CN102466637A - Method for measuring static ion removal rate of hydroxamic acid type polymeric chelant - Google Patents
Method for measuring static ion removal rate of hydroxamic acid type polymeric chelant Download PDFInfo
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- CN102466637A CN102466637A CN2010105421174A CN201010542117A CN102466637A CN 102466637 A CN102466637 A CN 102466637A CN 2010105421174 A CN2010105421174 A CN 2010105421174A CN 201010542117 A CN201010542117 A CN 201010542117A CN 102466637 A CN102466637 A CN 102466637A
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Abstract
The invention discloses a method for measuring the static ion removal rate of a hydroxamic acid type polymeric chelant. The method comprises the steps of: placing the hydroxamic acid type polymeric chelant in a reaction container; adding a metal ion solution with a concentration of C; taking out the supernatant liquors after agitation; measuring the concentration C1 of metal ions of the processed supernatant liquors; and calculating the static ion removal rate Q according to C and C1. The method disclosed by the invention can be used for rapidly measuring the static ion removal rate of the hydroxamic acid type polymeric chelant, has high measurement precision and simple measurement steps, is beneficial to reduction of the measurement cost and provides good data support for researches on the hydroxamic acid type polyacrylamide.
Description
Technical field
The present invention relates to a kind of static clearance assay method of ion of hydroxamic acid type high-molecular chelating agent.
Background technology
In the face of China environmental protection present situation and pressure that international green fort brought, carry out the R and D of oil field environmental protection technology in China, the great environmental protection problem that solves in puzzlement Chinese society and the economic development seems very urgent.
Petroleum gas enterprise adopts oil gas well such as drilling well to go into operation and measure such as raising the output in the oil-gas exploration and development process in a large number, has produced a large amount of drilling waste waters, and every mouthful of well produces drilling waste water 400～500m during drilling well
3, waste drilling fluid 500～700m
3The pollution problem that solves sewage has at present become one of important subject of each industrial sector environmental protection.Drilling waste water is the potpourri of drilling mud dilution for many times, and its complicated component contains the various components in the drilling mud, like clay, organic polymer, oils, inorganic salts, drilling cuttings, drilling mud additives etc.Environmental pollutants in drilling waste water load is high, and suspension content is everlasting more than the 2000mg/L, sometimes even more than 5000mg/L.These are colloidal by the suspension of bringing in the drilling fluid, add the protective colloid effect of drilling fluid, make it become special stabilising system, in water body, can not sink for a long time, cause the havoc of water ecology and influence the use of water; COD exceeds standard tens to hundred times, enters water body and will cause serious eutrophication, and the water blackout is smelly, can not use at all; The content of oily substance does not wait to several ten thousand mg/L from tens mg/L, will cause the serious decline of environmental quality behind the discharging environment; In addition,, or, contain multiple hazardous substances such as salt and some heavy metal elements (like Pb, Cu, Cd, Hg, Ni, Ba and Cr etc.) in the drilling waste water, biology is had very strong toxic action by drilling cuttings and the introducing of stratum mineral owing to bringing into of various mud additives.
Other industrial sector also has great amount of wastewater to discharge, and often contains various heavy metal ion in these waste water.For example: in textile waste, contain a large amount of Cu ions, in waste water from plating plant, contain the Cr ion, in electrolysis soda plant waste water, contain the Hg ion, in steel-making iron-smelter waste water, contain the Fe ion ... Deng.The hazardous waste that contains heavy metal at present is recovered as the master with refinement except cupric, lead etc., and remaining mostly is changed to the master with the enclosure storeroom.These discarded objects issue biochemical variation in the environmental baseline effect, can get into water body through washing away also of the rainwater or the day water again.
Heavy metal is one type of pollutant with potential hazard in the environment; It can not be decomposed by the microorganism in the environment; On the contrary; Biosome such as fish can be rich in heavy metal, and heavy metal is accumulated in environment, even some heavy metal can also be converted into the bigger organic compound of toxicity under action of microorganisms.The fearful chronicity that also is its harm of heavy metal pollution at the initial stage that heavy metal accumulates in environment, is difficult for discovering for people; Opposite with prussiate, general organic self purification, heavy metal contaminants can't pass through the degradation self-cleaning, but can be through biological food chain enrichment.In this course, be prone to residual heavy metal if get in the human body through food difficult the decomposition, can make people's slow poisoning in a certain position accumulation of human body, is difficult to cure, and greatly endangering health and Environmental security.Precious metal causes the economic loss and the wasting of resources again if can not recycle in the industrial waste water in addition.So the improvement to containing heavy metal wastewater thereby is extremely urgent.
Heavy metal ions in wastewater is polluted human formation with other life has been constituted huge threat.As occur in the polluting " Mad Hatter's disease " cause and pollute " Itai-itai diseases " incident that causes by Cd of Japan by Hg; In recent years some countries have also reported the serious consequence that heavy metal pollution produces successively in Europe, make the research of heavy metal pollution and control extremely pay attention to.
Heavy metal can accumulate in soil, and it can not be degraded by microorganisms, and the several different methods that in environmental improvement, adopts at present can only shift its location and change its physics, chemical form, and can not be with its basic elimination.Therefore, heavy metal is a kind of pollutant of eternal property.For heavy metal wastewater thereby, must carry out proper process.At first should manage to reduce wastewater flow rate, regain its useful metal as far as possible, waste water recycle after suitably handling is not arranged or few effluent as far as possible.Waste water to discharging carries out purified treatment, makes it to reach emission standard.To handling mud and the concentrate that produces, be not worth as having to recycle, also should carry out harmless treatment, in order to avoid produce secondary pollution.
Hydroxamic acid is because its particular structural and corresponding physical and chemical performance make the hydroxamic acid chemistry become chemical field research problem comparatively widely.Hydroxamic acid compound normally prepares with carboxylic acid or its derivant and azanol (or salt of azanol) reaction, and the carboxylic acid derivates of use has ester, acid amides, acid anhydrides, carboxylic acid halides.In addition, can also adopt sulfuric acid oxidation primary amine method, preparation such as the rearrangement method of nitroparaffins hydroxamic acid compound.Because the reaction conditions of ester and carboxylic acid halides and azanol is gentle, process is controlled easily, and is the most commonly used in commercial production.
Hydroxamic acid is one type of organic sequestering agent, because of being used as mineral flotation agent, extractant and analysis developer with metallic ion flocculating agent chelating.Long-term practice proves; Hydroxamic acid is that a kind of collecting property is strong, the good preferably collecting agent of selectivity; It can to multiple burning ore deposit and some non-ferrous metal oxide minerals and part oxidized sulphide ore all have good collecting performance, be cupric oxide ore, rare-earth mineral, tantalum niobium concentrate, one of the good collecting agent of iron ore, cassiterite, wolframite etc. of admiring.It has efficiently, low toxicity, good selective.
Although low molecule hydroxamic acid has obtained development rapidly and used widely, and is then few about the report of macromolecule hydroxamic acid type flocculating agent.The mid-1960s, the Masahirio Hatano of Japan etc. makes the methyl acrylate type high-molecular chelating agent of oxygen-containing nitrolic acid group.The mid-1970s, the acrylic amide modified hydroxamic acid group content that makes of apparatus such as Clauss is about 8% hydroxamic acid property polyacrylamide, and is applied to the selectively flocculate of technics of cassiterite clay.Nineteen eighty-two Vernon etc. has synthesized the high-molecular chelating agent that a series of N of containing replace hydroxamic acid.Spitzer in 1988 have synthesized the polymkeric substance of oxygen-containing nitrolic acid group, and in red-mud settlement, are able to subsequently use.
Polyacrylamide is a kind of good modified feedstock.In polyacrylamide (PAM) molecule; Pi-electron and the not share electron pair on the amino nitrogen atom on the acylamino-in the two keys of carbon back form the pi-conjugated system of p-; Cloud density decreases on the nitrogen-atoms, and the hydrogen atom that links to each other with it is become vivaciously, and multiple reaction can take place.Because it has performances such as good flocculation, thickening, drag reduction, bonding, scale inhibition, is widely used in industry such as papermaking, coating, oil recovery.
The polyacrylamide of different purposes, different to the requirement of its molecular mass size.The polyacrylamide of high molecule mass and ultra-high molecular weight is mainly used in flocculating agent or oilwell water shutoff, the displacement of reservoir oil etc., and domestic and international research also mainly concentrated on synthesizing of hydroxamic acid type high molecular polymer at present.But on some are used, like macromolecule emulsifier, then need hang down the preparation of the hydroxamic acid high molecular polymer of molecular mass, mainly adopt two kinds of methods: the first is carried out the polymerization of acrylic amide in the WS with the molecular mass control method; It two is to carry out the sedimentation polymerization with organic solvent.The method that this test is adopted is in the solution of water, to carry out the polymerization of acrylic amide, through the addition and the certain operations condition of control reagent, such as, monomer and initiator concentration, temperature, reaction time etc., reach the purpose of controlling the high-polymer molecular quality.
The polyacrylamide of different purposes, different to the requirement of the size of its molecular weight.According to the purpose of this paper, desire prepares low-molecular-weight polyacrylamide.For low-molecular-weight Preparation of Polyacrylamide, the following several method of main employing: (1) is not having under the situation of chain transfer according to the kinetics equation of polyreaction, and the square root of kinetics of polymerization reaction chain length and initiator concentration is inversely proportional to both at home and abroad.Therefore, increase initiator concentration and can make low-molecular-weight polyacrylamide.But it is too fast that the increase initiator concentration can make reaction carry out, and implode takes place, and is difficult to control.(2) in polyreaction, add molecular weight regulator, by the chain transfer control molecular weight of molecular weight regulator.Such as using isopropyl alcohol, sodium formate equimolecular quantity correctives carries out the polymerization of acrylic amide in the WS, but the polyacrylamide that makes has certain degree of crosslinking and degree of hydrolysis.(3) precipitation polymerization that carries out with organic solvent.Because employed organic solvent is very active chain-transferring agent to the polymerization of acrylic amide in the precipitation polymerization process; And most of organic solvents all are the precipitation agents of polyacrylamide;, the strand of polymkeric substance just can precipitate after rising to certain-length; Limited the further growth of strand, so the products therefrom molecular weight is lower, narrow molecular weight distribution.The organic solvent that was studied mainly contains isopropyl alcohol, acetone and water, acetone etc.
By acrylic amide modified hydroxamic acid macromolecule, its red mud in oil drilling, alumina producing is well used in separating because of having rapid and firm chelation with ferric ion.With flocculating agent, hydroxamic acid type polymeric flocculant will become very promising one type of flocculating agent from whole heavy metal sedimentation.
Flocculence occupies important status in water treatment, the use of flocculating agent has determined the effect of flocculation.Organic polymer coargulator appears at the 1950's, begins to be applied to the environmental protection field sixties, and it is big that it has a molecular weight; The adsorption bridging ability is strong, and a plurality of functional groups are arranged, and flocculating effect is good; The floc unit easy filtration that forms, consumption is few, forms the few and easy processing of sludge quantity; Do not receive advantages such as pH value and Influence of Temperature; But also can be to the character of handling waste water, through change functional group, functional group electrically, control molecular weight etc. selectively synthesizes, so organic polymer coargulator is widely used in water treatment at present.
The strong dentate of heavy metal ion is introduced in the organic polymer coargulator molecule sequestrant that can obtain to have the heavy metals trapping function---macromolecular heavy metal chelating agent.The hydroxamic acid group contains coordination atoms such as O, N; Can form the very high chelate of stability constant with many heavy metal ion; Be incorporated into this group and promptly obtain hydroxamic acid family macromolecule heavy metal chelant in the organic polymer sequestrant, the advantage of its existing organic polymer coargulator has good capture performance to heavy metal ion again; Can capture some heavy metal ion in the water body stable, efficiently, therefore in water pollution control, have potential extensive use.Compare with traditional chemical precipitation method; Macromolecular heavy metal chelating agent has the following advantages: dosing is few; Need not regulate the pH value, simple to operate, heavy metal ion can not separated out from mud because of the variation of pH value once more; Do not have secondary pollution, it can also reduce the content that causes absurd creature matter in the water through " flocculation of building bridge " effect of former polymeric flocculant.Therefore use it for the flocculation unit of water treatment, can reduce the subsequent treatment unit number, reduce processing cost, make treatment of heavy metal ions become simple, can be heavy metal pollution control and open up new way, new technology is provided.
Summary of the invention
The objective of the invention is to overcome the shortcoming and defect of above-mentioned prior art; A kind of static clearance assay method of ion of hydroxamic acid type high-molecular chelating agent is provided; This assay method can record the static clearance of ion of hydroxamic acid type high-molecular chelating agent fast, and measuring accuracy is high, and measuring process is simple; Reduced the measurement cost, for the research of hydroxamic acid type polyacrylamide provides good data support.
The object of the invention is realized through following technical proposals: the static clearance assay method of a kind of ion of hydroxamic acid type high-molecular chelating agent may further comprise the steps:
(a) get hydroxamic acid type high-molecular chelating agent and place reaction vessel;
(b) adding concentration is the metal ion solution of C;
(c) stir a period of time, get the upper strata settled solution;
(d) measure its concentration of metal ions C after treatment
1
(e) according to C and C
1Calculate the static clearance Q of ion.
In the said step (a), reaction vessel is a beaker.
In the said step (b), the metal ion solution volume of adding is 100ml.
In the said step (c), whipping temp is a room temperature.
In the said step (d), through the spectrophotometer measurement concentration of metal ions.
In sum; The invention has the beneficial effects as follows: can record the static clearance of ion of hydroxamic acid type high-molecular chelating agent fast, and measuring accuracy is high, measuring process is simple; Reduced the measurement cost, for the research of hydroxamic acid type polyacrylamide provides good data support.
Embodiment
Below in conjunction with embodiment, the present invention is done further detailed description, but embodiment of the present invention is not limited only to this.
Embodiment:
The static clearance assay method of the ion of a kind of hydroxamic acid type high-molecular chelating agent that the present invention relates to may further comprise the steps:
(a) get hydroxamic acid type high-molecular chelating agent and place reaction vessel;
(b) adding concentration is the metal ion solution of C;
(c) stir a period of time, get the upper strata settled solution;
(d) measure its concentration of metal ions C after treatment
1
(e) according to C and C
1Calculate the static clearance Q of ion.
In the said step (a), reaction vessel is a beaker.
In the said step (b), the metal ion solution volume of adding is 100ml.
In the said step (c), whipping temp is a room temperature.
In the said step (d), through the spectrophotometer measurement concentration of metal ions.
Above-mentioned steps (e) is according to C and C
1The formula that calculates the static clearance Q of ion is: Q=(C-C
1)/C.
The static clearance assay method of the ion of above-mentioned hydroxamic acid type high-molecular chelating agent can record the static clearance of ion of hydroxamic acid type high-molecular chelating agent fast; And measuring accuracy is high; Measuring process is simple; Reduced the measurement cost, for the research of hydroxamic acid type polyacrylamide provides good data support.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction, and every foundation technical spirit of the present invention, any simple modification, equivalent variations to above embodiment did all fall within protection scope of the present invention.
Claims (5)
1. the static clearance assay method of the ion of a hydroxamic acid type high-molecular chelating agent is characterized in that, may further comprise the steps:
(a) get hydroxamic acid type high-molecular chelating agent and place reaction vessel;
(b) adding concentration is the metal ion solution of C;
(c) stir a period of time, get the upper strata settled solution;
(d) measure its concentration of metal ions C after treatment
1
(e) according to C and C
1Calculate the static clearance Q of ion.
2. the static clearance assay method of the ion of a kind of hydroxamic acid type high-molecular chelating agent according to claim 1 is characterized in that in the said step (a), reaction vessel is a beaker.
3. the static clearance assay method of the ion of a kind of hydroxamic acid type high-molecular chelating agent according to claim 1 is characterized in that in the said step (b), the metal ion solution volume of adding is 100ml.
4. the static clearance assay method of the ion of a kind of hydroxamic acid type high-molecular chelating agent according to claim 1 is characterized in that in the said step (c), whipping temp is a room temperature.
5. the static clearance assay method of the ion of a kind of hydroxamic acid type high-molecular chelating agent according to claim 1 is characterized in that, in the said step (d), through the spectrophotometer measurement concentration of metal ions.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499029A (en) * | 2020-03-11 | 2020-08-07 | 深圳清华大学研究院 | Two-stage method for quickly removing copper ions in copper ammonia complex wastewater |
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2010
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111499029A (en) * | 2020-03-11 | 2020-08-07 | 深圳清华大学研究院 | Two-stage method for quickly removing copper ions in copper ammonia complex wastewater |
| CN111499029B (en) * | 2020-03-11 | 2022-05-13 | 深圳清华大学研究院 | Two-stage method for quickly removing copper ions in copper ammonia complexing wastewater |
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Application publication date: 20120523 |