CN104396949A - Method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent - Google Patents
Method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent Download PDFInfo
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- CN104396949A CN104396949A CN201410650994.1A CN201410650994A CN104396949A CN 104396949 A CN104396949 A CN 104396949A CN 201410650994 A CN201410650994 A CN 201410650994A CN 104396949 A CN104396949 A CN 104396949A
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- release agent
- chloroaluminate
- hydrated calcium
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Abstract
The invention discloses a method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent. The method includes: firstly calcining synthetic hydrated aluminum chloroaluminate dry powder in a crucible to obtain calcined aluminum chloroaluminate; then dispersing the calcined aluminum chloroaluminate in a solution containing original pesticide to obtain a suspension solution; then adjusting the pH of the obtained suspension solution with an acidity adjustment solution, and finally carrying out reaction, filtering, washing and drying so as to obtain the nano-controlled release agent. According to the method for structural reconstruction of hydrated aluminum chloroaluminate to synthesize pesticide controlled release agent, the pesticide controlled release agent has the characteristics of simple synthesis, low cost, easy separation and reusability. Hydrotalcite is employed to remove heavy metals in water, the specific surface area is large, and stronger adsorption capacity makes the adsorption effect remarkable. The method eliminates the metal salt inorganic anions competing with organic anions intercalation, and can be used for preparation of pillared hydrotalcite. The calcined hydrotalcite has very good adsorption and regeneration effects.
Description
Technical field
The present invention relates to a kind of hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method, belong to chemical synthetic pesticide sustained release agent field.
Background technology
The multiple metal hydroxides of stratiform is called for short LDHs, is an anionoid lamellar compound, and also known as hydrotalcite, it has acid and basic character, memory effect, the interchangeability of interlayer anion and microcellular structure.Since first relevant hydrotalcite-based compound in 1970 prepares the patent appearance of hydrogenation catalyst, hydrotalcite-based compound causes the great interest of people.It is widely used in the fields such as catalysis, absorption, ion exchange, in recent years, along with the further research to this kind of material, has opened up again its application in medicine, coating, agricultural chemicals, functional high molecule material, oil field development etc.
The multiple metal hydroxides (LDHs) of stratiform is anion type laminated compound, and interlayer has tradable anion, mainly comprises hydrotalcite, houghite and intercalation pillared hydrotalcite.Its structure is as sandwich, and both sides are made up of the metal ion positive charge sheet of divalence and trivalent, and centre is anion and hydrone.Each anionoid, as inorganic and organic anion, with many and heteropolyanion and metallic compound anion introducing hydrotalcite layers, just can obtain pillared hydrotalcite.Because this kind of material has anion interchangeability and the laminate cation collocation property of unique anion pillared layer structure and uniqueness, therefore, by metal ion and the anion of modulation, the variation of molecule assembling can be realized, in other words, under certain condition, some functional species can overcome lamellar compound active force between layers and insert bedding void changeably, and then modulation structural parameters and character on a large scale, as layer charge density, interlamellar spacing, laminate two-dimensional etc., derive rich and varied performance and function, meet the designing requirement of various functional material.
The most basic character of LDHs is alkalescence, and its stronger alkalescence shows often in its calcined product, the Acidity of Different L DHs is relevant with the alkalescence power of Divalent metal hydroxide with the Acidity of trivalent metal hydroxides in composition, and the acidity of pillared hydrotalcite also comes from pillaring anions sometimes.The heat endurance of LDHs is different because of composition, but substantially close; Only lose water of crystallization when being heated to uniform temperature, and its layer structure is not destroyed; When being heated to uniform temperature again, laminate hydroxyl shrinks and removes anion A
n-, cause LDHs micropore quantity sharply to increase, specific surface area also increases; At a higher temperature, more stable bimetallic oxide can be formed, when being heated beyond a certain temperature, along with hydroxyl and A
n-remove, LDHs is transitioned into the crystal structure being similar to metal oxide gradually from layered crystal structure.The mixture of metal oxide starts sintering, thus surface area is reduced greatly, and pore volume reduces, and alkalescence weakens.LDHs also has exclusive " memory effect ", namely changes after its structure through certain approach, reversibly returns to original structure again under certain condition.In general, high-valence anion is easy to the low price anion between switching layer.In addition, the bimetallic oxide compounds that hydrotalcite-based compound obtains after calcining under 500 DEG C of conditions, the anion adsorbed in environment can be rebuild by layer structure, therefore, hydrotalcite-based compound, particularly its calcined product and pillared hydrotalcite have larger specific surface area and pore volume, and acceptant object, can be used as adsorbent.
Calcining restoring method is based on development preparation method out on hydrotalcite " memory effect " characteristic basis, the memory effect of so-called hydrotalcite refer to the hydrotalcite sample calcined under uniform temperature join containing certain anion the aqueous solution or be placed in vapor atmosphere, then the reconstruction of hydrotalcite layer pole structure will be there is, anion enters interlayer, forms new pillared hydrotalcite.Therefore its preparation process is that the hydrotalcite of generation is fired to uniform temperature in atmosphere, after generating stratiform bimetallic oxide, then is placed in the anion solutions for inserting and carries out structural remodeling, form new lamellar compound.Finally filtered, washed, dry, obtain new hydrotalcite-like material.This process eliminate the slaine inorganic anion competing intercalation with organic anion, be usually used in preparing pillared hydrotalcite.Calcined state hydrotalcite has extraordinary absorption and regeneration effect, but the phenomenon that crystalline phase is not single or brilliant property is bad easily appears in sample.
Through calcination processing and non-calcination processing LDHs therebetween the otherness that manifests may be relevant with following truth: (1) calcination processing can increasing specific surface area, (2) calcination processing can improve pore volume, and (3) calcination processing can the content of carbanion between lower layer.In addition, this otherness also may the different absorption mechanisms of each oxo-anions relevant, for the LDHs through calcination processing, its absorption mechanism comprises the special adsorption of the rehydration of composite metal oxide material and the oxo-anions of generation simultaneously to rebuild LDHs structure, and for the LDHs without calcination processing, its absorption mechanism is only the ion exchange of interlayer anion.In adsorbing capacity, for the LDHs of non-calcination processing, its absorption mechanism is mainly anion exchange, and for the LDHs through calcination processing, its absorption mechanism is mainly the special adsorption of anion, if the anion therefore in original LDHs is not easy out replaced, then its adsorbing capacity of LDHs of non-calcination processing will far below the adsorbing capacity of the LDHs through calcination processing.In absorption power, for the LDHs of non-calcination processing, ion-exchange mechanism will comprise diffusion two steps in membrane diffusion and hole, but for the LDHs through calcination processing, structural remodeling and anion intercalatedly almost simultaneously to occur, therefore will shorten dramatically through its time of equilibrium adsorption of the LDHs of calcination processing.
Hydrotalcite-like material is the general designation of hydrotalcite, houghite and intercalated houghite, because of its there is special layer structure, specific surface area is large, and synthesize simple, with low cost, be easy to be separated and can reuse, in environmental pollution improvement, as adsorbent, there are quite large potentiality.Relevant reported in literature, relates to the Adsorption usefulness of hydrotalcite-like material to anionic pollutant mostly, removes Heavy Metals in Waters for employing hydrotalcite, especially with the removal of the heavy metal contaminants of cationic form existence, and the current less report of document.Make it on heavy metal ion-containing waste water clarificant, still have quite large using value using its significant adsorption effect and cheap cost.
Summary of the invention
The object of this invention is to provide a kind of hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method, to solve a still unsolved difficult problem in above-mentioned prior art.
Research finds: calcining hydrated calcium chloroaluminate, namely calcined hydrotalcite or calcining houghite interlayer anion after high temperature treatment almost all remove, and be converted into composite metal oxide, and discharging a large amount of gas, the hydrotalcite therefore after calcining has the specific surface area larger compared with its parent and stronger adsorption ability.Calcined state hydrotalcite not only can anion in adsorbent solution but also Liquidity limit simultaneously, and it can adsorb at relatively high temperatures, has incomparable advantage compared with other adsorbents.
The technical solution used in the present invention is: hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method, and its innovative point is: first the hydrated calcium chloroaluminate dry powder of synthesis is put into crucible calcination, obtain calcination calcium chloroaluminate; Then get calcination calcium chloroaluminate, be dispersed in the solution containing pesticide original medicine, obtain suspension; Then the pH acidity adjustment solution of gained suspension is adjusted, finally successively through reacting, filtering, wash and dry and obtain nano slow release agent.
Further, comprise calcining step and synthesis step, concrete steps are as follows:
(1) calcining step: synthesized hydrated calcium chloroaluminate dry powder is put into crucible, arranging heating rate is 10 DEG C/30min, keeps constant temperature after being heated to 300 ~ 700 DEG C, and calcining at constant temperature 2 ~ 8h obtains calcining hydrated calcium chloroaluminate;
(2) synthesis step: by described calcining hydrated calcium chloroaluminate, be dispersed in the solution containing pesticide original medicine 0.025 ~ 0.02g/ml, forming concentration is the suspension of 0.01 ~ 0.025g/ml, the PH regulating suspension with acidity adjustment solution is 4 ~ 12, then insulation reaction three days at reaction temperature is 20 ~ 100 DEG C, finally filter, and after spending deionized water 2 ~ 3 times, the pesticide slow-releasing agent of nano hybrid can be obtained.
Further, the general structure of described hydrated calcium chloroaluminate is 3CaOAl
2o
3caCl
210H
2o or Ca
4al
2(OH)
12c
l2(H
2o)
4, wherein, Ca:Al=1.5 ~ 6:1.
Further, the Ca:Al=2 ~ 4:1 in described hydrated calcium chloroaluminate.
Further, described the pesticide solution is the aqueous solution or the solution with organic solvent allotment.
Further, described acidity adjustment solution comprises inorganic acid and ackd salt thereof or inorganic base and basic salt thereof.
Further, the PH of suspension is regulated to be 6 ~ 10 with acidity adjustment solution in described synthesis step.
Further, the temperature arranging insulation reaction in described synthesis step is 35 ~ 80 DEG C.
Further, the time arranging insulation reaction in described calcining step is 3 ~ 5h, and temperature is 480 ~ 600 DEG C.
Beneficial effect of the present invention:
(1) this hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method of the present invention, pesticide slow-releasing agent synthesis simple, with low cost, be easy to be separated and can reuse, hydrotalcite is adopted to remove Heavy Metals in Waters, specific surface area is large, and stronger adsorption ability makes adsorption effect remarkable.
(2) general structure of the first hydrated calcium chloroaluminate calcined at a certain temperature of method of the present invention is 3CaOAl2O3CaCl210H2O or Ca4Al2 (OH) 12Cl2 (H2O) 4, wherein, Ca:Al=1.5 ~ 6:1, then join containing certain anion the aqueous solution or be placed in vapor atmosphere, then the reconstruction of hydrotalcite layer pole structure will be there is, anion enters interlayer, forms new pillared hydrotalcite, and during the Ca:Al=2 ~ 4:1 of hydrated calcium chloroaluminate, effect is better.Therefore its preparation process is that the hydrotalcite of generation is fired to uniform temperature in atmosphere, after generating stratiform bimetallic oxide, then is placed in the anion solutions for inserting and carries out structural remodeling, form new lamellar compound.Finally filtered, washed, dry, obtain new hydrotalcite-like material.
(3) this method eliminates the slaine inorganic anion competing intercalation with organic anion, can be used for preparing pillared hydrotalcite.Calcined state hydrotalcite has extraordinary absorption and regeneration effect.
Embodiment
Implementation column below can make those skilled in the art more fully understand the present invention, but does not therefore limit the present invention among described scope of embodiments.
embodiment 1
Prepare hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method:
(1) first calcination hydrated calcium chloroaluminate is prepared: get synthesized hydrated calcium chloroaluminate dry powder and put into crucible, rise to 500 DEG C with the speed of 10 DEG C/30min, constant temperature calcination 4h, obtains calcination hydrated calcium chloroaluminate, i.e. calcination calcium chloroaluminate;
Get 1g calcination hydrated calcium chloroaluminate, be dispersed in 40ml ethanol/water (volume ratio is (the 1:1)) solution of the indolebutyric acid containing 0.8mol/ml, after testing, the PH of suspension is greater than 8.5, uses HNO
3be adjusted to 8.0, then at room temperature react three days, filter, spend deionized water 2 times, indolebutyric acid nano slow release agent.
Based on the pesticide slow-releasing agent that the present embodiment method is produced, pesticide slow-releasing agent synthesis is simple, with low cost, be easy to be separated and can reuse, and adopt hydrotalcite to remove Heavy Metals in Waters, specific surface area is large, and stronger adsorption ability makes adsorption effect remarkable.
embodiment 2
A kind of hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method:
On the basis of embodiment 1, the 1g that Example 1 prepares calcines calcium chloroaluminate, is dispersed in the 100ml aqueous solution containing 0.5g dicamba.The pH HNO of suspension
3be adjusted to 8.0.Then, reaction 24 hours is at room temperature descended.Filter, wash with water, dicamba nano slow release agent.
Based on the pesticide slow-releasing agent that the present embodiment method is produced, pesticide slow-releasing agent synthesis is simple, with low cost, be easy to be separated and can reuse, and adopt hydrotalcite to remove Heavy Metals in Waters, specific surface area is large, and stronger adsorption ability makes adsorption effect remarkable.
embodiment 3
A kind of hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method:
On the basis of embodiment 1, the 1g that Example 1 prepares calcines calcium chloroaluminate, is dispersed in the 60ml aqueous solution containing 0.1g 2,4-dichlorphenoxyacetic acid.The pH of suspension is adjusted to 8.0 with HNO3.Then, reaction 12 hours is at room temperature descended.Filter, wash with water, 2,4-D nano slow release agents.
Based on the pesticide slow-releasing agent that the present embodiment method is produced, pesticide slow-releasing agent synthesis is simple, with low cost, be easy to be separated and can reuse, and adopt hydrotalcite to remove Heavy Metals in Waters, specific surface area is large, and stronger adsorption ability makes adsorption effect remarkable.
Above-described embodiment is only in order to illustrate technical scheme of the present invention; but not design of the present invention and protection domain are limited; those of ordinary skill of the present invention is modified to technical scheme of the present invention or equivalent replacement; and not departing from aim and the scope of technical scheme, it all should be encompassed in right of the present invention.
Claims (9)
1. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method, is characterized in that: first the hydrated calcium chloroaluminate dry powder of synthesis is put into crucible calcination, obtain calcination calcium chloroaluminate; Then get calcination calcium chloroaluminate, be dispersed in the solution containing pesticide original medicine, obtain suspension; Then the pH acidity adjustment solution of gained suspension is adjusted, finally successively through reacting, filtering, wash and dry and obtain nano slow release agent.
2. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 1, is characterized in that: comprise calcining step and synthesis step, concrete steps are as follows:
(1) calcining step: synthesized hydrated calcium chloroaluminate dry powder is put into crucible, arranging heating rate is 10 DEG C/30min, keeps constant temperature after being heated to 300 ~ 700 DEG C, and calcining at constant temperature 2 ~ 8h obtains calcining hydrated calcium chloroaluminate;
(2) synthesis step: by described calcining hydrated calcium chloroaluminate, be dispersed in the solution containing pesticide original medicine 0.025 ~ 0.02g/ml, forming concentration is the suspension of 0.01 ~ 0.025g/ml, the PH regulating suspension with acidity adjustment solution is 4 ~ 12, then insulation reaction three days at reaction temperature is 20 ~ 100 DEG C, finally filter, and after spending deionized water 2 ~ 3 times, the pesticide slow-releasing agent of nano hybrid can be obtained.
3. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 1 and 2, is characterized in that: the general structure of described hydrated calcium chloroaluminate is 3CaOAl
2o
3caCl
210H
2o or Ca
4al
2(OH)
12cl
2(H
2o)
4, wherein, Ca:Al=1.5 ~ 6:1.
4. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 3, is characterized in that: the Ca:Al=2 ~ 4:1 in described hydrated calcium chloroaluminate.
5. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 1 and 2, is characterized in that: described the pesticide solution is the aqueous solution or the solution with organic solvent allotment.
6. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 1 and 2, is characterized in that: described acidity adjustment solution comprises inorganic acid and ackd salt thereof or inorganic base and basic salt thereof.
7. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 2, is characterized in that: regulate the PH of suspension to be 6 ~ 10 with acidity adjustment solution in described synthesis step.
8. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 2, is characterized in that: the temperature arranging insulation reaction in described synthesis step is 35 ~ 80 DEG C.
9. hydrated calcium chloroaluminate structural remodeling synthetic pesticide sustained release agent method according to claim 2, is characterized in that: the time arranging insulation reaction in described calcining step is 3 ~ 5h, and temperature is 480 ~ 600 DEG C.
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Cited By (6)
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| CN114467952A (en) * | 2022-02-25 | 2022-05-13 | 茂名市和亿化工有限公司 | Method for synthesizing slow-release herbicide by using bispyribac-sodium intercalated hydrated calcium chloroaluminate |
| CN114467953A (en) * | 2022-02-25 | 2022-05-13 | 茂名市和亿化工有限公司 | Method for synthesizing bispyribac-sodium slow-release agent by reconstructing hydrated calcium chloroaluminate structure |
| CN114521552A (en) * | 2022-02-25 | 2022-05-24 | 茂名市和亿化工有限公司 | Method for synthesizing slow release agent by one-step intercalation assembly of oxyfluorfen-calcium chloroaluminate |
| CN114600895A (en) * | 2022-02-25 | 2022-06-10 | 茂名市和亿化工有限公司 | Method for synthesizing slow release agent by one-step intercalation assembly of bispyribac-sodium-calcium chloroaluminate |
| CN114804174A (en) * | 2022-02-25 | 2022-07-29 | 茂名市和亿化工有限公司 | Method for synthesizing oxyfluorfen sustained release agent by reconstructing hydrated calcium chloroaluminate structure |
| CN115430395A (en) * | 2022-09-28 | 2022-12-06 | 山东国舜建设集团有限公司 | Method for circularly removing chloride ions in wastewater by using mayenite material |
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| CN114467952A (en) * | 2022-02-25 | 2022-05-13 | 茂名市和亿化工有限公司 | Method for synthesizing slow-release herbicide by using bispyribac-sodium intercalated hydrated calcium chloroaluminate |
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| CN114804174A (en) * | 2022-02-25 | 2022-07-29 | 茂名市和亿化工有限公司 | Method for synthesizing oxyfluorfen sustained release agent by reconstructing hydrated calcium chloroaluminate structure |
| CN115430395A (en) * | 2022-09-28 | 2022-12-06 | 山东国舜建设集团有限公司 | Method for circularly removing chloride ions in wastewater by using mayenite material |
| CN115430395B (en) * | 2022-09-28 | 2023-12-29 | 山东国舜建设集团有限公司 | Method for circularly removing chloride ions in wastewater by using calcium aluminum stone material |
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Application publication date: 20150311 |