CN110551324A - Preparation method and application of nanoscale transition metal oxide loaded expanded graphite particles - Google Patents
Preparation method and application of nanoscale transition metal oxide loaded expanded graphite particles Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2110/00—Foam properties
- C08G2110/0025—Foam properties rigid
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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Abstract
The invention relates to modified expanded graphite, in particular to a preparation method and application of nano-scale transition metal oxide loaded expanded graphite particles. The preparation method of the nanometer transition metal oxide loaded expanded graphite particles comprises the steps of firstly preparing the nanometer transition metal oxide, adding expanded graphite particles into the nanometer transition metal oxide after calcining, placing the nanometer transition metal oxide in an ultrasonic-microwave linkage instrument for oscillation reaction in the presence of a dispersing agent, and preparing the nanometer transition metal oxide loaded expanded graphite particles by an intercalation method.
Description
Technical Field
The invention relates to modified expanded graphite, in particular to a preparation method and application of nano-scale transition metal oxide loaded expanded graphite particles.
Background
The hard polyurethane foam plastic has light weight, high specific strength, small heat conductivity coefficient, excellent forming and processing performance and certain mechanical strength, and is widely applied to the heat insulation and preservation fields of building industry, refrigeration equipment, industrial pipelines, industrial equipment and the like. Rigid polyurethane foam as a class of organic polymer materials has the fatal disadvantage of being very flammable. And a large amount of toxic smoke can be generated in the combustion process, so that people are easy to suffocate and die and the atmosphere is easy to pollute. Therefore, the use of non-flame-retardant rigid polyurethane foam has great potential safety hazard, and simultaneously, the further development of the rigid polyurethane foam is severely restricted.
In the rigid polyurethane foam, the expanded graphite can improve the flame retardant property of the material, but the smoke emission is not reduced or increased, which is caused by insufficient carbon formation and incompact carbon layer.
CN 104709882A discloses a preparation method of transition metal oxide nanoparticles, which comprises the steps of adding soluble transition metal salt into water or ethanol, uniformly dispersing the soluble transition metal salt, adding micromolecular alkali or alkaline solvent containing amino groups, placing the mixed solution into an oil bath pot, heating and refluxing the mixed solution until solid precipitates are generated, cooling the precipitates after the precipitates are not increased, and filtering, washing and drying the solid precipitates to obtain the transition metal oxide nanoparticles.
CN 102649162 a discloses a method for preparing a noble metal nanomaterial or a transition metal oxide nanomaterial, which utilizes an electrode reaction to obtain the noble metal nanomaterial or the transition metal oxide nanomaterial on the cathode of a flat electrode.
CN101521119A discloses a preparation method of an expanded graphite metal oxide composite material, (a) uniformly dispersing transition metal oxide nanoparticles into an aqueous solution through a surfactant to prepare a stable dispersion of inorganic nanoparticles; (B) and (3) dipping the expanded graphite into the stable dispersion liquid of the inorganic nanoparticles in the step (A), standing at room temperature for 10-24 hours, and then drying at 100-200 ℃ for 4-20 hours to obtain the expanded graphite/metal oxide composite material.
As can be seen from the above, the prior art discloses a method for preparing transition metal oxide nanomaterials, and also discloses a method for modifying expanded graphite with transition metal oxide nanoparticles. However, the application of the modified expanded graphite to the improvement of the flame retardant property of the material has not been found at present.
Disclosure of Invention
The invention aims to provide a preparation method of nano-scale transition metal oxide loaded expanded graphite particles, wherein the nano-scale transition metal oxide loaded expanded graphite particles prepared by an intercalation method have more excellent flame-retardant and char-forming functions than expanded graphite, and have flame-retardant and smoke-inhibiting effects on rigid polyurethane foam; the invention also provides the application of the nano-scale transition metal oxide loaded expanded graphite particles.
The preparation method of the nanometer transition metal oxide loaded expanded graphite particles comprises the steps of firstly preparing the nanometer transition metal oxide, adding expanded graphite particles into the nanometer transition metal oxide after calcining, placing the nanometer transition metal oxide in an ultrasonic-microwave linkage instrument for oscillation reaction in the presence of a dispersing agent, and preparing the nanometer transition metal oxide loaded expanded graphite particles by an intercalation method.
The nanometer transition metal oxide is M x O y, preferably one or more of Cu 2 O, Fe 2 O 3, Ni 2 O 3, Co 2 O 3, MnO 2, TiO 2 or La 2 O, and the particle size of the nanometer transition metal oxide is 0.1-0.5 mu M.
The calcination is carried out at 200-800 ℃ for 1-6 h.
The mass ratio of the nano-scale transition metal oxide to the expanded graphite particles is 1-3:1-4, and the expanded graphite particles are 50-300 meshes.
The dispersant is one or more of propylene carbonate or chloroethylene alcohol, and the dispersant is used in the conventional amount well known to those skilled in the art.
The oscillation reaction time is 8-16h, and the oscillation reaction temperature is 25-35 ℃.
The application of the nanoscale transition metal oxide loaded expanded graphite particles is to prepare the flame-retardant rigid polyurethane foam by taking the nanoscale transition metal oxide loaded expanded graphite particles as an additive flame retardant.
The addition part of the nano-scale transition metal oxide loaded expanded graphite particles is 10-50 parts based on 100 parts of raw material polyether used in the preparation of the flame-retardant rigid polyurethane foam.
The nanometer transition metal oxide has Lewis acid catalysis carbon forming effect, can be used as a synergist to be used with an intumescent flame retardant to improve the carbon forming amount of rigid polyurethane foam and improve the carbon layer structure, and simultaneously has the effect of catalyzing and oxidizing CO, and can oxidize CO into CO 2, thereby reducing the content of toxic gas in smoke.
The invention can insert the nanometer transition metal oxide into the expanded graphite layer structure by the intercalation method with the help of the energy of ultrasonic-microwave linkage without damaging the structure, so that the prepared transition metal oxide modified expanded graphite particles have the advantages of flame retardance and smoke suppression.
In the invention, the structural formula of the nano-scale transition metal oxide loaded expanded graphite particles is as follows:
The invention has the following beneficial effects:
The invention provides a preparation method of a nano-scale transition metal oxide loaded expanded graphite particle and application of the nano-scale transition metal oxide loaded expanded graphite particle in flame retardance and smoke suppression in rigid polyurethane foam.
The nano-scale transition metal oxide loaded expanded graphite particles have more excellent flame retardant and char forming functions than common expanded graphite. The formation principle of the nanoscale transition metal oxide loaded expanded graphite particles is as follows: the method takes expanded graphite as a host material, transition metal oxide nano particles as an intercalation agent, and organic solvents such as propylene carbonate and chloroethylene alcohol as dispersion media, and inserts nano particles by ultrasonic-microwave linkage energy, so that the distance between layers of graphite is increased by oscillation reaction, and the van der Waals force between the graphite layers is weakened. The nano particles are inserted into the graphite layer to enable the graphite layer to be negatively charged, and electrostatic repulsion is generated, so that the graphite layer is easily stripped and separated to obtain a target product. Compared with the traditional graphite intercalation method and the solution impregnation method, the method improves the loading efficiency without damaging the structure, and the prepared nano-scale transition metal oxide loaded expanded graphite particles have the advantages of flame retardance and smoke suppression. The modified expanded graphite is used as an additive flame retardant, so that the prepared hard polyurethane foam has good flame retardant and smoke suppression effects.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
(1) The tail gas reaction of plasma arc is adopted to evaporate Cu 2 O particles and liquefy impurities, and then Cu 2 O vapor enters a condensation chamber to be quenched and condensed into nano-scale transition metal oxide with the particle size of 0.1-0.3 mu m.
(2) And (3) calcining the nanoscale Cu 2 O in a muffle furnace at 300 ℃ for 6 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano-Cu 2 O, fully mixing the mixture in propylene carbonate, and placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 8 hours at 30 ℃ to obtain nano-transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano-Cu 2 O to the expanded graphite particles is 1: 1.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 2
(1) The tail gas reaction of plasma arc is adopted to evaporate Fe 2 O 3 particles and liquefy impurities, then Fe 2 O 3 vapor enters a condensation chamber and is quenched, and the nanometer transition metal oxide with the particle size of 0.2-0.4 mu m is condensed.
(2) And (3) calcining the nanoscale Fe 2 O 3 in a muffle furnace at 500 ℃ for 4 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nanoscale Fe 2 O 3, fully mixing the mixture in propylene carbonate, placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 8 hours at 32 ℃ to obtain nanoscale transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nanoscale Fe 2 O 3 to the expanded graphite particles is 1: 2.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 3
(1) The tail gas reaction of plasma arc is adopted to evaporate Ni 2 O 3 particles and liquefy impurities, then the Ni 2 O 3 vapor enters a condensation chamber and is quenched, and the nanometer transition metal oxide with the particle size of 0.1-0.4 mu m is condensed.
(2) And (3) calcining the nanoscale Ni 2 O 3 in a 400 ℃ muffle furnace for 5 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano-Ni 2 O 3, fully mixing the mixture in chloroethylene, placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 6 hours at 31 ℃ to obtain nano-transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano-Ni 2 O 3 to the expanded graphite particles is 2: 1.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 4
(1) The tail gas reaction of plasma arc is adopted to evaporate Co 2 O 3 particles and liquefy impurities, then the Co 2 O 3 vapor enters a condensation chamber and is quenched, and the nanometer transition metal oxide with the particle size of 0.3-0.4 mu m is condensed.
(2) And (3) calcining the nanoscale Co 2 O 3 in a 400 ℃ muffle furnace for 3 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano-Co 2 O 3, fully mixing the mixture in chloroethylene, placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 10 hours at 25 ℃ to obtain nano-transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano-Co 2 O 3 to the expanded graphite particles is 3: 2.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 5
(1) The tail gas reaction of plasma arc is adopted to evaporate MnO 2 particles and liquefy impurities, then MnO 2 vapor enters a condensation chamber and is quenched and condensed into nanometer transition metal oxide with the particle size of 0.1-0.4 mu m.
(2) And (3) calcining the nanoscale MnO 2 in a muffle furnace at 500 ℃ for 4 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano MnO 2, fully mixing the mixture in chloroethylene, and placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 8 hours at the temperature of 27 ℃ to obtain nano transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano MnO 2 to the expanded graphite particles is 3: 4.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 6
(1) The tail gas reaction of plasma arc is adopted to evaporate TiO 2 particles and liquefy impurities, and TiO 2 vapor is rapidly cooled after entering a condensation chamber and condensed into nano-scale transition metal oxide with the particle size of 0.1-0.5 mu m.
(2) And (3) calcining the nanoscale TiO 2 in a muffle furnace at 500 ℃ for 5 hours.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano TiO 2, fully mixing the mixture in propylene carbonate, and placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 7 hours at 28 ℃ to obtain nano transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano TiO 2 to the expanded graphite particles is 3: 2.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Example 7
(1) The tail gas reaction of plasma arc is adopted to evaporate La 2 O particles and liquefy impurities, and La 2 O vapor enters a condensation chamber and is quenched and condensed into nano-scale transition metal oxide with the particle size of 0.3-0.5 mu m.
(2) And (3) calcining the nano-scale La 2 O in a 400 ℃ muffle furnace for 5 h.
(3) And adding 50-300 mesh expanded graphite particles into the calcined nano-La 2 O, fully mixing the mixture in vinyl chloride, and placing the mixture in an ultrasonic-microwave linkage instrument to perform oscillation reaction for 8 hours at 30 ℃ to obtain nano-transition metal oxide loaded expanded graphite particles, wherein the mass ratio of the calcined nano-La 2 O to the expanded graphite particles is 2: 3.
(4) And (3) taking the prepared nano-scale transition metal oxide loaded expanded graphite particles as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
Application examples and comparative examples
The nano-scale transition metal oxide-supported expanded graphite particles prepared in example 1 are used as an additive flame retardant to prepare a flame-retardant rigid polyurethane foam. Wherein the addition parts of the nano-scale transition metal oxide loaded expanded graphite particles are 10 parts, 30 parts and 50 parts in sequence to form a formula of 5-7. The remaining formulations 1-4 serve as comparative examples. The specific formulation is shown in table 1:
TABLE 1 parameter table
taking formula No. 2 as an example, the concrete steps for preparing the rigid polyurethane foam are as follows: polyether 4110, Expanded Graphite (EG), distilled water, silicone oil, a tertiary amine catalyst and cyclopentane are fully and uniformly mixed in a 1000 ml plastic beaker by adopting a laboratory one-step free foaming technology, isocyanate (PAPI) is added, the mixture is rapidly stirred for 10s, and then the mixture is poured into a mold to be freely foamed. After foaming, the mixture is put into an oven with the temperature of 80 ℃ for curing for 2 hours, and then cured for 24 hours at normal temperature. Other numbered foam samples were prepared according to the above preparation procedure.
As can be seen from formula 1 in Table 1, the rigid foam Oxygen Index (OI) of the polyurethane prepared by adding only polyether 4110 is 19.1%, the vertical burning UL-94 grade is stepless, and the smoke density grade is 78.4, which indicates that the material belongs to combustible materials and generates a large amount of smoke during burning.
As can be seen from formulas 2 to 4 in Table 1, the amount of smoke released by the foam after EG addition is significantly increased and the smoke density grade is greatly improved.
As can be seen from formulas 5-7 in Table 1, the more the parts of EG-Cu 2 O are added, the higher the oxygen index of the rigid polyurethane foam is, the better the flame retardant property is, and the lower the smoke density grade is, compared with the equal parts of EG added, the flame retardant property and the smoke suppression property of the foam are both obviously improved after the EG-Cu 2 O is added, and the generation of smoke is suppressed while the flame retardant property of the rigid polyurethane foam is improved by adding EG-Cu 2 O.
The results of the application examples and the comparative examples show that the rigid polyurethane foam belongs to flammable materials and generates a large amount of smoke during combustion, and the addition of EG-Cu 2 O can obviously improve the flame retardant property of the rigid polyurethane foam, inhibit the generation of smoke and be beneficial to fire suppression and evacuation and escape of people.
Claims (10)
1. A preparation method of nanometer transition metal oxide loaded expanded graphite particles is characterized by comprising the following steps: firstly, preparing a nano-scale transition metal oxide, calcining, adding expanded graphite particles, placing in an ultrasonic-microwave interlocking instrument for oscillation reaction in the presence of a dispersing agent, and preparing the nano-scale transition metal oxide loaded expanded graphite particles by an intercalation method.
2. The process for producing nano-sized transition metal oxide-supported expanded graphite particles according to claim 1, wherein the nano-sized transition metal oxide is M x O y.
3. The method for preparing nano-sized transition metal oxide-supported expanded graphite particles according to claim 2, wherein the nano-sized transition metal oxide is one or more of Cu 2 O, Fe 2 O 3, Ni 2 O 3, Co 2 O 3, MnO 2, TiO 2 or La 2 O.
4. The method for producing nanoscale transition metal oxide-supported expanded graphite particles according to claim 1, characterized in that: the particle size of the nanometer transition metal oxide is 0.1-0.5 μm.
5. The method for producing nanoscale transition metal oxide-supported expanded graphite particles according to claim 1, characterized in that: the calcination is carried out at 200-800 ℃ for 1-6 h.
6. The method for producing nanoscale transition metal oxide-supported expanded graphite particles according to claim 1, characterized in that: the mass ratio of the nano-scale transition metal oxide to the expanded graphite particles is 1-3:1-4, and the expanded graphite particles are 50-300 meshes.
7. The method for producing nanoscale transition metal oxide-supported expanded graphite particles according to claim 1, characterized in that: the dispersant is one or more of propylene carbonate or chloroethylene.
8. The method for producing nanoscale transition metal oxide-supported expanded graphite particles according to claim 1, characterized in that: the oscillation reaction time is 8-16h, and the oscillation reaction temperature is 25-35 ℃.
9. Use of the nano-sized transition metal oxide-supported expanded graphite particles according to any one of claims 1 to 8, wherein: the nanometer transition metal oxide loaded expanded graphite particles are used as an additive flame retardant to prepare the flame-retardant rigid polyurethane foam.
10. use of the nano-sized transition metal oxide-supported expanded graphite particles according to claim 9, wherein: the addition part of the nano-scale transition metal oxide loaded expanded graphite particles is 10-50 parts based on 100 parts of raw material polyether used in the preparation of the flame-retardant rigid polyurethane foam.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113980452A (en) * | 2021-12-13 | 2022-01-28 | 深圳市华美龙电子应用材料有限公司 | Antibacterial anti-static film |
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| CN113980452A (en) * | 2021-12-13 | 2022-01-28 | 深圳市华美龙电子应用材料有限公司 | Antibacterial anti-static film |
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