CN105347310B - A kind of method for preparing high-purity calcium based hydrotalcite - Google Patents
A kind of method for preparing high-purity calcium based hydrotalcite Download PDFInfo
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Abstract
The invention discloses a kind of method for preparing high-purity calcium based hydrotalcite.The present invention has crystallinity and purity higher, and the preparation method by being exchanged using low-temperature ion using calcium based hydrotalcite precursor prepared by nucleation/crystallization isolation method, controls suitable CO3 2‑Add speed, it is to avoid Ca2+With CO3 2‑With reference to generation CaCO3Precipitation, overcomes calcic hydrotalcite and CaCO is easily produced in preparation process3The shortcoming of impurity, obtains crystal phase structure well, purity calcium based hydrotalcite higher.The inventive method preparation process is simple, effect is significant can provide reference for the large-scale industrial production of high-purity calcium based hydrotalcite.And the calcium based hydrotalcite of gained can be widely used in the fields such as PVC Guan Cai ﹑ Xing Cai ﹑ electricity line electricity Lan ﹑ Yi Qi Xie ﹑ films as the high effect nontoxic heat stabilizer of a new generation, the traditional lead salt of replacement and expensive organo-tin het stabilizer.
Description
Technical field：
The invention belongs to hydrotalcite preparing technical field, more particularly to a kind of method for preparing high-purity calcium based hydrotalcite.
Background technology：
Hydrotalcite (Layered Double Hydroxides, abbreviation LDHs) is that a class has shepardite Mg (OH)2Type is just
The anionic clay of octahedral structure.Chemical general formula is:[M2+ 1-xM3+ x(OH)2]z+[An-]z/n·mH2O, wherein M2+﹑ M3+Point
Divalence and trivalent metal cation are not represented, and x refers to M3+The shared molar fraction in metal ion.Hydrotalcite has as a class
The layered inorganic functional material of special construction, with can the composition of modulation and the structure of uniqueness and performance, ion exchange, absorption
Separate, catalysis, medicine and other fields are used widely selectivity, the infrared absorbance that particularly hydrotalcite-like materials have
With some properties such as ion exchangeable, it is set to be widely used to PE agricultural films (heat preserving agent) as novel inorganic functional material
In PVC (non-toxic heat stabilizer) Polymer material.
Calcium based hydrotalcite, [M2+ xCa2+ yM3+(OH)2]+(CO3)2- 1/2·mH2O, belongs to laminar dual hydroxy composite metal oxidation
Thing, is a kind of houghite, and it is that will have to introduce cation laminate, layer compared with the calcium ion of strong metal and larger ionic radius
Between anion be common CO3 2-.So its structure is similar with LDHs structures.Numerous studies show, due to the particularity of calcium constituent
Matter, calcium based hydrotalcite shows preferable thermal stability.
Document [1]：Gupta S,Agarwal D D,Banerjee S.Synthesis and characterization
of hydrotalcites:Potential thermal stabilizers for PVC.Indian Journal of
Chemistry,2008,47(7):Ca-Al-CO is referred in 1004-10083- LDH is that a kind of potential efficient PVC is thermally-stabilised
Agent, but have a large amount of CaCO in its preparation process3Impurity is generated, and greatly reduces the purity and experimental result of target hydrotalcite
Accuracy.
Document [2]：Frost R L,Palmer S J,Theiss F.Synthesis and Raman
spectroscopic characterisation of hydrotalcites based on the formula Ca6Al2
(CO3)(OH)16·4H2O.Journal of Raman Spectroscopy,2011,42(5):Using coprecipitated in 1163-1167
Shallow lake method prepares Ca6Al2-CO3- LDH, gained target hydrotalcite equally exists a large amount of CaCO3Impurity, has a strong impact on experimental result
Accuracy.
From above-mentioned document it can be seen that in calcium based hydrotalcite preparation process easily with the CO of interlayer3 2-It is miscellaneous with reference to generating
Matter CaCO3, substantially reduce the purity and performance of calcium based hydrotalcite.Therefore impurity CaCO how is avoided3Generation be current people's urgency
The problem that need to be solved.
The content of the invention：
It is an object of the invention to provide a kind of method for preparing high-purity calcium based hydrotalcite.The method does not have in preparation process
There is CaCO3Impurity is generated, and product shows good crystal phase structure and purity higher.
The present invention is obtained nitrate anion intercalation calcium based hydrotalcite precursor by using nucleation/crystallization isolation method, then specific
Carbonate solution is added under flow velocity carries out ion exchange, and final assembling obtains the calcium base neatly that crystal phase structure is good, purity is higher
Stone.
The method for preparing high-purity calcium based hydrotalcite of the present invention is concretely comprised the following steps：
A. it is in molar ratio M by divalent metal nitrate and trivalent metal nitrate2+/M3+=2-4 is dissolved in deionized water
Mixing salt solution is made into, NaOH is dissolved in deionized water the aqueous slkali for being made into same volume, wherein n (NaOH)/[n (M2+)+n
(M3+)]=2-2.5, the molal quantity of n (NaOH) expressions NaOH, n (M2+) represent bivalent metal ion molal quantity, n (M3+) represent
The molal quantity of trivalent metal ion；At room temperature by mixing salt solution and aqueous slkali with identical flow velocity addition rotation membrane reactor
Fast nucleation 2-10min, the slurries that will be obtained move to flask, 60-100 DEG C crystallization 6-10 hours, centrifuge washing to pH is 7, is obtained
To nitrate anion intercalation calcium based hydrotalcite precursor；
B. by nitrate anion intercalation calcium based hydrotalcite precursor dispersion to except CO2Deionized water in compound concentration be 0.02-
The suspension of 0.2mol/L；It is subsequently adding the carbonate solution that concentration is 0.02-0.2mol/L, the molal quantity and nitric acid of carbonate
Nitrate anion molal quantity ratio in root intercalation calcium based hydrotalcite precursor is 1-4：1, coutroi velocity at the uniform velocity adds in 15min-60min
It is complete；Under nitrogen protection, crystallization is stirred 0.5-12 hours at 0-60 DEG C, filtering, washing is dried to obtain high-purity calcium based hydrotalcite.
Described carbonate is selected from Na2CO3、K2CO3、(NH4)2CO3In one or more.
Described M2+It is Mg2+、Ni2+、Co2+、Zn2+、Cu2+In one or more and Ca2+, wherein Ca2+In M2+In rub
You are more than 25% at content；Described M3+It is Al3+、Cr3+、Fe3+、Sc3+In one or more.
The advantage of the invention is that：The calcium based hydrotalcite precursor prepared using nucleation/crystallization isolation method has knot higher
Brilliant degree and purity, and by the preparation method using low temperature-ion exchange, control suitable CO3 2-Add speed, it is to avoid Ca2+
With CO3 2-With reference to generation CaCO3Precipitation, overcomes calcic hydrotalcite and CaCO is easily produced in preparation process3The shortcoming of impurity, obtains
Good, the purity calcium based hydrotalcite higher to crystal phase structure.The inventive method preparation process is simple, effect is significant can be high-purity
The large-scale industrial production for spending calcium based hydrotalcite provides reference.And the calcium based hydrotalcite of gained can be used as the efficient nothing of a new generation
Scorchingly hot stabilizer, substitutes traditional lead salt and expensive organo-tin het stabilizer and is widely used in PVC Guan Cai ﹑ Xing Cai ﹑
The electricity line electricity Lan ﹑ Yi fields such as Qi Xie ﹑ films.
Brief description of the drawings
Fig. 1 is the XRD spectra of high-purity calcium based hydrotalcite prepared by embodiment 1.
Fig. 2 is the Mg directly prepared using nucleation/crystallization isolation method0.5Ca1.5Al-CO3The XRD spectra of-LDHs.
Specific embodiment
Embodiment 1：
Step A：Solid Mg (the NO of 10.26g (0.04mol) are weighed respectively3)2·6H2The solid of O ﹑ 28.3g (0.12mol)
Ca(NO3)2·4H2Solid Al (the NO of O and 30.01g (0.08mol)3)3·9H2O, is dissolved in except CO2Deionized water in, prepare
Into the mixing salt solution of 150mL；The NaOH of 19.2g is weighed, is dissolved in except CO2In deionized water, 150mL aqueous slkalis are made into；Room temperature
It is lower that by two kinds of solution, with fast nucleation 10min in identical flow velocity addition rotation membrane reactor, (reactor rotating speed is as 5000r/
Min), the slurries that will be obtained move to 500mL flasks, 100 DEG C of crystallization 10 hours, and centrifuge washing is about 7 to pH, obtains MgCaAl-
NO3- LDHs precursors, wherein Mg2+/Ca2+/Al3+=0.5:1.5:1；
Step B：Take MgCaAl-NO3- LDHs precursor 13.78g (0.015molNO3 —) used in there-necked flask and remove CO2Go
Ionized water ultrasonic disperse, is configured to 150mL suspension；Weigh 0.79g (0.0075mol) solids Na2CO3, make NO3 —With object
CO3 2-Than being 1:1,150mL is dissolved in except CO2Deionized water in, prepare Na under rapid mixing conditions2CO3Solution；
Step C：Under nitrogen protection, the Na for rapidly preparing step B2CO3Solution dropwise (1 drop per second) be added to it is suspended
In liquid, the crystallization 1h at 40 DEG C, centrifugation, with except CO2Deionized water wash to pH and be about 7,70 DEG C of dryings 12 hours, obtain
To high-purity calcium based hydrotalcite, chemical formula is：Mg0.5Ca1.5Al(OH)6CO3·2.4H2O。
High-purity calcium based hydrotalcite to obtaining has carried out following sign：Characterized by X-ray powder diffraction (XRD), shown
Show CO3 2-Hydrotalcite layers have been assembled into it and in the absence of impurity CaCO3Characteristic diffraction peak.
Embodiment 2：
Step A：Solid Mg (the NO of 20.52g (0.08mol) are weighed respectively3)2·6H2The solid of O ﹑ 18.9g (0.08mol)
Ca(NO3)2·4H2Solid Al (the NO of O and 30.01g (0.08mol)3)3·9H2O, is dissolved in except CO2Deionized water in, prepare
Into the mixing salt solution of 150mL；The NaOH of 19.2g is weighed, is dissolved in except CO2In deionized water, 150mL aqueous slkalis are made into；Room temperature
It is lower that by two kinds of solution, with fast nucleation 10min in identical flow velocity addition rotation membrane reactor, (reactor rotating speed is as 5000r/
Min), the slurries that will be obtained move to 500mL flasks, 100 DEG C of crystallization 10 hours, and centrifuge washing is about 7 to pH, obtains MgCaAl-
NO3- LDHs precursors, wherein Mg2+/Ca2+/Al3+=1:1:1.
Take above-mentioned product 13.78g (0.015molNO3 —) used in there-necked flask and remove CO2Deionized water ultrasonic disperse, match somebody with somebody
It is made 150mL suspension.
Step B：Weigh 0.79g (0.0075mol) solids Na2CO3, make NO3 —With object CO3 2-Than being 1:1, it is dissolved in 150mL
Except CO2Deionized water in, prepare Na under rapid mixing conditions2CO3Solution.
Step C：Under nitrogen protection, dropwise (1 drop is per second) is added to step A preparations to the solution rapidly prepared step B
Precursor slurry in, the crystallization 1h at 40 DEG C, centrifugation, with except CO2Deionized water wash to pH and be about 7,70 DEG C of dryings
12 hours, high-purity calcium based hydrotalcite is obtained, molecular structure is：MgCaAl(OH)6CO3·2.4H2O。
High-purity calcium based hydrotalcite to obtaining has carried out following sign：Characterized by X-ray powder diffraction (XRD), shown
Show CO3 2-Hydrotalcite layers have been assembled into it and in the absence of impurity CaCO3Characteristic diffraction peak.
Embodiment 3：
Step A：Solid Mg (the NO of 30.77g (0.12mol) are weighed respectively3)2·6H2The solid of O ﹑ 9.45g (0.04mol)
Ca(NO3)2·4H2Solid Al (the NO of O and 30.01g (0.08mol)3)3·9H2O, is dissolved in except CO2Deionized water in, prepare
Into the mixing salt solution of 150mL；The NaOH of 19.2g is weighed, is dissolved in except CO2In deionized water, 150mL aqueous slkalis are made into；Room temperature
It is lower that by two kinds of solution, with fast nucleation 10min in identical flow velocity addition rotation membrane reactor, (reactor rotating speed is as 5000r/
Min), the slurries that will be obtained move to 500mL flasks, 100 DEG C of crystallization 10 hours, and centrifuge washing is about 7 to pH, obtains MgCaAl-
NO3- LDHs precursors, wherein Mg2+/Ca2+/Al3+=3:1:2.
Take above-mentioned product 13.78g (0.015molNO3 —) used in there-necked flask and remove CO2Deionized water ultrasonic disperse, match somebody with somebody
It is made 150mL suspension.
Step B：Weigh 0.79g (0.0075mol) solids Na2CO3, make NO3 —With object CO3 2-Than being 1:1, it is dissolved in 150mL
Except CO2Deionized water in, prepare Na under rapid mixing conditions2CO3Solution.
Step C：Under nitrogen protection, dropwise (1 drop is per second) is added to step A preparations to the solution rapidly prepared step B
Precursor slurry in, the crystallization 1h at 40 DEG C, centrifugation, with except CO2Deionized water wash to pH and be about 7,70 DEG C of dryings
12 hours, high-purity calcium based hydrotalcite is obtained, molecular structure is：Mg1.5Ca0.5Al(OH)6CO3·2.4H2O。
High-purity calcium based hydrotalcite to obtaining has carried out following sign：Characterized by X-ray powder diffraction (XRD), shown
Show CO3 2-Hydrotalcite layers have been assembled into it and in the absence of impurity CaCO3Characteristic diffraction peak.
Embodiment 4：
Step A：Solid Mg (the NO of 10.26g (0.04mol) are weighed respectively3)2·6H2The solid of O ﹑ 28.3g (0.12mol)
Ca(NO3)2·4H2Solid Fe (the NO of O and 32.32g (0.08mol)3)3·9H2O, is dissolved in except CO2Deionized water in, prepare
Into the mixing salt solution of 150mL；The NaOH of 19.2g is weighed, is dissolved in except CO2In deionized water, 150mL aqueous slkalis are made into；Room temperature
It is lower that by two kinds of solution, with fast nucleation 10min in identical flow velocity addition rotation membrane reactor, (reactor rotating speed is as 5000r/
Min), the slurries that will be obtained move to 500mL flasks, 100 DEG C of crystallization 10 hours, and centrifuge washing is about 7 to pH, obtains MgCaFe-
NO3- LDHs precursors, wherein Mg2+/Ca2+/Fe3+=0.5:1.5:1.
Take above-mentioned product 13.78g (0.015molNO3 —) used in there-necked flask and remove CO2Deionized water ultrasonic disperse, match somebody with somebody
It is made 150mL suspension.
Step B：Weigh 0.79g (0.0075mol) solids Na2CO3, make NO3 —With object CO3 2-Than being 1:1, it is dissolved in 150mL
Except CO2Deionized water in, prepare Na under rapid mixing conditions2CO3Solution.
Step C：Under nitrogen protection, dropwise (1 drop is per second) is added to step A preparations to the solution rapidly prepared step B
Precursor slurry in, the crystallization 1h at 40 DEG C, centrifugation, with except CO2Deionized water wash to pH and be about 7,70 DEG C of dryings
12 hours, high-purity calcium based hydrotalcite is obtained, molecular structure is：Mg0.5Ca1.5Fe(OH)6CO3·2.4H2O。
High-purity calcium based hydrotalcite to obtaining has carried out following sign：Characterized by X-ray powder diffraction (XRD), shown
Show CO3 2-Hydrotalcite layers have been assembled into it and in the absence of impurity CaCO3Characteristic diffraction peak.
Embodiment 5：
Step A：Solid Zn (the NO of 14.36g (0.04mol) are weighed respectively3)2·6H2The solid of O ﹑ 28.3g (0.12mol)
Ca(NO3)2·4H2Solid Al (the NO of O and 30.01g (0.08mol)3)3·9H2O, is dissolved in except CO2Deionized water in, prepare
Into the mixing salt solution of 150mL；The NaOH of 19.2g is weighed, is dissolved in except CO2In deionized water, 150mL aqueous slkalis are made into；Room temperature
It is lower that by two kinds of solution, with fast nucleation 10min in identical flow velocity addition rotation membrane reactor, (reactor rotating speed is as 5000r/
Min), the slurries that will be obtained move to 500mL flasks, 100 DEG C of crystallization 10 hours, and centrifuge washing is about 7 to pH, obtains MgCaAl-
NO3- LDHs precursors, wherein Zn2+/Ca2+/Al3+=0.5:1.5:1.
Take above-mentioned product 13.78g (0.015molNO3 —) used in there-necked flask and remove CO2Deionized water ultrasonic disperse, match somebody with somebody
It is made 150mL suspension.
Step B：Weigh 0.79g (0.0075mol) solids Na2CO3, make NO3 —With object CO3 2-Than being 1:1, it is dissolved in 150mL
Except CO2Deionized water in, prepare Na under rapid mixing conditions2CO3Solution.
Step C：Under nitrogen protection, dropwise (1 drop is per second) is added to step A preparations to the solution rapidly prepared step B
Precursor suspension in, the crystallization 1h at 40 DEG C, centrifugation, with except CO2Deionized water wash to pH be about 7,70 DEG C do
Dry 12 hours, high-purity calcium based hydrotalcite is obtained, molecular structure is：Zn0.5Ca1.5Al(OH)6CO3·2.4H2O。
High-purity calcium based hydrotalcite to obtaining has carried out following sign：Characterized by X-ray powder diffraction (XRD), shown
Show CO3 2-Hydrotalcite layers have been assembled into it and in the absence of impurity CaCO3Characteristic diffraction peak.
In order to be contrasted, Mg is directly prepared using nucleation/isolation crystallization method0.5Ca1.5Al-CO3-LDHs。
Result of the test shows：The calcium based hydrotalcite prepared using the inventive method is more straight than corresponding nucleation/isolation crystallization method
The calcium based hydrotalcite for connecing preparation shows more preferable crystal phase structure and Geng Gao material purities.
Claims (2)
1. a kind of method for preparing high-purity calcium based hydrotalcite, it is characterised in that the method is concretely comprised the following steps：
A. it is in molar ratio M by divalent metal nitrate and trivalent metal nitrate2+/M3+=2-4 is made into being dissolved in deionized water
Mixing salt solution, NaOH is dissolved in deionized water the aqueous slkali for being made into same volume, wherein n (NaOH)/[n (M2+)+n(M3 +)]=2-2.5, the molal quantity of n (NaOH) expressions NaOH, n (M2+) represent bivalent metal ion molal quantity, n (M3+) represent three
The molal quantity of valence metal ion；At room temperature by mixing salt solution and aqueous slkali with fast in identical flow velocity addition rotation membrane reactor
Rapid-result core 2-10min, the slurries that will be obtained move to flask, 60-100 DEG C crystallization 6-10 hours, centrifuge washing to pH is 7, is obtained
Nitrate anion intercalation calcium based hydrotalcite precursor；
B. by nitrate anion intercalation calcium based hydrotalcite precursor dispersion to except CO2Deionized water in compound concentration be 0.02-0.2mol/L
Suspension；It is subsequently adding the carbonate solution that concentration is 0.02-0.2mol/L, molal quantity and the nitrate anion intercalation calcium of carbonate
Nitrate anion molal quantity ratio in based hydrotalcite precursor is 1-4：1, coutroi velocity is at the uniform velocity added in 15min-60min；Nitrogen
Under protection, crystallization is stirred 0.5-12 hours at 0-60 DEG C, filtering, washing is dried to obtain high-purity calcium based hydrotalcite；
Described M2+It is Mg2+、Ni2+、Co2+、Zn2+、Cu2+In one or more and Ca2+, wherein Ca2+In M2+In mole contain
Amount is more than 25%；Described M3+It is Al3+、Cr3+、Fe3+、Sc3+In one or more.
2. method according to claim 1, it is characterised in that described carbonate is selected from Na2CO3、K2CO3、(NH4)2CO3
In one or more.
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| CN110078103A (en) * | 2019-05-27 | 2019-08-02 | 肇庆学院 | A kind of calcium aluminium houghite and preparation method thereof |
| CN111533148A (en) * | 2020-05-06 | 2020-08-14 | 马德君 | Method for purifying artificially synthesized carbonate hydrotalcite compound |
| CN115260588B (en) * | 2021-04-29 | 2024-02-13 | 中国石油化工股份有限公司 | Quaternary intercalation structure acid absorbent, preparation method and application thereof |
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Effective date of registration: 20220907 Address after: South of Weiqi Road, Industrial Park, Delingha City, Haixi Mongolian and Tibetan Autonomous Prefecture, Qinghai Province 817000 Patentee after: Qinghai West Mine Magnesium-based Ecological Material Technology Co.,Ltd. Address before: 100029 Beijing University of Chemical Technology, 15 North Third Ring Road, Beijing, Chaoyang District Patentee before: BEIJING University OF CHEMICAL TECHNOLOGY |