CN106582550A - Lignin xanthate bentonite composite ball and preparation method thereof - Google Patents

Lignin xanthate bentonite composite ball and preparation method thereof Download PDF

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Publication number
CN106582550A
CN106582550A CN201610990137.5A CN201610990137A CN106582550A CN 106582550 A CN106582550 A CN 106582550A CN 201610990137 A CN201610990137 A CN 201610990137A CN 106582550 A CN106582550 A CN 106582550A
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lignin
xanthate
bentonite
composite balls
lignin xanthate
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葛圆圆
李志礼
孔言
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Guangxi University
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Guangxi University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/24Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12Naturally occurring clays or bleaching earth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/22Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26Synthetic macromolecular compounds
    • B01J20/262Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016Particle form
    • B01J20/28019Spherical, ellipsoidal or cylindrical
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/281Treatment of water, waste water, or sewage by sorption using inorganic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/285Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • C02F1/286Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof

Abstract

The invention discloses a lignin xanthate bentonite composite ball which is mainly prepared from, by weight, 5-20 parts of lignin xanthate, 90-120 parts of bentonite, 2-12 parts of dispersing agent, 18-45 parts of sodium alginate and 3-15 parts of regulator. According to the lignin xanthate bentonite composite ball, the bentonite and the lignin are natural inorganic mineral adsorbing material and organic adsorbing material respectively, the cost is low, the reserve volume is rich, and some progresses are made in the aspects of treating heavy metal and antibiotic pollutants in waste water. Because the lignin has weak adsorption capacity to the heavy metal, the modified lignin xanthate bentonite is taken as an active matter; the lignin xanthate bentonite and the bentonite are compounded, so that higher adsorption capacity to the heavy metal is realized.

Description

Lignin xanthate bentonite composite balls and preparation method thereof
Technical field
The invention belongs to field of composite material preparation, biomass resource field, more particularly to a kind of heavy metal, antibiotic Sewage has lignin xanthate bentonite composite balls of preferable adsorption capacity and preparation method thereof.
Background technology
In China, metal plating, process hides, dyestuff, dig up mine, papermaking and some other chemical industry achieve quick sending out Exhibition, but generate in these industrial processes containing the substantial amounts of waste water containing heavy metal ion (such as mercury, zinc, lead Deng), these waste water are also just directly or indirectly discharged without the effective process of sewage department without the monitoring of environment monitoring department To in environment, serious water pollution problems is caused.Because these heavy metal ion in water cannot be voluntarily in biotic environment Decomposition and conversion, will eventually be entered in human body body by the effect of food chain, cause uncomfortable people, poisoning or even cause Cancer, the serious body harm for endangering the mankind of heavy metal ion.
Every year, antibiotic is used the substantial amounts of production of China is simultaneously also substantial amounts of, and yield, consumption occupy world's first. At present, for the use of antibiotic is also without strict limit standard, the antibiosis in people's use, for animals and pharmaceuticals industry production waste water If element is just directly entered the pollution that can equally cause water body in water without effective process indirectly.The a large amount of of antibiotic make Obtaining the resistance to the action of a drug of human body pathogen strengthens, and the immunity for giving people body brings negative effect, can be inhaled by body into after human body Receive, a series of metabolic process of small part Jing generates inactive metabolite, the action time and metabolism time of antibiotic compared with Long, for the antibiotic for entering water environment, it still has biologically active, and can further form mother in the environment Body.Remaining antibiotic can cause the Soil Microorganism resistance to the action of a drug to strengthen in soil, precipitation, gravitational settling and other one A little approach can cause antibiotic to enter in water body, if people's class reference these contain the water of antibiotic, can cause it is uncomfortable very To some other diseases.Antibiotic is the another kind of important pollution sources in water pollution, and the water pollution problems of initiation already becomes Obtain extremely severe.
Lignin also known as lignin, are one of main components of lignocellulose biomass, are storage capacity second on the earth Biomass resource.The annual paper-making industry in the whole world produces 50,000,000 tons of lignin, but the lignin less than 10% is utilized.It is wooden Plain complex structure, not yet known to the mankind, structure is mainly macromolecular group to its concrete structure, mainly contains lignum-vitae base junction The logical basic structure seen of 3 kinds of structure, lilac based structures and p-hydroxyphenyl structure.Lignin contains phenolic hydroxyl group, alcoholic hydroxyl, carbonyl The functional groups such as base, carboxyl and methoxyl group, this has in terms of showing heavy metal of the lignin as low-cost sorbent in eliminating water is gone Great potentiality.But lignin is three-dimensional non-linearity macromolecular compound, it is easy to form intermolecular hydrogen bonding, make it can not Launch in water and be intertwined, form stable flocculate.
Bentonite is the nonmetallic minerals with montmorillonite as main component, is called bentonite, bentonite or swelling rock, due to There are some cations, such as K, Na, Mg in the layer structure of montmorillonite, the effect of these cations and montmorillonite is not sacrifices consisting of an ox, a sheep and a pig Gu, easily by other cation exchanges, thus with certain adsorption capacity.But bentonite hydrophily is strong, there is height in water Expansion, it is easily occupied between layers by hydrone and hydrated ion so as to be difficult to and the heavy metal ion and antibiosis in sewage Plain pollutant is fully contacted, and has had a strong impact on its absorption property.
Conventional powder shape adsorbent easily disperses in water, processes and is susceptible to be lost in now during the pollutant in waste water As, settling velocity is slow, to process be difficult after waste water and separate with water body, adsorbed and be difficult to recycle and reuse after pollutant, Secondary pollution is produced in water.At present, in the correlative study of adsorbent, by being fixed of adsorbent improving its rate of recovery With solve separation of solid and liquid a difficult problem become study hotspot, compared with powdered form adsorbent, spherical adsorbent have good machinery, Mass transfer diffusion, and be easily recycled and recycle, application prospect is boundless in terms of water pollution is processed.
The information for being disclosed in the background section is merely intended to increase the understanding of the general background to the present invention, and should not When the prior art for being considered to recognize or imply in any form the information structure well known to persons skilled in the art.
The content of the invention
It is an object of the invention to provide a kind of lignin xanthate bentonite composite balls, so as to overcome powder sorbent Settling velocity is slow, and later separation is difficult, reclaim the shortcoming being difficult.
Another object of the present invention is to the preparation method of lignin xanthate bentonite composite balls.
For achieving the above object, the invention provides a kind of lignin xanthate bentonite composite balls, by weight Meter, is mainly made up of following material component:5~20 parts of lignin xanthate;90~120 parts of bentonite;Dispersant 2~12 Part;3~15 parts of 18~45 parts of Na-alginate and conditioning agent.
Preferably, in above-mentioned technical proposal, the dispersant is sodium carboxymethylcellulose, neopelex, hard One or more of resin acid monoglyceride.
Preferably, in above-mentioned technical proposal, the conditioning agent be polyvinyl alcohol, n-butanol, polyethylene glycol in one kind or It is various.
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
(2) lignin xanthate and dispersant, bentonite obtained in step (1) are added to the water and are mixed and stirred for It is even, obtain lignin xanthate bentonite composite mortar;
(3) sodium alginate is added to the water and stirs sodium alginate and fully dissolved, be subsequently adding the step (2) obtained Lignin xanthate swelled ground compound slurry and conditioning agent, and stir, obtain mixture of viscous form;
(4) step (3) is obtained into mixture of viscous form and instills CaCl2In solution, and stir, then stand, completely Composite balls are obtained after solidification.
Preferably, in above-mentioned technical proposal, the step (1) prepares lignin xanthate and comprises the following steps:
A. it is lignin and NaOH mixing is soluble in water, formalin is then added dropwise, stir, it is 70-90 in temperature range Under conditions of DEG C, isothermal reaction 2-5 hours;
B. when temperature is down to 30-50 DEG C, then carbon disulfide is added dropwise, reacts 2-4 hours, after the completion of reaction, standing cooling, Filter, then drying obtains yellow-brown solid powder lignin xanthate.
Preferably, in above-mentioned technical proposal, the mass ratio of lignin and NaOH is 7-11 in the step (a):11;It is described Step (b) drying is to be vacuum dried 10-14 hours under conditions of temperature is for 55-65 DEG C.
Preferably, in above-mentioned technical proposal, the temperature of reaction is 40-60 DEG C in the step (2), continuous in course of reaction Stirring 2-4 hours.
Preferably, in above-mentioned technical proposal, reaction is that water-bath is anti-under conditions of temperature 80-100 DEG C in the step (3) Should, it is stirred continuously in course of reaction.
Preferably, in above-mentioned technical proposal, the step (4) is obtained after the composite balls after solidification and is dried, and dries and is 18-24 hours are dried under conditions of temperature is for 50-70 DEG C, final products are obtained after drying.
Preferably, in above-mentioned technical proposal, CaCl in the step (4)2Solution is the CaCl that mass fraction is 1-5%2It is molten Liquid;It is described to stand to stand 20-30 hours.
Compared with prior art, the present invention has the advantages that:
(1) lignin xanthate bentonite composite balls of the present invention, bentonite and lignin are respectively natural inorganic ore deposit Thing sorbing material and organic adsorption material, cheap, rich reserves, the heavy metal and antibiotic pollutant in waste water is processed Aspect is all in progress achieved with some.But because lignin heavy metal adsorption capacity is weaker, the present invention takes modified lignin resin yellow Ortho esters is active matter;Lignin xanthate and bentonite are combined, heavy metal has stronger adsorption capacity.
(2) after due to powder sorbent absorption water pollutant, it is difficult to separate with purified water, and powdered form adsorbent is inhaled It is difficult to recycle and reuse after heavy metal and antibiotic pollutant in attached complete waste water, is unfavorable for economizing on resources.Therefore, the present invention By sodium alginate, lignin xanthate bentonite is carried out into interspersed fixation, prepare lignin xanthate bentonite and be combined Bead, you can have preferable adsorption effect to the heavy metal of low concentration in water, also solves the problem that powder sorbent is met water and easily disperses, sinks The difficult problem of drop poor performance, subsequent treatment separation of solid and liquid.
Specific embodiment
With reference to specific embodiment, the specific embodiment of the present invention is described in detail, it is to be understood that this Bright protection domain is not limited by specific embodiment.
Embodiment 1
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
Under normal pressure, the addition 90g lignin in being furnished with the there-necked flask of electromagnetic agitation and reflux condensing tube, 110g NaOH, Distilled water 1000mL, stirring makes lignin fully dissolve, and controlling reaction temperature is 80 DEG C, is slowly added dropwise the formalin of 90mL, Continue to stir, isothermal reaction 3 hours.Reactant liquor is cooled to into 40 DEG C, the carbon disulfide of 100mL is slowly added dropwise, is stirred 3 hours. Question response is completed, and is stood cooling, is filtered, and is dried 12 hours in 60 DEG C of vacuum drying chambers, obtains yellow-brown solid powder wood Quality xanthate.
(2) the lignin xanthate 20g for weighing (1) preparation is added in 800ml water, and adds dispersant detergent alkylate Sodium sulfonate 6g, glyceryl monostearate 6g, stirring makes its fully dispersed, then weighs 120g bentonites and be added thereto, at 60 DEG C Being stirred continuously is sufficiently mixed it, continuously stirs 4h.The lignin xanthate bentonite composite mortar being uniformly mixed.
(3) 25g sodium alginates are added in 200ml water, heats under 100 DEG C of water-baths and constantly stirred with magnetic stirring apparatus Mixing makes sodium alginate fully dissolve, and the lignin xanthate bentonite as obtained in (2) is added after sodium alginate is completely dissolved Compound slurry, while adding conditioning agent polyvinyl alcohol 5g, n-butanol 5g, polyethylene glycol 5g, is kept stirring for so as to which dispersion is equal It is even, obtain thick mixture.
(4) the thick mixed liquor as obtained in (3) is drawn with syringe, is slowly dropped into the CaCl that mass fraction is 5%2It is molten In liquid, and it is gently mixed, after 30h is stood, is fully cured generation composite balls, with distilled water cyclic washing to neutrality, will be combined Ball is placed in vacuum drying chamber, is dried at 70 DEG C after 22h and is obtained final product final products.
Embodiment 2
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
Under normal pressure, the addition 90g lignin in being furnished with the there-necked flask of electromagnetic agitation and reflux condensing tube, 110g NaOH, Distilled water 1000mL, stirring makes lignin fully dissolve, and controlling reaction temperature is 80 DEG C, is slowly added dropwise the formalin of 90mL, Continue to stir, isothermal reaction 3 hours.Reactant liquor is cooled to into 40 DEG C, the carbon disulfide of 100mL is slowly added dropwise, is stirred 3 hours. Question response is completed, and is stood cooling, is filtered, and is dried 12 hours in 60 DEG C of vacuum drying chambers, obtains yellow-brown solid powder wood Quality xanthate.
(2) the lignin xanthate 15g for weighing (1) preparation is added in 700ml water, and adds dispersant carboxymethyl cellulose Plain sodium 10g, stirring makes its fully dispersed, then weighs 100g bentonites and be added thereto, and being stirred continuously at 50 DEG C makes it fully mix Close, continuously stir 3h.The lignin xanthate bentonite composite mortar being uniformly mixed;
(3) 35g sodium alginates are added in 300ml water, heats under 90 DEG C of water-baths and constantly stirred with magnetic stirring apparatus Mixing makes sodium alginate fully dissolve, and the lignin xanthate bentonite as obtained in (2) is added after sodium alginate is completely dissolved Compound slurry, while adding conditioning agent polyvinyl alcohol 10g, is kept stirring for so as to be uniformly dispersed, and obtains thick mixture.
(4) the thick mixed liquor as obtained in (3) is drawn with syringe, is slowly dropped into the CaCl that mass fraction is 4%2It is molten In liquid, and it is gently mixed, after 24h is stood, is fully cured generation composite balls, with distilled water cyclic washing to neutrality, will be combined Ball is placed in vacuum drying chamber, is dried at 60 DEG C after 20h and is obtained final product final products.
Embodiment 3
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
Under normal pressure, the addition 90g lignin in being furnished with the there-necked flask of electromagnetic agitation and reflux condensing tube, 110g NaOH, Distilled water 1000mL, stirring makes lignin fully dissolve, and controlling reaction temperature is 80 DEG C, is slowly added dropwise the formalin of 90mL, Continue to stir, isothermal reaction 3 hours.Reactant liquor is cooled to into 40 DEG C, the carbon disulfide of 100mL is slowly added dropwise, is stirred 3 hours. Question response is completed, and is stood cooling, is filtered, and is dried 12 hours in 60 DEG C of vacuum drying chambers, obtains yellow-brown solid powder wood Quality xanthate.
(2) the lignin xanthate 5g for weighing (1) preparation is added in 600ml water, and adds glyceryl monostearate 2g, Stirring makes its fully dispersed, then weighs 90g bentonites and be added thereto, and being stirred continuously at 40 DEG C is sufficiently mixed it, continuously stirs Mix 2h.The lignin xanthate bentonite composite mortar being uniformly mixed.
(3) 18g sodium alginates are added in 400ml water, heats under 80 DEG C of water-baths and constantly stirred with magnetic stirring apparatus Mixing makes sodium alginate fully dissolve, and the lignin xanthate bentonite as obtained in (2) is added after sodium alginate is completely dissolved Compound slurry, while adding conditioning agent polyethylene glycol 3g, is kept stirring for so as to be uniformly dispersed, and obtains thick mixture.
(4) the thick mixed liquor as obtained in (3) is drawn with syringe, is slowly dropped into the CaCl that mass fraction is 1%2It is molten In liquid, and it is gently mixed, after 20h is stood, is fully cured generation composite balls, with distilled water cyclic washing to neutrality, will be combined Ball is placed in vacuum drying chamber, is dried at 50 DEG C after 24h and is obtained final product final products.
Embodiment 4
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
Under normal pressure, the addition 90g lignin in being furnished with the there-necked flask of electromagnetic agitation and reflux condensing tube, 110g NaOH, Distilled water 1000mL, stirring makes lignin fully dissolve, and controlling reaction temperature is 80 DEG C, is slowly added dropwise the formalin of 90mL, Continue to stir, isothermal reaction 3 hours.Reactant liquor is cooled to into 40 DEG C, the carbon disulfide of 100mL is slowly added dropwise, is stirred 3 hours. Question response is completed, and is stood cooling, is filtered, and is dried 12 hours in 60 DEG C of vacuum drying chambers, obtains yellow-brown solid powder wood Quality xanthate.
(2) the lignin xanthate 10g for weighing (1) preparation is added in 500ml water, and adds dispersant carboxymethyl cellulose Plain sodium 2g, glyceryl monostearate 6g, stirring makes its fully dispersed, then weighs 100g bentonites and be added thereto, at 50 DEG C not Disconnected stirring is sufficiently mixed it, continuously stirs 5h.The lignin xanthate bentonite composite mortar being uniformly mixed.
(3) 45g sodium alginates are added in 500ml water, heats under 90 DEG C of water-baths and constantly stirred with magnetic stirring apparatus Mixing makes sodium alginate fully dissolve, and the lignin xanthate bentonite as obtained in (2) is added after sodium alginate is completely dissolved Compound slurry, while adding conditioning agent polyvinyl alcohol 5g, polyethylene glycol 7g, is kept stirring for so as to be uniformly dispersed, and obtains thick Mixture.
(4) the thick mixed liquor as obtained in (3) is drawn with syringe, is slowly dropped into the CaCl that mass fraction is 3%2It is molten In liquid, and it is gently mixed, after 26h is stood, is fully cured generation composite balls, with distilled water cyclic washing to neutrality, will be combined Ball is placed in vacuum drying chamber, is dried at 55 DEG C after 20h and is obtained final product final products.
Embodiment 5
A kind of preparation method of lignin xanthate bentonite composite balls, comprises the following steps:
(1) lignin xanthate is prepared;
Under normal pressure, the addition 90g lignin in being furnished with the there-necked flask of electromagnetic agitation and reflux condensing tube, 110g NaOH, Distilled water 1000mL, stirring makes lignin fully dissolve, and controlling reaction temperature is 80 DEG C, is slowly added dropwise the formalin of 90mL, Continue to stir, isothermal reaction 3 hours.Reactant liquor is cooled to into 40 DEG C, the carbon disulfide of 100mL is slowly added dropwise, is stirred 3 hours. Question response is completed, and is stood cooling, is filtered, and is dried 12 hours in 60 DEG C of vacuum drying chambers, obtains yellow-brown solid powder wood Quality xanthate.
(2) the lignin xanthate 18g for weighing (1) preparation is added in 600ml water, and adds dispersant carboxymethyl cellulose Plain sodium 5g, neopelex 3g, stirring makes its fully dispersed, then weighs 95g bentonites and be added thereto, at 55 DEG C not Disconnected stirring is sufficiently mixed it, continuously stirs 3h.The lignin xanthate bentonite composite mortar being uniformly mixed;
(3) 30g sodium alginates are added in 400ml water, heats under 95 DEG C of water-baths and constantly stirred with magnetic stirring apparatus Mixing makes sodium alginate fully dissolve, and the lignin xanthate bentonite as obtained in (2) is added after sodium alginate is completely dissolved Compound slurry, while adding conditioning agent polyvinyl alcohol 5g, n-butanol 4g, is kept stirring for so as to be uniformly dispersed, and obtains thick Mixture.
(4) the thick mixed liquor as obtained in (3) is drawn with syringe, is slowly dropped into the CaCl that mass fraction is 3.5%2 In solution, and it is gently mixed, after 24h is stood, is fully cured generation composite balls, with distilled water cyclic washing to neutrality, will answers Close ball to be placed in vacuum drying chamber, be dried at 65 DEG C after 22h and obtain final product final products.
Service condition
The lignin xanthate bentonite composite balls prepared using the present invention process the clearance of mercury-containing waste water.Mercury concentration For 20mg/L, adsorption time 32h, operation temperature is 28 DEG C.As shown in table 1.
Clearance of the different adsorbents of table 1 to mercury pollution waste water
As shown in Table 1, unmodified bentonite and lignin xanthate bentonite composite balls have to mercury pollution waste water Except effect, but under same amount, lignin xanthate bentonite composite balls are substantially better than unmodified bentonite, in addition During amount more than 5.6g/L, composite balls are to the clearance of mercury waste water more than 90%.
Using absorption of the lignin xanthate bentonite composite balls of present invention preparation to Doxycycline Hyclate in waste water Amount.Doxycycline Hyclate initial concentration 1200mg/L, adsorbent addition 8.0g/L, adsorption time 32h, 28 DEG C of operation temperature. As shown in table 2.
Adsorbance of the different adsorbents of table 2 to Doxycycline Hyclate waste water
As shown in Table 2, how western unmodified bentonite and lignin xanthate bentonite composite balls are to the hydrochloric acid in waste water Ring have suction-operated, but under same concentrations, absorption of the lignin xanthate bentonite composite balls to Doxycycline Hyclate Amount is much higher than unmodified bentonite in more than 200mg/g.
It is aforementioned to the present invention specific illustrative embodiment description be in order to illustrate and illustration purpose.These descriptions It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned teaching, can be much changed And change.The purpose of selecting and describing the exemplary embodiment is that explaining that the certain principles and its reality of the present invention should With so that those skilled in the art can realize and using the present invention a variety of exemplaries and A variety of selections and change.The scope of the present invention is intended to be limited by claims and its equivalents.

Claims (10)

1. a kind of lignin xanthate bentonite composite balls, it is characterised in that count by weight, mainly by following raw material group Part is made:
2. lignin xanthate bentonite composite balls according to claim 1, it is characterised in that the dispersant is carboxylic Sodium carboxymethylcellulose pyce, neopelex, one or more of glyceryl monostearate.
3. lignin xanthate bentonite composite balls according to claim 1, it is characterised in that the conditioning agent is poly- One or more in vinyl alcohol, n-butanol, polyethylene glycol.
4. a kind of preparation method of lignin xanthate bentonite composite balls as claimed in claim 1, it is characterised in that bag Include following steps:
(1) lignin xanthate is prepared;
(2) lignin xanthate and dispersant, bentonite obtained in step (1) are added to the water and are mixed and stirred for uniformly, obtaining To lignin xanthate bentonite composite mortar;
(3) sodium alginate is added to the water and stirs sodium alginate and fully dissolved, be subsequently adding wooden obtained in the step (2) Plain xanthate swelled ground compound slurry and conditioning agent, and stir, obtain mixture of viscous form;
(4) step (3) is obtained into mixture of viscous form and instills CaCl2In solution, and stir, then stand, after being fully cured Obtain composite balls.
5. the preparation method of lignin xanthate bentonite composite balls according to claim 1, it is characterised in that described Step (1) prepares lignin xanthate and comprises the following steps:
A. it is lignin and NaOH mixing is soluble in water, formalin is then added dropwise, stir, it is 70-90 DEG C in temperature range Under the conditions of, isothermal reaction 2-5 hours;
B. when temperature is down to 30-50 DEG C, then carbon disulfide is added dropwise, reacts 2-4 hours, after the completion of reaction, stand cooling, mistake Filter, then drying obtains yellow-brown solid powder lignin xanthate.
6. the preparation method of lignin xanthate bentonite composite balls according to claim 5, it is characterised in that described The mass ratio of lignin and NaOH is 7-11 in step (a):11;Step (b) drying is in the condition that temperature is 55-65 DEG C Lower vacuum drying 10-14 hours.
7. the preparation method of lignin xanthate bentonite composite balls according to claim 1, it is characterised in that described The temperature of reaction is 40-60 DEG C in step (2), and 2-4 hours are continuously stirred in course of reaction.
8. the preparation method of lignin xanthate bentonite composite balls according to claim 1, it is characterised in that described Reaction is the water-bath under conditions of temperature 80-100 DEG C in step (3), is stirred continuously in course of reaction.
9. the preparation method of lignin xanthate bentonite composite balls according to claim 1, it is characterised in that described Step (4) is obtained after the composite balls after solidification and is dried, and it in temperature is that to be dried 18-24 little under conditions of 50-70 DEG C that drying is When, final products are obtained after drying.
10. the preparation method of lignin xanthate bentonite composite balls according to claim 1, it is characterised in that institute State CaCl in step (4)2Solution is the CaCl that mass fraction is 1-5%2Solution;It is described to stand to stand 20-30 hours.
CN201610990137.5A 2016-11-10 2016-11-10 Lignin xanthate bentonite composite ball and preparation method thereof Pending CN106582550A (en)

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CN107162145A (en) * 2017-05-23 2017-09-15 湖南工业大学 A kind of heavy metal chelant flocculant containing xanthogen and its preparation and application
CN108654582A (en) * 2018-05-25 2018-10-16 合肥慧谷农业科技有限公司 A kind of biological adsorption agent prepared using Thallus Laminariae (Thallus Eckloniae) extract
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CN116813356A (en) * 2023-07-22 2023-09-29 佛山市奥林万达新型建材有限公司 Ceramic body reinforcing agent and preparation method thereof
CN116813356B (en) * 2023-07-22 2024-04-19 佛山市奥林万达新型建材有限公司 Ceramic body reinforcing agent and preparation method thereof

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Application publication date: 20170426