CN110227421A - A kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel - Google Patents

A kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel Download PDF

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Publication number
CN110227421A
CN110227421A CN201910525536.8A CN201910525536A CN110227421A CN 110227421 A CN110227421 A CN 110227421A CN 201910525536 A CN201910525536 A CN 201910525536A CN 110227421 A CN110227421 A CN 110227421A
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China
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active carbon
shinyleaf yellowhorn
yellowhorn shell
shell active
based aquagel
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CN201910525536.8A
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Chinese (zh)
Inventor
郝一男
王任飞
王喜明
红岭
丁立军
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Inner Mongolia Agricultural University
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Inner Mongolia Agricultural 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
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/261Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
    • 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
    • B01J20/28047Gels
    • 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
    • C02F1/283Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them

Abstract

The present invention relates to technical field of function materials, disclose a kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel, and charing that shinyleaf yellowhorn shell powder is heated up in the case where completely cutting off air conditions obtains shinyleaf yellowhorn shell active carbon;It takes shinyleaf yellowhorn shell active carbon powder, polyvinyl alcohol and sodium alginate to add water mixed dissolution in a reservoir, and carries out ultrasonic wave and disperse to obtain uniform suspension;By suspension water-bath in heat, CaCl is added dropwise in container when there is dope2Solution is cooled into spherical hydrogel after keeping the temperature after completion of dropwise addition;Finally hydrogel is dried, is crushed.The present invention prepares active carbon using shinyleaf yellowhorn shell, then space net structure is formed using polyethylene glycol and sodium alginate to coat active carbon, form the spheric active carbon based aquagel that surface has oxygen-containing functional group, selective absorption can be carried out to the dye substance in water, also evade the problem of be easy to causeing adsorbent to be lost when directlying adopt active carbon particle.

Description

A kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel
Technical field
The present invention relates to technical field of function materials, and in particular to a kind of preparation side of shinyleaf yellowhorn shell active carbon based aquagel Method and its application.
Background technique
There is data to suggest that total weight is discharged China's dyeing waste water day at 300-400 tons, and every 1 ton of untreated dyestuff Discharge of wastewater will result in the pollution of 20 tons of natural environment water bodys into environment[17].The world today, there are about 1,400,000,000 populations not to have Direct drinking water resource, more than 80 countries' (greater than 40% of world population) lack originally water resource[18].2000, joint State organizes oneself that China is classified as one of 13 poor-water states, the world.Waste water from dyestuff coloration is big, high organic content, complicated component, can The features such as biochemical is poor makes waste water from dyestuff have bigger harmfulness.If untreated waste water from dyestuff is allowed to enter water body environment, Huge prestige rib can be brought to natural water environment, natural environment, the existence of the mankind or even the sustainable development of economic society.
Active carbon is a kind of porous functional material, active carbon be considered as be arranged in it is similar with graphite carbon crystal " helical form layered structure ".Active carbon has a series of features and advantages, such as: huge void ratio and huge specific surface Product, the corrosion resistance of strength can resist high temperature, not be afraid of the ability of acid and alkali corrosion, and electric conductivity is very outstanding, chemistry Stability and biocompatibility are also high, and to the excellent adsorptivity of physical property and chemical property.Active carbon and people's It lives closely bound up, sizable effect can be played in every field, for example in power industry, active carbon is due to stronger suction Attached ability can accomplish desulfurization and dephosphorization;In chemical industry, the harmful substances such as CO that absorption smeltery generates;Food safety row Industry, may be used as desiccant makes food have the longer shelf-life;Also there is relatively broad application in environmental protection industry.
But the absorption of active carbon is a physical adsorption process, and Powdered Activated Carbon has unique excellent in the treatment of waste water Gesture, but it the shortcomings that it is also obvious that because the partial size very little of Powdered Activated Carbon, quality also very little, hold very much in use It easily just goes in air, causes to be lost, to increase cost.Moreover, being difficult and moisture after the completion of absorption in sewage treatment It separates out and, this is also current problem to be solved.Prepare at this stage in addition active carbon material largely select timber into Row production, consumes a large amount of timber resources, is unfavorable for environment.
Summary of the invention
Based on problem above, the present invention provides a kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel, Active carbon is prepared using shinyleaf yellowhorn shell, is reduced resource waste, shinyleaf yellowhorn shell active carbon has very big specific surface area and aperture; Then it forms space net structure using polyethylene glycol and sodium alginate to coat active carbon, forming surface has oxygen-containing official The spheric active carbon based aquagel that can be rolled into a ball can carry out selective absorption to the dye substance in water;The grain of particle is increased simultaneously Diameter has evaded the problem of be easy to causeing adsorbent to be lost when directlying adopt active carbon particle.
In order to solve the above technical problems, the present invention provides a kind of preparation method of shinyleaf yellowhorn shell active carbon based aquagel, Include the following steps:
S1: crushing after shinyleaf yellowhorn shell is dried, and smashed shinyleaf yellowhorn shell powder is risen in the case where completely cutting off air conditions Temperature charing, obtains shinyleaf yellowhorn shell active carbon;
S2: taking out the shinyleaf yellowhorn shell active carbon distilled water repeated flushing prepared, be then filtered, then will filtering The shinyleaf yellowhorn shell active carbon obtained afterwards is placed in 100 DEG C of baking oven and is dried, and is cooled to room temperature after drying spare;
S3: dry 100 parts of shinyleaf yellowhorn shell active carbon powder, 15 parts of polyvinyl alcohol and seaweed after cooling are taken by mass fraction 15 parts of sour sodium, is then blended in the container for filling 500 parts of distilled water, and container is placed in ultrasonic dispersing machine and carries out ultrasonic wave After dispersing 10~20min, uniform suspension is obtained;
S4: suspension is placed in 80 DEG C of water-bath and is heated, constantly stirred with glass bar in heating process, work as appearance When dope, 500 parts of 10%CaCl is added dropwise into container2Solution keeps the temperature 60~120min, then is cooled into after completion of dropwise addition Spherical hydrogel, is finally dried hydrogel, obtains shinyleaf yellowhorn shell active carbon based aquagel.
Further, the carbonization process temperature control in step S1 are as follows: by room temperature to 120 DEG C, keep the temperature 30min;So Temperature is risen to 200 DEG C afterwards, and keeps the temperature 60min;600 DEG C are finally warming up to, 120min is kept the temperature.
Further, heating rate is 10 DEG C/min in carbonization process.
Further, CaCl in step S42The rate of addition of solution is 3~5 parts/min.
To solve the above problems, the present invention also provides a kind of applications of shinyleaf yellowhorn shell active carbon based aquagel, including with Lower step: it takes in liquid of the shinyleaf yellowhorn shell active carbon based aquagel adsorbent material investment containing dye substance, adjusting pH value of solution is 3 ~5,1~3h is reacted at 10 DEG C~60 DEG C;After adsorption reaction, it is separated by filtration shinyleaf yellowhorn shell active carbon based aquagel.
Compared with prior art, the beneficial effects of the present invention are: the present invention prepares active carbon using shinyleaf yellowhorn shell, reduce Then the wasting of resources forms space net structure using polyethylene glycol and sodium alginate and coats to active carbon, forms surface Spheric active carbon based aquagel with oxygen-containing functional group can carry out selective absorption to the dye substance in water;Increase simultaneously The partial size of particle, has evaded the problem of be easy to causeing adsorbent to be lost when directlying adopt active carbon particle.
Detailed description of the invention
Fig. 1 is the preparation method flow chart that embodiment Chinese is preced with active fruit shell carbon based aquagel;
Fig. 2 is the infrared spectrogram of 2 Chinese hat active fruit shell carbon and shinyleaf yellowhorn shell active carbon based aquagel of embodiment;
Fig. 3 is the nitrogen adsorption curve of 2 Chinese hat active fruit shell carbon and shinyleaf yellowhorn shell active carbon based aquagel of embodiment;
Fig. 4 is the graph of pore diameter distribution of 2 Chinese hat active fruit shell carbon and shinyleaf yellowhorn shell active carbon based aquagel of embodiment.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below with reference to embodiment and attached drawing, to this Invention is described in further detail, and exemplary embodiment of the invention and its explanation for explaining only the invention, are not made For limitation of the invention.
Embodiment 1:
Referring to Fig. 1, a kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel include the following steps:
S1: crushing after shinyleaf yellowhorn shell is dried, and smashed shinyleaf yellowhorn shell powder is risen in the case where completely cutting off air conditions Temperature charing, obtains shinyleaf yellowhorn shell active carbon (hereinafter abbreviated as " XSBAC ");
S2: the XSBAC distilled water repeated flushing prepared is taken out, for removing the ashy substance in XSBAC, Yi Mianying Ring its absorption property;Then it is filtered, then the XSBAC obtained after filtering is placed in 100 DEG C of baking oven and is dried, It is cooled to room temperature after drying spare;
S3: taking dry 100 parts of XSBAC powder after cooling, 15 parts of polyvinyl alcohol and 15 parts of sodium alginate by mass fraction, Then be blended in the container for filling 500 parts of distilled water, by container be placed in ultrasonic dispersing machine carry out ultrasonic wave dispersion 10~ After 20min, uniform suspension is obtained;During this, sodium alginate and polyvinyl alcohol are dissolved in formation sodium alginate-polyethylene after water Alcohol colloidal solution, sodium alginate-polyvinyl alcohol are space net structure;XSBAC powder after ultrasonic wave disperses is suspended in glue In shape solution;
S4: suspension is placed in 80 DEG C of water-bath and is heated, constantly stirred with glass bar in heating process, work as appearance When dope, 500 parts of 10%CaCl is added dropwise into container2Solution keeps the temperature 60~120min, then is cooled into after completion of dropwise addition Spherical hydrogel;CaCl during this2As crosslinking agent, effect is exactly to generate chemical bond between the molecule of line style, makes line Type molecule is connected with each other, make suspension formed granular sodium alginate-polyvinyl alcohol-active carbon have reticular structure Small spherical particles are finally dried hydrogel, obtain shinyleaf yellowhorn shell active carbon based aquagel (hereinafter abbreviated as " XSBACH ").
The present invention prepares active carbon using shinyleaf yellowhorn shell, reduces resource waste, XSBAC have very big specific surface area and Aperture;Then it forms space net structure using polyethylene glycol and sodium alginate to coat active carbon, forming surface has The spheric active carbon based aquagel of oxygen-containing functional group can carry out selective absorption to the dye substance in water;It increases simultaneously The partial size of grain, has evaded the problem of be easy to causeing adsorbent to be lost when directlying adopt active carbon particle.
Embodiment 2:
S1: crushing after shinyleaf yellowhorn shell is dried, and smashed shinyleaf yellowhorn shell powder is risen in the case where completely cutting off air conditions Temperature charing, the control of carbonization process temperature are as follows: by room temperature to 120 DEG C, keep the temperature 30min;Then temperature is risen to 200 DEG C, And keep the temperature 60min;600 DEG C are finally warming up to, 120min is kept the temperature, controlling heating rate in the process is 10 DEG C/min, is obtained XSBAC;Gradient increased temperature is used in carbonization process, can reduce the temperature stress that reticular structure active carbon generates in temperature-rise period, Charcoal framework collapse is prevented, to guarantee its pore structure abundant.
S2: taking out the XSBAC distilled water repeated flushing prepared, be then filtered, and then will obtain after filtering XSBAC is placed in 100 DEG C of baking oven and is dried, and is cooled to room temperature after drying spare;
S3: taking dry 100 parts of XSBAC powder after cooling, 15 parts of polyvinyl alcohol and 15 parts of sodium alginate by mass fraction, Then be blended in the container for filling 500 parts of distilled water, by container be placed in ultrasonic dispersing machine carry out ultrasonic wave dispersion 10~ After 20min, uniform suspension is obtained;
S4: suspension is placed in 80 DEG C of water-bath and is heated, constantly stirred with glass bar in heating process, work as appearance When dope, 500 parts of 10%CaCl is added dropwise into container2Solution, rate of addition are 3~5 parts/min, to guarantee into ball particle Uniformly, 60~120min is kept the temperature after completion of dropwise addition, then is cooled into spherical hydrogel, after hydrogel is dried, obtain XSBACH。
Using 27 type infrared spectrometer of TENSOR respectively to the shiny-leaved yellowhorn active carbon XSBAC and shiny-leaved yellowhorn in the present embodiment The functional group of active carbon hydrogel XSBACH is characterized, as a result as shown in Figure 2.From Figure 2 it can be seen that XSBACH is in 3330cm-1, 3058cm-1、1554cm-1、1337cm-1、528cm-1Apparent absorption peak at 5 is shared, is-OH, C-H, C=O, C-O-C respectively On stretching motion and phenyl ring caused by C-H deformation vibration, and XSBAC is in 528cm-1But without apparent absorption peak.Explanation XSBACH produces new absorption peak here.The absorption peak of-OH stretching vibration is by the 3388cm on XSBAC-1It is moved to 3330cm-1.The symmetrical stretching vibration peak of C=O by XSBAC 1604cm-1It is moved to 1554cm-1, the group absorptions peak of XSBACH Comparison XSBAC has apparent enhancing;In 500cm-1-600cm-1Between, XSBACH is generated newly continuously herein Absorption peak, reason be exactly C-H bending motion and aromatic ring CH deformation vibration caused by, and XSBAC is not so much.Explanation The number and type ratio XSBAC's of the functional group of XSBACH is more, and the adsorption effect of XSBACH will be more preferable.
Using Mai Qike Baeyer miniII type physical adsorption appearance to shiny-leaved yellowhorn active carbon XSBAC and shiny-leaved yellowhorn active carbon water-setting The specific surface area of glue XSBACH and aperture are analyzed, as a result as shown in Figure 3,4.Use N2As adsorbing medium -196.15 Nitrogen absorption measurement is carried out at DEG C.Specific surface area and hole the volume product of XSBACH is respectively 52.41m2/g-1And 0.04m3/g-1。 XSBAC specific surface area and hole volume product are respectively 12.42m2/g-1And 0.005m3/g-1.The average pore size of XSBAC and XSBACH is equal About 9.64nm.And XSBACH central hole structure is more flourishing, and possesses stable skeleton structure, specific surface area is bigger, and adsorbance is more By force.Therefore, XSBACH can effectively adsorb the dye substance in water.
Embodiment 3
It takes in aqueous solution of the shinyleaf yellowhorn shell active carbon based aquagel adsorbent material investment containing dye substance obtained, adjusts PH value of solution is 3~5, and 1~3h is reacted at 10 DEG C~60 DEG C;After adsorption reaction, it is separated by filtration shinyleaf yellowhorn shell active carbon base Hydrogel takes filtrate to measure its adsorbance with ultraviolet specrophotometer.
Shinyleaf yellowhorn shell active carbon based aquagel adsorbent material 0.02g obtained in the present embodiment Example 2, investment alkalinity Pinkish red concentration is in the aqueous solution of 700mg/L, and adjusting pH value of solution is 4, reacts 3h at 60 DEG C;After adsorption reaction, with from Scheming separates 5 minutes, is moved to a small amount of supernatant liquor in conical flask with pipette, after 100 times of dilution, uses uv-spectrophotometric Meter measures its adsorbance.As a result are as follows: XSBACH is up to 285.6mg/g to the adsorbance of basic fuchsin.
It as above is the embodiment of the present invention.Design parameter in above-described embodiment and embodiment is merely to understand table Invention verification process is stated, the scope of patent protection being not intended to limit the invention, scope of patent protection of the invention is still with it It is all to change with equivalent structure made by specification and accompanying drawing content of the invention subject to claims, it should all similarly wrap Containing within the scope of the present invention.

Claims (5)

1. a kind of preparation method of shinyleaf yellowhorn shell active carbon based aquagel, which comprises the steps of:
S1: crushing after shinyleaf yellowhorn shell is dried, and smashed shinyleaf yellowhorn shell powder is heated up charcoal in the case where completely cutting off air conditions Change, obtains shinyleaf yellowhorn shell active carbon;
S2: taking out the shinyleaf yellowhorn shell active carbon distilled water repeated flushing prepared, be then filtered, and then will obtain after filtering To shinyleaf yellowhorn shell active carbon be placed on 100 DEG C baking oven in be dried, be cooled to room temperature after drying spare;
S3: dry 100 parts of shinyleaf yellowhorn shell active carbon powder, 15 parts of polyvinyl alcohol and sodium alginate after cooling are taken by mass fraction It 15 parts, is then blended in the container for filling 500 parts of distilled water, container is placed on progress ultrasonic wave dispersion in ultrasonic dispersing machine After 10~20min, uniform suspension is obtained;
S4: suspension being placed in 80 DEG C of water-bath and heated, constantly stirred with glass bar in heating process, sticky when occurring When object, 500 parts of 10%CaCl is added dropwise into container2Solution keeps the temperature 60~120min, then is cooled into spherical after completion of dropwise addition Hydrogel is finally dried hydrogel, obtains shinyleaf yellowhorn shell active carbon based aquagel.
2. the preparation method of shinyleaf yellowhorn shell active carbon based aquagel according to claim 1, which is characterized in that in step S1 Carbonization process temperature control are as follows: by room temperature to 120 DEG C, keep the temperature 30min;Then temperature is risen to 200 DEG C, and kept the temperature 60min;600 DEG C are finally warming up to, 120min is kept the temperature.
3. the preparation method of shinyleaf yellowhorn shell active carbon based aquagel according to claim 2, it is characterised in that: carbonization process Middle heating rate is 10 DEG C/min.
4. the preparation method of shinyleaf yellowhorn shell active carbon based aquagel according to claim 1, it is characterised in that: in step S4 CaCl2The rate of addition of solution is 3~5 parts/min..
5. a kind of application based on shinyleaf yellowhorn shell active carbon based aquagel described in Claims 1 to 4 any one, feature exist In, comprising the following steps: it takes in liquid of the shinyleaf yellowhorn shell active carbon based aquagel adsorbent material investment containing dye substance, adjusts PH value of solution is 3~5, and 1~3h is reacted at 10 DEG C~60 DEG C;After adsorption reaction, it is separated by filtration shinyleaf yellowhorn shell active carbon base Hydrogel.
CN201910525536.8A 2019-06-18 2019-06-18 A kind of preparation method and applications of shinyleaf yellowhorn shell active carbon based aquagel Pending CN110227421A (en)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN115073866A (en) * 2022-06-15 2022-09-20 郭逸晨 Biochar-embedded composite hydrogel capable of adsorbing active dye and preparation method thereof

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