CN1772622A - Surfactant intercalated magnetic hydrotalcite material and its prepn - Google Patents
Surfactant intercalated magnetic hydrotalcite material and its prepn Download PDFInfo
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- CN1772622A CN1772622A CNA2005100865661A CN200510086566A CN1772622A CN 1772622 A CN1772622 A CN 1772622A CN A2005100865661 A CNA2005100865661 A CN A2005100865661A CN 200510086566 A CN200510086566 A CN 200510086566A CN 1772622 A CN1772622 A CN 1772622A
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Abstract
The present invention provides one kind of surfactant intercalated magnetic hydrotalcite material and its preparation, and belongs to the field of hydrotalcite material technology. The surfactant intercalated magnetic hydrotalcite has chemical expression of (M2+)1-x(N3+)x(OH)2(Surf)a(Bn+)b.mH2O/M'Fe2O4. Its preparation process includes the first preparation of nanometer level magnetic kernel and mixing the magnetic kernel with corresponding slat solution, the subsequent co-precipitation process of assembling surfactant into interlayer of hydrotalcite to obtain surfactant intercalated hydrotalcite with magnetic kernel. The present invention is superior in that during use, externally applied magnetic field may have magnetic field strength and direction controlled to realize the high dispersion and target location of magnetic hydrotalcite and organic compound, originally being hard to intercalate, may be assembled into interlayer of hydrotalcite.
Description
Technical field
The invention belongs to the hydrotalcite material technical field, a kind of surfactant intercalated magnetic hydrotalcite material and preparation method thereof particularly is provided; Be specially dodecyl sodium sulfonate intercalated magnetic hydrotalcite, Witco 1298 Soft Acid intercalated magnetic hydrotalcite and dodecyl sulphate intercalated magnetic hydrotalcite; They can be applied as a kind of ion-exchanger, sorbent material, pharmaceutical carrier, support of the catalyst and biosensor etc. as a kind of base mateiral.
Background technology
(Layered double hydroxides is a kind of anionic inorganic clay material LDHs) to hydrotalcite, has laminate metallic element Modulatory character and interlayer anion interchangeability.Utilize the interchangeability of its interlayer anion, can be with between the organic molecule interposed layer.Change reaction conditionss such as temperature, crystallization time, pH value, interlayer object, main body laminate, can obtain various organic-hydrotalcite composite material, make it all have unique advantage in preparation routine and aspects such as nanometer composite organic-inorganic material, biosensor.
Because the peculiar amphipathic property of tensio-active agent makes surfactant intercalated hydrotalcite be with a wide range of applications.People such as Crepaldi have reported tensio-active agent dodecyl sulphate and Witco 1298 Soft Acid intercalation zinc chrome hydrotalcite 429～442 pages of Journal of Colloid and Interface the 248th phases of Science in 2002, and studied its different zinc chromes than the time chemical structure and thermostability.People such as Zhang Hui and Wang Bin has reported 190～196 pages of the 92nd phases of Materials Chemistry and Physics in 2005 and has utilized coprecipitation method synthetic surfactant dodecyl sodium sulfonate and Witco 1298 Soft Acid intercalation magnesium aluminum-hydrotalcite, the author utilizes the property of tensio-active agent that hydrotalcite has been carried out modification, and the hydrophobic non-ionic type agricultural chemicals Chlorpyrifos 94 of script is assembled into hydrotalcite layers.
Magnetic hydrotalcite material can utilize externally-applied magnetic field to increase its dispersiveness owing to have magnetic, and reaches convenient recovery and the localized purpose of target.People such as Duan Xue and Zhang Hui has reported for 752～757 pages at Chinese Science Bulletin the 8th phase the 50th volume in 2005 and has utilized synthetic captopril and the 5-aminosalicylic acid intercalated houghite with magnetic of chemical coprecipitation technique, utilize externally-applied magnetic field can increase its dispersiveness, and can make it be fixed on diseased region to reach the localized purpose of target.Duan Xue and Zhang Hui patent (application number: reported magnetic hydrotalcite 200410009903.2) as a kind of gastric antiacids intermediate, its have good in and the performance of hydrochloric acid in gastric juice and bigger magnetic.Still the document and the patent report that do not have relevant surfactant intercalated magnetic hydrotalcite material at present both at home and abroad.
Summary of the invention:
The object of the present invention is to provide a kind of surfactant intercalated magnetic hydrotalcite material and preparation method thereof, promptly the dodecyl sodium sulfonate intercalated magnetic hydrotalcite (DSO-LDHs/M ' Fe
2O
4), the Witco 1298 Soft Acid intercalated magnetic hydrotalcite (DBS-LDHs/M ' Fe
2O
4) and the dodecyl sulphate intercalated magnetic hydrotalcite (DS-LDHs/M ' Fe
2O
4).Can be applied as ion-exchanger, sorbent material, pharmaceutical carrier, support of the catalyst, biosensor etc. as a kind of base mateiral, and in use can realize target setting control effect, increase dispersed and improve the rate of recovery by the magneticstrength and the direction of control externally-applied magnetic field.Having solved in the past the ortho-water talc materials disperses undesirable and problem such as can't locate.
The prepared surfactant intercalated magnetic hydrotalcite material of the present invention is a supramolecular structure, and its crystalline structure is the crystalline structure of houghite material, and chemical formula is:
(M
2+)
1-x(N
3+)
x(OH)
2(Surf)
a(B
n-)
b·mH
2O/M’Fe
2O
4。Be a kind of organic and inorganic composite functional material with magnetic, wherein the quality percentage composition of tensio-active agent is 0～40%, and specific saturation magnetization is 2～75AM
2/ Kg; Coercivity H is 0～400kA/m.(M wherein
2+)
1-x(N
3+)
x(OH)
2(Surf)
a(B
N-)
bMH
2O (can be abbreviated as Surf-LDHs), M ' Fe
2O
4Be magnetic species, Surf-LDHs is for being coated on M ' Fe
2O
4Outer surfactant intercalated hydrotalcite.Its quality percentage composition is:
M’Fe
2O
4：5％～50％，
Surf-LDHs：95％～50％；
M wherein
2+Be divalent-metal ion Zn
2+, Mg
2+, Ni
2+, Cu
2+, Ca
2+, Mn
2+In any;
N
3+Be trivalent metal ion Al
3+, Fe
3+, Cr
3+, Ga
3+In any.
M ' is Co
2+, Mg
2+, Ba
2+, Ni
2+Wherein any of divalent-metal ion, M
2+Can be the same or different with M '.
Surf represents interlayer surface promoting agent negatively charged ion.
B
N-For carrying capacity is the inorganic anion of n, B in the Surf-LDHs chemical formula
N-Can not exist or for CO
3 2-, NO
3 -, Cl
-, OH
-, H
2PO
4 -In any, two kinds or three kinds.
X=N
3+/ (M
2++ N
3+), 0＜x＜1; A, b are respectively Surf, B
N-Quantity, and satisfy a+n * b=x, m is the crystallization water number, can be any real number.
The concrete preparation process of surfactant intercalated magnetic hydrotalcite material of the present invention is:
A, nano-magnetic nuclear M ' Fe
2O
4Powder preparing
The soluble inorganic salt and two of M ', ferric soluble inorganic salt are mixed with mixing solutions, wherein (M '+Fe
2+)/Fe
3+Mol ratio is 1～5, M '/Fe
2+Mol ratio is 0.5～2.The volumetric molar concentration of M ' is 0.1～2.5M, Fe
3+Volumetric molar concentration be 0.2～5.0M; Use the NaOH alkaline solution, wherein the NaOH volumetric molar concentration is 0.1～5.0M; Under nitrogen protection, alkali lye splashed in the salts solution to the pH value and equal 6～8; 15～60 ℃ of crystallization are 4～72 hours in water-bath; reaction solution is filtered; wash with water; use absolute ethanol washing again; vacuum-drying, grind to form powdery, obtain particle size range at the M ' of 200～800nm Fe through 800～1200 ℃ of high-temperature roastings
2O
4Powder.Obtain powder uniformly with the standard sieve screening.
Wherein M ' is Co
2+, Mg
2+, Ba
2+, Ni
2+Wherein any of divalent-metal ion.All reaction solutions and bath water are the decarbonation deionized water.
The preparation of b, surfactant intercalated magnetic hydrotalcite
Step 1: solubility divalent metal salt, trivalent metal salt are pressed M
2+/ N
3+Be the mixing salt solution A that 1～9 mol ratio is made into, in addition with an amount of NaOH proportionaling alkali-forming solution B, the concentration of solution A, B is 0.0001～1mol/L, with an amount of tensio-active agent and magnetic core M ' Fe
2O
4Be configured to mixed solution C, wherein [the N in the A solution
3+]/[surfactant soln Surf] mol ratio is 1～3, the M in the A solution
2+/ M ' Fe
2O
4Mass ratio be 2～48;
M wherein
2+Can be Zn
2+, Mg
2+, Ni
2+, Cu
2+, Ca
2+, Mn
2+In any; N
3+Can be Al
3+, Fe
3+, Cr
3+, Ga
3+In any; Soluble M
2+, N
3+The negatively charged ion of salt can be NO
3 -, Cl
-, OH
-:
Step 2: with the reaction vessel that solution C places band to stir, being simultaneously mixing salt solution A and alkaline solution B slowly to be added under 0.001～1ml/s condition in titration speed, is 6.5～11 to stop to the pH of gained slurries, changes in the crystallizing kettle;
Perhaps above-mentioned solution A and solution C being mixed and put into crystallizing kettle, is under 0.001～1ml/s condition in titration speed, and solution B is splashed in the crystallizing kettle, obtains pH and be 6.5～11 slurries;
Step 3: in crystallizing kettle, use N
2Protection makes slurries crystallization 18～72 hours under 35～100 ℃ of temperature.Again through suction filtration, be washed to neutrality, 25～100 ℃ of dry 12h～72 hour, obtain Surf-LDHs/M ' Fe
2O
4
The quality percentage composition of tensio-active agent is 0～40% in this surfactant intercalated magnetic hydrotalcite material; Specific saturation magnetization is 2～75AM
2/ Kg; Coercivity H is 0～400kA/m.Because this surfactant intercalated magnetic hydrotalcite material has magnetic, in use can realize the high dispersing and the target location of operation system magnetic hydrotalcite, disperse undesirable and shortcoming such as can't locate thereby solved in the past the ortho-water talc materials by control magneticstrength of externally-applied magnetic field and direction; And, because the amphipathic property of tensio-active agent, can with originally can't intercalation or the non-ionic type and/or the hydrophobic type organic molecule of very difficult intercalation be assembled into hydrotalcite layers.
Advantage of the present invention is:
[1] prepared a kind of new surfactant intercalated magnetic hydrotalcite material, owing to have magnetic, can accurate localization and the dispersion of height; Because the amphipathic property of tensio-active agent, can with originally can't intercalation or the non-ionic type and/or the hydrophobic type organic molecule of very difficult intercalation be assembled into hydrotalcite layers.
[2] by changing Surf-LDHs/M ' Fe
2O
4Assembling condition, as changing the mol ratio of magnetic nuclear and hydrotalcite, the hydrotalcite that can obtain having different magnetic.
Embodiment:
Embodiment 1
(1) magnetic core MgFe
2O
4The preparation of nano-powder
With magnesium/ferrous iron/ferric iron mol ratio is 2: 1: 1 ratio, takes by weighing 8.47g Mg (NO
3)
26H
2O and 6.666g Fe (NO
3)
39H
2O and 3.29g FeCl
24H
2O is dissolved in the 100ml water and is made into mixing salt solution, takes by weighing 6.02g NaOH and 7.43g Na
2CO
3Be dissolved in the 100ml water and be made into mixed ammonium/alkali solutions; Alkaline solution dropwise splashed in the salts solution to the pH value equal 6,50 ℃ of crystallization are 4 hours in water-bath, and reaction solution is filtered, wash with water, use absolute ethanol washing again, vacuum-drying, grind to form powdery, roasting 4 hours in 800 ℃, air atmosphere again, 10 ℃/minute of temperature rise rates make magnetic nuclear MgFe
2O
4, obtaining powder uniformly with the standard sieve screening, all reaction solutions and bath water are the decarbonation deionized water.
(2) magnetic DSO-LDHs/MgFe
2O
4Preparation
With 5.77g Mg (NO
3)
26H
2O, 2.81g Al (NO
3)
39H
2O is mixed with the 50ml mixing salt solution; Weighing 3.6g NaOH is mixed with 50ml alkali lye more in addition; The solution that in addition the 2.04g sodium laurylsulfonate is mixed with 150ml places the four-hole boiling flask of 500ml, adds the magnetic nuclear of 0.12g simultaneously, makes Mg (NO
3)
26H
2O/MgFe
2O
4=48 mass ratioes.At 35 ℃, N
2Under gas shiled and the stirring condition, mixing salt solution and alkaline solution be added drop-wise to simultaneously contain sodium laurylsulfonate and MgFe
2O
4Four-hole boiling flask in, the pH value is 10 ± 0.3.80 ℃ of crystallization 18 hours are washed to neutrality and surfactant-free, and are centrifugal, put into 80 ℃ of oven dryings 14 hours, obtain DSO-LDHs/MgFe
2O
4
Record this DSO-LDHs/MgFe
2O
4The coercivity H value be 8kA/m, specific saturation magnetization σ
sBe 2.04AM
2/ Kg, all reaction solutions and bath water are the decarbonation deionized water.
Embodiment 2
(1) magnetic core NiFe
2O
4The preparation of nano-powder
With nickel/ferrous iron/ferric iron mol ratio is 2: 1: 1 ratio, takes by weighing 10.10g NiSO
46H
2O, 4.50gFeSO
47H
2O and 6.40g Fe
2(SO
4)
37H
2O is dissolved in the 150ml water and is made into mixing salt solution, takes by weighing 8.00g NaOH and is dissolved in the 100ml water and is made into mixed ammonium/alkali solutions; Under nitrogen protection, alkali lye splashed in the salts solution to the pH value and equal 8; 15 ℃ of crystallization are 48 hours in water-bath; reaction solution is filtered; wash with water; use absolute ethanol washing again, vacuum-drying, grind to form powdery, roasting 2 hours in 1200 ℃, air atmosphere again; 10 ℃/minute of temperature rise rates make magnetic nuclear NiFe
2O
4, obtaining powder uniformly with the standard sieve screening, all reaction solutions and bath water are the decarbonation deionized water.
(2) magnetic DBS-LDHs/NiFe
2O
4
With 8.92g Zn (NO
3)
26H
2O and 4.00g Cr (NO
3)
39H
2O is mixed with the 50ml mixing salt solution; Weighing 4g NaOH is mixed with 50ml alkali lye in addition; The solution that weighing 3.48g Sodium dodecylbenzene sulfonate is mixed with 150ml places the 500ml four-hole boiling flask, and adds 3.57g magnetic core NiFe
2O
4, make Zn (NO
3)
26H
2O/NiFe
2O
4Mass ratio be 2.5; At 35 ℃, N
2Under gas shiled and the stirring condition, mixing salt solution and alkaline solution be added drop-wise to simultaneously contain DBS and magnetic core NiFe
2In the 500ml four-hole boiling flask of O, the pH value maintains in 7 ± 0.5 scopes, and 35 ℃ of crystallization 72 hours are centrifugal, washs to neutrality and 65 ℃ of dryings of surfactant-free 24 hours, obtains DSO-LDHs/NiFe
2O
4
Record this magnetic DBS-LDHs/NiFe
2O
4The coercivity H value be 48kA/m, specific saturation magnetization σ
sBe 30.73AM
2/ Kg, all reaction solutions and bath water are the decarbonation deionized water.
Embodiment 3
(1) magnetic core CoFe
2O
4The preparation of nano-powder
With cobalt/ferrous iron/ferric iron mol ratio is 1.5: 1: 1 ratio, takes by weighing 5.05g CoSO
46H
2O, 2.78gFeSO
47H
2O and 4.00g Fe
2(SO
4)
37H
2O is dissolved in the 150ml water and is made into mixing salt solution, takes by weighing 8.00g NaOH and is dissolved in the 100ml water and is made into mixed ammonium/alkali solutions; Under nitrogen protection, alkali lye splashed in the salts solution to the pH value and equal 7; 40 ℃ of crystallization are 16 hours in water-bath; reaction solution is filtered; wash with water; use absolute ethanol washing again, vacuum-drying, grind to form powdery, roasting 4 hours in 900 ℃, air atmosphere again; 10 ℃/minute of temperature rise rates make magnetic nuclear CoFe
2O
4, obtaining than uniformed powder with the standard sieve screening, all reaction solutions and bath water are the decarbonation deionized water.
(2) magnetic DBS-LDHs/CoFe
2O
4
Weighing 8.92g Zn (NO
3)
26H
2O (0.03mol) and 3.75g Al (NO
3)
39H
2O (0.01mol) is mixed with the 50ml mixing salt solution; Weighing 4.00g NaOH is mixed with 50ml alkali lye in addition; The solution that weighing 3.49g Sodium dodecylbenzene sulfonate is mixed with 150ml places the four-hole boiling flask of 500ml, and the magnetic nuclear that adds 0.46g simultaneously makes Zn (NO
3)
26H
2O/CoFe
2O
4Mass ratio be 19.4; 45 ℃, N
2Under gas shiled and the stirring condition, mixing salt solution and alkaline solution are added drop-wise in the four-hole boiling flask simultaneously, the pH value maintains in 7.5 ± 0.3 scopes; 80 ℃ of crystallization 24 hours, centrifugal, wash to neutrality and surfactant-free; 65 ℃ of dryings 24 hours obtain DBS-LDHs/CoFe
2O
4
Survey magnetic DBS-LDHs/CoFe
2O
4The coercivity H value be 84kA/m, specific saturation magnetization σ
sBe 7.69AM
2/ Kg, all reaction solutions and bath water are the decarbonation deionized water.
Embodiment 4
(1) magnetic core NiFe
2O
4The preparation of nano-powder
With nickel/ferrous iron/ferric iron mol ratio is 2: 1: 1 ratio, takes by weighing 10.10g NiSO
46H
2O, 4.50gFeSO
47H
2O and 6.40g Fe
2(SO
4)
37H
2O is dissolved in the 150ml water and is made into mixing salt solution, takes by weighing 8.00g NaOH and is dissolved in the 100ml water and is made into mixed ammonium/alkali solutions; Under nitrogen protection, alkali lye splashed in the salts solution to the pH value and equal 8; 15 ℃ of crystallization 48h in water-bath; reaction solution is filtered; wash with water; use absolute ethanol washing again, vacuum-drying, grind to form powdery, roasting 2 hours in 900 ℃, air atmosphere again; 10 ℃/minute of temperature rise rates make magnetic nuclear NiFe
2O
4, obtaining powder uniformly with the standard sieve screening, all reaction solutions and bath water are the decarbonation deionized water.
(2) magnetic DS-LDHs/NiFe
2O
4
Weighing 8.76g Ni (NO
3)
26H
2O and 3.75g Al (NO
3)
39H
2O is mixed with the 50ml mixing salt solution; Weighing 4.00g NaOH is mixed with 50ml alkali lye in addition; The solution that the 2.88g sodium lauryl sulphate is mixed with 150ml places the four-hole boiling flask of 500ml, adds 0.75g magnetic nuclear simultaneously and makes Ni (NO
3)
26H
2O/NiFe
2O
4Mass ratio be 11.6; 45 ℃, N
2Under gas shiled and the stirring condition, mixing salt solution and alkaline solution are added drop-wise in the four-hole boiling flask simultaneously, the pH value maintains in 8.0 ± 0.3 scopes; 80 ℃ of crystallization 24 hours, centrifugal, wash to neutrality and surfactant-free; 65 ℃ of dryings 24 hours obtain DS-LDHs/NiFe
2O
4
Survey magnetic DS-LDHs/NiFe
2O
4The coercivity H value be 33kA/m, specific saturation magnetization σ
sBe 11.12AM
2/ Kg.All reaction solutions and bath water are the decarbonation deionized water.
Claims (2)
1. surfactant intercalated magnetic hydrotalcite material, its crystalline structure is the crystalline structure of houghite material, it is characterized in that: chemical formula is: (M
2+)
1-x(N
3+)
x(OH)
2(Surf)
a(B
N-)
bMH
2O/M ' Fe
2O
4, be a kind of organic and inorganic composite functional material with magnetic, wherein the quality percentage composition of tensio-active agent is 0～40%, specific saturation magnetization is 2～75AM
2/ Kg; Coercivity H is 0～400kA/m; (M wherein
2+)
1-x(N
3+)
x(OH)
2(Surf)
a(B
N-)
bMH
2O is for being coated on M ' Fe
2O
4Outer surfactant intercalated hydrotalcite; M ' Fe
2O
4Be magnetic species; Its quality percentage composition is: M ' Fe
2O
4: 5%～50%, Sul-LDHs:95%～50%; M wherein
2+Be divalent-metal ion Zn
2+, Mg
2+, Ni
2+, Cu
2+, Ca
2+, Mn
2+In any; N
3+Be trivalent metal ion Al
3+, Fe
3+, Cr
3+, Ga
3+In any; M ' is Co
2+, Mg
2+, Ba
2+, Ni
2+Wherein any of divalent-metal ion, M
2+Identical or different with M '; On behalf of interlayer, Surf bear monovalence tensio-active agent negatively charged ion; B
N-For carrying capacity is the inorganic anion of n, B in the Sul-LDHs chemical formula
N-Be CO
3 2-, NO
3 -, Cl
-, OH
-, H
2PO
4 -In any 1～3 kind or do not exist; X=N
3+/ (M
2++ N
3+), 0＜x＜1; A, b are respectively Surf, B
N-Quantity, and satisfy a+n * b=x, m is the crystallization water number, is any real number;
2. method for preparing the described surfactant intercalated magnetic hydrotalcite material of claim 1, adopt coprecipitation method to prepare nano-scale magnetic nuclear earlier, with this magnetic core and corresponding salt solution mix, tensio-active agent is assembled into hydrotalcite layers, obtains having the surfactant intercalated hydrotalcite of magnetic simultaneously; Concrete technology is:
A, nano-magnetic nuclear M ' Fe
2O
4Powder preparing
With M, soluble inorganic salt and two, ferric soluble inorganic salt be mixed with mixing solutions, wherein (M '+Fe
2+)/Fe
3+Mol ratio is 1～5, M '/Fe
2+Mol ratio is 0.5～2; The volumetric molar concentration of M ' is 0.1～2.5M, Fe
3+Volumetric molar concentration be 0.2～5.0M; Use the NaOH alkaline solution, wherein the NaOH volumetric molar concentration is 0.1～5.0M; Under nitrogen protection, alkali lye splashed in the salts solution to the pH value and equal 6～8; 15～60 ℃ of crystallization are 4～72 hours in water-bath; reaction solution is filtered; wash with water; use absolute ethanol washing again; vacuum-drying, grind to form powdery, obtain particle size range at the M ' of 200～800nm Fe through 800-1200 ℃ of high-temperature roasting
2O
4Powder obtains powder uniformly with the standard sieve screening; Wherein M ' is Co
2+, Mg
2+, Ba
2+, Ni
2+Wherein any of divalent-metal ion; All reaction solutions and bath water are all used the decarbonation deionized water;
The preparation of b, surfactant intercalated magnetic hydrotalcite
Step 1: solubility divalent metal salt, trivalent metal salt are pressed M
2+/ N
3+Be the mixing salt solution A that the mol ratio of 1-9 is made into, in addition with an amount of NaOH proportionaling alkali-forming solution B, the concentration of solution A, B is 0.0001-1mol/L, with tensio-active agent and magnetic core M ' Fe
2O
4Be configured to mixed solution C, wherein [N
3+]/[tensio-active agent] mol ratio be 1-3, the M salt/M ' Fe in the A solution
2O
4Mass ratio be 2～48; M wherein
2+Be Zn
2+, Mg
2+, Ni
2+, Cu
2+, Ca
2+, Mn
2+In any; N
3+Be Al
3+, Fe
3+, Cr
3+, Ga
3+In any; Soluble M
2+, N
3+The negatively charged ion of salt is NO
3 -, Cl
-, OH
-
Step 2: with the reaction vessel that solution C places band to stir, be simultaneously mixing salt solution A and alkaline solution B slowly to be added under the 0.001-1ml/s condition in titration speed, to the pH of gained slurries be that 6.5-11 stops, changing in the crystallizing kettle;
Perhaps above-mentioned solution A and solution C mixing being put into crystallizing kettle, is under the 0.001-1ml/s condition in titration speed, and solution B is splashed in the crystallizing kettle, obtains the slurries that pH is 6.5-11;
Step 3: in crystallizing kettle, use N
2Protection makes slurries crystallization 18～72 hours under 35-100 ℃ of temperature; Again through suction filtration, be washed to neutrality, 25-100 ℃ of drying 12～72 hours, obtain Sul-LDHs/M ' Fe
2O;
Reaction solution and bath wateies all in step 1～3 are all used the decarbonation deionized water.
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| JP4729213B2 (en) * | 2001-11-09 | 2011-07-20 | 戸田工業株式会社 | Li-Al layered double hydroxide particle powder and method for producing the same |
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|---|---|---|---|---|
| WO2010025630A1 (en) * | 2008-09-05 | 2010-03-11 | 北京化工大学 | Sodium cholate-included prednisone intercalated layered double hydroxides and preparation method thereof |
| CN101775277B (en) * | 2009-12-31 | 2012-07-11 | 北京化工大学 | Photosensitive composite film and preparation method thereof |
| CN105854747A (en) * | 2016-04-29 | 2016-08-17 | 南京工程学院 | Monodisperse melamine resin magnetic microsphere and preparation method thereof |
| CN105854747B (en) * | 2016-04-29 | 2019-02-15 | 南京工程学院 | A kind of monodisperse melamine resin magnetic microsphere and preparation method thereof |
| CN111215075A (en) * | 2018-11-25 | 2020-06-02 | 中国科学院大连化学物理研究所 | Catalyst for eliminating ethylene coupling nitrous oxide produced by oxidative dehydrogenation of ethane and preparation and application thereof |
| CN111215075B (en) * | 2018-11-25 | 2023-01-24 | 中国科学院大连化学物理研究所 | Catalyst for coupling elimination of nitrous oxide in preparation of ethylene through oxidative dehydrogenation of ethane and preparation and application thereof |
| CN110898796A (en) * | 2019-11-27 | 2020-03-24 | 清华大学深圳国际研究生院 | Preparation method of magnetic layered double hydroxide, magnetic layered double hydroxide and application thereof |
| CN113104872A (en) * | 2021-05-24 | 2021-07-13 | 北京化工大学 | Method for preparing organic molecule intercalation hydrotalcite array by one-step method |
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