CN107349910A - A kind of preparation method and applications of Pyromellitic Acid anhydride modification mao bamboon adsorbent - Google Patents
A kind of preparation method and applications of Pyromellitic Acid anhydride modification mao bamboon adsorbent Download PDFInfo
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- CN107349910A CN107349910A CN201710614224.5A CN201710614224A CN107349910A CN 107349910 A CN107349910 A CN 107349910A CN 201710614224 A CN201710614224 A CN 201710614224A CN 107349910 A CN107349910 A CN 107349910A
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- mao bamboon
- adsorbent
- acid anhydride
- pyromellitic acid
- fiber dust
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of preparation method and applications of Pyromellitic Acid anhydride modification mao bamboon adsorbent.Mao bamboon is pre-processed to obtain pretreated mao bamboon fiber dust, pretreated mao bamboon fiber dust is subjected to double alkalisation with the NaOH solution that concentration is 2 ~ 6mol/L, double alkalisation mao bamboon fiber dust is made；Raw material is weighed according to following mass percent concentration：DMF is 76 ~ 96%, pyromellitic dianhydride is 2 ~ 5%, and double alkalisation mao bamboon fiber dust is 2 ~ 18%, and three's sum is 100%, pyromellitic dianhydride is added in DMF, until completely dissolved, double alkalisation mao bamboon fiber dust is added, after stirring reaction, filter, washing is repeatedly to neutrality, and most after drying 1 h in 85 DEG C of baking oven, it is Pyromellitic Acid anhydride modification mao bamboon adsorbent to obtain powdered product.The Pyromellitic Acid anhydride modification mao bamboon adsorbent of the present invention is applied to the lead ion in adsorbing separation water, and adsorption capacity is high, and cost is cheap, and technique is simple, for solving environmental pollution, promoting refuse reclamation significant.
Description
Technical field
The invention belongs to changing waste into resources utilization and water-treatment technology field, more particularly to a kind of Pyromellitic Acid anhydride modification
The preparation method and applications of mao bamboon adsorbent.
Background technology
In recent years, developing rapidly with industry, heavy metal pollution of water body getting worse, it has also become generally close the world today
One of environmental problem of note.Lead is a kind of common and poisonous heavy metal contaminants, from various industrial activities such as metal electricity
The discharge of industrial wastewater caused by plating, oil refining and battery manufacture etc..Lead ion can be by sucking, taking in or skin is absorbed into
Human body, be mainly collected in human skeleton, brain, kidney and muscle, cause serious anaemia, kidney trouble, sacred disease and
Vomiting is even dead.Therefore, the side for being adapted to remove industrial wastewater ion is found to harm caused by the mankind for lead ion
Method, can qualified discharge, to protection human health and ecological environment have great importance.
Biosorption process is a kind of cost-effective heavy-metal ion removal biosorption technology of new cost.Biology is inhaled
Attached dose of abundance, kind is more and cost is relatively low, and used adsorption plant is simple during absorption, operation side
Just, and with adsorption rate is fast, adsorbance is big, good selective, particularly 1~100 mg/L heavy metal wastewater therebies are being handled
When adsorption effect it is fine, the biological adsorption agent after desorption is reusable.Therefore, natural reproducible resource, development environment are utilized
Friendly product and technology are by as the inexorable trend of sustainable development.Mao bamboon contains substantial amounts of cellulose, hemicellulose and wood
The fibers such as quality, fiber therein are in bundle-shaped, laterally there is section line, and there is lumen cross section, and surface is fluted, and this is probably mao bamboon
The main reason for adsorption capacity, the modified structural void for causing mao bamboon increase, and specific surface area increase, have cellulose base day
The exclusive advantage of right high polymer material.Main component cellulose in mao bamboon can handle the heavy metal ion in waste water, and
Guangxi bamboo resource enriches, and the more such as throwaway chopsticks of discarded mao bamboon product, it is i.e. variable useless to be prepared into biological adsorption agent
For treasured, the secondary pollution to environment is turn avoid, there is wide exploit potentialities.
Mao bamboon can be enriched with more heavy metal ion by being modified after introducing active function groups on its surface.Prepare
The advantages that modified mao bamboon fiber adsorbing substance absorption property stabilization, advantages of good adsorption effect, high adsorption capacity, for largely discarded mao bamboon money
Source have found the theoretical foundation to turn waste into wealth.
Pyromellitic dianhydride structure is special, and chemism is very high, and the suction of heavy metal ion can be controlled by the value of system
Echo selection.This patent carries out chemical modification using mao bamboon as raw material, using pyromellitic dianhydride, and introducing carboxyl on mao bamboon surface lives
Property functional group, make its strengthen heavy metal ion adsorption capacity.
The content of the invention
, should it is an object of the invention to provide a kind of preparation method and applications of Pyromellitic Acid anhydride modification mao bamboon adsorbent
Pyromellitic Acid anhydride modification mao bamboon adsorbent is bigger to the adsorption capacity of heavy metal ion in water.
Prepare concretely comprising the following steps for Pyromellitic Acid anhydride modification mao bamboon adsorbent：
(1) mao bamboon is sawn into block, cleaning, crushed after being dried in 80 DEG C, and cross 60 mesh sieves, the mao bamboon powder that then will be obtained
End is totally submerged in n-hexane solvent, reacts 4 h under conditions of 55 DEG C and 150 rpm, be washed with deionized water it is net, in 55 ~
4 ~ 8 h are dried under the conditions of 65 DEG C, obtain pretreated mao bamboon fiber dust.
(2) the pretreated mao bamboon fiber dust that step (1) obtains is mixed with concentration for 2 ~ 6mol/L NaOH solution
Close, it is desirable to which the mass ratio of pretreated mao bamboon fiber dust and NaOH that step (1) obtains is 2 ~ 6:1, then in 25 ~ 35 DEG C
And 150 react 24 h under conditions of rpm, then clean 4 ~ 6 times with deionized water, ethanol, acetone successively, by products therefrom again
Mixed with the NaOH solution that concentration is 2 ~ 6mol/L, it is desirable to which products therefrom and NaOH mass ratio are 2 ~ 6:1, then in 25 ~ 35
DEG C and 150 rpm under conditions of react 24 h, then cleaned 4 ~ 6 times with deionized water, ethanol, acetone successively, double alkalisation be made
Mao bamboon fiber dust.
(3) raw material is weighed according to following mass percent concentration：DMF is 76 ~ 96%, and pyromellitic dianhydride is 2 ~ 5%, step
(2) double alkalisation mao bamboon fiber dust made from is 2 ~ 18%, and three's sum is 100%.
(4) pyromellitic dianhydride that step (3) weighs is added in DMF, until completely dissolved, adds step (3) and claim
The double alkalisation mao bamboon fiber dust taken, 4 ~ 20h is then reacted under conditions of 70 ± 5 DEG C and 120 ~ 150 rpm, after suction filtration,
Successively with DMF, deionized water, saturation NaHCO3Solution, ethanol, acetone washing are repeatedly to neutrality, most after in 85 DEG C of baking oven
1 h is dried, it is Pyromellitic Acid anhydride modification mao bamboon adsorbent to obtain powdered product.
The Pyromellitic Acid anhydride modification mao bamboon adsorbent of the present invention is applied to the lead ion in adsorbing separation water.
The advantage of the invention is that：The adsorption capacity of the Pyromellitic Acid anhydride modification mao bamboon adsorbent of the present invention is high, absorption
After the completion of process, directly it is filtered to remove, renewable Reusability, stable mechanical performance, cost is cheap, and technique is simple, the present invention
Used mao bamboon is a kind of adsorbent of natural green, for solving environmental pollution, promoting from discarded disposable bamboo chopsticks
It is significant to enter refuse reclamation.
Brief description of the drawings
Fig. 1 is the dosage of the Pyromellitic Acid anhydride modification mao bamboon adsorbent prepared in the embodiment of the present invention in the aqueous solution
The influence variation diagram of Pb (II) ionic adsorption effect.
Fig. 2 is the Pyromellitic Acid anhydride modification mao bamboon adsorbent prepared in the embodiment of the present invention to water under different pH condition
Pb (II) Adsorption Effect variation diagram in solution.
Embodiment
Embodiment：
The preparation of Pyromellitic Acid anhydride modification mao bamboon adsorbent：
Mao bamboon is sawn into block, cleaning, crushed after being dried in 80 DEG C, and crosses 60 mesh sieves, obtains mao bamboon powder.In reactor
In, add 10.0 g mao bamboons powder and 60 ml n-hexanes, mao bamboon powder is totally submerged in n-hexane solvent, in 55 DEG C and
4 h are reacted under conditions of 150 rpm, is then washed with deionized water only, is dried 6h under the conditions of 55 DEG C, obtain pretreated
Mao bamboon fiber dust.
In the reactor, above-mentioned pretreated mao bamboon fiber dust is added into the NaOH that 250 ml concentration are 4 mol/L
In solution, it is desirable to which the mass ratio of pretreated the mao bamboon fiber dust and NaOH of addition is 4:1, then in 25 DEG C and 150
24 h are reacted under conditions of rpm, then are washed 5 times with deionized water, ethanol, acetone successively, products therefrom is added 250 again
Ml concentration be 4 mol/L NaOH solution in, then react 24 h under conditions of 25 DEG C and 150 rpm, then spend successively from
Sub- water, ethanol, acetone wash 5 times, and double alkalisation mao bamboon fiber dust is made.
In the reactor, it is 1 in mass ratio by 5.0 g pyromellitic dianhydrides and 250 ml DMF:47 mixing, treat completely molten
Xie Hou, 5.0 g double alkalisation mao bamboon fiber dusts obtained above are added, react 20 h in 75 DEG C and 150 rpm, filter
Afterwards, products therefrom is washed repeatedly to neutrality with DMF, deionized water, saturated sodium bicarbonate solution, ethanol, acetone successively, and in
1 h is dried in 85 DEG C of baking oven, it is Pyromellitic Acid anhydride modification mao bamboon adsorbent to obtain powdered product, and pack is standby.
Pyromellitic Acid anhydride modification mao bamboon adsorbent made from the present embodiment is applied to lead ion adsorption experiment, specific mistake
Journey is as follows：
Application example 1：Weigh Pyromellitic Acid anhydride modification mao bamboon made from 50,75,100,125,150,200 mg the present embodiment
It is that 100 mg/L contain in Pb (II) solion that adsorbent, which is respectively placed in the 50mL concentration that adjusted good pH is 5.0,（0.1mol/L
HNO3Or NaOH regulations pH）, at 25 DEG C, rotating speed be 150 rpm shake the h of bed reaction 4 after, with 0.45 μm of membrane filtration,
With icp mses measure Pb (II) concentration.As a result it is as shown in Figure 1.
Application example 2：Pyromellitic Acid anhydride modification mao bamboon adsorbent made from 50 mg the present embodiment is weighed to be respectively placed in
It is that 100 mg/L contain in Pb (II) solion to regulate the 50 mL concentration that pH is 2.0,3.0,4.0,5.0 and 6.0（0.1mol/
L HNO3Or NaOH regulations pH）, at 25 DEG C, rotating speed be 150 rpm shake the h of bed reaction 4 after, with 0.45 μm of filter membrane mistake
Filter, Pb (II) concentration is determined with icp mses.As a result it is as shown in Figure 2.
Claims (2)
1. a kind of preparation method of Pyromellitic Acid anhydride modification mao bamboon adsorbent, it is characterised in that concretely comprise the following steps：
(1) mao bamboon is sawn into block, cleaning, crushed after being dried in 80 DEG C, and cross 60 mesh sieves, the mao bamboon powder that then will be obtained
End is totally submerged in n-hexane solvent, reacts 4 h under conditions of 55 DEG C and 150 rpm, be washed with deionized water it is net, in 55 ~
4 ~ 8 h are dried under the conditions of 65 DEG C, obtain pretreated mao bamboon fiber dust；
(2) the pretreated mao bamboon fiber dust that step (1) obtains is mixed with the NaOH solution that concentration is 2 ~ 6mol/L,
The mass ratio for seeking pretreated the mao bamboon fiber dust and NaOH that step (1) obtains is 2 ~ 6:1, then in 25 ~ 35 DEG C and 150
24 h are reacted under conditions of rpm, then are cleaned 4 ~ 6 times with deionized water, ethanol, acetone successively, by products therefrom again with concentration
Mixed for 2 ~ 6mol/L NaOH solution, it is desirable to which products therefrom and NaOH mass ratio are 2 ~ 6:1, then in 25 ~ 35 DEG C and 150
24 h are reacted under conditions of rpm, then are cleaned 4 ~ 6 times with deionized water, ethanol, acetone successively, double alkalisation mao bamboon fiber is made
Powder；
(3) raw material is weighed according to following mass percent concentration：DMF is 76 ~ 96%, and pyromellitic dianhydride is 2 ~ 5%, step (2)
Obtained double alkalisation mao bamboon fiber dust is 2 ~ 18%, and three's sum is 100%；
(4) pyromellitic dianhydride that step (3) weighs is added in DMF, until completely dissolved, adds what step (3) weighed
Double alkalisation mao bamboon fiber dust, 4 ~ 20h is then reacted under conditions of 70 ± 5 DEG C and 120 ~ 150 rpm, after suction filtration, successively
With DMF, deionized water, saturation NaHCO3Solution, ethanol, acetone washing are repeatedly to neutrality, most after in 85 DEG C of baking oven dry 1
H, it is Pyromellitic Acid anhydride modification mao bamboon adsorbent to obtain powdered product.
2. the application of the Pyromellitic Acid anhydride modification mao bamboon adsorbent prepared according to the method for claim 1, its feature exist
It is applied to the lead ion in adsorbing separation water in the Pyromellitic Acid anhydride modification mao bamboon adsorbent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111545177A (en) * | 2020-04-15 | 2020-08-18 | 济南大学 | Preparation method of modified magnetic bamboo fiber composite adsorbent |
| CN115634672A (en) * | 2022-11-03 | 2023-01-24 | 内蒙古农业大学 | Pyromellitic anhydride modified polyvinylamine gel, and preparation method, application and regeneration method thereof |
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| CN103920466A (en) * | 2014-05-05 | 2014-07-16 | 湖南大学 | Preparation method and application of modified ramie fiber adsorbent |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111545177A (en) * | 2020-04-15 | 2020-08-18 | 济南大学 | Preparation method of modified magnetic bamboo fiber composite adsorbent |
| CN115634672A (en) * | 2022-11-03 | 2023-01-24 | 内蒙古农业大学 | Pyromellitic anhydride modified polyvinylamine gel, and preparation method, application and regeneration method thereof |
| CN115634672B (en) * | 2022-11-03 | 2024-01-26 | 内蒙古农业大学 | Pyromellitic anhydride modified polyvinyl amine gel and preparation method, application and regeneration method thereof |
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