CN107456951A - A kind of rice straw adsorbent of modification and its preparation method and application - Google Patents
A kind of rice straw adsorbent of modification and its preparation method and application Download PDFInfo
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- CN107456951A CN107456951A CN201710743317.8A CN201710743317A CN107456951A CN 107456951 A CN107456951 A CN 107456951A CN 201710743317 A CN201710743317 A CN 201710743317A CN 107456951 A CN107456951 A CN 107456951A
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- rice straw
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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
-
- 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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
-
- 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
-
- 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
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses rice straw adsorbent of a kind of modification and its preparation method and application, adsorbent is the rice straw by amino modified；Preparation method is as follows：（1）Crush or grind after rice straw is gone into the removal of impurity, cleaning, drying first, sieving；（2）Weigh step（1）The middle rice straw through processing, epoxychloropropane and dimethylformamide are added, 1 2h is stirred under the conditions of 90 100 DEG C, it is fully reacted；Diethylenetriamines is then added, continues to stir 1 2h；Finally, triethylamine is added, keeping temperature continues to react 2 3h；Resulting materials are separated by filtration, and rinsed well with water；（3）By step（2）In rinse well material drying, produce.Modified adsorbent raw material is rice straw in the present invention, and its is cheap, and it is convenient to obtain；For adsorbent by the chromium and nickel in physical method Adsorption water, adsorption efficiency is high, and non-secondary pollution thing generates during whole Adsorption, and the harmful material of the person is not produced.
Description
Technical field
The invention belongs to water-treatment technology field, rice straw adsorbent of more particularly to a kind of modification and preparation method thereof
And application.
Background technology
With the fast development of industrial production and human society, problem of environmental pollution increasingly aggravates.Countless polluters
It is discharged into water environment, wherein heavy metal pollutants have hypertoxicity or carcinogenicity, and are difficult to biodegradation.This
Outside, heavy metal is easily enriched with and and then accumulated by food chain in organism or human body in vivo.
Chromium and nickel ion are widely used in leather, plating, cement manufacture, dye industry etc..In view of the harmfulness of chromium and nickel
With its extensive use in various industrial productions, manufacturing process, effective removal chromium and nickel have important from industrial wastewater
Meaning.Removing the conventional processing method of chromium and nickel in water body mainly has two classes, and one kind is traditional treatment method, including chemistry
(reduction) precipitation method, electrochemical process, membrane filter method, ion-exchange etc.；One kind is absorption method.Traditional treatment method treatment effeciency
Low, investment and processing cost are higher, and operate inconvenience.And compared with numerous traditional treatment methods, absorption method generally utilizes absorption
Harmful substance in sewage is fixed on its surface so as to be removed by the porous of material, while has Non-energy-consumption, without secondary
The advantages that polluting, be easily operated.It is of crucial importance thus to seek the adsorbent that cost is cheap and adsorption efficiency is high.
Being had been reported that the raw material of industry such as recent years, activated carbon, graphene and the adsorbent of their material modified preparation more,
Heavy metal also has certain suction-operated to the industrial wastes such as flyash, scrap rubber after treatment, and China is that agricultural production is big
Whether state, the researcher of agriculture field also can prepare advantages of good adsorption effect, easily operated in thinking using agriculture waste material
Adsorbent.Application number CN2012105884866 Chinese patent application discloses a kind of oleic acid modified peanut adsorbent, will
Peanut shell is modified using oleic acid, n-hexane and sulfuric acid after peanut shell pretreatment, produces modified peanut shell adsorbent.The application
The main hydroxyl using in the carboxyl and peanut shell in carboxylic acid carries out esterification, the carboxyl that esterification product ionizes out in water
Can heavy metal ion form suction-operated, but the adsorption effect of this application heavy metal lead is more preferable, and the processing to chromium and nickel is simultaneously
Do not refer to.
The content of the invention
For the deficiency of existing issue, it is an object of the invention to provide a kind of rice straw adsorbent of modification and its preparation
Methods and applications, raw material are easy to get, and preparation technology is simple, and gained adsorbent has good adsorption effect, for the dirt in waste water
Dye heavy metal has good absorption, removes effect, can be used for solving prior art to chromium in waste water and nickel contamination thing difficulty
The problem of reason.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of rice straw adsorbent of modification, first pre-processes rice straw through pulverization, then by pretreated straw
Stalk carries out amino modified reaction at high temperature with modifying agent, cleaning, drying, produces.
A kind of preparation method of the rice straw adsorbent of modification, comprises the following steps：
(1) pretreatment of rice straw：Crush or grind, mistake after rice straw is gone into the removal of impurity, cleaning, drying first
Sieve；
(2) modification of rice straw：Treated rice straw in step (1) is weighed, modifying agent is added and carries out high temperature
Modified, the addition sequence of modifying agent is：Epoxychloropropane and dimethylformamide are first added, 1- is stirred under the conditions of 90-100 DEG C
2h, it is set fully to react；Diethylenetriamines is then added, insulation continues to stir 1-2h；Finally, triethylamine, phase equality of temperature are added
2-3h is stirred under the conditions of degree；Resulting materials are separated by filtration, and rinsed well with water；
(3) material rinsed well in step (2) is dried, produced.
As a kind of optimal technical scheme of the application, in the step (1), after rice straw distilled water flushing, put
20-24h is dried in 80-100 DEG C of baking oven, 40-200 mesh sieves are crossed after the straw crushing, grinding after drying.
As a kind of optimal technical scheme of the application, in the step (2), the quality 9-10g of rice straw is often weighed
When add modifying agent 31-36mL, wherein, the volume ratio of epoxychloropropane and dimethylformamide, diethylenetriamines, triethylamine is
3~3.6：2.5~3：1~1.2：2.5~3；Rinse water is deionized water or distilled water.
As a kind of optimal technical scheme of the application, magnetic stirrer is used in the step (2).
As a kind of optimal technical scheme of the application, in the step (3), drying temperature is 80-100 DEG C, during drying
Between be 20-24h.
The present invention also provides a kind of rice straw adsorbent of the modification prepared using the above method weight in waste water is adsorbed
The application of metal.
Rice straw is made up of cellulose, hemicellulose and lignin etc., can effectively adsorb heavy metal in the solution, profit
By the use of discarded Agricultural Materials as adsorbent, discarded resource can not only be made full use of, and absorption effect can be improved by modified
Fruit is as the high-efficiency adsorbent application in water process；Amine is easy to protonate in sour environment, by electrostatic attraction and from
Sub- exchange adsorption metal ion improves adsorption efficiency.Based on above-mentioned good characteristic, rice straw can be used for the absorption of chromium and nickel,
Rice straw after amino modified has more excellent absorption property.
Compared with prior art, the invention has the advantages that：
(1) the Agricultural Materials rice straw in the present invention as raw material, its is cheap, and it is convenient to obtain；
(2) material modified no danger, nonstaining property, sorbent preparation method are simple to operation；
(3) final product is whole to the adsorption efficiency of chromium and nickel height by the chromium and nickel in physical method Adsorption water
The generation of non-secondary pollution thing during individual Adsorption, the harmful material of the person is not produced；
(4) present invention makes full use of material, makes the best use of everything, and reaches the purpose of energy-conserving and environment-protective.
Embodiment
The present invention is described in further details with reference to embodiments.Agents useful for same or the unreceipted production of instrument and equipment
Manufacturer, it is accordingly to be regarded as the conventional products that can be bought by market.
Embodiment 1
A kind of preparation method of the rice straw adsorbent of modification, comprises the following steps：
(1) pretreatment of rice straw：The rice straw distilled water flushing that will be collected into first, then as 80 DEG C of bakings
24h is dried in case.100 mesh sieves will be crossed after the straw crushing of drying, grinding again；
(2) modification of rice straw：Taking in 10g steps 1 has rice straw to be modified to be placed in round-bottomed flask, and adds
10.8mL epoxychloropropane and 9mL dimethylformamides, then flask is placed under the conditions of 100 DEG C and stirs 1h, make it fully anti-
Should.3.6mL diethylenetriamines is then added in flask, continues to stir 2h under the conditions of 95 DEG C；Finally, added in flask
9mL triethylamines, 3h is stirred under the conditions of 90 DEG C.Then, resulting materials are separated by filtration, and cleaned with deionized water；
(3) step 2 resulting materials are placed in 100 DEG C of baking ovens and dry 20h, produced.
Dusty material prepared by the above method is modified rice straw adsorbent, and the adsorbent is placed in drier
Store for future use.
Embodiment 2
A kind of preparation method of the rice straw adsorbent of modification, comprises the following steps：
(1) pretreatment of rice straw：The rice straw distilled water flushing that will be collected into first, then as 80 DEG C of bakings
24h is dried in case.40 mesh sieves will be crossed after the straw crushing of drying, grinding again；
(2) modification of rice straw：Taking in 9g steps 1 has rice straw to be modified to be placed in round-bottomed flask, and adds
12mL epoxychloropropane and 10mL dimethylformamides, then flask is placed under the conditions of 90 DEG C and stirs 2h, it is fully reacted.
4mL diethylenetriamines is then added in flask, continues to stir 1h under the conditions of 100 DEG C；Finally, 10mL tri- is added in flask
Ethamine, 2h is stirred under the conditions of 100 DEG C.Then, resulting materials are separated by filtration, and cleaned with deionized water；
(3) step 2 resulting materials are placed in 80 DEG C of baking ovens and dry 24h, produced.
Dusty material prepared by the above method is modified rice straw adsorbent, and the adsorbent is placed in drier
Store for future use.
Embodiment 3
A kind of preparation method of the rice straw adsorbent of modification, comprises the following steps：
(1) pretreatment of rice straw：The rice straw distilled water flushing that will be collected into first, then as 100 DEG C
24h is dried in baking oven.200 mesh sieves will be crossed after the straw crushing of drying, grinding again；
(2) modification of rice straw：Taking in 9.1g steps 1 has rice straw to be modified to be placed in round-bottomed flask, and adds
Enter 10mL epoxychloropropane and 8.8mL dimethylformamides, then flask is placed under the conditions of 95 DEG C and stirs 1.4h, makes its abundant
Reaction.3.3mL diethylenetriamines is then added in flask, continues to stir 1.6h under the conditions of 90 DEG C；Finally, add in flask
Enter 9mL triethylamines, 2.5h is stirred under the conditions of 95 DEG C.Then, resulting materials are separated by filtration, and cleaned with deionized water；
(3) step 2 resulting materials are placed in 95 DEG C of baking ovens and dry 22h, produced.
Dusty material prepared by the above method is modified rice straw adsorbent, and the adsorbent is placed in drier
Store for future use.
Using the rice straw (MRS) of the modification obtained in embodiment 1-3 and unmodified rice straw (RS) as absorption
Contrast test is done in agent, verifies both the above adsorbent effect of Adsorption of Chromium and nickel in water.Specially：
The different chromium of concentration (VI), nickel (II) solution, absorption effect of the test adsorbent to chromium (VI), nickel (II) is respectively configured
Should.It is 0.2g, 0.3g and 0.4g to take adsorbent mass respectively；Chromium (VI) solution concentration is 20mg/L, 40mg/L and 60mg/L；Nickel
(II) solution concentration is 20mg/L, 40mg/L and 60mg/L.Chromium (VI) solution and nickel (II) liquor capacity are 50mL.
In the case where other conditions keep constant, different quality adsorbent is to various concentrations in test example and comparative example
Chromium (VI) solution, nickel (II) corresponding absorption property, respectively as shown in table 1 below, table 2.
Table 1 rice straw adsorbent chromium (VI) treatment effect
Table 2 rice straw adsorbent nickel (II) treatment effect
With reference to Tables 1 and 2, rice straw is to chromium adsorpting data related to nickel after contrast before modified, it can be seen that modified
Its absorption property of rice straw afterwards has obtained largely being lifted, and adsorption efficiency also greatly increases.
As shown in above-mentioned table, chromium (VI) and nickel (II) initial concentration are higher, and the adsorbance of corresponding adsorbent is more；So
And the dosage of adsorbent is nonlinear for the adsorption effect of adsorbate, after reaching certain dosage, even if increase adsorbent is used
Amount, adsorption effect also increases limited.
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (7)
1. the rice straw adsorbent of a kind of modification, it is characterised in that first rice straw is pre-processed through pulverization, then will be located in advance
Stalk after reason carries out amino modified reaction at high temperature with modifying agent, cleaning, drying, produces.
2. the preparation method of the rice straw adsorbent of the modification described in claim 1, it is characterised in that comprise the following steps：
（1）The pretreatment of rice straw：Crush or grind after rice straw is gone into the removal of impurity, cleaning, drying first, sieving；
（2）The modification of rice straw：Weigh step（1）In treated rice straw, add modifying agent carry out it is high temperature modified,
The addition sequence of modifying agent is：Epoxychloropropane and dimethylformamide are first added, 1-2h is stirred under the conditions of 90-100 DEG C, makes it
Fully reaction；Diethylenetriamines is then added, insulation continues to stir 1-2h；Finally, triethylamine is added, under identical temperature conditionss
Stir 2-3h；Resulting materials are separated by filtration, and rinsed well with water；
（3）By step（2）In rinse well material drying, produce.
3. the preparation method of the rice straw adsorbent of modification according to claim 2, it is characterised in that the step
（1）In, after rice straw distilled water flushing, it is placed in 80-100 DEG C of baking oven and dries 20-24h, straw crushing after drying, grinds
40-200 mesh sieves are crossed after mill.
4. the preparation method of the rice straw adsorbent of modification according to claim 2, it is characterised in that the step
（2）In, modifying agent 31-36mL is added when often weighing the quality 9-10g of rice straw, wherein, epoxychloropropane and dimethyl acyl
Amine, diethylenetriamines, the volume ratio of triethylamine are 3 ~ 3.6：2.5~3：1~1.2：2.5~3；Rinse water be deionized water or
Distilled water.
5. the preparation method of the rice straw adsorbent of modification according to claim 2, it is characterised in that the step
（2）It is middle to use magnetic stirrer.
6. the preparation method of the rice straw adsorbent of modification according to claim 2, it is characterised in that the step
（3）In, drying temperature is 80-100 DEG C, drying time 20-24h.
7. the rice straw adsorbent of the modification described in claim 1 is in the application of absorption heavy metal in waste water.
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Cited By (3)
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| CN109174067A (en) * | 2018-11-06 | 2019-01-11 | 齐鲁工业大学 | A method of hexavalent chromium adsorbent is prepared by raw material of Alocasia ordora |
| CN109513425A (en) * | 2018-09-25 | 2019-03-26 | 山东大学 | A kind of peanut shell graphene composite aerogel oil absorption material and preparation method thereof |
| CN112023889A (en) * | 2020-08-28 | 2020-12-04 | 西安工程大学 | Method for microwave-assisted in-situ one-step modification of activated carbon by oleic acid |
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| CN109513425A (en) * | 2018-09-25 | 2019-03-26 | 山东大学 | A kind of peanut shell graphene composite aerogel oil absorption material and preparation method thereof |
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| CN112023889A (en) * | 2020-08-28 | 2020-12-04 | 西安工程大学 | Method for microwave-assisted in-situ one-step modification of activated carbon by oleic acid |
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Application publication date: 20171212 |