CN109289813A - The adsorbent material of nitrous oxide, preparation method and applications in a kind of Wheat Growing Soils - Google Patents
The adsorbent material of nitrous oxide, preparation method and applications in a kind of Wheat Growing Soils Download PDFInfo
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- CN109289813A CN109289813A CN201811098634.XA CN201811098634A CN109289813A CN 109289813 A CN109289813 A CN 109289813A CN 201811098634 A CN201811098634 A CN 201811098634A CN 109289813 A CN109289813 A CN 109289813A
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- nitrous oxide
- adsorbent material
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- wheat growing
- growing soils
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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
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid 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
- B01J20/28016—Particle form
Abstract
The invention discloses the adsorbent materials of nitrous oxide, preparation method and applications in a kind of Wheat Growing Soils.The method is specifically: including obtaining calcination after nitrogen butyl-pyridinium isoleucine salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel mixing;The temperature of the calcination is 120~170 DEG C;Nitrogen butyl-pyridinium isoleucine salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel mass ratio are 2:7:1.The present invention prepares the adsorbent material method rapid and convenient, has very high targeting and arresting efficiency using special ion liquid, salt and grafting chelating gel, obtained adsorbent material when preparation, this method is to the permeability of nitrous oxide in wheatland up to 98.9%.Wide with the range of linearity, detection limit is low, and relative standard deviation is smaller, is able to satisfy detection requirement of the country for nitrous oxide in wheatland.
Description
Technical field
The invention belongs to field of environment protection, and in particular to the adsorbent material of nitrous oxide, preparation in a kind of Wheat Growing Soils
Method and its application.
Background technique
Nitrous oxide (N2O) it is a kind of gas with greenhouse effects, is 6 kinds of greenhouse gases as defined in Kyoto Protocol
One of.The retention time of nitrous oxide in an atmosphere is long, and can transport stratosphere, be cause ozone layer depletion substance it
One.Compared with carbon dioxide, N2The content of O in an atmosphere is very low, but its unimolecule heats 310 that potentiality is carbon dioxide
Times, it will be more and more significant in future to the warming effect of global climate.
Soil is the Major Natural source of nitrous oxide, and wherein agricultural soil discharges nitrous oxide about 3 × 10-6t every year.
In China, wheat planting area accounts for 22% or so of China's cereal crops gross area, is accounted for by the nitrous oxide that Wheat Growing Soils discharge
According to a big chunk of nitrous oxide total release.Therefore, the discharge for further control greenhouse gases nitrous oxide mentions
For convenient monitoring means, how fast and accurately to measure and capture the nitrous oxide generated in wheatland and also result in extensive weight
Depending on.
Adsorption and oxidation Asia nitrogen is usually adsorbed with different biomass carbon raw materials (moso bamboo powder, straw) in Wheat Growing Soils, but
Biomass carbon raw material is indifferent to the specific adsorption of nitrous oxide, and adsorption rate is not high.
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 nitrous oxide, therefore there is far-reaching influence to the research of the system.
Summary of the invention
It is long for there are detection times in the determination method of the nitrous oxide in existing wheatland, sensitivity is lower,
Complicated for operation, the disadvantages of stability is poor, the object of the present invention is to provide a kind of adsorption materials of nitrous oxide in Wheat Growing Soils
Material, preparation method and applications.The material can greatly improve the capturing efficiency of nitrous oxide in Wheat Growing Soils, while have line
Property range is wide, and detection limit is low, the lesser feature of relative standard deviation.
In order to realize that above-mentioned task, the present invention take following technical solution:
The preparation method of the adsorbent material of nitrous oxide in a kind of Wheat Growing Soils, including by nitrogen butyl-pyridinium isoleucine
Calcination obtains after salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel mixing;
The temperature of the calcination is 120~170 DEG C;
The mass ratio of nitrogen butyl-pyridinium isoleucine salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel is
2:7:1。
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 nitrous oxide in the Wheat Growing Soils 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: sodium acetate and nitrogen butyl-pyridinium isoleucine salt are mixed to get aqueous two-phase
Extraction system, then polyacrylamide-ethylenediamine 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 nitrous oxide in the Wheat Growing Soils after vacuum dried.
The adsorbent material of nitrous oxide in a kind of Wheat Growing Soils, the capture material use preparation method system of the present invention
It is standby to obtain.
The adsorbent material of nitrous oxide is for adsorbing nitrous oxide in Wheat Growing Soils in Wheat Growing Soils of the present invention
Using.
Optionally, using nitrous oxide in the adsorbent material absorption Wheat Growing Soils of nitrous oxide in Wheat Growing Soils of the invention
Method include: to mix soil to be adsorbed with adsorbent material, by mass percentage, the additive amount of adsorbent material is in soil
0.5%.
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 nitrous oxide in wheatland
Permeability up to 98.9%, have the range of linearity wide, detection limit is low, and relative standard deviation is smaller, be both able to satisfy country for
The detection requirement of nitrous oxide in wheatland.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph for the adsorbent material being prepared in embodiment 1;
Fig. 2 is the electromicroscopic photograph for the adsorbent material being prepared in embodiment 8;
Fig. 3 is the electromicroscopic photograph for the adsorbent material being prepared in embodiment 9;
The present invention is further explained below in conjunction with the drawings and specific embodiments.
Specific embodiment
The present invention is in preparing Wheat Growing Soils using special ion liquid, salt and grafting chela when the adsorbent material of nitrous oxide
Gel is closed, obtained round block shape active adsorbing material has very high targeting and arresting efficiency, and this method in wheatland to aoxidizing
The permeability of sub- nitrogen has the range of linearity wide, detection limit is low, and relative standard deviation is smaller, ionic liquid nitrogen fourth up to 98.9%
Yl pyridines isoleucine salt ([BPy] ILE): sodium acetate (CH3COONa): polyacrylamide-ethylenediamine grafting chelating gel
(EDA-PAM-Gel) mass ratio of three is 2:7:1.
Specific preparation method can be with are as follows: the ILE and 15 part of quality of ionic liquid [BPy] for being 21% by 65 parts of mass fractions
The CH3COONa that score is 16% is uniformly mixed, and obtains two phase aqueous extraction system, and adding 20 parts of mass fractions is 41%
EDA-PAM-Gel obtains gelatinous mixture, by above-mentioned gelatinous mixture at 120~170 DEG C calcination two hours, calcination temperature
120~170 DEG C of degree, obtains particle powder after calcination, the particle powder obtained after calcination is then stored in 20~40 DEG C true
24~48 hours are stood in empty drying box, the adsorbent material is made.
Ionic liquid nitrogen butyl-pyridinium isoleucine salt ([BPy] ILE): upper marine origin victory Chemical Co., Ltd.
Polyacrylamide-ethylenediamine grafting chelating gel (EDA-PAM-Gel):, with polyacrylamide gel (PAM-Gel,
Gongyi City source Yu Runhai water-purifying material Co., Ltd) it is skeleton, it is to connect with ethylenediamine (Jinan century sensible Chemical Co., Ltd.)
Branch chelating agent reacts in formaldehyde presence according to Mannich, and chelation group is made and is grafted gel;
In order to realize that the purpose for improving the capture rate of nitrous oxide in wheatland, the present invention devise a series of experiments to obtain
To preferably technological parameter:
Embodiment 1:
The CH3COONa for being 16% by ILE and 15 part of mass fraction of ionic liquid [BPy] that 65 parts of mass fractions are 21%
It is uniformly mixed, obtains two phase aqueous extraction system, adding the EDA-PAM-Gel that 20 parts of mass fractions are 41%, to obtain gel mixed
Close object, by above-mentioned gelatinous mixture at 120 DEG C calcination two hours, be then stored at quiet in 20 DEG C of vacuum oven
It sets 24 hours, the adsorbent material is made.
The adsorbent material is taken out, for capturing the nitrous oxide in Wheat Growing Soils, specific acquisition procedure is, will be to be adsorbed
Soil is mixed with adsorbent material and is adsorbed, and the additive amount of adsorbent material is preferably 0.5% (mass fraction), 27 DEG C of decentralizations in soil
Set 20min.
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 [BPy] DCN (2,2'- bipyridyl decorin) in the present embodiment, remaining condition is constant, note
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 1- carboxymethyl -3- methylimidazole hexafluorophosphate ([cmmim] [PF6]) 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 that adsorbent material intermediate ion liquid is changed it can be seen from above-described embodiment and table one, for separating wheat
The permeability of Tanaka's nitrous oxide is respectively 98.9%, 74.3%, 59.3%, so when using [BPy] ILE as ionic liquid
Maximum to the permeability of nitrous oxide in wheatland, 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 sodium chloride (NaCl), 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 potassium acetate (CH3COOK), remaining condition is constant, and the permeability of record capture front and back object is shown in Table one.
The type for changing salt it can be seen from above-described embodiment and table one, for separating the infiltration of nitrous oxide in wheatland
Rate is respectively 98.9%, 40.7%, 59.9%, so the permeability using nitrous oxide in wheatland when CH3COONa is maximum, is seeped
Saturating 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 10%, 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 32%, 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 the oxygen in wheatland
The permeability for changing sub- nitrogen is respectively 98.9%, 80.0%, 79.4%, thus the use of mass fraction is 21% ionic liquid when wheat
The permeability of the nitrous oxide of Tanaka is maximum, and 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 DEAE- agarose, remaining condition is constant, the infiltration of record capture front and back object nitrous oxide
Rate 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 SDS-PAGE, remaining condition is constant, the permeability of record capture front and back object nitrous oxide
It 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 the Asia of the oxidation in wheatland
The permeability of nitrogen is respectively 98.9%, 61.0%, 80.1%, so using the nitrous oxide in wheatland when EDA-PAM-Gel
Permeability is maximum, and osmotic effect is best.
When gel is EDA-PAM-Gel in adsorbent material it can be seen from Fig. 1,2 and 3, round block structure can be formed, and
Change the adsorbent material single structure that gel variations are then prepared to change, 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 21%, 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, and difference is only that preparation process conditional is different, the present embodiment
In the mass fraction of gel be changed to 61%, 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 the Asia of the oxidation in wheatland
The permeability of nitrogen is respectively 98.9%, 72.3%, 69.5%, so the oxygen when mass fraction using gel is 41% in wheatland
The permeability for changing sub- nitrogen is maximum, and 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 methane, 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 carbon dioxide, 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 nitrous oxide in wheatland
Claims (7)
1. the preparation method of the adsorbent material of nitrous oxide in a kind of Wheat Growing Soils, which is characterized in that including by nitrogen butyl-pyridinium
Calcination obtains after isoleucine salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel mixing;
The temperature of the calcination is 120~170 DEG C;
Nitrogen butyl-pyridinium isoleucine salt, sodium acetate and polyacrylamide-ethylenediamine grafting chelating gel mass ratio are 2:7:
1。
2. the preparation method of the adsorbent material of nitrous oxide in Wheat Growing Soils 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 nitrous oxide in the Wheat Growing Soils after vacuum dried.
3. the preparation method of the adsorbent material of nitrous oxide in Wheat Growing Soils 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 nitrous oxide, feature exist in Wheat Growing Soils according to claim 1,2 or 3
In the method is specifically: sodium acetate and nitrogen butyl-pyridinium isoleucine salt are mixed to get two phase aqueous extraction system, then
Polyacrylamide-ethylenediamine grafting chelating gel is added in two phase aqueous 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 nitrous oxide in the Wheat Growing Soils after vacuum dried.
5. the adsorbent material of nitrous oxide in a kind of Wheat Growing Soils, which is characterized in that the capture material is appointed using claim 1-4
Preparation method described in one claim is prepared.
6. the adsorbent material of nitrous oxide is for adsorbing nitrous oxide in Wheat Growing Soils in Wheat Growing Soils described in claim 5
Using.
7. application according to claim 6 adsorbs wheat using the adsorbent material of nitrous oxide in Wheat Growing Soils of the invention
The method of nitrous oxide includes: to mix soil to be adsorbed with adsorbent material in the soil of field, by mass percentage, is inhaled in soil
The additive amount of enclosure material is 0.5%.
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2018
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