CN108946773A - A kind of carbonate form hydrotalcite-based compound raw powder's production technology - Google Patents
A kind of carbonate form hydrotalcite-based compound raw powder's production technology Download PDFInfo
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Abstract
The present invention provides a kind of preparation methods of carbonate form hydrotalcite-based compound, this method is using bivalent metal oxide or hydroxide and trivalent metal hydroxides as primary raw material, compounding is with bivalent metal oxide or the bivalent metal carbonate (normal salt or subcarbonate) of hydroxide same metal for providing carbonate, the direct composite structure of hydro-thermal reaction assisted through a step ultrasonic wave is regular, even-grained hydrotalcite-based compound, this technique belongs to atom economic reaction, reaction speed is fast, process no waste discharge, product washed can not directly be dried, water resource is greatly saved.This method has the characteristics that process flow is simple, environmentally protective, easy to industrialized production.
Description
Technical field
The invention belongs to the preparation fields of inorganic functional material, and in particular to a kind of carbonate form hydrotalcite-based compound powder
The preparation method of body.
Background technique
LDHs is the abbreviation of layered composite metal hydroxides (layered double hydroxides), also known as neatly
Stone class compound is a kind of anion type laminated complex hydroxide of two dimension, by the nanoscale laminate and interlayer of similar shepardite
Anion is constituted, and general formula isWherein M, N be divalent and trivalent metal from
Son (M=Mg2+、Ni2+、Co2+、Zn2+Deng N=Al3+、Fe3+、Cr3+Deng), An-For interlayer anion (such as CO3 2-、Cl-、OH-、
PO4 3-、NO3 -Deng), x N3+/(M2++N3+) ratio, m be the crystallization water quantity.LDHs material have acid-base property, memory effect,
Microcellular structure, laminate cation is adjustable therefore many unique properties such as denaturation and interlayer anion interchangeability are applied to
The numerous areas such as absorption, ion exchange, catalysis, medicine bioengineering, functional polymer material.Wherein, interlayer anion CO3 2-'s
Carbonate form LDHs is most common.
It include solvable using primary raw material currently, preparing the preparation method of carbonate form LDHs still based on coprecipitation
Property divalent and trivalent metal salt, be co-precipitated by mixing salting liquid and alkali by certain way, then pass through crystallization process
Prepare LDHs.Hydro-thermal method is also to prepare a kind of important method of LDHs, using slightly solubility divalent and trivalent metal oxide or
Hydroxide is main material, in enclosed system, is taken water as a solvent, and at a certain temperature, under the spontaneous pressure of water, is carried out anti-
It answers.Above two method generally requires longer reaction time (counting as unit of day), while requiring that hydrogen is added in the process
Sodium oxide molybdena, sodium carbonate or urea etc. provide alkaline environment and carbonate, need to go using a large amount of water in subsequent washing process
Except remaining foreign ion, serious waste is caused to water resource, there are subsequent sewage handling problems.Therefore, exploitation energy conservation
Clean LDHs technology of preparing is of great significance.
Aspect is cleaned in carbonate form LDHs preparation process, Chinese invention patent (CN 1994888A) is with divalent, trivalent
The hydroxide and CO of metal2For raw material, high-temperature stirring, which is reacted, is made carbonate form LDHs.This reaction needs to be continually fed into CO2Dimension
Hold CO3 2-Concentration simultaneously guarantees to react required pressure, needs to expend a large amount of CO2, restrictive condition is more, requires consersion unit high.In
State's patent (102701241 A of CN) is using one of Divalent metal hydroxide, carbonate or subcarbonate and trivalent
Metal hydroxides mixing dispersion, heating stirring is reacted in closed reactor, and obtaining interlayer is CO3 2-LDHs.But hydro-thermal method
Using the Divalent metal hydroxide of indissoluble is raw material there are dissolution of raw material degree is low, and reaction speed is slow, and partial size, which is easy to grow up, etc. asks
Topic.
Chinese patent (102350288 A of CN), which is reported, prepares high dispersion dose partial size with ultrasonic wave-hydrothermal reaction coupling technology
Uniform TiO2Nanotube, but ultrasonic technology is used to synthesize LDHs mainly as a kind of dispersing method, is only being co-precipitated at present
The precipitation process of method or LDHs product dispersion process introduce ultrasonic wave, but hydro-thermal method preparation LDHs in introduce ultrasonic wave auxiliary
There is not been reported for the research of reaction, nucleation and dispersion.
Summary of the invention
The purpose of the present invention is overcoming the problems, such as that existing Solid raw materials are more existing during preparing LDHs, one is provided
Kind process cleans, reaction speed is fast, product cut size is uniform, average grain diameter is small and the carbonate form hydrotalcite chemical combination of high degree of dispersion
The preparation method of powder.
The present invention prepares carbonate form LDHs using hydrothermal technique combination ultrasonic radiation (supersonic, water-heating), using divalent metal
Oxide or hydroxide, trivalent metal hydroxides and bivalent metal carbonate (normal salt or subcarbonate) are raw material, warp
After supersonic, water-heating reaction, product LDHs can be obtained.The aquation of bivalent metal oxide and water, surface are formed than more loose
Hydroxide, can make its reactivity improve；All raw materials participate in reaction in reaction, belong to atom economic reaction；Instead
It answers process without using the additive for generating foreign ion, therefore does not need to carry out water washing to product after separation of solid and liquid process；
Ultrasonic technique is added during the reaction, can not only accelerate to react, but also can effectively control the particle diameter distribution of LDHs.
LDHs synthetic method of the present invention sequentially includes the following steps:
(1) mix: by bivalent metal oxide or hydroxide, trivalent metal hydroxides, bivalent metal carbonate or
Divalent metal subcarbonate and deionized water be mixed into solid content be not higher than 20wt% suspension, wherein divalent metal and
The molar ratio of trivalent metal is 2-4, and the molar ratio range of divalent metal and carbonate is 3-15, bivalent metal oxide or hydrogen-oxygen
Compound is identical as the divalent metal in bivalent metal carbonate or divalent metal subcarbonate；
(2) react: the mixture in step (1) is added in supersonic, water-heating reaction kettle in 120-230 DEG C of temperature range, surpasses
It is reacted 0.5-12 hours under conditions of acoustical power 300-1500W, to get interlayer is CO after being separated by solid-liquid separation, being dry3 2-LDHs powder
Body.
Reaction temperature in preparation method of the present invention, in step (1) in the molar ratio and solid-to-liquid ratio, step (2) of material
Degree and time, ultrasound intensity and time etc. are all the key factors for influencing LDHs structure.
In the step (1), bivalent metal oxide has: Mg2+、Ca2+、Co2+、Ni2+Or Zn2+Deng oxide in one
Kind, Divalent metal hydroxide Mg2+、Ca2+、Co2+、Ni2+Or Zn2+One of hydroxide；Trivalent metal hydroxides
Have: Al3+、Fe3+、Co3+、Cr3+、V3+、Ga3+Deng one of hydroxide；Bivalent metal carbonate is Mg2+、Ca2+、Co2+、
Ni2+Or Zn2+One of carbonate, divalent metal subcarbonate is Mg2+、Ca2+、Co2+、Ni2+Or Zn2+Basic carbonate
One of salt.Material purity is technical pure or more.
When solid content is higher than 20wt% in the step (1), material concentration is too high, and raw material reaction is incomplete, to reduce
The conversion ratio of raw material increases the difficulty of purifying products.
The molar ratio of divalent metal and trivalent metal is lower than 2 in the step (1) or divalent metal and carbonate rub
When you are than lower than 3, side reaction occurs for trivalent metal hydroxides, is partially converted into hydroxyl trivalent metal oxide；When divalent gold
Belong to and the molar ratio of trivalent metal be higher than 4 or divalent metal and carbonate molar ratio higher than 15 when, divalent metal hydroxide
The generation or residue of object, to reduce the purity of product, increase the difficulty of purifying products due to the presence of these side reactions.
In the step (2), ultrasonic wave improves dispersibility using mechanical effect, heterogeneous reaction can be made to go on smoothly.
Ultrasonic wave needs energy carrier medium to be propagated, and in the reaction system, water is as medium, and there are positive and negative pressure in transmitting
Alternating cycles generate hydrone to squeeze and increase its original density in positive phase, and when minus phase, hydrone is sparse, discrete water
Density reduces, and sound wave cavitation is generated between water and sample, the formation, growth and explosion of bubble in solution is caused to be compressed,
To make bivalent metal oxide or hydroxide, trivalent metal hydroxides, bivalent metal carbonate or divalent metal alkali formula
The dispersion of the solid samples such as carbonate, increases the contact area between sample and water, improves object from solid phase and is transferred to liquid phase
Mass transfer rate；The second order effect machinery of ultrasound, which shake, emulsifies, spreading, smashing etc., to be all conducive to the comprehensive of reactant and sufficiently mixes
It closes, it is more more effective than general unidirectional mixing effect.
Ultrasonic power, which cannot achieve the reaction system lower than 300W, in the step (2) accelerates Solid raw materials reaction speed
The purpose of rate after ultrasonic power is more than 1500W, since ultrasonic energy is greater than the enthalpy change that product decomposes in the reaction system, is led
Cause can not synthesize product.
In the step (2) range of reaction temperature be 120-230 DEG C, beyond the range all can not complete synthesis it is completely pure
Hydrotalcite, when being lower than 120 DEG C, Solid raw materials reactivity is low to be led to not generate hydrotalcite, when being higher than 230 DEG C, trivalent gold
Belonging to hydroxide can occur to generate the side reaction of hydroxyl trivalent metal oxide, to reduce the purity of product, it is pure to increase product
The difficulty of change.
In the step (2) reaction time range be 0.5-12h, reaction be lower than 0.5h, Solid raw materials can not fully reacting,
The heat of system itself is added, hydrotalcite has the tendency that reunion since ultrasound generates the accumulation of heat for a long time more than 12h.
Drying temperature in the step (2) is not higher than 150 DEG C, is higher than this temperature, and hydrotalcite is easy dehydration, and structure is collapsed
The actual conditions for collapsing, and drying are not higher than 0.5wt% by the final moisture content of product, qualified products water content.
The present invention shows the prior art compared to having the advantages that
1) one-step method directly synthesizes the regular LDHs of layer structure, does not use NaOH, Na2CO3Equal raw materials, using raw material institute
The atom utilization of the LDHs of preparation is high, while simplifying production technology (no washing process) and save water, no waste water,
Abraum salt, water can reuse, reduce pollution to environment, greatly reduce cost；
2) the LDHs uniform particle sizes obtained and narrow distribution (P [D50-σ≤X≤D50+ σ] > 70%, i.e. average grain diameter and mark
70%) probability in the section of quasi- difference is greater than, crystal development is complete, and the use of ultrasonic technique solves product cut size wider distribution
The problem of, and good dispersion (reunion index≤5)；
3) ultrasonic use accelerates the process of reaction, improves 3-6 times than traditional reaction time；
4) it in addition, present invention process is simple and easy, applied to mass production of cheap and can prepare high-grade
LDHs。
Detailed description of the invention
Fig. 1 is the XRD diagram of embodiment 1；
Fig. 2 is that the FT-IR of embodiment 1 schemes；
Fig. 3 is the TG-DTA figure of embodiment 1 (solid line is TG curve, and dotted line is DTA curve)；
Fig. 4 is that the SEM of embodiment 1 schemes；
Fig. 5 is that (solid line is the grain size distribution of embodiment 1, and dotted line is the grain of comparative example 1 for the grain size distribution of embodiment 1
Diameter distribution map)；
Fig. 6 is the XRD diagram of comparative example 1 (solid line is the XRD diagram reacted after 1h, and dotted line is the XRD diagram reacted after 4h).
Specific embodiment
Following present invention is for the purpose of the controllable carbonate form LDHs of the particle diameter distribution for preparing high-quality, it should be understood that
It is that the specific embodiments described herein are merely illustrative of the invention, is not intended to restrict the invention.
Reaction is carried out substantially according to following equation:
MO+H2O→M(OH)2 (1)
M2++N3++OH–+CO3 2-+H2O→LDHs (5)
Below will by embodiment, the present invention will be described in detail, in the examples below, using Rigaku public affairs
The Mini Flex II type x-ray powder diffraction instrument (XRD) of department carries out the characterization of crystal structure to sample；Using Brooker company
Tensor II type Fourier infrared spectrograph (FT-IR) qualitative analysis is carried out to the infrared absorption of sample；Using Rigaku
The TG8120 type thermal analyzer of company investigates the thermal decomposition situation of sample；It is scanned using the JSM-7001F type of Japan Electronics Corporation
The pattern and particle size of electron microscope (SEM) observing samples；Using the Autosorb-iQ2 type of Kang Ta instrument company of the U.S.
The specific surface area of sample is measured；Using the Bettersize2000 type Particle Size Analyzer of Dandong Bai Te company to sample
Equivalent grain size distribution is tested.
Embodiment 1:
By MgO, Al (OH)3、MgCO3·Mg(OH)2·H2O is mixed to join the anti-of 1.2L by the molar ratio of 7:4:3 respectively
It answers in kettle, addition 975mL deionized water, solid content 7.5wt%, it is warming up to 165 DEG C after mixing evenly, in ultrasonic power
Supersonic, water-heating reacts 1h under 300W, it is cooling after product be separated by solid-liquid separation, dry after obtain MgAl-CO3 2-- LDHs powder.By XRD
As a result as shown in Figure 1, each characteristic diffraction peak peak type point is alarmmed, baseline is smooth, free from admixture peak, illustrates that the product crystal phase is single and crystallizes
Property is good.Qualitative analysis is carried out for the sample using infrared spectroscopy, as a result as shown in Fig. 2, 3464cm-1The absorption peak at place be by
Caused by the stretching vibration of hydroxyl on laminate.3069cm-1The absorption peak at place is by interlayer CO3 2-On the laminate of intermediary water
Caused by the hydrogen bond action of hydroxyl, 1611cm-1The absorption peak at place is attributed to H2The bending vibration of-OH in O, and 1363cm-1The suction at place
It receives peak and is attributed to CO3 2-C-O stretching vibration characteristic peak, 778cm-1And 682cm-1It is attributed to CO respectively3 2-Out-of-plane deformation C-O
Stretching vibration characteristic peak and in-plane bending C-O stretching vibration characteristic peak, 552cm-1, 447cm-1Locating absorption peak is interlayer oxygen lattice
The characteristic peak that vibration generates, and 447cm-1Absorption peak is mainly the relevant vibration peak of chemical bond between metal and oxygen atom.It should
There is three endothermic peaks, 246 DEG C of suction as shown in figure 3, can be seen that the sample from DTA curve in the thermal gravimetric analysis results of product
Thermal spike Master Home is the removing of the crystallization water of interlayer, with the rising of temperature, occurs two suctions again at 313 DEG C and 427 DEG C
Thermal spike is attributed to the removing of laminate hydroxyl and the removing of interlayer carbonate respectively.Using the shape of the scanning electron microscope observation sample
Looks, as a result as shown in figure 4, the product is typical LDHs sheet-like morphology, particle size is distributed in 1 μm or so.Using granularity point
Analyzer tests the equivalent grain size of the LDHs, as shown in figure 5, it is clear that with ultrasonic preparation is not added from figure
Sample (D50=10.9 μm) it compares, not only average grain diameter is small for the sample of supersonic, water-heating synthesis, but also particle diameter distribution is relatively narrow, the sample
The average grain diameter D of product50=1.23 μm (P [X]=87.6%), reunion index is 3.6, analysis result and sem analysis result one
It causes.The specific surface area of the sample is 30m2/g。
Comparative example 1:
By MgO, Al (OH)3、MgCO3·Mg(OH)2·H2O is mixed to join the anti-of 1.2L by the molar ratio of 7:4:3 respectively
It answers in kettle, addition 975mL deionized water, solid content 7.5wt%, it is warming up to 165 DEG C after mixing evenly, hydro-thermal difference is anti-
Answer 1h and 4h, it is cooling after product be separated by solid-liquid separation, dry after obtain the characterization that powder carries out XRD, as shown in fig. 6, hydro-thermal reaction
1h, raw material A l (OH)3There are no fully reactings, and hydro-thermal reaction 4h, all raw material fully reactings can synthesize pure water
Ultrasound is not added compared with Example 1 in talcum, and the hydro-thermal reaction time extends 4 times, while product average grain diameter D50=10.9 μm of (P
[X]=51.5%), reunion index is 11.2.
Embodiment 2:
By Mg (OH)2、Al(OH)3、MgCO3·Mg(OH)2·H2O is mixed to join 1.2L by the molar ratio of 4:2:1 respectively
Reaction kettle in, 975mL deionized water is added, solid content 5wt% is warming up to 120 DEG C, in ultrasonic power after mixing evenly
Supersonic, water-heating reacts 0.5h under 1200W, it is cooling after product be separated by solid-liquid separation, dry after obtain MgAl-CO3 2-- LDHs powder.It should
The average grain diameter D of product50=1.81 μm (P [X]=85.3%), reunion index is 3.5.
Embodiment 3:
By Ca (OH)2、Al(OH)3、CaCO3It is mixed to join in the reaction kettle of 1.2L by the molar ratio of 28:11:2 respectively,
975mL deionized water is added, solid content 20wt% is warming up to 200 DEG C after mixing evenly, ultrasonic at ultrasonic power 500W
Hydro-thermal reaction 8h, it is cooling after product be separated by solid-liquid separation, dry after obtain CaAl-CO3 2-- LDHs powder, the average grain diameter of the product
D50=3.67 μm (P [X]=78%), reunion index is 4.1.
Embodiment 4:
By CoO, Al (OH)3、CoCO3·H2O is mixed to join in the reaction kettle of 1.2L by the molar ratio of 3:1:1 respectively, is added
Enter 975mL deionized water, solid content 10.9wt% is warming up to 180 DEG C after mixing evenly, ultrasonic at ultrasonic power 500W
Hydro-thermal reaction 2h, it is cooling after product be separated by solid-liquid separation, dry after obtain CoAl-CO3 2-- LDHs powder, the average grain diameter of the product
D50=2.36 μm (P [X]=82.6%), reunion index is 3.9.
Embodiment 5:
By ZnO, Al (OH)3、2ZnCO3·3Zn(OH)2The reaction of 1.2L is mixed to join by the molar ratio of 5:5:2 respectively
In kettle, 975mL deionized water is added, solid content 6.8wt% is warming up to 220 DEG C after mixing evenly, in ultrasonic power 800W
Lower supersonic, water-heating reacts 4h, it is cooling after product be separated by solid-liquid separation, dry after obtain ZnAl-CO3 2-- LDHs powder, the product are put down
Equal partial size D50=2.85 μm (P [X]=81%), reunion index is 3.7.
Embodiment 6:
By Ni (OH)2、Al(OH)3、2Ni(OH)2·NiCO3It is mixed to join 1.2L's by the molar ratio of 25:10:2 respectively
In reaction kettle, 975mL deionized water is added, solid content 5wt% is warming up to 140 DEG C, in ultrasonic power after mixing evenly
Supersonic, water-heating reacts 6h under 600W, it is cooling after product be separated by solid-liquid separation, dry after obtain NiAl-CO3 2-- LDHs powder, the product
Average grain diameter D50=2.43 μm (P [X]=79%), reunion index is 3.9.
Embodiment 7:
By CoO, Fe (OH)3、CoCO3·H2O is mixed to join in the reaction kettle of 1.2L by the molar ratio of 4:3:2 respectively, is added
Enter 975mL deionized water, solid content 15wt% is warming up to 180 DEG C after mixing evenly, ultrasonic at ultrasonic power 1500W
Hydro-thermal reaction 2h, it is cooling after product be separated by solid-liquid separation, dry after obtain CoFe-CO3 2-- LDHs powder, the average grain diameter of the product
D50=1.09 μm (P [X]=89%), reunion index is 3.2.
Claims (4)
1. a kind of carbonate form hydrotalcite-based compound raw powder's production technology, it is characterised in that include the following steps:
(1) it mixes: by bivalent metal oxide or hydroxide, trivalent metal hydroxides, bivalent metal carbonate or divalent
Basic metal carbonates and deionized water are mixed into the suspension that solid content is not higher than 20wt%, wherein divalent metal and trivalent
The molar ratio of metal is 2-4, and the molar ratio range of divalent metal and carbonate is 3-15, bivalent metal oxide or hydroxide
It is identical as the divalent metal in bivalent metal carbonate or divalent metal subcarbonate；
(2) react: mixture in step (1) is added in supersonic, water-heating reaction kettle in 120-230 °C of temperature range, ultrasonic function
It is reacted 0.5-12 hours under conditions of rate 300-1500W, to get interlayer is CO after being separated by solid-liquid separation, being dry3 2-LDHs powder.
2. a kind of carbonate form hydrotalcite-based compound raw powder's production technology as described in claim 1, it is characterised in that step
Suddenly (1) bivalent metal oxide is Mg2+、Ca2+、Co2+、Ni2+Or Zn2+One of oxide, Divalent metal hydroxide
For Mg2+、Ca2+、Co2+、Ni2+Or Zn2+One of hydroxide.
3. a kind of carbonate form hydrotalcite-based compound raw powder's production technology as described in claim 1, it is characterised in that step
Suddenly (1) trivalent metal hydroxides are Al3+、Fe3+、Co3+、Cr3+、V3+Or Ga3+One of hydroxide.
4. a kind of carbonate form hydrotalcite-based compound raw powder's production technology as described in claim 1, it is characterised in that step
Suddenly (1) bivalent metal carbonate is Mg2+、Ca2+、Co2+、Ni2+Or Zn2+One of carbonate, divalent metal basic carbonate
Salt is Mg2+、Ca2+、Co2+、Ni2+Or Zn2+One of subcarbonate.
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| Publication number | Priority date | Publication date | Assignee | Title |
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