkyl thiophosphate.
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| CN201710897269.8A CN108285215A (en) | 2017-09-28 | 2017-09-28 | A kind of natural gas waste water method for removing hydrargyrum |
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| CN201710897269.8A CN108285215A (en) | 2017-09-28 | 2017-09-28 | A kind of natural gas waste water method for removing hydrargyrum |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511798A (en) * | 2019-08-13 | 2019-11-29 | 青岛华友恒新能源材料技术研究院有限公司 | A kind of purifying treatment method of mercurous natural gas fluid |
| CN112694159A (en) * | 2019-10-22 | 2021-04-23 | 中国石油化工股份有限公司 | Wastewater treatment agent containing metal sulfide and wastewater treatment method |
| CN114538656A (en) * | 2022-02-23 | 2022-05-27 | 湖北楚星化工股份有限公司 | Device and method for controlling adding amount of mercury removing agent for mercury-containing wastewater treatment |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110511798A (en) * | 2019-08-13 | 2019-11-29 | 青岛华友恒新能源材料技术研究院有限公司 | A kind of purifying treatment method of mercurous natural gas fluid |
| CN112694159A (en) * | 2019-10-22 | 2021-04-23 | 中国石油化工股份有限公司 | Wastewater treatment agent containing metal sulfide and wastewater treatment method |
| CN114538656A (en) * | 2022-02-23 | 2022-05-27 | 湖北楚星化工股份有限公司 | Device and method for controlling adding amount of mercury removing agent for mercury-containing wastewater treatment |
| CN114538656B (en) * | 2022-02-23 | 2023-12-22 | 湖北楚星化工股份有限公司 | Device and method for controlling addition amount of mercury removing agent in mercury-containing wastewater treatment |
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