CN1151224C - Selective infrared absorbing material of anionic laminated column structure and its preparing process - Google Patents
Selective infrared absorbing material of anionic laminated column structure and its preparing process Download PDFInfo
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- CN1151224C CN1151224C CNB001035517A CN00103551A CN1151224C CN 1151224 C CN1151224 C CN 1151224C CN B001035517 A CNB001035517 A CN B001035517A CN 00103551 A CN00103551 A CN 00103551A CN 1151224 C CN1151224 C CN 1151224C
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Abstract
The present invention relates to a selective infrared absorbing material of an anionic laminated column structure and a preparing method thereof. In the present invention, the material of an anionic laminated column structure ([M(II)1-xM(III)x(OH)2]Aa/nBb/nmH2O), which has favorable selective infrared absorption performance and adjustable selective infrared absorption range, is prepared by changing raw material sorts and adjusting raw material composition, concentration, proportion, crystallizing temperature, a solution pH value, crystallizing time, a feeding sequence, etc. according to the adjustable and changeable characteristic of the composition and the structure of the anionic laminated material and on the basis of an intercalation chemistry principle. The material has the characteristics of high selective infrared absorption performance, favorable crystal phase, uniform particle diameter distribution and controllable particle diameter size. Meanwhile, the preparing method of the present invention has the advantages of simple technology, little investment equipment, short production time, low energy consumption, no environment pollution and wide application range.
Description
The present invention relates to a kind of preparation method of selective infrared absorbing material of anionic laminated column structure.
At present, the infrared absorbing material that widely adopts in the plastic sheeting for farm use is mainly natural inorganic products such as talcum powder both at home and abroad, performances such as its infrared absorption effect (heat retaining property of film) and visible light transmissivity can't be taken into account, the talcum powder addition is few, infrared absorption effect (heat retaining property of film) is poor, addition is big, then causes the transmitance that reduces visible light significantly.
Negatively charged ion stratiform structured material has become emerging in the world research focus in recent years, and its chemical constitution of anion laminated material is [M
2+ 1-xM
3+ x(OH)
2] A
N- X/nMH
2O, wherein: M
2+And M
3+Be divalence and trivalent metal ion, A
N-Be n valency negative ion, its most typical constitutional features is: the vertical ordered arrangement of the two-dimentional laminate of nanometer scale forms three-dimensional crystalline structure, is covalent bonding between atom in the laminate, and interlayer is weak chemical bond, as ionic linkage, hydrogen bond.The laminate skeleton has positive charge, and interlayer is an opposite charges ion balance with it, and integral body is electric neutrality, and interlayer ion has interchangeability, and interlamellar spacing varies in size with interlayer ion and is regular and changes.Laminate chemical constitution, interlayer ion kind and quantity, interlamellar spacing etc. all can change with design requirements, therefore can show different and various physicochemical property, make it be widely used in (seeing Cavani et al. " Catal.Today " in the industries such as petrochemical complex, medicine, agricultural, 1997,11:173).Because this material has the infrared absorption performance in 7-14 mum wavelength (this is the heat radiation infra-red range) scope, can be used as selective infrared absorbing material, substitutes traditional heat preserving agent, is used for plastic sheeting for farm use etc., improves heat insulation effect.
But said structure ([M
2+ 1-xM
3+ x(OH)
2] A
N- X/nMH
2O) anion laminated material exists infrared absorbance range to fix and have defective and the low weakness of infrared absorption performance in the selectivity infrared absorbance range in 7-14 mum wavelength scope, has limited the widespread use of this inorganic non-metallic crystalline material.
Purpose of the present invention: the preparation method that a kind of selective infrared absorbing material of anionic laminated column structure is provided, make its more traditional infrared absorbing material in 7-14 mum wavelength scope, has the adjustable sex change energy of higher selectivity infrared absorption performance and selectivity infrared absorption, to be fit to different working conditionss.
Invention main points of the present invention:
A kind of selective infrared absorbing material of anionic laminated column structure, its chemical constitution and structure are:
[M (II)
1-xM (III)
x(OH)
2] A
N1- A/nB
N2- B/nMH
2O, wherein M (II) is a divalent-metal ion, M (III) is a trivalent metal ion, A
N1-And B
N2-Be different negatively charged ion or anionic group, n1, n2=1-3, a+b=x, 0＜a/b≤1,0.15≤x≤0.5, m is generally 1-20.It is a layer pole structure, and laminate is the oxyhydroxide of M (II) and M (III), and the interlayer support post is A
N1-And B
N2-
Above-mentioned divalent-metal ion M (II) is Mg
2+Zn
2+Cu
2+Ni
2+Fe
2+Mn
2+Ca
2+In any, trivalent metal ion M (III) is Al
3+Cr
3+Fe
3+V
3+Co
3+Ga
3+Ti
3+In any, A
N1-Be Cl
-CO
3 2-NO
3 -In any, B
N2-Be F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the organic sulfonic acid negatively charged ion.
The preparation method of above-mentioned selective infrared absorbing material of anionic laminated column structure, concrete steps are:
A: solubility divalence inorganic metal salt and solubility trivalent inorganic metal salt are mixed with mixing salt solution, and the volumetric molar concentration of divalent-metal ion is 0.2-2.5M, and the concentration of trivalent metal ion is 0.1-1.25M;
B: the mixing salt solution in the steps A is mixed with alkaline solution, obtain the slurries of pH value, have a kind of A of containing at least in two kinds of salt of steps A or the step B alkaline solution for 8.5-13
N1-
C: step B gained slurries are stirred crystallization down after 2-24 hour at 70-120 ℃; Add and contain B
N2-Acid solution, regulating pH value be 4.5-7.5, stirs 2-10 hour, filters then, washs, drying collection product.
Alkaline solution among the step B is preferably any or their mixing solutions in sodium hydroxide, ammoniacal liquor, yellow soda ash, the urea.
The present invention is according to the adjustable sex change characteristics of anion layer rod structure material The Nomenclature Composition and Structure of Complexes, utilize the intercalation chemistry principle, by changing raw material type and regulating raw material and form, concentration, ratio, crystallization temperature, the pH value of solution value, crystallization time, method assembles such as order of addition(of ingredients) have the anion layer column material of fine selectivity infrared absorption performance, material grains is evenly distributed and is tiny, compare with traditional anion laminated material, the prepared highly selective infrared absorption anion layer column material of the present invention has advantages such as higher selectivity infrared absorption performance and the scope of application is extensive.Preparation method's technology of the present invention is simple simultaneously, facility investment is few, the production time is short, energy consumption is low, non-environmental-pollution.Technology provided by the invention also can be used for the selective infrared absorbing material of anionic laminated column structure of synthetic different The Nomenclature Composition and Structure of Complexes.
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1: Mg
4Al
2(OH)
12CO
3MH
2The infrared absorption spectra of O
Fig. 2: Mg
4Al
2(OH)
12(CO
3)
0.4(SO
4)
0.6MH
2The infrared absorption spectra of O (embodiment 1)
Embodiment 1: magnalium-carbonate and sulfate anion pillared material synthetic
Choose 1.6 mol sulfuric acid magnesium and 0.8 mol sulfuric acid aluminium is made into 1 liter of salts solution, get 4.8 moles of NaOH and 2.5 moles of Na
2CO
3Be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=11.0, mixed serum adds sulfuric acid to slurries pH=7 100 ℃ of crystallization 4 hours, and crystallization is 2 hours again, filter, washing, drying, the product that obtains is Mg
4Al
2(OH)
12(CO
3)
0.4(SO
4)
0.6MH
2O.The product crystal phase structure is good, particle diameter 0.2 μ, and greater than 99%, ir-absorbance is greater than 85% for particle distribution (particle diameter=0.2 μ).
Embodiment 2: zinc-aluminium-carbonate and sulfate anion pillared material synthetic
Choose 1.0 mol sulfuric acid zinc and 0.5 mol sulfuric acid aluminium is made into 1 liter of salts solution, get 4 moles of NaOH and 1.5 moles of Na
2CO
3Be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=10.0, mixed serum adds sulfuric acid to slurries pH=6.8 80 ℃ of crystallization times 20 hours, and crystallization is 12 hours again, filters washing, drying.The product that obtains is Zn
4Al
2(OH)
12(CO
3)
0.5(SO
4)
0.5MH
2O.The product crystal phase structure is good, particle diameter 0.3 μ, and greater than 99%, ir-absorbance is greater than 85% for particle distribution (particle diameter=0.3 μ).
Embodiment 3: cobalt aluminium-nitrate radical and sulfate anion pillared material synthetic
Choose 1.2 molar nitric acid cobalts and 0.4 aluminum nitrate that rubs and be made into 1 liter of salts solution, get 3.5 moles of NaOH and be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=9.5, mixed serum 140 ℃ of crystallization times 6 hours, is added sulfuric acid to slurries pH=6.5, and crystallization is 4 hours again, filter washing, drying.The product that obtains is Co
6Al
2(OH)
16(NO
3)
0.2(SO
4)
0.8MH
2O.The product crystal phase structure is good, particle diameter 0.3 μ, and greater than 99%, ir-absorbance is greater than 90% for particle distribution (particle diameter=0.3 μ)
Embodiment 4: nickel aluminium-nitrate radical and azochlorosulfonate acid anion pillared material synthetic
Choose 2.2 molar nitric acid nickel and 1.1 molar nitric acid aluminium are made into 1 liter of salts solution, get 8.5 moles of NaOH and be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=9, mixed serum 100 ℃ of crystallization times 6 hours, is added sulfonic acid to slurries pH=6.7, and crystallization is 4 hours again, filter washing, drying.The product that obtains is Ni
4Al
2(OH)
12(NO
3)
0.4(A)
0.6MH
2O, A are sulfonate radical.The product crystal phase structure is good, particle diameter 0.3 μ, and greater than 99%, ir-absorbance is greater than 90% for particle distribution (particle diameter=0.3 μ).
Embodiment 5: manganese aluminium-nitrate radical and Phenylsulfonic acid root anion layer column material synthetic
Choose 1.6 molar nitric acid manganese and 0.8 molar nitric acid aluminium is made into 1 liter of salts solution, get 9 moles of NaOH and be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=9, mixed serum 80 ℃ of crystallization times 24 hours, is added Phenylsulfonic acid to slurries pH=5.0, and crystallization is 2 hours again, filter washing, drying.The product that obtains is Mn
4Al
2(OH)
12(NO
3)
0.1(B)
0.9MH
2O, B are the Phenylsulfonic acid root.The product crystal phase structure is good, particle diameter 0.3 μ, and greater than 99%, ir-absorbance is greater than 90% for particle distribution (particle diameter=0.3 μ).
Embodiment 6: zinc-magnesium aluminium-carbonate and sulfate anion pillared material synthetic
Choose 0.8 mole of magnesium chloride and 0.8 mole of zinc chloride (mole of magnesium and zinc form can at 0-1 scope modulation) and 0.8 mole of aluminum chloride and be made into 1 liter of salts solution, get 4.8 moles of NaOH and 1.2 moles of Na
2CO
3Be made into 1 liter of alkaline solution, two solution are mixed, mixed serum pH=12 100 ℃ of crystallization times 4 hours, adds sulfuric acid to slurries pH=7 with mixed serum, and crystallization is 4 hours again, filters washing, drying.The product that obtains is Mg
2Zn
2Al
2(OH)
12(NO
3)
0.3(SO
4)
0.7MH
2O.The product crystal phase structure is good, particle diameter 0.3 μ, and greater than 99%, ir-absorbance is greater than 85% for particle distribution (particle diameter=0.3 μ).
Claims (3)
1. the preparation method of a selective infrared absorbing material of anionic laminated column structure, its chemical constitution of said selective infrared absorbing material of anionic laminated column structure and structure are:
[M (II)
1-xM (III)
x(OH)
2] A
N1- A/nB
N2- B/nMH
2O, wherein M (II) is a divalent-metal ion, M (III) is a trivalent metal ion, A
N1-And B
N2-Be different negatively charged ion or anionic group, n1, n2=1-3, a+b=x, 0＜a/b≤1,0.15≤x≤0.5, m=1-20, it is a layer pole structure, and laminate is the oxyhydroxide of M (II) and M (III), and the interlayer support post is A
N1-And B
N2-
Concrete steps are:
A: solubility divalence inorganic metal salt and solubility trivalent inorganic metal salt are mixed with mixing salt solution, and the volumetric molar concentration of divalent-metal ion is 0.2-2.5M, and the volumetric molar concentration of trivalent metal ion is 0.1-1.25M;
B: mixing salt solution in the steps A is mixed with alkaline solution, obtain the slurries of pH value, have a kind of A of containing at least in two kinds of salt of steps A or the step B alkaline solution for 8.5-13
N1-
C: descend stirring after 2-24 hour at 70-120 ℃ in step B gained slurries; Add and contain B
N2-Acid solution, regulating pH value be 4.5-7.5, stirs 2-10 hour, filters then, washs, drying collection product.
2. according to the preparation method of claim 1, it is characterized in that: M (II) is Mg
2+Zn
2+Cu
2+Ni
2+Fe
2+Mn
2+Ca
2+In any, M (III) is Al
3+Cr
3+Fe
3+V
3+Co
3+Ga
3+Ti
3+In any, A
N1-Be Cl
-CO
3 2-NO
3 -In any, B
N2-Be F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the organic sulfonic acid negatively charged ion.
3. according to the preparation method of claim 1 or 2, it is characterized in that: the alkaline solution among the step B is any or their mixing solutions in sodium hydroxide, ammoniacal liquor, yellow soda ash, the urea.
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|---|---|---|---|
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|---|---|---|---|
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|---|---|
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| CN1151224C true CN1151224C (en) | 2004-05-26 |
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|---|---|---|---|---|
| CN100365093C (en) * | 2005-10-25 | 2008-01-30 | 上海师范大学 | Infrared absorbing material and its prepn |
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Granted publication date: 20040526 |