CN106693914A - Method for hydrothermally preparing chromium blocking and control adsorbent from biomass and application - Google Patents
Method for hydrothermally preparing chromium blocking and control adsorbent from biomass and application Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The invention belongs to the fields of materials, metallurgy and resources and environments and in particular relates to a method for hydrothermally preparing a chromium blocking and control adsorbent from biomass and application. The method comprises the following steps: firstly, after washing a biomass template, crushing the biomass template for later use; secondly, immersing the crushed biomass into a chromate solution; finally, putting a mixture of the biomass and the chromate solution into a high-pressure reaction kettle; after reacting, obtaining a chromium-based composite compound with a nano structure. The adsorbent provided by the invention keeps a regular multi-grade structure in the biomass and can also form a blocking and control effect on chromium; the adsorbent is suitable for purifying an impurity element in a chromium solution. The chromium blocking and control adsorbent is filtered, washed and dried for later use. The chromium blocking and control adsorbent can be used for efficiently and selectively adsorbing impurities including vanadium, arsenic, antimony, aluminum, iron and the like in the chromium solution and a blocking and control effect on a chromium element in a mother solution is formed, so that the purification effect of the chromium solution is realized. The preparation method of the adsorbent is simple to operate and low in cost, and a ppb-grade purification effect can be realized.
Description
Technical field
The invention belongs to material, metallurgical and resource and environment filed, and in particular to a kind of biomass template method Hydrothermal Synthesiss system
The method of standby efficiently resistance control Adsorbent and the application in element purification, micro miscellaneous of adsorbing separation especially in chromium solution
Prime element.
Background technology
Chromium is important strategic resource, is widely used in the research fields such as national defense industry, chemical industry, superconductor and hydrogen bearing alloy.
In the process of chrome ore, because vanadium and chromium are adjacent element in the periodic table of elements, therefore property is more similar, generally
It is present in vanadium titano-magnetite in the way of symbiosis, affects the purification process of chromium and the purity of final products.Additionally, with work
Skill is goed deep into, and chrome ore leachate also remains other elements such as aluminium, iron, arsenic, antimony etc..The presence of these impurity can also influence chromium to produce
The purity and quality of product.In mineral process, if the main component of generation is discharged for the waste water of chromium without treatment, a side
Face can pollute to environment, threaten human health；On the other hand also result in the waste of chromium resource.Therefore, chromium solution is reduced
In impurity content, purifying chromium solution there is important meaning for improving the quality and the recycling of chromate waste water of chromium product
Justice.
For containing vanadium and chromium solution, the separation method of current vanadium chromium mainly has extraction, ion-exchange, chemical precipitation method
Deng.In the Chinese patent of Publication No. CN 102534266A, propose one kind with Liquid-Liquid-Liquid Systems extract and separate vanadium chromium
Method.Phase salt and polymer are added into vanadium chromium solution first, aqueous two-phase body is formed after into phase salt and polymer dissolving
System, then adds organic phase in above-mentioned double-aqueous phase system.Three-phase system is obtained by vibration, split-phase, standing, it is possible to achieve vanadium
The separation of chromium.It has the disadvantage, in operation in order to extend the service life of extractant, the requirement to the pH of solution is more tight
Lattice.In the patent of Publication No. CN103773956A, propose that a kind of method using reduction-precipitation-calcining-dissolution is molten to vanadium chromium
Vanadium chromium in liquid is separated, while chrome green and vanadic anhydride product has been obtained, but the technological process is long, behaviour
Make cumbersome.In the patent of Publication No. CN 102925686A, propose from containing Selective Separation in vanadium, the solution of chromium and extraction vanadium
With the method for chromium, realize vanadium and chromium efficiently separate and high-purity is extracted, but the process need to apply to ion exchange resin, need
The chromium that will be remained in using detergent in exchange column is washed, and technique is relatively complicated.Li Hong Qe etc. were in 2014《Steel vanadium
Titanium》One kind is reported on the 3rd phase of magazine page 5 with anion exchange resin selective absorption vanadium so as to separate and extract vanadium and chromium
Method, and elaborate the mechanism of the resin adsorption vanadium and the separation principle of vanadium chromium.But the technique is in ion exchange resin conversion and regeneration step
Need to consume substantial amounts of acid in rapid, and a large amount of waste water can be produced during regeneration.Wei Guang leaves in 2013 et al. exist《China YouSe metallography
Report》The progress of aluminum removing method in chrominm salt production technology is reported in the 6th phase page 1712 of volume 23.It is main from solid phase method in text
Reviewed with two aspects of liquid phase method various except the method characteristic of aluminium, and inquired into the developing direction of aluminum removing method.It is molten for chromium
Other micro impurity elements in liquid, such as arsenic, antimony etc. are separated, and presently relevant document report is less.
2015, Canadian scholar Ridha existed《Chemical Engineering Journal》On volume 274 page 69
One is reported with biomass such as maple leaf, white corks as template, Ca (OH) is successfully synthesized2Base nano particle, the material is to two
Carbonoxide has the performance of enhancing absorption.2015, Xie Yinde etc. existed《Zhengzhou University's journal》Reported in the phase page 34 of volume 36 6
Synthesize the research of iron cobalt nano material on biological template method, use apoferritin be biological template in text, with cobalt nitrate with
Iron ammonium sulfate is raw material, has synthesized the iron cobalt nano material of protein envelope for reducing agent using sodium borohydride.In January, 2015
Huang Xin etc. exists《Sichuan Teachers University journal》Biological template method in the phase page 148 of volume 38 1 is summarized in preparing the text of nano material one
87 domestic and foreign literatures, are all to form nano material using the masterplate effect of element dipping, for being catalyzed, the energy and detection etc.
Field, and the group for biomass is not reported with the reduction of Cr VI, while to the resistance control effect and solution of element
Purification still without reference to.
Biomass-based one side can serve as template, complete the template effect in adsorbent self assembling process, that is, synthesize
The features such as target product can inherit the chemical constituent and multilevel hierarchy of template；On the other hand, the biomass-based reducing agent that serves as can
Redox reaction is carried out with Cr VI, chromium base complex chemical compound is formed.This reaction hydrothermal condition can next step complete, no
Need to additionally introduce reducing agent, biomass-based this dual-use function is not reported also.Therefore, the present invention is pure for chromium solution
Change the adsorbent proposed using biomass water hot preparation chromium resistance control effect, have for the impurity element in purification chromium solution certain
Practical significance.
The content of the invention
The purpose of the present invention is to overcome above-mentioned not enough problem, macroscopically establishes overall offer mass exchange passage, microcosmic
On by nano-particle build cluster, to solution host ions formed resistance control impurity purify new system physical model；It is chemically sharp
The chromium base complex chemical compound with nanostructured, the organic matter in biomass are constructed with the chemical property of chromium and the reaction of cell
Can be under hydrothermal conditions trivalent chromium by hexavalent chrome reduction, chromium in advance all occupies the adsorption site of adsorbent, and provides mesh
Mark the adsorption site of ion.Therefore, it is template using biomass such as tangleweed etc. that this patent is proposed a kind of, Hydrothermal Synthesiss are net
Change preparation and the purification method of chromium solution adsorbent.On the one hand, the adsorbent remains the regular multilevel hierarchy inside biomass,
On the other hand being formed has the high-efficiency adsorbent of resistance control effect, can be used for the depth of the impurity such as vanadium in chromium solution, arsenic, antimony, aluminium, iron
Degree purification.The technological process is simple, and the selective absorption to impurity is good, can be processing by the chromium solution after purified treatment
High-purity chromium product provides technical support.Simultaneously there is process to be easily controlled, waste water and gas discharge is few, the advantage such as environmental friendly.
Technical scheme：
A kind of method of biomass water hot preparation chromium resistance control adsorbent, step is as follows：
(1) compound concentration is the chromatedsolution of 0.1~1.5mol/L, and it is 2~6 to adjust pH；
(2) biomass are cleaned and is broken into 0.5~5.0cm2Fritter, is added to immersion in chromatedsolution；30~
Soaked 2~36 hours under 70 DEG C of temperature conditionss, obtain biomass potassium chromate mixture；Wherein, biomass and chromatedsolution
Mass volume ratio be 1:2~8；
(3) the biomass potassium chromate mixture for obtaining step (2) is transferred in reactor, in 120~220 DEG C of temperature strips
It is aged 2~8 hours under part, obtains chromium resistance control adsorbent；The chromium resistance control adsorbent washing that will be obtained, filtering, drying for standby.
Described biomass are sea-tangle, stalk, wood chip, leaf or pericarp；
Described chromatedsolution is potassium chromate or sodium chromate；
A kind of application of chromium resistance control adsorbent, described chromium resistance controls adsorbent with chromium solution to be clean according to quality volume
Than being 1:150~500 concussions are stirred, and are reacted 4~5 hours.
Mixed solution is by after purification, vanadium, arsenic, antimony, aluminium, iron ion degree of purification therein is up to ppb ranks.
The chemical composition of chromium resistance control adsorbent is mainly chromium and the oxide and nitride of carbon are (former by biomass of sea-tangle
Material).The high-efficiency adsorbent of chromium resistance control effect prepared by biomass sea-tangle hydro-thermal, the Nano-cluster configuration with marshalling is shown in figure
1-3；400 times of electron micrographs of Fig. 1 keep original interchange channel environment after showing chromium modification, focus primarily upon " thin
The internal integration of born of the same parents' module "；The scanning electron microscope (SEM) photograph of Fig. 2 shows that the cluster is built by three-dimensional order network structure, so that
Quid pro quo qualitative change, realizes the directional migration of the object ion under new soln environment；Fig. 3 is that the transmission electron microscope of the adsorbent shines
Piece, shows that build three-dimensional net structure is the nanometer rods of 10-30nm, and this nanometer rods are mainly chromium with alginic cell wall through thing
The chromium base complex formed after Physicochemical effect.Resistance control can be played a part of to the chromium in solution, so that oriented attachment solution
In other impurity.Entanglement based on matrix can form nanocluster, overcome the single easily disperse of nano-particle, interface group
It is based on hydroxyl, carbonyl and chromium oxide；The infrared spectrogram of Fig. 4 chromium resistance control adsorbent.
Beneficial effects of the present invention：The synthetic route of selective absorbent of the present invention is simple, and easy to operate, corrosivity is low,
It is with low cost, it is environment-friendly.Adsorbent can carry out selective absorption to the trace impurity in the chrome liquor containing magazines such as vanadium, be adapted to
In chromium solution trace element purification with separate, the selective absorption process will not produce secondary pollution, selective absorption impurity
The effect of element is good.
Brief description of the drawings
Fig. 1 is 400 magnification micrographs of adsorbent prepared by the present invention.
Fig. 2 is the cluster scanning electron microscope (SEM) photograph of adsorbent prepared by the present invention.
Fig. 3 is that the cluster of adsorbent prepared by the present invention constitutes microcosmic particle transmission electron microscope picture.
The infrared spectrogram of Fig. 4 chromium resistance control adsorbent.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment, but the invention is not limited in specific implementation
Example.
Embodiment 1：
After sea-tangle is cleaned, the water of excess surface is drained, sea-tangle is broken into about 1cm with scissors2Fritter.Weigh 50g seas
Band fritter, is immersed in the potassium chromate solution of 100mL 0.3mol/L, is placed in 50 DEG C of baking ovens and soaks 2 hours.Again will be above-mentioned mixed
Compound is transferred in autoclave, and 180 DEG C are aged 2 hours.After reaction terminates, the filtering of the solid sample that will obtain, washing, 80 DEG C do
Dry 24 hours standby.The element composition of chromium resistance control agent is shown in Table 1
Table 1 is constituted and basic content with the essential element that sea-tangle prepares chromium resistance control adsorbent as biological raw material
| Element | Weight % | Atom % |
| C | 14.06 | 23.01 |
| N | 2.61 | 3.66 |
| O | 48.07 | 59.08 |
| Na | 1.87 | 0.10 |
| Cr | 33.20 | 12.56 |
| Other | 0.19 | |
| Total amount | 100.0 |
Weigh 0.5g adsorbents and be added to 150mL, during pH value is 8.15 chromium (VI), vanadium (V) mixed liquor, vanadium in mixed liquor
(V), chromium (VI) concentration is respectively 9.803mg/L, 88.79mg/L.Concussion 4h, after being separated by filtration adsorbent, remains in analytical solution
The content of Yu Ge (VI), vanadium (V), calculates adsorbent to chromium (VI), the adsorption capacity of vanadium (V), as a result as follows：
Embodiment 2：
After sea-tangle is cleaned, the water of excess surface is drained, sea-tangle is broken into about 4cm with scissors2Fritter.Weigh 100g seas
Band fritter, is immersed in the potassium chromate solution of 200mL 0.6mol/L, is placed in 60 DEG C of baking ovens and soaks 3 hours.Again will be above-mentioned mixed
Compound is transferred in autoclave, and 180 DEG C are aged 2 hours.After reaction terminates, the filtering of the solid sample that will obtain, washing, 80 DEG C do
Dry 24 hours standby.
Weigh 1g adsorbents and be added to 500mL, during pH value is 9.20 chromium (VI), vanadium (V) mixed liquor, chromium in mixed liquor
(VI), vanadium (V) concentration is respectively 91.44mg/L, 1.164mg/L.Stirring 6h, after being separated by filtration adsorbent, remains in analytical solution
The content of Yu Ge (VI), vanadium (V), calculates by vanadium (V) concentration after sorbent treatment, as a result as follows：
| Initial concentration (mg/L) | Concentration (mg/L) after 6h | Clearance (%) | |
| Vanadium | 1.164 | 0.048 | 95.87 |
| Chromium | 91.44 | ---- | ---- |
Embodiment 3：
After orange peel is cleaned, dry naturally 6 hours, orange peel is broken into about 3cm with pocket knife2Fritter.Weigh 50g seas
Band fritter, is immersed in the potassium chromate solution of 150mL 0.15mol/L, is placed in 80 DEG C of baking ovens and soaks 3 hours.Again will be above-mentioned mixed
Compound is transferred in autoclave, and 200 DEG C are aged 4 hours.After reaction terminates, the filtering of the solid sample that will obtain, washing, 80 DEG C do
Dry 24 hours standby.
Weigh 1g adsorbents and be added to 500mL, during pH value is 5.40 chromium (VI), arsenic (V) mixed liquor, chromium in mixed liquor
(VI), the concentration of arsenic (V) is respectively 93.53mg/L, 8.20mg/L.Stirring 12h, after being separated by filtration adsorbent, in analytical solution
Remaining chromium (VI), the content of arsenic (V), calculate clearance of the adsorbent to arsenic (V), as a result as follows：
| Initial concentration (mg/L) | Concentration (mg/L) after 6h | Clearance (%) | |
| Chromium | 93.53 | ---- | ---- |
| Arsenic | 8.20 | 0.016 | 99.80 |
Embodiment 4：
The stalk cleaned after drying is cut into about 1cm fritters.50g stalk blocks are weighed, is immersed in 150mL0.6mol/L's
In chromium acid sodium solution, it is placed in 80 DEG C of baking ovens and soaks 3 hours.Said mixture is transferred in autoclave again, 200 DEG C of ageings 4
Hour.After reaction terminates, the filtering of the solid sample that will obtain, washing, 80 DEG C of dryings 24 hours are standby.
Weigh 1g adsorbents and be added to 500mL, during pH value is 8.79 chromium (VI), antimony (V) mixed liquor, chromium in mixed liquor
(VI), the concentration of antimony (V) is respectively 93.53mg/L, 8.20mg/L.Stirring 18h, after being separated by filtration adsorbent, in analytical solution
Remaining chromium (VI), the content of antimony (V), calculate clearance of the adsorbent to antimony (V), as a result as follows：
| Initial concentration (mg/L) | Concentration (mg/L) after 18h | Clearance (%) | |
| Chromium | 110.50 | ---- | ---- |
| Antimony | 11.06 | 0.035 | 99.68 |
Embodiment 5：
1-2cm is broken into after maple leaves is cleaned into drying2Piece.30g maple leaves fragments are weighed, 50mL0.1mol/L is immersed in
Potassium chromate solution in, be placed in 50 DEG C of baking ovens soak 2 hours.Said mixture is transferred in autoclave again, 220 DEG C of ageings
6 hours.After reaction terminates, the filtering of the solid sample that will obtain, washing, 80 DEG C of dryings 24 hours are standby.
Weigh 2g adsorbents and be added to 300mL, during pH value is 3.05 chromium (VI), aluminium (III) mixed liquor, chromium in mixed liquor
(VI), the concentration of aluminium (III) is respectively 105.20mg/L, 6.17mg/L.It is put into shaking table and shakes 26h, centrifugation adsorbent,
The content of residual Al (III) in supernatant analytical solution is taken, as a result such as following table：
| Initial concentration (mg/L) | Concentration (mg/L) after 18h | Clearance (%) | |
| Chromium | 105.20 | ---- | ---- |
| Aluminium | 6.17 | 0.037 | 99.40 |
Embodiment 6：
50g wood dusts are weighed, is immersed in the chromium acid sodium solution of 150mL 0.4mol/L, be placed in 80 DEG C of baking ovens and soak 8
Hour.Said mixture is transferred in autoclave again, 210 DEG C are aged 5 hours.After reaction terminates, the solid sample that will be obtained
Filtering, washing, 80 DEG C of dryings 24 hours are standby.
Weigh 1g adsorbents and be added to 500mL, during pH value is 2.50 chromium (VI), iron (III) mixed liquor, chromium in mixed liquor
(VI), the concentration of iron (III) is respectively 120.95mg/L, 16.91mg/L.Magnetic agitation 12h, after being separated by filtration adsorbent, inspection
The content of remaining iron (III) in solution is surveyed, 1g adsorbents, magnetic agitation 12h is added in this solution, then detects solution
Iron (III) concentration, it is as a result as shown in the table：
| Initial concentration (mg/L) | Concentration (mg/L) after 18h | Concentration (mg/L) after 24h | Clearance (%) | |
| Chromium | 120.95 | ---- | ---- | ---- |
| Iron | 16.91 | 0.175 | 0.042 | 99.75 |
Claims (5)
1. a kind of method that adsorbent is controlled in biomass water hot preparation chromium resistance, it is characterised in that step is as follows：
(1) compound concentration is the chromatedsolution of 0.1~1.5mol/L, and it is 2~6 to adjust pH；
(2) biomass are cleaned and is broken into 0.5~5.0cm2Fritter, is added to immersion in chromatedsolution；At 30~70 DEG C
Soaked 2~36 hours under temperature conditionss, obtain biomass potassium chromate mixture；Wherein, the quality of biomass and chromatedsolution
Volume ratio is 1:2~8；
(3) the biomass potassium chromate mixture for obtaining step (2) is transferred in reactor, under 120~220 DEG C of temperature conditionss
Ageing 2~8 hours, obtains chromium resistance control adsorbent；The chromium resistance control adsorbent washing that will be obtained, filtering, drying for standby.
2. method according to claim 1, it is characterised in that described biomass be sea-tangle, stalk, wood chip, leaf or
Pericarp.
3. method according to claim 1 and 2, it is characterised in that described chromatedsolution is potassium chromate or sodium chromate.
4. the application of the chromium resistance control adsorbent that a kind of method described in claim 1 or 2 is obtained, it is characterised in that described chromium
Resistance control adsorbent is 1 according to mass volume ratio with chromium solution to be clean:150~500 concussions are stirred, and are reacted 4~5 hours.
5. the application of the chromium resistance control adsorbent that a kind of method described in claim 3 is obtained, it is characterised in that described chromium resistance control
Adsorbent is 1 according to mass volume ratio with chromium solution to be clean:150~500 concussions are stirred, and are reacted 4~5 hours.
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| CN201611020782.0A CN106693914B (en) | 2016-11-14 | 2016-11-14 | A kind of method and application of biomass water hot preparation chromium resistance control adsorbent |
| PCT/CN2017/075455 WO2017162013A1 (en) | 2016-03-25 | 2017-03-02 | Preparation and application method for ion blocking and controlling adsorbent |
| US15/776,985 US11071967B2 (en) | 2016-03-25 | 2017-03-02 | Method of preparation and application of ion-keeper adsorbent |
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| CN201611020782.0A CN106693914B (en) | 2016-11-14 | 2016-11-14 | A kind of method and application of biomass water hot preparation chromium resistance control adsorbent |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014027953A1 (en) * | 2012-08-17 | 2014-02-20 | Su Holding Ab | Magnetic activated carbon and methods for preparing and regenerating such materials |
| CN104587969A (en) * | 2015-02-03 | 2015-05-06 | 吉林大学 | Preparation method of carbon-base adsorbing material capable of selectively adsorbing copper ions |
| CN104649246A (en) * | 2013-11-18 | 2015-05-27 | 湖南师范大学 | Low temperature hydrothermal preparation method of biomass carbon microsphere / nanosphere |
| CN106076275A (en) * | 2016-06-29 | 2016-11-09 | 山东农业大学 | A kind of porous magnetic Cr VI adsorbent and preparation method thereof |
-
2016
- 2016-11-14 CN CN201611020782.0A patent/CN106693914B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014027953A1 (en) * | 2012-08-17 | 2014-02-20 | Su Holding Ab | Magnetic activated carbon and methods for preparing and regenerating such materials |
| CN104649246A (en) * | 2013-11-18 | 2015-05-27 | 湖南师范大学 | Low temperature hydrothermal preparation method of biomass carbon microsphere / nanosphere |
| CN104587969A (en) * | 2015-02-03 | 2015-05-06 | 吉林大学 | Preparation method of carbon-base adsorbing material capable of selectively adsorbing copper ions |
| CN106076275A (en) * | 2016-06-29 | 2016-11-09 | 山东农业大学 | A kind of porous magnetic Cr VI adsorbent and preparation method thereof |
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