CN1358691A - All return mixing-liquid film reactor and use in prepairng ultrafine anion layer shape material - Google Patents
All return mixing-liquid film reactor and use in prepairng ultrafine anion layer shape material Download PDFInfo
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Abstract
The present invention relates to an all return mixing-liquid membrane reactor and its application in preparation of ultrafine anionic laminer material. In said invention, an all return mixing liquid membrane reactor is designed according to basic process for preparing anionic laminar material by coprecipitation method and utilizing the principle of crystal chemistry, in which the forced micromixing technique is adopted to make two liquid reactants quickly fully mix and contact in the gap between the rotor and stator of reactor, after reaction said material can be quickly separated from reactor to implement simultaneous nucleation and synchronous growth of particles so as to make the material possess the characteristics of small particle size and uniform distribution, its particle size can be up to 10-100 nm.
Description
The present invention relates to a kind of full back-mixing liquid film reactor and the application in the preparation super fine anion laminated material thereof.
The 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, negatively charged ion stratiform structured material has become emerging in the world research focus in recent years.When the grain-size of above-mentioned materials little when certain size becomes ultra-fine (nano level) anion laminated material, can make the variation of the performance generation essence of material, so that break through, show the many and general distinct performance of material, such as high strength, high rigidity and ceramic superplasticity etc.The property that has just because of this material makes it be used widely at aspects such as petrochemical complex, matrix material, agricultural, military affairs.
As anion laminated material the most frequently used preparation method-salts solution and alkaline solution coprecipitation method (sol-gel method), institute's employing equipment also is conventional tank reactor, because salt is realized with the mode of mixing by stirring of alkali in reactor, mix very insufficient, reaction interface is little, exist concentration gradient, speed of response and velocity of diffusion slow, therefore earlier form new precipitation particles on the sedimentary particle, exist in the time of new and old particle, cause particle size distribution extremely inhomogeneous.Make the size of particles of synthetic materials and all disperse performance to be subjected to very big influence, its crystalline size also is difficult to reach nanometer scale, has greatly limited the application of this type of material.
Purpose of the present invention: formulate a kind of full back-mixing liquid film reactor, and use it in the preparation super fine anion laminated material, thereby a kind of novel method for preparing super fine anion laminated material is provided.Make that reactant makes its synchronous nucleation at the moment thorough mixing in the coprecipitation reaction, reach into the homogeneity of nuclear particle,, make crystal grain reach nanometer scale, and crystal grain is evenly distributed in conjunction with the temperature programmed control dynamic crystallization.
Main points of the present invention: a kind of full back-mixing liquid film reactor that is used for liquid-liquid two-phase coprecipitation reaction, by one the sealing casing as stator, one rotatable cone-shaped rotor is arranged in the stator, the outside surface of rotor and inner surface of stator have groove respectively, stator is provided with raw material fluid inlet and discharge port, fluid inlet is positioned at the long-pending little end of rotor cross-section, and discharge port is positioned at the long-pending big end of rotor cross-section, and the end that cross-sectional area is little on the rotor has liquid distributor.Leave the slit that can regulate size between stator inner surface and the rotor outer surface, gap size can be by variation modulation between the 1-20 micron of rotor and stator relative position.
Rotor is cone-shaped, and its tapering (angle on hypotenuse and base on the longitudinal cross-section) is the 50-70 degree, and the inner chamber of stator is identical with the rotor tapering cone-shaped.The outside surface of rotor is identical with groove shapes, number on the inner surface of stator, can for radially, multiple arrangement such as inclination, the groove of stator inner surface shape in the shape of a spiral preferably, the groove of rotor outer surface is rightabout spirrillum.
Above-mentioned reactor can be used for liquid-liquid coprecipitation method and prepare super fine anion laminated material, and its concrete steps are:
A: solubility divalence inorganic metal salt and solubility trivalent inorganic metal salt are mixed with mixing salt solution, the mol ratio of divalent-metal ion and trivalent metal ion is 1-4.5, 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 and alkaline solution are added respectively in the reactor of claim 1 or 2 simultaneously, and after liquid distributor disperseed, place, the slit thorough mixing between rotor and stator was discharged to crystallizing kettle through discharge port; The rotating speed of control rotor is 1000-8000rpm, and the flow of discharge port is 100-1000kg/h, the consumption of alkaline solution with salt solution mix after pH at 8.5-13 for suitable;
C: the mixed serum in the crystallizing kettle stirs under 70-180 ℃, crystallization 2-24h, with the material after the crystallization after filtration, wash, be drying to obtain anion laminated material.
The described solubility divalent metal salt of steps A is Mg
2+Zn
2+Cu
2+Ni
2+Fe
2+Mn
2+Ca
2+With Cl
-CO
3 2-NO
3 -B
N2-F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the soluble salt that the organic sulfonic acid negatively charged ion is formed; The solubility trivalent metal salt is Al
3+Cr
3+Fe
3+V
3+Co
3+Ga
3+Ti
3+With Cl
-CO
3 2-NO
3 -B
N2-F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the soluble salt that the organic sulfonic acid negatively charged ion is formed; Alkaline solution among the step B is any or their mixing solutions in sodium hydroxide, ammoniacal liquor, yellow soda ash, the urea.
Effect of the present invention: the present invention prepares the basic technology of anion laminated material from coprecipitation method, utilize the crystal chemistry principle, designed a kind of full back-mixing liquid film reactor, adopt and force the microcosmic hybrid technology, nucleation and crystallization are separated, make reactant rapid thorough mixing in reactor, reaction back material hightails reactor, nucleation, synchronous growth when realizing particle, thus make material have the characteristic that size of particles is little and be evenly distributed, and the size of particle can reach 10-100nm.
The invention will be further described below in conjunction with drawings and Examples:
Fig. 1: the structural representation of the full back-mixing liquid film reactor of the present invention
Fig. 2: liquid distributor sectional view
Fig. 3: rotor plane is launched synoptic diagram
Fig. 1 is the structural representation of the full back-mixing liquid film reactor of the present invention, and rotor 4 is one to be installed in the cone on the motor shaft 7, and tapering α is the 50-70 degree, be 60 degree among Fig. 1, its outside surface has helical groove, and Fig. 1 further groove cross section is a rectangle, groove width is 1-5 with the groove depth ratio: 1, and be 4: 1 among Fig. 1; The spiral fluted number is 2-3 with the ratio of the cms of the large section one end diameter of rotor: 1, and among Fig. 1 3-1.Stator 3 is a right cylinder that inner chamber is a cone, and its internal surface has and the reciprocal helical groove of rotor, and the number of groove, shape are identical with rotor.As can be seen from Figure 1 stator 3 is by the slit between screw thread 5 adjustings and the rotor, and the adjustable extent in slit is the 1-20 micron.As can be seen from Figure 2 liquid distributor is the disk that has 4 rectangular paddle 8, is connected with rotor by pin 9.
When above-mentioned reactor is used for the preparation of anion laminated material, the mixing salt solution that solubility divalence inorganic metal salt and solubility trivalent inorganic metal salt are formed and alkaline solution pass through two opening for feeds 1 on the stator 3 respectively behind liquid distributor 2, place, slit thorough mixing between rotor 4 and stator 3 is discharged to crystallizing kettle through discharge port 6.Embodiment 1: magnalium-carbonate anion stratified material synthetic
Choose 1.6 mole of magnesium chloride and 0.4 mol sulfuric acid aluminium is made into 1 liter of solution, get 3.8 moles of NaOH and 1.6 moles of Na
2CO
3Be made into 1 liter solution, two solution are mixed reactor slit 11 μ m in full back-mixing liquid film reactor, rotor speed is 3000r/min, and discharge port place liquid flow rate is 500kg/h, mixed serum pH=11.0, mix rear slurry in 100 ℃ of crystallization 6 hours, filtration, washing, drying.
The product crystal phase structure is good, average particle diameter 0.1 μ m, particle distribution D
90(90% particle) is less than 0.12 μ m.Embodiment 2: zinc-aluminium-carbonate anion stratified material synthetic
Choose 1.6 mol sulfuric acid zinc and 0.2 mol sulfuric acid aluminium, get 4.2 moles of NaOH and 1.6 moles of Na
2CO
3Be made into 1 liter of solution, two solution are mixed reactor slit 8 μ m in full back-mixing liquid film reactor, rotor speed 1500r/min, discharge port place liquid flow rate is 200kg/h, mixed serum pH=10.5, mixed serum filters 100 ℃ of crystallization 4 hours, washing, drying.
The product crystal phase structure is good, average particle diameter 0.08 μ m, particle distribution D
90Less than 0.1 μ m.Embodiment 3: cobalt aluminium-nitrate anion stratified material synthetic
Choose 1.6 molar nitric acid cobalts and 0.4 aluminum nitrate that rubs and be made into 1 liter of solution, get 5.0 moles of NaOH and be made into 1 liter of solution, two solution are mixed in full back-mixing liquid film reactor, reactor slit 10 μ m, rotor speed 4000r/min, discharge port place liquid flow rate is 700kg/h, mixed serum pH=9.5, mixed serum filters 100 ℃ of crystallization 6 hours, washing, drying.
The product crystal phase structure is good, average particle diameter 0.13 μ m, particle distribution D
90Less than 0.15 μ m.Embodiment 4: nickel aluminium-carbonate anion stratified material synthetic
Choose 1.6 molar nitric acid nickel and 0.4 molar nitric acid aluminium is made into 1 liter of solution, get 3.5 moles of NaOH and 1.6 moles of Na
2CO
3Be made into 1 liter of solution, two solution are mixed reactor slit 16 μ m in full back-mixing liquid film reactor, rotor speed 9000r/min, the liquid flow rate 900kg/h of discharge port place, mixed serum pH=9.0, mixed serum filters 100 ℃ of crystallization 8 hours, washing, drying.
The product crystal phase structure is good, average particle diameter 0.2 μ m, particle distribution D
90Less than 0.25 μ m.Embodiment 5: manganese aluminium-nitrate anion stratified material synthetic
Choose 1.6 molar nitric acid manganese and 0.4 molar nitric acid aluminium is made into 1 liter of solution, get 4.8 moles of NaOH and be made into 1 liter of solution, two solution are mixed in full back-mixing liquid film reactor, reactor slit 5 μ m, rotor speed 2000r/min, discharge port place liquid flow rate is 300kg/h, mixed serum pH=10.0, mixed serum filters 100 ℃ of crystallization 6 hours, washing, drying.
The product crystal phase structure is good, average particle diameter 0.07 μ m, particle distribution D
90Less than 0.11 μ m.Embodiment 6: zinc-magnesium aluminium-carbonate anion stratified material synthetic
Choose 0.8 mol sulfuric acid magnesium and 0.4 mol sulfuric acid zinc and 0.2 mol sulfuric acid aluminium and be made into 1 liter of solution, get 40.5 moles of NaOH and 2.0 moles of Na
2CO
3Be made into 1 liter of solution, two solution are mixed reactor slit 12 μ m in full back-mixing liquid film reactor, rotor is pass on fast 3500r/min, the liquid flow rate 450kg/h of discharge port place, mixed serum pH=10.5, mixed serum filters 100 ℃ of crystallization 5 hours, washing, drying.
The product crystal phase structure is good, average particle diameter 0.09 μ m, particle distribution D
90Less than 0.11 μ m.
Claims (4)
1. full back-mixing liquid film reactor that is used for liquid-liquid two-phase coprecipitation reaction, by one the sealing casing as stator, one rotatable cone-shaped rotor is arranged in the stator, the outside surface of rotor and inner surface of stator have groove respectively, the long-pending little end of rotor cross-section has liquid distributor, stator is provided with raw material fluid inlet and discharge port, fluid inlet is positioned at the long-pending little end of rotor cross-section, discharge port is positioned at the long-pending big end of rotor cross-section, it is characterized in that: leave the slit that can regulate size between stator inner surface and the rotor outer surface, gap size can be by variation modulation between the 1-20 micron of rotor and stator relative position.
2. according to the reactor of claim 1, it is characterized in that: the tapering of rotor is the 50-70 degree, the inner chamber of stator is identical with the rotor tapering cone-shaped, the groove of stator inner surface is shape in the shape of a spiral, the groove of rotor outer surface and the groove shapes of stator, number are identical, but be rightabout spirrillum, the groove width of groove is 1-5 with the groove depth ratio: 1, and the number of supratrochlear depression groove is 2-3 with the ratio of the cms of the maximum diameter of rotor: 1.
3. a method of utilizing the reactor made super fine anion laminated material of claim 1 or 2 adopts the coprecipitated method of deciding, and concrete steps are:
A: solubility divalence inorganic metal salt and solubility trivalent inorganic metal salt are mixed with mixing salt solution, the mol ratio of divalent-metal ion and trivalent metal ion is 1-4.5, 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 and alkaline solution are added respectively in the reactor of claim 1 or 2 simultaneously, and after liquid distributor disperseed, place, the slit thorough mixing between rotor and stator was discharged to crystallizing kettle through discharge port; The rotating speed of control rotor is 1000-8000rpm, and the flow of discharge port is 100-1000kg/h, the consumption of alkaline solution with salt solution mix after pH at 8.5-13 for suitable;
C: the mixed serum in the crystallizing kettle stirs under 70-180 ℃, crystallization 2-24h, with the material after the crystallization after filtration, wash, be drying to obtain anion laminated material.
4. according to the method for claim 3, it is characterized in that: the described solubility divalent metal salt of steps A is Mg
2+Zn
2+Cu
2+Ni
2+Fe
2+Mn
2+Ca
2+With Cl
-CO
3 2-NO
3 -B
N2-F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the soluble salt that the organic sulfonic acid negatively charged ion is formed; The solubility trivalent metal salt is Al
3+Cr
3+Fe
3+V
3+Co
3+Ga
3+Ti
3+With Cl
-CO
3 2-NO
3 -B
N2-F
-Br
-I
-SO
4 2-ClO
3 -OH
-H
2PO
4 -WO
4 2-Any in the soluble salt that the organic sulfonic acid negatively charged ion is formed; 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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