CN115160645A - Preparation method of vermiculite compound flame retardant material - Google Patents
Preparation method of vermiculite compound flame retardant material Download PDFInfo
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/041—Carbon nanotubes
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- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
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Abstract
The invention discloses a preparation method of a vermiculite compound flame retardant material, wherein the vermiculite compound flame retardant material comprises vermiculite, carbon nano tubes, boron phosphate and tin hydroxide. The preparation method prepares the vermiculite carbon nano tube composite material by pretreating vermiculite, prepares the vermiculite flame retardant material by crystallization, mixes the organic plastic material and adds the curing agent to prepare the plastic finished product with high flame retardant property. The method for preparing the flame retardant material has simple process and easy popularization, utilizes the vermiculite laminate structure, inserts the organic flame retardant and the inorganic flame retardant to realize the compounding of various flame retardants, constructs the high-performance flame retardant material, has certain infrared and ultraviolet blocking capability besides the flame retardant performance of a plastic finished product, and is suitable for large-scale popularization.
Description
Technical Field
The invention relates to the technical field of flame retardant materials, in particular to a preparation method of a vermiculite compound flame retardant material.
Background
Vermiculite is one of nonmetal minerals with better resource prospect and potential advantages in China, is an important nonmetal mineral, is also a magnesium-containing aluminosilicate secondary metamorphic mineral with a layered structure, belongs to layered silicate, and is low in price and easy to obtain. The vermiculite is high temperature resistant and has good electrical insulation; expanded vermiculite is prone to water and moisture absorption; it expands at high temperature and is easy to peel. Vermiculite has the characteristics of good interlayer cation exchange capacity, expansion capacity, adsorption capacity, sound insulation, heat insulation, fire resistance, freezing resistance and the like, is stable in chemical property, is insoluble in water, is nontoxic and tasteless, has no side effect, and is mainly used for treating wastewater containing heavy metals and organic cations by utilizing good adsorption performance and ion exchange performance in industry, preparing antibacterial materials and heat insulation materials, vermiculite filter aid, purifying agents, organic vermiculite and the like.
At present, vermiculite is almost made into expanded vermiculite and then is used for building heat insulation materials in China, the value is very low, an industrial chain for effectively utilizing vermiculite resources is not established all the time, and the problems of vermiculite development and utilization in China are as follows compared with the problems in China: 1) The application range is narrow: the application of the domestic vermiculite is mainly limited to building materials, and the application of the domestic vermiculite in agriculture, electromechanics, chemical industry and environmental protection is little. Besides the above five departments of industry, the device is also applied to the mechanical, electronic and metallurgical industries, and the application field is obviously wide. 2) The product variety is few: the vermiculite patent products in China are obviously fewer in varieties than those in foreign countries, and have great difference in the fields of agricultural building materials and petrochemical industry. 3) The processing method is simple: in China, the vermiculite is generally utilized by directly utilizing raw ore after being calcined and expanded. Different processing methods are often adopted for different applications abroad, the processing technical method is more advanced, novel and diversified, and the widening of the utilization field and the development of new products are correspondingly promoted. 4) The utilization rate of the fine-grained vermiculite is low: the application of coarse-grained vermiculite in China has a good foundation, but the utilization rate of fine-grained vermiculite with the granularity less than 0.3mm is low, so that the resource waste is caused. In view of international technology trade barriers and intellectual property protection, the advanced vermiculite processing technology is difficult to be directly introduced from abroad. From the sustainable development perspective, the research on the deep processing technology and the application technology of vermiculite must be strengthened at present, the industrial innovation is accelerated, and a novel functionalized new material is prepared, so that a new vermiculite product with higher added value is obtained.
Polymer materials such as EVA, PP, PE, PVC and the like have great influence on social development and life of people, the flame retardance of polymer ionomer materials is always concerned by people since the last century, and substances which can stop combustion reaction through chemical action when the polymer ionomer materials are not combusted or are combusted, namely flame retardants, are added into high polymer materials to prepare the composite materials by utilizing the high compatibility of the polymer high polymer materials, so that the flame retardance of the composite materials is improved. Epoxy resins are widely used as base resins for electronic laminates, encapsulating materials, electronic parts of electronic and electrical appliances, and coatings, and in order to ensure fire safety in applications, flammable epoxy resins must be subjected to flame retardant treatment. Although the halogen flame retardant has high flame retardant efficiency, the flame retardant material can release a large amount of smoke, toxic and corrosive gases during combustion, and is harmful to human bodies and the environment. Therefore, the research on new environment-friendly and efficient flame-retardant materials has become a development trend in the flame-retardant field.
Therefore, in combination with the above problems, it is an urgent need to solve the problems of the art to provide a preparation method of a vermiculite compound flame retardant material.
Disclosure of Invention
In view of the above, the invention provides a preparation method of a vermiculite compound flame retardant material, the vermiculite compound flame retardant material prepared by the invention has high stability and good flame retardant effect, and the flame retardant material prepared by the invention has the advantages of simple process, easiness in popularization and obvious economic value.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a vermiculite compound flame retardant material comprises vermiculite, carbon nano tubes, boron phosphate and tin hydroxide, and comprises the following steps:
s1, pretreating vermiculite: calcining raw ore vermiculite to prepare expanded vermiculite, and removing impurities in the expanded vermiculite after water washing and flotation; shearing and crushing the prepared expanded vermiculite by a crusher to obtain particles with the particle size of 100-10000 meshes, soaking the vermiculite powder in 20-30% ferric chloride solution, modifying the vermiculite for 1-56h at the rotating speed of 100-20000rpm, wherein the volume ratio of the vermiculite to the ferric chloride solution is 1-5-15, the modification reaction temperature is 25-100 ℃, washing and drying, and the treated modified vermiculite powder is reserved;
s2, preparing the vermiculite carbon nanotube composite material: the modified vermiculite powder obtained in the step S1 and a carbon source are subjected to ultrasonic boiling and are uniformly mixed and placed into a high-temperature tubular furnace reactor, inert gas is introduced, the temperature rise rate is 1-20 ℃/min, the reaction is carried out at the temperature of 600-1000 ℃, and the non-agglomerated vermiculite/carbon nano tube composite material is obtained through the reaction;
s3, preparing a vermiculite flame retardant material: putting the vermiculite/carbon nano tube composite material obtained in the step S2 into a hydrothermal kettle, firstly adding 0.0001-0.1mol/L boric acid and sodium pyrophosphate, stirring for 5-100min, then adding 0.0001-0.01mol/L sulfanilic acid, wherein the volume ratio of the vermiculite/carbon nano tube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the sulfanilic acid is 1;
s4, mixing an organic plastic material: dispersing the vermiculite compound flame retardant material obtained in the step S3 in an absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite compound flame retardant material to the absolute ethyl alcohol solution is 1:5-15, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 3-5 times, adding absolute ethyl alcohol, stirring, carrying out ultrasonic-assisted dispersion, mixing with the organic plastic material, stirring, carrying out ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging, and drying to obtain a mixture of the vermiculite compound flame retardant material and the organic plastic material;
s5, preparing a finished vermiculite compound flame retardant material: and (5) adding a curing agent into the mixture of the vermiculite flame retardant material and the organic plastic material obtained in the step (S4), and performing thermal treatment molding to obtain a plastic product with high flame retardant property.
Preferably, the ferric chloride solution in step S1 may also be a cobalt chloride solution or a nickel chloride solution.
Preferably, the calcining temperature in the step S1 is 550-900 ℃, and the calcining time is 1-100min; the shearing and pulverizing time of the pulverizer is 1-200min, the rotation speed is 1000-20000rpm, the reaction time is 1-48h, the drying temperature is 40-180 ℃, and the drying time is 0.5-24h.
Preferably, the carbon source in step S2 includes, but is not limited to, melamine, pyridine, pyrrole, dicyandiamide.
Preferably, the sulfanilic acid in step S3 may also be an amino acid, DOPO or maleic acid.
Preferably, the organic plastic material is mixed in the step S4, and then stirred for 1-55min at 500-1800 rpm.
Preferably, the organic plastic material in step S4 includes, but is not limited to, ethylene oxide, propylene oxide, polyethylene, polypropylene, polyvinyl chloride, polyvinyl alcohol, polyurethane.
Preferably, in the step S5, the mass ratio of the mixture of the vermiculite flame retardant material and the organic plastic material to the curing agent is 2-5:5.
preferably, the heat treatment molding conditions in the step S5 are set at a temperature of 100-300 ℃ and a treatment time of 1-100min.
Preferably, the curing agent in step S5 includes, but is not limited to, ethylene oxide, propylene oxide, glycerin, dioctyl phthalate.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
according to the technical scheme, vermiculite is used as a main base material, vermiculite is used as a layered material and mainly comprises elements such as silicon, magnesium, aluminum and the like, organic and inorganic flame retardants are inserted into a vermiculite layer plate or between layers to realize compounding of various flame retardants, a high-performance and three-dimensional flame retardant is constructed, carbon nano tubes grow on the vermiculite layer plate, an intercalated multi-level structure flame retardant is constructed by a coprecipitation method, and the composite flame retardant material is prepared, so that modification and preparation of the surface of fine particle vermiculite are realized. The novel flame-retardant material is constructed by a synthetic method, and a new thought is provided for the development of the preparation research of the vermiculite flame-retardant material.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Example 1:
calcining raw ore vermiculite at 900 ℃ to prepare expanded vermiculite, and removing impurities in the expanded vermiculite after water washing and flotation; shearing and crushing the prepared expanded vermiculite for 10min to 650 meshes at the rotation speed of 10000rpm, taking 2g of vermiculite powder, soaking the vermiculite powder in 30ml of 30% ferric chloride solution, reacting for 24h at the rotation speed of 4000rpm, wherein the reaction temperature is 40 ℃, washing for 3 times by deionized water after reaction, and drying for 18h at the temperature of 125 ℃.
And (2) carrying out ultrasonic boiling and uniform mixing on the iron modified vermiculite powder and 2g of melamine, putting the mixture into a high-temperature tubular furnace reactor, introducing inert gas, heating at a speed of 5 ℃/min to 700 ℃, and reacting for 2 hours to obtain the vermiculite-carbon nanotube composite material.
Putting the vermiculite carbon nanotube composite material into a hydrothermal kettle, firstly adding 0.001mol/L boric acid and sodium pyrophosphate, stirring for 15min, then adding 0.0001mol/L sulfanilic acid, wherein the volume ratio of the vermiculite carbon nanotube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the sulfanilic acid is 1.
Putting the vermiculite composite flame retardant material into an absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite composite flame retardant material to the absolute ethyl alcohol solution is 1:10, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 5 times, adding absolute ethyl alcohol, carrying out stirring and ultrasonic-assisted dispersion, mixing with the organic plastic material, carrying out stirring and ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging at the rotating speed of 1000rpm for 10min, separating, and drying at the temperature of 60 ℃ for 24h to obtain a mixture of the vermiculite flame retardant material and the organic plastic material.
Taking a mixture of a vermiculite flame retardant material and a PVC plastic material, adding DOP, wherein the mass ratio of the mixture of the vermiculite flame retardant material and the PVC plastic material to a curing agent is 1:1, carrying out hot-pressing treatment and molding at 180 ℃ to obtain the vermiculite compound flame retardant material with high flame retardant property. The limiting oxygen index LOI is at most 35.4%.
Example 2:
pretreating vermiculite: calcining raw ore vermiculite at 900 ℃ to prepare expanded vermiculite, and removing impurities in the expanded vermiculite by washing and flotation; shearing and crushing the prepared expanded vermiculite to 700 meshes, soaking 2g of vermiculite powder in 30ml of 30% ferric chloride solution, reacting for 24 hours at the rotating speed of 3000rpm, wherein the reaction temperature is 40 ℃, washing for 3 times by using deionized water after reaction, and drying at the temperature of 130 ℃ for 20 hours.
And (2) carrying out ultrasonic boiling and mixing on the iron modified vermiculite powder and 1.5g of dicyandiamide uniformly, putting the mixture into a high-temperature tubular furnace reactor, introducing inert gas, heating at the rate of 5 ℃/min to 760 ℃ and reacting for 2 hours to obtain the vermiculite carbon nanotube composite material.
Putting the vermiculite carbon nanotube composite material into a hydrothermal kettle, firstly adding 0.001mol/L boric acid and sodium pyrophosphate, stirring for 15min, then adding 0.0001mol/L sulfanilic acid, wherein the volume ratio of the vermiculite carbon nanotube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the sulfanilic acid is 1.
Dispersing the vermiculite composite flame retardant material in an absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite composite flame retardant material to the absolute ethyl alcohol solution is 1:10, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 5 times, adding absolute ethyl alcohol, carrying out stirring ultrasonic-assisted dispersion, mixing with the organic plastic material, carrying out stirring ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging at the rotating speed of 1000rpm for 10min, separating, and drying at the temperature of 60 ℃ for 24h to obtain the mixture of the vermiculite flame retardant material and the organic plastic material.
Taking a mixture of a vermiculite flame retardant material and a PVC plastic material, adding DOP, wherein the mass ratio of the mixture of the vermiculite flame retardant material and the PVC plastic material to a curing agent is 1:1, carrying out hot-pressing treatment and molding at 190 ℃ to obtain the vermiculite compound flame retardant material with high flame retardant property. The limiting oxygen index LOI is at most 35.4%.
Example 3:
calcining raw ore vermiculite at 900 ℃ to prepare expanded vermiculite, and removing impurities in the expanded vermiculite after washing and flotation; shearing and crushing the prepared expanded vermiculite at 10000rpm for 15min to 800 meshes, taking 2g of vermiculite powder, soaking the vermiculite powder in 30ml of 30% cobalt chloride solution, reacting for 24h at 2000rpm, wherein the reaction temperature is 40 ℃, washing for 3 times by using deionized water after reaction, and drying at 120 ℃ for 24h.
And (2) uniformly mixing the cobalt modified vermiculite powder and 1.5g of dicyandiamide by ultrasonic boiling, putting the mixture into a high-temperature tubular furnace reactor, introducing inert gas, heating at a speed of 5 ℃/min to 800 ℃ and reacting for 2 hours to obtain the vermiculite-carbon nanotube composite material.
Putting the vermiculite carbon nanotube composite material into a hydrothermal kettle, firstly adding 0.001mol/L boric acid and sodium pyrophosphate, stirring for 15min, then adding 0.0001mol/L maleic acid, wherein the volume ratio of the vermiculite carbon nanotube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the maleic acid is 1.
Dispersing the vermiculite composite flame retardant material in 100ml of absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite composite flame retardant material to the absolute ethyl alcohol solution is 1:10, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 5 times, adding absolute ethyl alcohol, carrying out stirring and ultrasonic-assisted dispersion, mixing with the organic plastic material, carrying out stirring and ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging at the rotating speed of 1000rpm for 10min, separating, and drying at the temperature of 60 ℃ for 24h to obtain a mixture of the vermiculite flame retardant material and the organic plastic material.
Taking a mixture of a vermiculite flame retardant material and a PVC plastic material, adding DOP, wherein the mass ratio of the mixture of the vermiculite flame retardant material and the PVC plastic material to a curing agent is 1:1, performing heat treatment molding at 200 ℃ to obtain the vermiculite compound flame retardant material with high flame retardant property. The limiting oxygen index LOI is at most 35.4%.
Example 4:
calcining raw ore vermiculite at 900 ℃ to prepare expanded vermiculite, and removing impurities in the expanded vermiculite after water washing and flotation; shearing and crushing the prepared expanded vermiculite at 10000rpm for 10min to 750 meshes, taking 2g of vermiculite powder, soaking the vermiculite powder in 30ml of 30% nickel chloride solution, reacting at the rotation speed of 3000rpm for 24h, wherein the reaction temperature is 40 ℃, washing the vermiculite powder for 3 times by using deionized water after reaction, and drying the vermiculite powder at the temperature of 110 ℃ for 16h.
The preparation method comprises the steps of carrying out ultrasonic boiling and uniform mixing on nickel modified vermiculite powder and 1.5g of melamine, then placing the mixture into a high-temperature tubular furnace reactor, introducing inert gas, heating at a rate of 5 ℃/min to 700 ℃, and reacting for 2 hours to obtain the vermiculite-carbon nanotube composite material.
Putting the vermiculite carbon nanotube composite material into a hydrothermal kettle, firstly adding 0.001mol/L boric acid and sodium pyrophosphate, stirring for 15min, then adding 0.0001mol/L DOPO, wherein the volume ratio of the vermiculite carbon nanotube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the DOPO is 1.
Dispersing the vermiculite composite flame retardant material in 100ml of absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite composite flame retardant material to the absolute ethyl alcohol solution is 1:10, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 5 times, adding absolute ethyl alcohol, carrying out stirring ultrasonic-assisted dispersion, mixing with the organic plastic material, carrying out stirring ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging at the rotating speed of 1000rpm for 10min, separating, and drying at the temperature of 60 ℃ for 24h to obtain the mixture of the vermiculite flame retardant material and the organic plastic material.
Taking a mixture of a vermiculite flame retardant material and a PVC plastic material, adding DOP, wherein the mass ratio of the mixture of the vermiculite flame retardant material and the PVC plastic material to a curing agent is 1:1, heat treating and forming at 190 ℃ to prepare the vermiculite compound flame retardant material with high flame retardant property. The limiting oxygen index LOI is at most 35.4%.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation method of a vermiculite compound flame retardant material comprises vermiculite, carbon nano tubes, boron phosphate and tin hydroxide, and is characterized by comprising the following steps:
s1, pretreating vermiculite: calcining raw ore vermiculite to prepare expanded vermiculite, and removing impurities in the expanded vermiculite after water washing and flotation; shearing and crushing the prepared expanded vermiculite by a crusher to obtain particles with the particle size of 100-10000 meshes, soaking the vermiculite powder in 20-30% ferric chloride solution, carrying out iron modification for 1-56h at the rotating speed of 100-20000rpm, wherein the volume ratio of the vermiculite to the ferric chloride solution is 1-15, the modification reaction temperature is 25-100 ℃, washing and drying, and the treated modified vermiculite powder is reserved;
s2, preparing the vermiculite carbon nanotube composite material: ultrasonically boiling and uniformly mixing the modified vermiculite powder obtained in the step S1 and a carbon source, putting the mixture into a high-temperature tubular furnace reactor, introducing inert gas, heating at the rate of 1-20 ℃/min, reacting at the temperature of 600-1000 ℃, and reacting to obtain a non-agglomerated vermiculite/carbon nanotube composite material;
s3, preparing a vermiculite flame retardant material: putting the vermiculite/carbon nano tube composite material obtained in the step S2 into a hydrothermal kettle, firstly adding 0.0001-0.1mol/L boric acid and sodium pyrophosphate, stirring for 5-100min, then adding 0.0001-0.01mol/L sulfanilic acid, wherein the volume ratio of the vermiculite/carbon nano tube composite material to the mixed liquid of the boric acid, the sodium pyrophosphate and the sulfanilic acid is 1;
s4, mixing an organic plastic material: dispersing the vermiculite compound flame retardant material obtained in the step S3 in an absolute ethyl alcohol solution, wherein the volume ratio of the vermiculite compound flame retardant material to the absolute ethyl alcohol solution is 1:5-15, uniformly stirring, carrying out ultrasonic-assisted centrifugal washing for 3-5 times, adding absolute ethyl alcohol, stirring, carrying out ultrasonic-assisted dispersion, mixing with the organic plastic material, stirring, carrying out ultrasonic-assisted dispersion to obtain a uniform suspension, centrifuging, and drying to obtain a mixture of the vermiculite compound flame retardant material and the organic plastic material;
s5, preparing a finished vermiculite compound flame retardant material: and (5) adding a curing agent into the mixture of the vermiculite flame retardant material and the organic plastic material obtained in the step (S4), and performing thermal treatment molding to obtain a plastic product with high flame retardant property.
2. The method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the ferric chloride solution in step S1 can also be a cobalt chloride solution or a nickel chloride solution.
3. The preparation method of the vermiculite compound flame retardant material according to claim 1, wherein in the step S1, the calcination temperature is 550-900 ℃, and the calcination time is 1-100min; the shearing and pulverizing time of pulverizer is 1-200min, rotation speed is 1000-20000rpm, reaction time is 1-48h, drying temperature is 40-180 deg.C, and drying time is 0.5-24h.
4. The method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the carbon source in step S2 includes but is not limited to melamine, pyridine, pyrrole, dicyandiamide.
5. The method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the sulfanilic acid in step S3 may also be amino acid, DOPO or maleic acid.
6. The method for preparing the vermiculite compound flame retardant material according to claim 1, wherein the mixture obtained in step S4 is mixed with the organic plastic material and then stirred at 500-1800rpm for 1-55min.
7. The method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the organic plastic material in step S4 includes but is not limited to ethylene oxide, propylene oxide, polyethylene, polypropylene, polyvinyl chloride, polyvinyl alcohol, polyurethane.
8. The preparation method of the vermiculite compound flame retardant material according to claim 1, wherein the mass ratio of the mixture of the vermiculite flame retardant material and the organic plastic material to the curing agent in the step S5 is 2-5:5.
9. the method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the heat treatment molding conditions in step S5 are set at 100-300 ℃ for 1-100min.
10. The method for preparing a vermiculite compound flame retardant material according to claim 1, wherein the curing agent in step S5 includes but is not limited to ethylene oxide, propylene oxide, glycerin, dioctyl phthalate.
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