CN110028090B - Hydrotalcite-like compound and preparation method and application thereof - Google Patents

Hydrotalcite-like compound and preparation method and application thereof Download PDF

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CN110028090B
CN110028090B CN201910276543.9A CN201910276543A CN110028090B CN 110028090 B CN110028090 B CN 110028090B CN 201910276543 A CN201910276543 A CN 201910276543A CN 110028090 B CN110028090 B CN 110028090B
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hydrotalcite
chlorite
compound
trivalent metal
divalent metal
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CN110028090A (en
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翟朋达
吴海霞
王奎涛
杨迦
秦玉明
温冲
郭伟
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Andixsen medical technology Hebei Co.,Ltd.
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Hebei University of Science and Technology
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    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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Abstract

The invention relates to the technical field of hydrotalcite materials, and particularly discloses a hydrotalcite-like compound and a preparation method and application thereof. The compound comprises a layer structure formed by divalent metal hydroxide and trivalent metal hydroxide and interlayer anions, and the anions are chlorite. The preparation method at least comprises the following steps: mixing divalent metal salt and trivalent metal salt to prepare mixed salt water solution; mixing chlorite and alkaline substance to prepare coprecipitation water solution; and simultaneously adding the mixed saline solution and the coprecipitation aqueous solution into a reactor, and performing crystallization treatment to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function. The hydrotalcite-like compound obtained by the invention has stable performance, the release period of chlorine dioxide is long and reaches 90 days, the release amount is stable, and the initial release amount reaches 20mg every day.

Description

Hydrotalcite-like compound and preparation method and application thereof
Technical Field
The invention relates to the technical field of hydrotalcite materials, in particular to a hydrotalcite-like compound and a preparation method and application thereof.
Background
Hydrotalcite, also known as Layered Double Hydroxides (LDH), is an artificially synthesized Layered mineral material that has emerged in recent years and can be used as a catalyst and a catalyst carrier in the fields of chemistry and chemical engineering; the product is used as a new generation antacid and gastric mucosa protective agent in the pharmaceutical industry; in the plastic industry, can be used as an antibacterial agent, a flame retardant and a PVC stabilizer; in the field of environmental protection, the compounds have strong adsorption effect on a plurality of toxic and harmful anions, so the compounds have wide application prospect in the aspects of water quality purification, sewage treatment, pollution prevention, environmental remediation and the like; the material is used as an infrared and ultraviolet absorption and barrier material in the field of functional materials.
The chlorine dioxide has strong reaction activity and oxidation capacity, does not generate organic halogenated substances such as chloroform and the like and mutagenic substances in the application process, and has selectivity. Therefore, chlorine dioxide is widely used as a disinfectant, a bleaching agent, a deodorant, a cleaning agent, and the like in the related fields. Chlorine dioxide has been increasingly used over the last 20 years, primarily because chlorine dioxide has proven to be viable and effective as a disinfectant and bleach alternative to other disinfection processes, including from conventional liquid chlorine to ozone. However, the instability of chlorine dioxide brings great inconvenience to practical application, and the existing preparation or storage conditions are required to be harsh.
Disclosure of Invention
Aiming at the problem that the existing chlorine dioxide needs to be prepared or stored under harsh conditions at present, the invention provides a hydrotalcite-like compound.
And a method for preparing the hydrotalcite-like compound.
And the application of the hydrotalcite-like compound in the aspect of slowly releasing chlorine dioxide.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a hydrotalcite-like compound, which comprises a layer structure composed of a divalent metal hydroxide and a trivalent metal hydroxide, and an anion between the layers, wherein the anion is chlorite.
Compared with the prior art, the hydrotalcite-like compound provided by the invention has the following advantages:
the hydrotalcite-like compound is used as a chlorine dioxide slow release agent, the performance of the hydrotalcite-like compound is stable, the release period of chlorine dioxide is long, the release period reaches 90 days, the release amount is stable, and the initial release amount reaches 20mg every day.
Preferably, the divalent metal is Mg2+、Ni2+Or Cu2+。
Preferably, the trivalent metal is Al3+、Ti3+Or Fe3+。
Preferably, the molar ratio of the divalent metal to the trivalent metal is 0.9 to 4: 1.
The molar ratio of the divalent metal to the trivalent metal is controlled to be 0.9 to 4:1 because the hydrotalcite framework is easily formed and stable in this ratio range and anions are easily introduced into the interlayer.
Preferably, the amount of the chlorite species is 1.6 to 6.4 times the sum of the amounts of the divalent metal and trivalent metal species.
ClO prepared by different times2 -ClO in intercalated hydrotalcite2 -When the content is different, less than 1.6 times, the content is due to ClO2 -Too low a concentration and NO3 -、Cl-More easily into the interlayer, resulting in ClO2 -Cannot be inserted between layers; 6.4 times ClO2 -The maximum amount of intercalation is reached, and even if the sodium chlorite quality is increased, the interlaminar intercalation amount is not increased.
Further, the present invention also provides a method for preparing a hydrotalcite-like compound, comprising at least the following steps:
step A, mixing a divalent metal salt and a trivalent metal salt to prepare a mixed salt water solution;
step B, mixing chlorite and alkaline substances to prepare a coprecipitation aqueous solution;
and step C, simultaneously adding the mixed salt aqueous solution and the coprecipitation aqueous solution into a reactor, and performing crystallization treatment to obtain the hydrotalcite-like compound.
Compared with the prior art, the preparation method provided by the invention has the following advantages:
the invention utilizes the performance of hydrotalcite capable of being assembled by intercalation, adopts a coprecipitation method to assemble chlorite ions between hydrotalcite layers to prepare the hydrotalcite-like material with the interlayer object being the chlorite intercalation, and uses the hydrotalcite-like material as the chlorine dioxide slow release agent.
The hydrotalcite-like compound obtained by the invention has stable performance, the release period of chlorine dioxide is long and reaches 90 days, the release amount is stable, and the initial release amount reaches 20mg every day.
Preferably, the anion of the divalent metal salt is NO3 -、Cl-Or CO3 2-。
Preferably, the anion of the trivalent metal salt is NO3 -、Cl-Or SO4 2-。
Preferably, the divalent metal salt is magnesium nitrate, magnesium chloride, magnesium carbonate, nickel nitrate, copper chloride or copper nitrate.
Preferably, the trivalent metal salt is aluminum nitrate, aluminum chloride, aluminum sulfate, titanium sulfate, ferric chloride, ferric nitrate, or ferric sulfate.
Preferably, the total concentration of divalent metal and trivalent metal in the mixed brine solution is 0.2 to 1.0 mol/L.
Preferably, the total concentration of the chlorite and the alkaline substance in the coprecipitation aqueous solution is 0.68 to 20 mol/L.
Preferably, the chlorite is potassium chlorite, sodium chlorite, or ammonium chlorite.
Preferably, the alkaline substance is potassium hydroxide, sodium hydroxide or sodium phosphate
Preferably, the conditions of the crystallization treatment are as follows: the pH value is 8-10, the temperature is 20-80 ℃, and the treatment time is 2-24 h.
Preferably, CO is removed in the mixed salt aqueous solution, the coprecipitation aqueous solution and the crystallization treatment process2Preparing or treating the distilled water.
Preferably, the reactor employs a nitrogen atmosphere.
CO removal by extraction2Distilled water and N2Protection is due to the reaction solution being alkaline, preventing CO from reacting during the reaction2Into solution to generate CO3 2-，CO3 2-To ClO2 -More easily enter the hydrotalcite interlayer to generate CO3 2-Intercalated hydrotalcite, producing impurities; meanwhile, the chlorite ions are ensured to smoothly enter the interlayer of the hydrotalcite-like compound by controlling the crystallization treatment time and the pH value.
Filtering and drying are further carried out after the crystallization treatment, and CO is removed from a filter cake obtained by filtering2Washing the filter cake to be neutral by using distilled water, then washing for 1-2 times by using absolute ethyl alcohol, and drying for 10-14h at the temperature of 50-70 ℃.
Furthermore, the invention also provides the application of the hydrotalcite-like compound in the aspect of slowly releasing chlorine dioxide, and the hydrotalcite-like compound can be used as a long-acting disinfectant, a bleaching agent, a deodorant, a cleaning agent and the like.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a hydrotalcite XRD standard spectrum;
FIG. 2 is an XRD pattern of a hydrotalcite-like compound obtained in example 1 of the present invention;
FIG. 3 is an XRD pattern of a hydrotalcite-like compound obtained in example 2 of the present invention;
FIG. 4 is an XRD pattern of a hydrotalcite-like compound obtained in example 3 of the present invention;
FIG. 5 is an infrared spectrum of a hydrotalcite-like compound obtained in example 1 of the present invention;
FIG. 6 is an infrared spectrum of a hydrotalcite-like compound obtained in example 2 of the present invention;
FIG. 7 is an infrared spectrum of a hydrotalcite-like compound obtained in example 3 of the present invention;
fig. 8 is a chlorine dioxide release curve of the hydrotalcite-like compound obtained in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 12.82g of solid Mg (NO)3)2And 18.76g of solid Al (NO)3)3Mixed and dissolved in 500mL of de-CO2To obtain a mixed salt water solution;
and B: 24.78g of sodium chlorite and 9.6g of sodium hydroxide were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the mixed saline solution and the coprecipitation aqueous solution into a conical flask protected by nitrogen, adjusting the pH value to 8.8, crystallizing at 60 ℃ for 6h, filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake by using absolute ethyl alcohol once, and drying the filter cake for 12 hours at the temperature of 60 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalated Mg-Al hydrotalcite.
The obtained chlorite intercalated Mg-Al hydrotalcite is subjected to X-ray diffraction and infrared spectrum analysis, and the analysis results are respectively shown in fig. 2 and fig. 5.
Fig. 1 is a hydrotalcite XRD standard pattern, from which it can be seen that 003, 006 and 009 are characteristic peaks of hydrotalcite compounds.
Compared with the standard spectrum of hydrotalcite XRD in figure 1, the XRD spectrum of the chlorite intercalated Mg-Al hydrotalcite obtained in the embodiment has characteristic peaks of 003 hydrotalcite, 006 hydrotalcite and 009 hydrotalcite in figure 2, which shows that the product prepared in the embodiment is a hydrotalcite compound, but the graph line is unsmooth, the peak height is lower, the peak width is larger, and the crystallinity of the hydrotalcite is lower.
In the infrared spectrum of FIG. 5, 1384cm-The nearby absorption peak is a Cl-O-Cl vibration absorption peak, which indicates that anions in the interlayer part of the hydrotalcite are chlorite.
The content of the chlorite ion intercalated Mg-Al hydrotalcite obtained in the embodiment is detected by an iodometry method, and the detected content of the chlorite ion is 7.9%.
Example 2
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 25.64g of solid Cu (NO)3)2And 18.76g of solid Fe (NO)3)3Mixed and dissolved in 500mL of de-CO2To obtain a mixed salt water solution;
and B: 60.77 sodium chlorite and 14.6g sodium hydroxide were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the mixed saline solution and the coprecipitation aqueous solution into a conical flask protected by nitrogen, adjusting the pH value to 9, crystallizing at 60 ℃ for 6h, filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake by using absolute ethyl alcohol once, and drying the filter cake for 12 hours at the temperature of 60 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalation Cu-Fe hydrotalcite.
The obtained chlorite intercalated Cu-Fe hydrotalcite is subjected to X-ray diffraction and infrared spectrum analysis, and the analysis results are respectively shown in fig. 3 and fig. 6.
Compared with the standard hydrotalcite XRD pattern in FIG. 1, the XRD pattern 3 of the chlorite intercalated Cu-Fe hydrotalcite obtained in the embodiment shows characteristic peaks of 003 hydrotalcite, 006 hydrotalcite and 009 hydrotalcite, which indicates that the product prepared in the embodiment is a hydrotalcite compound, and has a smooth graph and higher characteristic peaks, thus indicating that the crystallinity of the hydrotalcite is better.
In the infrared spectrum of FIG. 6, 1384cm-The nearby absorption peak is a Cl-O-Cl vibration absorption peak, which indicates that anions in the interlayer part of the hydrotalcite are chlorite.
The content of the chlorite ion in the obtained chlorite ion intercalated Cu-Fe hydrotalcite is detected by an iodometry method, and the detected content of the chlorite ion is 9.8%.
In order to better illustrate the characteristics of the hydrotalcite-like compound with the chlorine dioxide slow-release function provided in the embodiment of the present invention, 20g of the chlorite intercalated Cu-Fe hydrotalcite prepared in the embodiment 2 is subjected to chlorine dioxide release detection, and the detection result is shown in fig. 8.
As can be seen from fig. 8, the release period of chlorine dioxide is long, reaching 90 days, the release amount is stable, and the initial release amount reaches 20mg per day.
Example 3
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 25.64g of solid Mg (NO)3)2And 18.76g of solid Al (NO)3)3Mixed and dissolved in 500mL of de-CO2To obtain a mixed salt water solution;
and B: 50.65 parts of sodium chlorite and 9.6 parts of sodium hydroxide were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the mixed saline solution and the coprecipitation aqueous solution into a conical flask protected by nitrogen, adjusting the pH value to 9.1, crystallizing at 60 ℃ for 7h, filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake by using absolute ethyl alcohol once, and drying the filter cake for 12 hours at the temperature of 60 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalated Mg-Al hydrotalcite.
The obtained chlorite intercalated Mg-Al hydrotalcite is subjected to X-ray diffraction and infrared spectrum analysis, and the analysis results are respectively shown in fig. 4 and 7.
Compared with the standard hydrotalcite XRD pattern in FIG. 1, the XRD pattern 4 of the chlorite intercalated Mg-Al hydrotalcite obtained in this example shows characteristic peaks of the hydrotalcite 003, 006 and 009, which indicates that the product prepared in this example is a hydrotalcite compound, but the pattern is not smooth, the peak height is low, and the crystallinity of the hydrotalcite is low.
In the infrared spectrum in FIG. 7, 1384cm-The nearby absorption peak is a Cl-O-Cl vibration absorption peak, which indicates that anions in the interlayer part of the hydrotalcite are chlorite.
The content of the chlorite ion intercalated Mg-Al hydrotalcite obtained in the embodiment is detected by an iodometry method, and the detected content of the chlorite ion is 8.8%.
Example 4
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 33.6g of solid MgCO3And 16.25g of solid FeCl3Mixed and dissolved in 500mL of de-CO2Obtaining a divalent and trivalent metal salt mixed solution in the distilled water;
and B: 286.24g of ammonium chlorite and 65.6g of sodium phosphate were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the divalent and trivalent metal salt mixed solution and the coprecipitation aqueous solution into a conical flask with nitrogen protection, adjusting pH to 8, crystallizing at 80 deg.C for 2h, vacuum filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake for 2 times by using absolute ethyl alcohol, and drying the filter cake for 10 hours at 70 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalation Mg-Fe hydrotalcite.
Example 5
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 54.9g of solid Ni (NO)3)2And 14.4g of solid Ti2(SO4)3Mixed and dissolved in 500mL of de-CO2Obtaining a divalent and trivalent metal salt mixed solution in the distilled water;
and B: 212g of potassium chlorite and 16.8g of potassium hydroxide were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the divalent and trivalent metal salt mixed solution and the coprecipitation aqueous solution into a conical flask with nitrogen protection, adjusting the pH value to 10, crystallizing at 20 ℃ for 24 hours, filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake for 1 time by using absolute ethyl alcohol, and drying the filter cake for 14 hours at 50 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalated Ni-Ti hydrotalcite.
Example 6
The embodiment of the invention provides a preparation method of a hydrotalcite-like compound, which comprises the following steps:
step A, 19g of solid MgCl2And 13.4g of solid AlCl3Mixed and dissolved in 500mL of de-CO2Obtaining a divalent and trivalent metal salt mixed solution in the distilled water;
and B: 108.6g of sodium chlorite and 164g of sodium phosphate were mixed and dissolved in 500mL of CO-removed solution2Obtaining a coprecipitation aqueous solution in the distilled water;
and C: adding the divalent and trivalent metal salt mixed solution and the coprecipitation aqueous solution into a conical flask with nitrogen protection, adjusting pH to 9, crystallizing at 40 deg.C for 10h, vacuum filtering, and removing CO2Washing the filter cake to be neutral by using distilled water, washing the filter cake for 1 time by using absolute ethyl alcohol, and drying the filter cake for 12 hours at the temperature of 55 ℃ to obtain the hydrotalcite-like compound with the chlorine dioxide slow release function, namely the chlorite intercalated Mg-Al hydrotalcite.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (7)

1. A method for preparing a hydrotalcite-like compound, characterized by: the preparation method at least comprises the following steps:
step A, mixing a divalent metal salt and a trivalent metal salt to prepare a mixed salt water solution;
step B, mixing chlorite and alkaline substances to prepare a coprecipitation aqueous solution;
step C, simultaneously adding the mixed salt aqueous solution and the coprecipitation aqueous solution into a reactor for crystallization treatment, wherein the crystallization treatment conditions are as follows: the pH value is 8-10, the temperature is 20-80 ℃, the processing time is 2-24h, and CO is removed in the processes of the mixed salt water solution, the coprecipitation water solution and crystallization processing2Preparing or treating the distilled water to obtain a hydrotalcite-like compound, wherein the hydrotalcite-like compound comprises a layered structure formed by divalent metal hydroxide and trivalent metal hydroxide and interlayer anions, and the anions are chlorite; the divalent metal is Mg2+、Ni2+Or Cu2+(ii) a The trivalent metal is Al3+、Ti3+Or Fe3+(ii) a The molar ratio of the divalent metal to the trivalent metal is 0.9-4: 1; the amount of the chlorite species is 1.6 to 6.4 times the sum of the amounts of the divalent metal and trivalent metal species.
2. The process for producing a hydrotalcite-like compound according to claim 1, wherein: the anion of the divalent metal salt is NO3 -、Cl-Or CO3 2-(ii) a And/or
The anion of the trivalent metal salt is NO3 -、Cl-Or SO4 2-。
3. The process for producing a hydrotalcite-like compound according to claim 2, characterized in that: the divalent metal salt is magnesium nitrate, magnesium chloride, magnesium carbonate, nickel nitrate, copper chloride or copper nitrate; and/or
The trivalent metal salt is aluminum nitrate, aluminum chloride, aluminum sulfate, titanium sulfate, ferric chloride, ferric nitrate or ferric sulfate.
4. The process for producing a hydrotalcite-like compound according to claim 1, wherein: the total concentration of the divalent metal and the trivalent metal in the mixed salt water solution is 0.2-1.0 mol/L; and/or
The total concentration of the chlorite and the alkaline substance in the coprecipitation aqueous solution is 0.68-20 mol/L.
5. The process for producing a hydrotalcite-like compound according to claim 1, wherein: the chlorite is potassium chlorite, sodium chlorite or ammonium chlorite; and/or
The alkaline substance is potassium hydroxide, sodium hydroxide or sodium phosphate.
6. The process for producing a hydrotalcite-like compound according to claim 1, wherein:
the crystallization treatment is carried out in a nitrogen atmosphere; and/or
Filtering and drying are further carried out after the crystallization treatment, and CO is removed from a filter cake obtained by filtering2Washing the filter cake to be neutral by using distilled water, then washing for 1-2 times by using absolute ethyl alcohol, and drying for 10-14h at the temperature of 50-70 ℃.
7. Use of the hydrotalcite-like compound obtained by the process according to any one of claims 1 to 6 for the sustained release of chlorine dioxide.
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CN111285384B (en) * 2020-02-23 2022-10-21 武汉工程大学 Method for preparing hydrotalcite-based composite flame retardant by decomposing phosphate tailings with organic phosphonic acid
CN114887582B (en) * 2022-05-12 2023-08-15 重庆文理学院 Method for recycling phosphite radical ions in wastewater
CN115043439B (en) * 2022-06-10 2023-11-17 青岛大学 Special anion intercalation modified nickel-titanium double-metal hydroxide and preparation method and application thereof
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