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CN104310676B - The method that mercury compound in waste liquid is removed under normal temperature and pressure - Google Patents

The method that mercury compound in waste liquid is removed under normal temperature and pressure Download PDF

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Publication number
CN104310676B
CN104310676B CN201410539774.1A CN201410539774A CN104310676B CN 104310676 B CN104310676 B CN 104310676B CN 201410539774 A CN201410539774 A CN 201410539774A CN 104310676 B CN104310676 B CN 104310676B
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Prior art keywords
hydrargyrum
under normal
waste liquid
mercury compound
normal temperature
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CN201410539774.1A
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CN104310676A (en
Inventor
李森
王良栋
李璐
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Xinjiang Chengrun Environmental Protection Technology Co.,Ltd.
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GUIZHOU MEIRUITE ENVIRONMENTAL PROTECTION TECHNOLOGY Co Ltd
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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
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • 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
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • 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
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • 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
    • C02F1/70—Treatment of water, waste water, or sewage by reduction
    • 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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  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a kind of method that mercury compound in waste liquid is removed under normal temperature and pressure, method comprises the following steps：Step 1：Under normal temperature and pressure, the waste liquid containing mercury compound is contacted with reaction carriers, and be irradiated by 170nm～400nm length ultraviolets line or visible light；Step 2：By photocatalyst catalytic action, mercury compound is decomposed into into monomer hydrargyrum, the monomer hydrargyrum after decomposition carries out Adsorption by adsorbent.By adopting the present invention, under normal operating conditions, can continuously and efficiently easily from the various waste liquids containing hydrargyrum in the case where room temperature and normal pressure is close to while removing all kinds of form hydrargyrums, hydrargyrum concentration is less than below 5ppb in making treatment fluid.Organic pollution to containing in waste water also has high removal efficiency simultaneously, can reach draining newest standards, in addition for the clearance of hydrargyrum in spent sorbents containing hydrargyrum can reach 99%, the hydrargyrum response rate can reach 96%, the characteristics of fully demonstrating high removal efficiency, environment-friendly and green, with wide application value.

Description

The method that mercury compound in waste liquid is removed under normal temperature and pressure
Technical field
The present invention relates to Pollutant Treatment recovery technology field, removes hydrargyrum in waste liquid under more particularly to a kind of normal temperature and pressure The method of compound.
Background technology
The necks such as production, petroleum refining and petrochemistry manufacture, the production of PVC chemical products in crude oil and natural gas Domain, for the amount and concentration of hydrargyrum can use very big difference according to the difference in the place of production, typically from several ppb to several ppm.In addition Not only there was only monomer hydrargyrum in the disposing waste liquid of gas field, the amount of mercury compound can much unnecessary list in some cases In body hydrargyrum, and these compounds, major part is organic mercury compound.Other containing in the waste water of PVC chlorine industries field Mercury pollution thing major part is chlorination hydrargyrum.And most of adsorbent can only remove hydrargyrum ion, to monomer hydrargyrum and organic water Silver does not have removal effect, does not reach newest discharge standard 5ppb of national mercurous waste liquid.For mercury compound decomposition and inversion is Monomer hydrargyrum, needs under hydrogen gasification process reaction condition more, and high temperature and high pressure, i.e. reaction temperature must be adopted to adopt 200～400 DEG C, 2～6MPa of pressure.And the adsorption reaction speed of adsorbent is low, absorbs the process of the spent sorbents of hydrargyrum And the recovery of hydrargyrum is also the necessary process of complexity.For in the waste liquid or waste water of petrochemical field, containing heavy Or Ultralight crude oil liquid, the partial organic substances in the middle of them be difficult degraded, do not reach water quality discharge standard.And need single Processing equipment.
The content of the invention
In view of this, it is an object of the invention to provide a kind of method that mercury compound in waste liquid is removed under normal temperature and pressure. Can it is continuous and efficiently easily from the various waste liquids containing hydrargyrum in the case where room temperature and normal pressure is close to while removing all kinds of form water Silver, reduces processing cost, and also having simultaneously for the persistent organic pollutants contained in waste water decompose well removal effect.
The purpose of the present invention is achieved through the following technical solutions：
The method that mercury compound in waste liquid is removed under the normal temperature and pressure, comprises the following steps：
Step 1：Under normal temperature and pressure, the waste liquid containing mercury compound is contacted with reaction carriers, and by 170nm～ The ultraviolet or visible light of 400nm wavelength is irradiated, irradiation time 5-10 minute；
Step 2：By photocatalyst catalytic action, mercury compound is decomposed into into monomer hydrargyrum, the monomer hydrargyrum after decomposition Adsorption is carried out by adsorbent.
Further, also including step 3：Hydrargyrum in adsorbent is reclaimed using Low Temperature Heat Treatment technology.
Further, the reaction carriers include one or more in aluminium oxide catalyst, natural crystal, zeolite and silica gel Combination.
Further, the adsorbent includes the adsorbent of the sulfide for main body of Mo-Fe systems.
Further, in the step 1, it is irradiated using 185nm～365nm length ultraviolet lines；
Further, in step 2, catalytic action is carried out by titanium system photocatalyst.
The invention has the beneficial effects as follows：By adopting the present invention, under normal operating conditions, can continuously and it is efficient easily In the case where room temperature and normal pressure is close to while removing all kinds of form hydrargyrums, hydrargyrum is dense in making treatment fluid from the various waste liquids containing hydrargyrum Degree can reach the newest mark of draining less than below 5ppb while the organic pollution to containing in waste water also has high removal efficiency Standard, in addition for the clearance of hydrargyrum in spent sorbents containing hydrargyrum can reach 99%, the hydrargyrum response rate can reach 96%.The present invention The characteristics of having fully demonstrated high removal efficiency, environment-friendly and green, with wide application value.
Other advantages of the present invention, target and feature will be illustrated to a certain extent in the following description, and And to a certain extent, based on being will be apparent to investigating hereafter to those skilled in the art, Huo Zheke To be instructed from the practice of the present invention.The present invention target and other advantages can be realized by description below and Obtain.
Description of the drawings
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with accompanying drawing the present invention is made into The detailed description of one step, wherein：
Fig. 1 be two kinds of model aluminium oxide catalyst carrier schematic diagrams, NK124 and NKHO24；
Fig. 2 is the aluminium oxide (Al used in invention203) and knot of the zeolite mixture under high scanning electron microscope SEM Composition；
Fig. 3 is the structure chart under high scanning electron microscope SEM of Mo-Fe systems solid sulfate in invention；
Fig. 4 is structure chart under high scanning electron microscope SEM of adsorbent in invention (a in figure:Aluminium oxide Al203And boiling The mixed carrier of stone；b:Mo-Fe systems solid sulfate).
Specific embodiment
Hereinafter with reference to accompanying drawing, the preferred embodiments of the present invention are described in detail.It should be appreciated that preferred embodiment Only for the explanation present invention, rather than in order to limit the scope of the invention.
The method that mercury compound in waste liquid is removed under the normal temperature and pressure of the present invention, comprises the following steps：
Step 1：Under normal temperature and pressure, the waste liquid containing mercury compound is contacted with reaction carriers, and by 170nm～ 400nm length ultraviolets line or visible light are irradiated, and irradiation time is 5-10 minutes；
Step 2：By photocatalyst catalytic action, mercury compound is decomposed into into monomer hydrargyrum, the monomer hydrargyrum after decomposition Adsorption is carried out by adsorbent.
Step 3：Hydrargyrum in adsorbent is reclaimed using Low Temperature Heat Treatment technology.
In step 1, there is provided an each form hydrargyrum organic compound for containing in said debris, with can make water Silver-colored organic compound conversions are the monomer hydrargyrum conversion processing stage contacted by the material of monomer hydrargyrum.It is described here The material that all kinds of hydrargyrum organic compound conversions are monomer hydrargyrum can be made to include aluminium oxide catalyst (Al2O3), as shown in figure 1, separately Outward, zeolite catalyst carrier, ceramic catalyst carrier, colloidal silica catalyst carrier, absorbent charcoal carrier, fiber carrier, porous glass with And natural crystal etc., for a kind of combination that can also be several in them, may be used to as reaction carriers.For natural Ore can be any one of Kaolin, montmorillonite, attapulgite, bentonite, kieselguhr, volcanic ash, zeolite, flyash or It is arbitrarily various to be mixed in proportion.In these decomposition catalyst carriers remove r- aluminium oxidies, beyond silicon and zeolite, as silicon- The big porous mass of specific surface area such as this kind of complex carrier of aluminium oxide is also used.Aluminium oxide-zeolite this combination is in practice Good reaction effect is embodied, the structure of high scanning electron microscope SEM of aluminium oxide-zeolite mixture is as shown in Figure 2.
For aluminium oxide catalyst carrier can be divided into the γ types of the α types and activated alumina of corundum etc. etc., possess here Contact degrading activity is γ types.The specific surface area of the γ type activated alumina catalyst carriers for being used here be 50～ 500m2/ g, preferably with 120～250m2/ g, 0.1～1.5cm of pore volume3/ g, preferably with 0.4～1.4cm3/g。
For zeolite or natural minerals, they are all crystalline aluminum silicate compounds so possessing various crystallization structure Make.H types, cation exchange and layer structure etc. are used and are all possible, but sometimes need to consider to decompose hydrocarbon solution Property activity control, so compared with other adopt layer structure more.The layered zeolite for using or the principal shape of natural minerals It is specific surface area in 150～700m2/ g, preferably with 350～500m2/ g, 0.1～0.5cm of pore volume3/ g, preferably with 0.2～0.4cm3/g。
In step 2) in, the present invention adopt middle-ultraviolet lamp or visible photocatalysis conversion energy, wavelength of light be 170nm～ 400nm, preferably with 185nm～365nm, in the present invention in uviol lamp or the tube outer wall of visible light, is entered with titanium photocatalyst The transparent adherence overlay film of row.In whole course of reaction, photocatalyst rises and decomposes catalytic action.In the present embodiment, using visible ray titanium light Wavelength can be adopted during catalyst to be irradiated for the visible ray of more than 300nm, carried out using the quartz burner of 185nm～365nm During irradiation, the preferential ultraviolet photocatalyst using titanium dioxide so can just react at normal temperatures and pressures, reduce operation Cost.
For the selection of adsorbent, in the present embodiment, adsorbent mainly adopts sulfide including Mo-Fe systems for main body Adsorbent.Adsorbent is mainly used in the solid absorbent with insoluble and slightly solubility metal sulfide for main body and is contacted, and makes list Body hydrargyrum occur vulcanizable cures reaction the sulfide removal stage, the adsorbent elements for using can be molybdenum, tungsten, vanadium, copper, ferrum, At least select in the metals such as nickel, zinc, cadmium it is a kind of can also be this metal alloy or two kinds and two or more metals, then Vulcanizing treatment is carried out to them, adsorbent product is obtained, such as Mo-Fe mixing is led to alumina carrier surface OH groups with species The control of excess temperature and pressure forms molecular layer, Fe3+Ionic replacement Al3+Ion occupies alumina surface position, and Mo6+From It is sub then combined with the oxonium ion in molecular layer, using newly-generated presoma by the oxidation state of its active component by temperature, pressure Power controls to be converted into sulphided state, and Mo with vulcanizing agent is added6+Ion and Fe3+Ion is changed into active specy by vulcanizing treatment； Can also use in the oxide of those metals, chloride, sulfide or polysulfide one or two and it is two or more mixed Compound, carries out process and obtains adsorbent product.During adsorbent use, carrier can be adopted, it is also possible to do not use carrier, Adsorbent can make the form such as powder, broken shape, cylindric, spherical, fibrous, cellular, according to practical service environment Carry out selection use.
In the present embodiment, adsorbent is allowed to be dispersed on carrier, with the increase of dispersibility, the effect of adsorbent in the present invention Become more preferable.Carrier is mixed into aluminium oxide-zeolite system particularly, and molten dispersion Mo-Fe systems solid of penetrating vulcanizes on this support Thing is optimal for the method for adsorbent.Structure such as Fig. 3 of high scanning electron microscope SEM of Mo-Fe systems solid sulfate It is shown.The structure of high scanning electron microscope SEM of the adsorbent on carrier with vulcanization reaction thing is as shown in Figure 4.
In practical operation, on carrier, the amount scope of Mo-Fe systems solid sulfate is 0.1～30wt%, especially with It is ideal in the case of 10～20wt%.If it exceeds this amount, the effect of carrier will reduce dispersibility to be reduced.If amount Very little, then the adsorption treatment effect of adsorbent will be deteriorated.
In the waste liquid that the present invention is adopted, the processing method containing each form hydrargyrum can substantially be divided into two stages：First Stage is each form hydrargyrum organic compound for containing in said debris, with can make hydrargyrum organic compound conversions be monomer The monomer hydrargyrum conversion processing stage contacted by the material of hydrargyrum；Second stage is vulcanized with insoluble and slightly solubility metal Thing is contacted for the solid absorbent of main body, makes monomer hydrargyrum that the sulfide removal stage of vulcanizable cures reaction to occur.This It is bright contain in the various waste liquids of efficient process whole form hydrargyrums while, the hardly degraded organic substance in waste water ultraviolet with And be decomposed in the presence of photocatalyst, the material after decomposition has the carrier adsorptions such as oxidized aluminum or activated carbon to remove.By adopting The method, the whole form hydrargyrums contained in various waste liquids after being separated with liquid effectively can be removed, and reach 5ppb standards with It is interior.
Low Temperature Heat Treatment can be carried out by the hydrargyrum solidfied material after solid-liquid separation in the present invention, hydrargyrum resource is reclaimed.Process In spent sorbents, residual water silver concentration is less than 0.1% afterwards, and the response rate of hydrargyrum can reach more than 96%.
In the present invention for the sulfuration hydrargyrum after solidification reclaims hydrargyrum therein using low-temperature heat, comprise the concrete steps that It is 200～300 DEG C that heating-up temperature is controlled in rotary kiln roasting smelting device, heating treatment time 40～60 minutes, and device is intrinsic pressure Power is 90～100kPa, and sufficient air will be provided when heating, and air velocity is 500～600ml/min.Material adsorbent In composition there must be ferrous compound, silicon dioxide and calcium dioxide.For ferrous compound can be oxygen Change ferrous, Iron sulfuret., ferrous chloride, ferrous sulfate, ferrous nitrate, in ferrous phosphate, and ferrous other compounds One kind, and two or more mixture, it is preferred to use iron sulfide.For silicon dioxide, mainly there is conduct The clay of adsorbent elements, zeolite, ceramics, porous glass, colloidal silica catalyst, a kind of thing in natural crystal and soil etc. Matter, or two kinds and two or more compounding substances.The combination of zeolite and aluminium oxide is used preferably as carrier.For calcium What compound was conventional is two kinds and two or more in calcium oxide, calcium hydroxide or Calcium Carbonate etc., and these compounds Compounding substances.In this condition with a temperature of, HgS is broken down into hydrargyrum simple substance through a series of reaction of catalytic chemistries, and with gaseous state shape Formula is escaped with tail gas, and other metallicses are then remained in waste residue.Jing rotations are distinguished at high temperature with the steam hydrargyrum that tail gas is escaped Wind dust-precipitator and bagroom gather dust after removal mercurial soot, then cooler, tubulation cooler and surge tank are cold in scripture mound respectively Congeal into liquid mercury, Jing water seals are slipped mercury tank and collected and enter collection mercury tank, then the packaging and storage by washing after mercury tank washes clean.It is buffered Tail gas after tank condensation demercuration Jing after the further demercuration of packed absorber introduces full factory's vent gas treatment workshop by blower fan again and processes.It is de- Waste residue after hydrargyrum is pumped to vacuum rewinding tank by vacuum pump Jing after the cooling of slag cooler, finally keeps in collection slag bath, according to demercuration Composition in slag is processed afterwards.
Specific embodiment：
1 Xinjiang of the experimental example treating waste liquid of hydrargyrum containing monomer
Total hydrargyrum amount (mg/L)
Before processing 1200
After adsorption treatment 0.00021
2 Shaanxi of the embodiment treating waste liquid of mercury pollution containing ion
Total hydrargyrum amount (mg/L)
Before processing 1.92
After adsorption treatment 0.0003
Embodiment 3
For the recovery of the hydrargyrum for wherein adsorbing after processing for spent sorbents low-temperature heat.Spent sorbents for testing come The adsorbent after absorption hydrargyrum from experiment, measures its content for 67g/kg
4 zunyi, guizhou mercury pollution containing ion waste liquid of embodiment
Total hydrargyrum amount (mg/L)
Before processing 1.52
After adsorption treatment 0.0045
Finally illustrate, above example is only unrestricted to illustrate technical scheme, although with reference to compared with Good embodiment has been described in detail to the present invention, it will be understood by those within the art that, can be to the skill of the present invention Art scheme is modified or equivalent, and without deviating from the objective and scope of the technical program, which all should be covered in the present invention Right in the middle of.

Claims (5)

1. the method that mercury compound in waste liquid is removed under normal temperature and pressure, it is characterised in that：The method comprising the steps of：
Step 1：Under normal temperature and pressure, the waste liquid containing mercury compound is contacted with reaction carriers, and by 170nm～ The ultraviolet or visible light of 400nm wavelength is irradiated, irradiation time 5-10 minute；
Step 2：By the photocatalyst catalytic action of the molten photocatalyst for penetrating attachment on reaction carriers, mercury compound is decomposed into into list Body hydrargyrum, the scattered adsorption agent on carrier, the adsorbed agent of the monomer hydrargyrum after decomposition absorb and are attached on carrier with adsorbent, Monomer hydrargyrum in waste water is removed；
Also include step 3：Hydrargyrum in adsorbent is reclaimed using Low Temperature Heat Treatment technology.
2. the method that mercury compound in waste liquid is removed under normal temperature and pressure according to claim 1, it is characterised in that：It is described Reaction carriers include zeolite catalyst carrier, ceramic catalyst carrier, colloidal silica catalyst carrier, absorbent charcoal carrier, fiber carrier, porous The combination of one or more in property glass and natural crystal.
3. the method that mercury compound in waste liquid is removed under normal temperature and pressure according to claim 1 and 2, it is characterised in that： The adsorbent includes the adsorbent of the sulfide for main body of Mo-Fe systems.
4. the method that mercury compound in waste liquid is removed under normal temperature and pressure according to claim 1, it is characterised in that：It is described In step 1, it is irradiated using 185nm～365nm length ultraviolet lines.
5. the method that mercury compound in waste liquid is removed under normal temperature and pressure according to claim 1, it is characterised in that：In step In rapid 2, catalytic action is carried out by titanium system photocatalyst.
CN201410539774.1A 2014-10-13 2014-10-13 The method that mercury compound in waste liquid is removed under normal temperature and pressure Active CN104310676B (en)

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US6858147B2 (en) * 2001-08-03 2005-02-22 Dispersion Technology, Inc. Method for the removal of heavy metals from aqueous solution by means of silica as an adsorbent in counter-flow selective dialysis
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TWI441783B (en) * 2010-12-14 2014-06-21 Super Dragon Technology Co Ltd Method of removing heavy metals from wastewater
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