CN109289817A - The adsorbent material of 2,4- Embutox, preparation method and applications in a kind of chernozem - Google Patents
The adsorbent material of 2,4- Embutox, preparation method and applications in a kind of chernozem Download PDFInfo
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- CN109289817A CN109289817A CN201811072401.2A CN201811072401A CN109289817A CN 109289817 A CN109289817 A CN 109289817A CN 201811072401 A CN201811072401 A CN 201811072401A CN 109289817 A CN109289817 A CN 109289817A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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Abstract
The invention discloses the adsorbent materials of 2,4- Embutox, preparation method and applications in a kind of chernozem, including calcination after potassium dihydrogen phosphate, polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and the mixing of tetrabutyl phosphorus chloride is obtained；The temperature of the calcination is 120~150 DEG C；The mass ratio of the potassium dihydrogen phosphate, polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and tetrabutyl phosphorus chloride is 7:2:1.The present invention prepares the adsorbent material method rapid and convenient, using special ion liquid, salt and grafting chelating gel when preparation, obtained ionic liquid active adsorbing material has very high targeting and arresting efficiency, and this method is to the permeability of 2,4- Embutox in chernozem up to 99.6%.Wide with the range of linearity, detection limit is low, and relative standard deviation is smaller, has both been able to satisfy detection requirement of the country for 2,4- Embutox in chernozem.
Description
Technical field
The invention belongs to field of environment protection, and in particular to the adsorbent material of 2,4- Embutox, preparation in a kind of chernozem
Method and its application.
Background technique
2,4- Embutox is as a kind of most important herbicide, always in occupation of critical role in entire chemical weed control.Closely
Its sustained production rises within several years, and use scope is also constantly expanding.One of main representative as phenoxy carboxylic acid herbicides, 2,
4- Embutox is easy to migrate in farmland ecosystem, and soil, atmosphere, water source etc. is caused to pollute, it is thus determined that it is detected
Method just seems especially urgent.
2,4- Embutoxs (2,4-DB) are absorbability selectivity medium poison herbicide, are mainly used for preventing and kill off gramineous crop
Broadleaf weed, nutgrass flatsedge and the certain malignant weeds of Tanaka.Sucking, intake have after skin absorbs to eyes, mucous membrane and skin
Skin generates the potential hazards such as stimulation, disturbance endocrine.There are specific residue limits (MRL) requirement in many countries to 2,4-DB.
2,4- Embutox in processing soil generallys use spreads quick lime, spray limewash or brassin class, first in the soil
Shell element substance, but often function and effect are low for above method, it is time-consuming and laborious.
For ionic liquid aqueous two-phase as a kind of novel green separation system occurred in recent years, itself has toxicity
It is small, the properties such as non-combustible, non-volatile, not oxidizable.It has been investigated that ionic liquid is on the one hand to the molten of inorganic and organic materials
Solution has selectivity, on the other hand immiscible with certain organic solvents, this feature may be used on the infiltration of liquid liquid, the micro- infiltration of liquid phase
Thoroughly, the micro- infiltration of solid phase, ionic liquid/supercritical CO2Infiltration etc..Again because it is short with the split-phase time, permeability is high, infiltration
Process is not easy the advantages that emulsifying and receives more and more attention.In addition, the main component of ionic liquid double-aqueous phase system two-phase is all
It is water, makes it have benign environment required for bioactive molecule, there is wide application on permeability and separation biological substance
Prospect.Up to the present, the data information about ionic liquid double-aqueous phase system as osmotic system also more lacks, meanwhile,
It is also not seen reported about ionic liquid infiltration 2,4- Embutox, therefore there is far-reaching influence to the research of the system.
Summary of the invention
It is long for there are times of penetration in existing 2,4- Embutox permeating method, equipment is expensive, complicated for operation, permeability
Low disadvantage, it is an object of the present invention to the adsorbent material of 2,4- Embutox, preparation method and applications in a kind of chernozem,
For separation and Extraction 2,4- Embutox.The material can capture most of, high-purity 2,4- Embutox, shorten 2,4- drop
The disengaging time of butyric acid, at the same have it is easy to operate, do not use large-scale instrument, reduce using traditional volatile organic solvent to keep away
Exempt from the characteristics of bringing secondary pollution.
In order to realize that above-mentioned task, the present invention take following technical solution:
The preparation method of the adsorbent material of 2,4- Embutox in a kind of chernozem, including by potassium dihydrogen phosphate, polyacrylamide
Calcination obtains after amine-diisopropanolamine (DIPA) grafting chelating gel and the mixing of tetrabutyl phosphorus chloride；
The temperature of the calcination is 120~150 DEG C；
The potassium dihydrogen phosphate, polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and the tetrabutyl phosphorus chloride matter
Amount is than being 7:2:1.
Optionally, the time of the calcination is 2h, and powdery granule object is obtained after calcination；
Then powdery granule object is obtained to the adsorbent material of 2,4- Embutox in the chernozem after vacuum dried.
Optionally, the vacuum drying temperature is 20~40 DEG C, and the vacuum drying time is 24~48h.
Optionally, the method is specifically: potassium dihydrogen phosphate and tetrabutyl phosphorus chloride are mixed to get aqueous two-phase extraction
System, then polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel is added in two phase aqueous extraction system and obtains gel mixture,
Calcination obtains powdery granule object to gel mixture under an inert atmosphere；
Then powdery granule object is obtained to the adsorbent material of 2,4- Embutox in the chernozem after vacuum dried.
The adsorbent material of 2,4- Embutox in a kind of chernozem, the adsorbent material use preparation method system of the present invention
It is standby to obtain.
The adsorbent material of 2,4- Embutox is for adsorbing 2,4- Embutox in chernozem in chernozem of the present invention
Using.
Optionally, specifically using 2,4- drop in the adsorbent material absorption chernozem of 2,4- Embutox in chernozem of the invention
The method of butyric acid includes: that specific adsorption method is that 1:3 is mixed by volume by adsorbent material and chernozem, is placed at 27 DEG C
30min。
Compared with prior art, advantages of the present invention are as follows:
Adsorbent material preparation method rapid and convenient of the present invention, it is solidifying using special ion liquid, salt and grafting chelating when preparation
Glue, obtained round block shape active adsorbing material have very high targeting and arresting efficiency, and this method is to 2,4- drop in chernozem
The permeability of butyric acid has the range of linearity wide, detection limit is low, and relative standard deviation is smaller, is both able to satisfy country up to 99.6%
Detection requirement for 2,4- Embutox in chernozem.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph for the adsorbent material that embodiment 1 is prepared；
Fig. 2 is the electromicroscopic photograph for the adsorbent material that embodiment 8 is prepared；
Fig. 3 is the electromicroscopic photograph for the adsorbent material that embodiment 9 is prepared；
The present invention is further explained below in conjunction with the drawings and specific embodiments.
Specific embodiment
The present invention is in preparing chernozem using special ion liquid, salt and grafting chela when the adsorbent material of 2,4- Embutox
Close gel, obtained round block shape active adsorbing material has very high targeting and arresting efficiency, this method in chernozem 2,
The permeability of 4- Embutox has the range of linearity wide, detection limit is low, and relative standard deviation is smaller, biphosphate up to 99.6%
The mass ratio of potassium, polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and tetrabutyl phosphorus chloride is 7:2:1
The KH for being 10% by Cl and 20 part of mass fraction of ionic liquid [TBP] that 60 parts of mass fractions are 24%2PO4Mixing
Uniformly, two phase aqueous extraction system is obtained, adding and accounting for total quality of materials score is that 20 parts of 45%DIPA-PAM-Gel obtain gel
Shape mixture forms above-mentioned gelatinous mixture calcination (calcination temperature be 120~150 DEG C) two hours under nitrogen protection
Then powdery granule is stored at standing 24~48 hours in 20~40 DEG C of vacuum oven, it is living that ionic liquid is made
Property adsorbent material.
Ionic liquid [TBP] Cl: upper marine origin victory Chemical Co., Ltd..
DIPA-PAM-Gel: polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel: DIPA-PAM-Gel, polyacrylamide
Amine-diisopropanolamine (DIPA) grafting chelating gel (DIPA-PAM-Gel), with polyacrylamide gel (PAM-Gel, Gongyi City Henan profit sea
Source water-purifying material Co., Ltd) --- it is skeleton, diisopropanolamine (DIPA) (Shanghai Hao Hua Chemical Co., Ltd.) is grafting chelating agent,
It under formaldehyde participates in, is reacted according to Mannich, chelation group is made and is grafted gel.
In order to realize that the capture rate for improving 2,4- Embutox in chernozem, the present invention devise a series of experiments to obtain
Preferably technological parameter:
Embodiment 1:
The KH2PO4 that Cl and 20 part of mass fraction of ionic liquid [TBP] that 60 parts of mass fractions are 24% is 10% is mixed
Uniformly, two phase aqueous extraction system is obtained, adding and accounting for total quality of materials score is that 20 parts of 45%DIPA-PAM-Gel obtain gel
Shape mixture, by above-mentioned gelatinous mixture, calcination two hours, calcination temperature are 120 DEG C under nitrogen protection, are formed powdered
Then particle is stored at standing 48 hours in 20 DEG C of vacuum oven, ionic liquid active adsorbing material, the suction is made
Enclosure material list electron microscope is shown in Fig. 1.
The adsorbent material is taken out, for capturing 2,4- Embutox in chernozem, by volume by adsorbent material and chernozem
1:3 is mixed, and places 30min at 27 DEG C.
The permeability of record capture front and back object is shown in Table one.
Embodiment 2:
The preparation method of the present embodiment is same as Example 1, distinguishes the ionic liquid type being only that in preparation process not
Together, ionic liquid is changed to [2-aemim] [PF6] (1- aminoethyl -3- methylimidazole hexafluorophosphate) in the present embodiment, remaining
Condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 3:
The preparation method of the present embodiment is same as Example 1, distinguishes the ionic liquid type being only that in preparation process not
Together, ionic liquid is changed to [cmmim] [PF6] (1- acetate -3- methylimidazole hexafluorophosphate) in the present embodiment, remaining
Part is constant, and the permeability of record capture front and back object is shown in Table one.
The ingredient of adsorbent material intermediate ion liquid is changed it can be seen from above-described embodiment and table one, it is black for separating
The permeability of 2,4- Embutox in calcium soil is respectively 99.6%, 74.3%, 59.3%, so using [TBP] Cl as ion
The permeability of 2,4- Embutox when liquid in chernozem is maximum, and osmotic effect is best.
Embodiment 4:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
Salt in example is changed to K2CO3, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 5:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
Salt in example is changed to (NH4)2SO4, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
The ingredient that salt is changed it can be seen from above-described embodiment and table one, for separating 2, the 4- drop fourth in chernozem
The permeability of acid is respectively 99.6%, 80.6%, 77.4%, so using KH2PO42,4- drop fourth when as salt in chernozem
The permeability of acid is maximum, and osmotic effect is best.
Embodiment 6:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of ionic liquid in example is changed to 14%, remaining condition is constant, and the permeability of record capture front and back object is shown in Table
One.
Embodiment 7:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of ionic liquid in example is changed to 34%, remaining condition is constant, and the permeability of record capture front and back object is shown in Table
One.
The mass fraction for changing ionic liquid it can be seen from above-described embodiment and table one, for separating in chernozem
The permeability of 2,4- Embutoxs is respectively 99.6%, 80.0%, 79.4%, so the ionic liquid for the use of mass fraction being 24%
When chernozem in 2,4- Embutox permeability it is maximum, osmotic effect is best.
Embodiment 8:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The type of gel in example is changed to sephadex, remaining condition is constant, and the electron microscope of the adsorbent material is shown in Fig. 2；
The permeability of record capture front and back object is shown in Table one.
Embodiment 9:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The type of gel in example is changed to 2-MEA-dithizone grafting chelating gel, remaining condition is constant, the electricity of the adsorbent material
Mirror figure is shown in Fig. 3；
The permeability of record capture front and back object is shown in Table one.
The type for changing three kinds of gels it can be seen from above-described embodiment and table one, for separating 2,4- in chernozem
The permeability of Embutox is respectively 99.6%, 63.0%, 84.1%, so using 2,4- in chernozem when DIPA-PAM-Gel
The permeability of Embutox is maximum, and osmotic effect is best.
The structure that change gel variations will lead to the adsorbent material being finally prepared it can be seen from Fig. 1,2 and 3 changes
Become, the capture rate of original active adsorbing material reduces.
Embodiment 10:
The preparation method of the present embodiment is same as Example 1, and difference is only that preparation process conditional is different, the present embodiment
In the mass fraction of gel be changed to 35%, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 11:
The preparation method of the present embodiment is same as Example 1, distinguishes the condition difference being only that in preparation process, this implementation
The mass fraction of gel in example is changed to 55%, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
The mass fraction for changing gel it can be seen from above-described embodiment and table one, for separating 2,4- in chernozem
The permeability of Embutox is respectively 99.6%, 77.4%, 89.5%, so accounting for the gel that total quality of materials is 45% using being added
When it is maximum to the permeability of 2, the 4- Embutox in chernozem, osmotic effect is best.
Embodiment 12:
The preparation method of the present embodiment is same as Example 1, and difference is only that the object of adsorbent material effect is different, this
Object in embodiment is changed to 2,4-D butyl ester, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Embodiment 13:
The preparation method of the present embodiment is same as Example 1, and difference is only that the object of adsorbent material effect is different, this
Object in embodiment is changed to butachlor, remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
Influence of one different condition of table to the permeability of the 2,4- Embutox in chernozem
Claims (7)
1. the preparation method of the adsorbent material of 2,4- Embutox in a kind of chernozem, which is characterized in that including by potassium dihydrogen phosphate,
Calcination obtains after polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and the mixing of tetrabutyl phosphorus chloride；
The temperature of the calcination is 120~150 DEG C；
The potassium dihydrogen phosphate, polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel and the tetrabutyl phosphorus chloride mass ratio
For 7:2:1.
2. the preparation method of the adsorbent material of 2,4- Embutox in chernozem according to claim 1, which is characterized in that institute
The time for stating calcination is 2h, and powdery granule object is obtained after calcination；
Then powdery granule object is obtained to the adsorbent material of 2,4- Embutox in the chernozem after vacuum dried.
3. the preparation method of the adsorbent material of 2,4- Embutox in chernozem according to claim 2, which is characterized in that institute
The vacuum drying temperature stated is 20~40 DEG C, and the vacuum drying time is 24~48h.
4. the preparation method of the adsorbent material of 2,4- Embutox, feature exist in chernozem according to claim 1,2 or 3
In the method is specifically: potassium dihydrogen phosphate and tetrabutyl phosphorus chloride being mixed to get two phase aqueous extraction system, then in Shuan Shui
Polyacrylamide-diisopropanolamine (DIPA) grafting chelating gel is added in phase extraction system and obtains gel mixture, gel mixture exists
Calcination obtains powdery granule object under inert atmosphere；
Then powdery granule object is obtained to the adsorbent material of 2,4- Embutox in the chernozem after vacuum dried.
5. the adsorbent material of 2,4- Embutox in a kind of chernozem, which is characterized in that the adsorbent material is appointed using claim 1-4
Preparation method described in one claim is prepared.
6. the adsorbent material of 2,4- Embutox is for adsorbing 2,4- Embutox in chernozem in chernozem described in claim 5
Using.
7. application according to claim 6 is specifically inhaled using the adsorbent material of 2,4- Embutox in chernozem of the invention
It is by adsorbent material and chernozem 1:3 by volume that the method for 2,4- Embutox, which includes: specific adsorption method, in attached chernozem
It mixes, places 30min at 27 DEG C.
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2018
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| CN103801271A (en) * | 2014-01-22 | 2014-05-21 | 长安大学 | Dithizone grafted chelating gel, preparation method thereof and method for treating mercury-containing wastewater |
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