CN114621771A - Preparation method of phytic acid modified magnalium hydrotalcite/montmorillonite nano material - Google Patents
Preparation method of phytic acid modified magnalium hydrotalcite/montmorillonite nano material Download PDFInfo
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- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052901 montmorillonite Inorganic materials 0.000 title claims abstract description 22
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 20
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 20
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 9
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 title abstract description 7
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 title abstract description 7
- 229940068041 phytic acid Drugs 0.000 title abstract description 7
- 235000002949 phytic acid Nutrition 0.000 title abstract description 7
- 239000000467 phytic acid Substances 0.000 title abstract description 7
- 229910001051 Magnalium Inorganic materials 0.000 title abstract description 3
- 229910020068 MgAl Inorganic materials 0.000 claims abstract description 88
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000000243 solution Substances 0.000 claims description 40
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 238000003756 stirring Methods 0.000 claims description 30
- 238000005303 weighing Methods 0.000 claims description 30
- FENRSEGZMITUEF-ATTCVCFYSA-E [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].OP(=O)([O-])O[C@@H]1[C@@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H](OP(=O)([O-])[O-])[C@H](OP(=O)(O)[O-])[C@H]1OP(=O)([O-])[O-] FENRSEGZMITUEF-ATTCVCFYSA-E 0.000 claims description 24
- 230000007935 neutral effect Effects 0.000 claims description 24
- 229940083982 sodium phytate Drugs 0.000 claims description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 16
- 239000004202 carbamide Substances 0.000 claims description 16
- MFUVDXOKPBAHMC-UHFFFAOYSA-N magnesium;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MFUVDXOKPBAHMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 16
- 239000002131 composite material Substances 0.000 claims description 12
- 230000002378 acidificating effect Effects 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- XNDZQQSKSQTQQD-UHFFFAOYSA-N 3-methylcyclohex-2-en-1-ol Chemical compound CC1=CC(O)CCC1 XNDZQQSKSQTQQD-UHFFFAOYSA-N 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 8
- 239000002184 metal Substances 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- 239000002243 precursor Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- GANNOFFDYMSBSZ-UHFFFAOYSA-N [AlH3].[Mg] Chemical class [AlH3].[Mg] GANNOFFDYMSBSZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005119 centrifugation Methods 0.000 claims description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003063 flame retardant Substances 0.000 abstract description 11
- 239000000779 smoke Substances 0.000 abstract description 11
- 239000010985 leather Substances 0.000 abstract description 10
- 239000011159 matrix material Substances 0.000 abstract description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 3
- 239000011574 phosphorus Substances 0.000 abstract description 3
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 abstract 3
- 238000012986 modification Methods 0.000 abstract 1
- 230000004048 modification Effects 0.000 abstract 1
- 239000011347 resin Substances 0.000 abstract 1
- 229920005989 resin Polymers 0.000 abstract 1
- 230000002195 synergetic effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 230000001629 suppression Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 229910003023 Mg-Al Inorganic materials 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000003763 carbonization Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000008408 compound extracted from plant Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K21/00—Fireproofing materials
- C09K21/02—Inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C14—SKINS; HIDES; PELTS; LEATHER
- C14C—CHEMICAL TREATMENT OF HIDES, SKINS OR LEATHER, e.g. TANNING, IMPREGNATING, FINISHING; APPARATUS THEREFOR; COMPOSITIONS FOR TANNING
- C14C9/00—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes
- C14C9/02—Impregnating leather for preserving, waterproofing, making resistant to heat or similar purposes using fatty or oily materials, e.g. fat liquoring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a preparation method of a phytic acid modified magnalium hydrotalcite/montmorillonite nano material. The method is characterized in that phytic acid from a biological source is adopted to perform surface modification on magnesium-aluminum hydrotalcite/montmorillonite prepared in the application number of CN202011524847.1, a phosphorus source in the phytic acid and the magnesium-aluminum hydrotalcite/montmorillonite are used for realizing synergistic flame retardance, the flame retardance of the magnesium-aluminum hydrotalcite/montmorillonite can be further improved, MgAl LDH-PA/MMT is added into an organic matrix as a flame-retardant smoke suppressant, and the flame-retardant smoke suppressant is applied to multiple fields of leather, resin, transportation and the like to endow the organic matrix with good flame-retardant and smoke-suppressant performances.
Description
Technical Field
The invention relates to a preparation method of a plant acid modified magnesium aluminum hydrotalcite/montmorillonite nano material.
Background
Alumina and magnesia formed by MgAl LDH in the combustion process have adsorbability to smoke and can be used as smoke suppressants, but the MgAl LDH is easy to agglomerate when being used independently; MMT is a layered silicate which forms SiO during combustion2The physical barrier has good flame resistance, the MMT is stripped, then MgAl LDH grows on the surface of the MMT, and finally the obtained MgAl LDH/MMT has certain flame resistanceThe flame retardance and smoke suppression of the flame-retardant and smoke-suppression composite material are still to be improved, and the flame retardance and smoke suppression of the flame-retardant and smoke-suppression composite material can be further improved by modifying the flame-retardant and smoke-suppression composite material with a phosphorus-containing environment-friendly flame retardant through catalytic carbonization.
PA, also known as phytic acid, having the molecular formula C6H18O24P6Is an organic phosphorus compound extracted from plant seeds. Because of containing phosphorus, the material can be used as an acid source of a flame retardant material in a combustion process and can be catalyzed into carbon, and the material is used in the field of flame retardance. Researchers intercalate PA between LDH layers by a coprecipitation method and apply the PA to polypropylene, and the result proves that the PA modified LDH has good flame retardance and char formation (Kalali E N, Montes A, Wang X, et al. Effect of polymeric acid-modified layered double hydroxide on a flat graphite and mechanical properties of an internal flame retardant polymeric system [ J].Fire and Materials,2018,42.)。
The difference of the patent in preparation method from other methods is that the MgAl LDH-PA/MMT is that on the basis of the earlier patent application, PA is loaded on the MgAl LDH/MMT by utilizing the adsorption effect of PA and MgAl LDH/MMT, and the obtained MgAl LDH-PA/MMT can be applied to a plurality of fields of leather, plastics, electronic devices, transportation and the like, and has good flame-retardant and smoke-suppression performance.
Disclosure of Invention
The invention aims to provide a preparation method of MgAl LDH-PA/MMT, and the material can further improve the flame retardance and smoke suppression of a matrix on the basis of the MgAl LDH/MMT and has good application prospect.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of MgAl LDH-PA/MMT comprises the following steps,
the following quantities are in parts by mass:
the method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in the patent (CN202011524847.1), 0.50-2.00 parts of MMT is weighed and mixed with 20-80mL of nitric acid aqueous solution, stirred for 4h at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain the acid-etched MMT. Weighing 1.50-4.50 parts of magnesium nitrate hexahydrate, 0.50-2.00 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT obtained after centrifugation in the step one with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and simultaneously fully dispersing the mixed solution in the ultrasonic process; weighing 2.00-4.50 parts of urea, adding into the mixed solution, stirring uniformly at room temperature, transferring to a hydrothermal reaction kettle, and reacting for 15h at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.1-0.5g of sodium phytate, dissolving with deionized water, dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value to 2-5 for later use.
Step three: weighing 0.80-1.60 parts of MgAl LDH/MMT, preparing 30-40mL of suspension by using deionized water, stirring for 20-50min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 3-6h at 70 ℃, and centrifuging until the supernatant is neutral to obtain the MgAl LDH-PA/MMT.
In the second step, the concentration of the dilute hydrochloric acid is 0.1 mol/L.
In the third step, the mass ratio of MgAl LDH/MMT to sodium phytate is 4: 1.
in step three, the final reaction temperature was 70 ℃.
The MgAl LDH-PA/MMT composite material is prepared according to the preparation method.
Drawings
FIG. 1 is an FTIR spectra of MgAl LDH/MMT and MgAl LDH-PA/MMT;
fig. 2 is an SEM photograph: (a) MgAl LDH/MMT; (b) MgAl LDH-PA/MMT; (c) EDS photographs of- (d) MgAl LDH-PA/MMT.
Compared with the prior art, the invention has the beneficial effects that:
by controlling the pH value of the sodium phytate solution, PA can fully occupy the active sites of MgAl LDH/MMT, and the PA is adsorbed to the surface of the MgAl LDH/MMT by utilizing the hydrogen bond and the electrostatic force between the PA and the MgAl LDH/MMT, so that the MgAl LDH-PA/MMT is obtained. The MgAl LDH-PA/MMT prepared by the method further improves the flame retardance and smoke suppression performance on the basis of the MgAl LDH/MMT.
The MgAl LDH-PA/MMT is introduced into the leather fatting agent and applied to leather fatting, and compared with the fatted crust leather without adding a flame-retardant material, the oxygen index of the fatted crust leather added with the MgAl LDH-PA/MMT can be improved from 23.5% to 29.5%; when the method is used for cone calorimetric detection, the total heat release amount is reduced by 62% compared with that of fatliquoring crust leather with a simple fatliquoring agent, and is reduced by 37% compared with that of MgAl LDH/MMT/fatliquoring crust leather; the maximum smoke yield is reduced by 75% compared with the greasing crust leather of a simple fatliquor and reduced by 53% compared with the greasing crust leather of MgAl LDH/MMT/the greasing agent. Therefore, the MgAl LDH-PA/MMT is added into the matrix, and the matrix can be endowed with better flame retardance, heat insulation and smoke suppression.
Detailed Description
The present invention is described in detail below with reference to examples, which are provided for further illustration of the present invention and are not to be construed as limiting the scope of the present invention.
The invention relates to a preparation method of MgAl LDH-PA/MMT, which is characterized in that on the basis of a patent of Mg-Al hydrotalcite modified montmorillonite nano material and a preparation method thereof (application number: CN202011524847.1), the flame retardance and smoke suppression of the MgAl LDH/MMT are further improved by modifying the MgAl LDH/MMT with the PA from a biological base. The preparation method comprises the following steps: (the raw materials are in parts by mass)
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in the patent (CN202011524847.1), 0.50-2.00 parts of MMT is weighed and mixed with 20-80mL of nitric acid aqueous solution, stirred for 4h at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain the acid-etched MMT. Weighing 1.50-4.50 parts of magnesium nitrate hexahydrate, 0.50-2.00 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT obtained after centrifugation in the step one with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and simultaneously fully dispersing the mixed solution in the ultrasonic process; weighing 2.00-4.50 parts of urea, adding into the mixed solution, stirring uniformly at room temperature, transferring into a hydrothermal reaction kettle, and reacting for 15h at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.1-0.5g of sodium phytate, dissolving with deionized water, dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value to 2-5 for later use.
Step three: weighing 0.80-1.60 parts of MgAl LDH/MMT, preparing 30-40mL of suspension by using deionized water, stirring for 20-50min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 3-6h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
In the second step, the concentration of the dilute hydrochloric acid is 0.10 mol/L.
In the third step, the mass ratio of MgAl LDH/MMT to sodium phytate is 4: 1.
in step three, the final reaction temperature was 70 ℃.
Example 1
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in patent (CN202011524847.1), 0.60 part of MMT is weighed and mixed with 50mL of nitric acid aqueous solution, stirred for 4 hours at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain acid-etched MMT. Weighing 1.80 parts of magnesium nitrate hexahydrate, 0.75 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT centrifuged in the step I with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and fully dispersing the mixed solution in an ultrasonic process; weighing 2.00 parts of urea, adding the urea into the mixed solution, stirring the urea evenly at room temperature, transferring the urea into a hydrothermal reaction kettle, and reacting the urea for 15 hours at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.10g of sodium phytate, dissolving with deionized water, then dropwise adding dilute hydrochloric acid into the dilute hydrochloric acid solution, and adjusting the pH value of the dilute hydrochloric acid solution to 2 for later use.
Step three: weighing 0.80 part of MgAl LDH/MMT, preparing 30mL of suspension by using deionized water, stirring for 20min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 3h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
Example 2
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in the patent (CN202011524847.1), 0.80 part of MMT is weighed and mixed with 60mL of nitric acid aqueous solution, stirred for 4 hours at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain the acid-etched MMT. Weighing 2.00 parts of magnesium nitrate hexahydrate, 0.85 part of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT centrifuged in the step I with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and fully dispersing the mixed solution in an ultrasonic process; weighing 2.20 parts of urea, adding the urea into the mixed solution, stirring the urea evenly at room temperature, transferring the urea into a hydrothermal reaction kettle, and reacting the urea for 15 hours at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.15g of sodium phytate, dissolving the sodium phytate with deionized water, then dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value of the solution to 2.5 for later use.
Step three: weighing 0.90 part of MgAl LDH/MMT, preparing 35mL of suspension by using deionized water, stirring for 20min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 3.5h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
Example 3
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in the patent (CN202011524847.1), 1.00 part of MMT is weighed and mixed with 70mL of nitric acid aqueous solution, stirred for 4 hours at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain the acid-etched MMT. Weighing 2.50 parts of magnesium nitrate hexahydrate, 1.25 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT centrifuged in the step I with 50ml of metal salt solution, uniformly stirring, stripping the MMT soil by adopting an ultrasonic method to obtain stripped MMT, and fully dispersing the mixed solution in an ultrasonic process; 2.50 parts of urea is weighed and added into the mixed solution, the mixed solution is stirred evenly at room temperature and then transferred to a hydrothermal reaction kettle, and the reaction is carried out for 15 hours at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.20g of sodium phytate, dissolving with deionized water, then dropwise adding dilute hydrochloric acid into the dilute hydrochloric acid solution, and adjusting the pH value of the dilute hydrochloric acid solution to 3 for later use.
Step three: weighing 1.10 parts of MgAl LDH/MMT, preparing 40mL of suspension by using deionized water, stirring for 25min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 4h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
Example 4
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in the patent (CN202011524847.1), 1.20 parts of MMT is weighed and mixed with 75mL of nitric acid aqueous solution, stirred for 4 hours at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain acid-etched MMT. Weighing 3.00 parts of magnesium nitrate hexahydrate, 1.50 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT centrifuged in the step I with 50ml of metal salt solution, uniformly stirring, stripping the MMT soil by adopting an ultrasonic method to obtain stripped MMT, and fully dispersing the mixed solution in an ultrasonic process; 3.00 parts of urea is weighed and added into the mixed solution, the mixed solution is stirred evenly at room temperature and then transferred into a hydrothermal reaction kettle, and the mixture is reacted for 15 hours at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.30g of sodium phytate, dissolving the sodium phytate with deionized water, then dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value of the solution to 3.5 for later use.
Step three: weighing 1.30 parts of MgAl LDH/MMT, preparing 40mL of suspension by using deionized water, stirring for 30min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 5h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
Example 5
The method comprises the following steps: referring to the preparation process of MgAl LDH/MMT in patent (CN202011524847.1), 2.00 parts of MMT is weighed and mixed with 80mL of nitric acid aqueous solution, stirred for 4 hours at 105 ℃, and centrifuged until the supernatant is neutral, so as to obtain acid-etched MMT. Weighing 4.50 parts of magnesium nitrate hexahydrate, 2.00 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT centrifuged in the step I with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and fully dispersing the mixed solution in an ultrasonic process; 4.50 parts of urea is weighed and added into the mixed solution, the mixed solution is stirred evenly at room temperature and then transferred to a hydrothermal reaction kettle, and the reaction is carried out for 15 hours at 140 ℃. And after the temperature is reduced to room temperature, centrifuging and collecting the obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material.
Step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.50g of sodium phytate, dissolving the sodium phytate with deionized water, then dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value of the solution to 4.0 for later use.
Step three: weighing 1.60 parts of MgAl LDH/MMT, preparing 40mL of suspension by using deionized water, stirring for 35min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 6h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
To demonstrate the feasibility of adsorbing phytic acid on the surface of MgAl LDH/MMT, the inventors performed the following analytical tests, and the analytical results are as follows:
FIG. 1 shows FTIR spectra of MgAl LDH/MMT and MgAl LDH-PA/MMT at 1096cm compared to MgAl LDH/MMT-1The peak width of absorption is changed from 1210cm-1The absorption peak of P-O, P ═ O shows that PA exists in MgAl LDH-PA/MMT, and the absorption peak of O-H is 3452cm-1Moving red to 3442cm-1It shows that hydrogen bonding exists between PA and MgAl LDH/MMT.
Shown in FIG. 2 are SEM pictures of MgAl LDH/MMT and MgAl LDH-PA/MMT, and EDS pictures of MgAl LDH-PA/MMT. As shown in FIG. 2(a), MgAl LDH/MMT has flower-like morphology. Partial dissolution of MgAl LDH-PA/MMT in FIG. 2(b) occurs because the reaction conditions are acidic, which has corrosive effect on MgAl LDH in MgAl LDH-PA/MMT, but still partially retains the original morphology. FIG. 2(c-d) energy spectrum analysis also demonstrated that PA was supported on the MgAl LDH/MMT surface. Both FIGS. 1 and 2 demonstrate the feasibility of preparing MgAl LDH-PA/MMT.
The invention is not limited to the examples, and any equivalent changes to the technical solution of the invention by a person skilled in the art after reading the description of the invention are covered by the claims of the invention.
Claims (4)
1. A preparation method of a plant acid modified magnesium aluminum hydrotalcite/montmorillonite nano material is characterized by comprising the following specific steps:
the method comprises the following steps: weighing 0.50-2.00 parts of montmorillonite (MMT) and 20-80mL of nitric acid aqueous solution, mixing, stirring at 105 ℃ for 4h, centrifuging until the supernatant is neutral, and obtaining acid-etched MMT; weighing 1.50-4.50 parts of magnesium nitrate hexahydrate, 0.50-2.00 parts of aluminum nitrate nonahydrate and deionized water to prepare 50ml of solution serving as a hydrotalcite precursor salt solution, mixing the MMT obtained after centrifugation in the step one with 50ml of metal salt solution, uniformly stirring, stripping the MMT by adopting an ultrasonic method to obtain stripped MMT, and simultaneously fully dispersing the mixed solution in the ultrasonic process; weighing 2.00-4.50 parts of urea, adding into the mixed solution, stirring uniformly at room temperature, transferring into a hydrothermal reaction kettle, and reacting for 15h at 140 ℃. After the temperature is reduced to room temperature, centrifugally collecting an obtained solid sample, washing the sample to be neutral by using deionized water, and freeze-drying to finally obtain the MgAl LDH/MMT composite material;
step two: firstly, preparing a dilute hydrochloric acid solution, weighing 0.1-0.5g of sodium phytate, dissolving the sodium phytate in deionized water, dropwise adding dilute hydrochloric acid into the solution, and adjusting the pH value of the solution to 2-5 for later use;
step three: weighing 0.80-1.60 parts of MgAl LDH/MMT, preparing 30-40mL of suspension by using deionized water, stirring for 20-50min when the temperature reaches 70 ℃, pouring the acidic sodium phytate solution obtained in the third step, stirring for 3-6h at 70 ℃, and centrifuging until the supernatant is neutral to obtain PA modified MgAl LDH/MMT (MgAl LDH-PA/MMT).
2. The method for preparing the plant acid modified magnesium aluminum hydrotalcite/montmorillonite nano material as claimed in claim 1, wherein the method comprises the following steps:
in the second step, the concentration of the dilute hydrochloric acid is 0.1 mol/L.
3. The method for preparing the plant acid modified magnesium aluminum hydrotalcite/montmorillonite nano material as claimed in claim 1, wherein the method comprises the following steps:
in the third step, the mass ratio of MgAl LDH/MMT to sodium phytate is 4: 1.
4. the method for preparing the plant acid modified magnesium aluminum hydrotalcite/montmorillonite nano material as claimed in claim 1, wherein the method comprises the following steps:
in step three, the final reaction temperature was 70 ℃.
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| CN117247634A (en) * | 2023-11-13 | 2023-12-19 | 江苏诺贝尔塑业股份有限公司 | High-temperature-resistant power tube and preparation method thereof |
| CN117247634B (en) * | 2023-11-13 | 2024-02-02 | 江苏诺贝尔塑业股份有限公司 | High-temperature-resistant power tube and preparation method thereof |
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