CN110862534A - Intercalation reinforced polyamide material and preparation method thereof - Google Patents
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F120/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
- C08F120/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F120/04—Acids; Metal salts or ammonium salts thereof
- C08F120/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
- C08G69/16—Preparatory processes
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- C—CHEMISTRY; METALLURGY
- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C—CHEMISTRY; METALLURGY
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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- C—CHEMISTRY; METALLURGY
- 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
- C08K9/02—Ingredients treated with inorganic substances
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/08—Ingredients agglomerated by treatment with a binding agent
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Abstract
The invention discloses an intercalation reinforcing polyamide material and a preparation method thereof, wherein the intercalation reinforcing polyamide material is prepared from the following raw materials in parts by weight: 10-16 parts of lignin, 40-50 parts of expanded perlite, 30-40 parts of sodium acrylate, 0.9-1 part of ammonium persulfate, 300 parts of caprolactam 200-sodium silicate, 1-2 parts of 2-mercaptobenzimidazole, 20-30 parts of thionyl chloride, 8-11 parts of stearic acid, 4-5 parts of antimony trioxide, 0.1-0.2 part of triethylamine, 4-6 parts of aluminum stearate and 3-5 parts of dicumyl peroxide. The material of the invention has good flame retardance and mechanical stability, and when the material is burnt in fire, the carbon layer burnt by lignin can be uniformly distributed among the layers of perlite to form an expanded carbon layer, thus playing the role of heat insulation and fire prevention and further improving the fire resistance.
Description
Technical Field
The invention belongs to the field of materials, and particularly relates to an intercalation reinforced polyamide material and a preparation method thereof.
Background
Polyamides are commonly known as nylons and are a generic name for polymers containing amide groups in the repeating units of the macromolecular main chain. The polyamide can be prepared by ring-opening polymerization of lactam, or polycondensation of diamine and diacid. The polyamide is a high polymer having a polar amide group (-CO-NH-) in the main chain. Originally used as a raw material for manufacturing fibers, the PA is later used as an engineering plastic widely applied in the industry at present due to toughness, wear resistance, self-lubrication and wide use temperature range. The PA can be widely used for replacing copper and nonferrous metals to manufacture mechanical, chemical and electrical parts, such as a fuel pump gear of a diesel engine, a water pump, a high-pressure sealing ring, an oil delivery pipe and the like. The DuPont company in the United states originally developed resins for fibers and was commercialized in 1939. In the 50 th of the 20 th century, injection molded products are developed and produced to replace metals to meet the requirements of light weight and cost reduction of downstream industrial products. The PA has good comprehensive properties including mechanical property, heat resistance, abrasion resistance, chemical resistance and self-lubricity, has low friction coefficient and certain flame retardance, is easy to process, is suitable for being filled with glass fiber and other fillers for reinforcing modification, improves the performance and expands the application range. The varieties of PA are various, including PA6, PA66, PA11, PA12, PA46, PA610, PA612, and PA PAl010, and new varieties such as semi-aromatic nylon PA6T and special nylon developed in recent years; however, the fireproof performance of the current polyamide is poor, and the application range of the polyamide is seriously influenced.
Disclosure of Invention
The invention aims to provide an intercalation reinforced polyamide material and a preparation method thereof aiming at the defects and shortcomings of the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an intercalation reinforced polyamide material, which is composed of the following raw materials in parts by weight: 10-16 parts of lignin, 40-50 parts of expanded perlite, 30-40 parts of sodium acrylate, 0.9-1 part of ammonium persulfate, 300 parts of caprolactam 200-sodium silicate, 1-2 parts of 2-mercaptobenzimidazole, 20-30 parts of thionyl chloride, 8-11 parts of stearic acid, 4-5 parts of antimony trioxide, 0.1-0.2 part of triethylamine, 4-6 parts of aluminum stearate and 3-5 parts of dicumyl peroxide.
The preparation method of the intercalation reinforced polyamide material comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(2) adding antimony trioxide into thionyl chloride, stirring uniformly, adding stearic acid, raising the temperature to 50-55 ℃, keeping the temperature and stirring for 1-2 hours, and distilling to remove the thionyl chloride to obtain antimony oxychloride;
(3) adding lignin into deionized water which is 35-40 times of the weight of the mixture, adding antimony oxychloride, uniformly stirring, adding triethylamine, feeding into an ice water bath, stirring for reacting for 3-5 hours, and discharging to obtain a lignin modified solution;
(4) adding sodium acrylate into the lignin modified solution, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate and the expanded perlite, keeping the temperature and stirring for 2-3 hours, filtering, washing the precipitate with water, and drying at the temperature of 50-60 ℃ for 100-3 minutes in vacuum to obtain the intercalated perlite;
(5) mixing 2-mercaptobenzimidazole and dicumyl peroxide, adding the mixture into anhydrous ethanol with the weight 37-40 times of that of the mixture, and uniformly stirring to obtain an alcohol dispersion liquid;
(6) mixing the intercalated perlite, the alcohol dispersion liquid and caprolactam, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65-75 ℃, preserving heat, stirring for 3-4 hours, discharging, filtering, washing precipitate with water, drying at normal temperature, mixing with aluminum stearate, uniformly stirring, feeding into an extruder, carrying out melt extrusion, and cooling to obtain the intercalated reinforced polyamide material.
The invention has the advantages that:
according to the invention, antimony trioxide is firstly subjected to acyl chlorination modification, then is blended with lignin, triethylamine is used as an acid-binding agent to obtain a lignin modified solution, sodium acrylate is used as a monomer, polymerization is carried out under the action of an initiator, expanded perlite is introduced in the polymerization process, so that intercalation of sodium polyacrylate to perlite is realized, modified lignin is introduced in the intercalation, and the attachment stability of lignin between perlite layers is realized.
Detailed Description
Example 1
An intercalation reinforced polyamide material, which is composed of the following raw materials in parts by weight: 10 parts of lignin, 40 parts of expanded perlite, 30 parts of sodium acrylate, 0.9 part of ammonium persulfate, 200 parts of caprolactam, 1 part of 2-mercaptobenzimidazole, 20 parts of thionyl chloride, 8 parts of stearic acid, 4 parts of antimony trioxide, 0.1 part of triethylamine, 4 parts of aluminum stearate and 3 parts of dicumyl peroxide.
The preparation method of the intercalation reinforced polyamide material comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight of 20 times of that of the ammonium persulfate, and uniformly stirring;
(2) adding antimony trioxide into thionyl chloride, stirring uniformly, adding stearic acid, raising the temperature to 50 ℃, keeping the temperature and stirring for 1 hour, and distilling to remove the thionyl chloride to obtain antimony trichloride;
(3) adding lignin into deionized water which is 35 times of the weight of the mixture, adding antimony oxychloride, uniformly stirring, adding triethylamine, feeding into an ice water bath, stirring for reaction for 3-5 hours, and discharging to obtain a lignin modified solution;
(4) adding sodium acrylate into the lignin modified solution, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the ammonium persulfate and the expanded perlite, keeping the temperature and stirring for 2 hours, filtering, washing the precipitate with water, and drying at the temperature of 50 ℃ for 100 minutes in vacuum to obtain the intercalated perlite;
(5) mixing 2-mercaptobenzimidazole and dicumyl peroxide, adding the mixture into anhydrous ethanol with the weight 37 times that of the mixture, and uniformly stirring to obtain an alcohol dispersion liquid;
(6) mixing the intercalated perlite, the alcohol dispersion liquid and caprolactam, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, keeping the temperature and stirring for 3 hours, discharging, filtering, washing the precipitate with water, drying at normal temperature, mixing with aluminum stearate, uniformly stirring, feeding into an extruder, melting and extruding, and cooling to obtain the intercalated reinforced polyamide material.
Example 2
An intercalation reinforced polyamide material, which is composed of the following raw materials in parts by weight: 16 parts of lignin, 50 parts of expanded perlite, 40 parts of sodium acrylate, 1 part of ammonium persulfate, 300 parts of caprolactam, 2-mercaptobenzimidazole, 2 parts of thionyl chloride, 30 parts of stearic acid, 11 parts of antimony trioxide, 0.2 part of triethylamine, 6 parts of aluminum stearate and 5 parts of dicumyl peroxide.
The preparation method of the intercalation reinforced polyamide material comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight 30 times that of the ammonium persulfate, and uniformly stirring;
(2) adding antimony trioxide into thionyl chloride, stirring uniformly, adding stearic acid, raising the temperature to 55 ℃, keeping the temperature and stirring for 2 hours, and distilling to remove the thionyl chloride to obtain antimony trichloride;
(3) adding lignin into deionized water 40 times of the weight of the mixture, adding antimony oxychloride, uniformly stirring, adding triethylamine, feeding into an ice-water bath, stirring for reaction for 5 hours, and discharging to obtain a lignin modified solution;
(4) adding sodium acrylate into the lignin modified solution, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 75 ℃, adding the ammonium persulfate and the expanded perlite, keeping the temperature and stirring for 3 hours, filtering, washing the precipitate with water, and drying at 60 ℃ in vacuum for 120 minutes to obtain the intercalated perlite;
(5) mixing 2-mercaptobenzimidazole and dicumyl peroxide, adding the mixture into anhydrous ethanol with the weight 37-40 times of that of the mixture, and uniformly stirring to obtain an alcohol dispersion liquid;
(6) mixing the intercalated perlite, the alcohol dispersion liquid and caprolactam, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 75 ℃, keeping the temperature and stirring for 4 hours, discharging, filtering, washing the precipitate with water, drying at normal temperature, mixing with aluminum stearate, uniformly stirring, feeding into an extruder, melting and extruding, and cooling to obtain the intercalated reinforced polyamide material.
Example 3
An intercalation reinforced polyamide material, which is composed of the following raw materials in parts by weight: lignin 12, expanded perlite 44, sodium acrylate 35, ammonium persulfate 0.9, caprolactam 270, 2-mercaptobenzimidazole 1.5, thionyl chloride 25, stearic acid 10, antimony trioxide 4.5, triethylamine 0.15, aluminum stearate 5 and dicumyl peroxide 4.
The preparation method of the intercalation reinforced polyamide material comprises the following steps:
(1) adding ammonium persulfate into deionized water with the weight being 26 times that of the ammonium persulfate, and uniformly stirring;
(2) adding antimony trioxide into thionyl chloride, stirring uniformly, adding stearic acid, raising the temperature to 50 ℃, keeping the temperature and stirring for 1.5 hours, and distilling to remove the thionyl chloride to obtain antimony oxychloride;
(3) adding lignin into deionized water 38 times the weight of the mixture, adding antimony oxychloride, uniformly stirring, adding triethylamine, feeding into an ice-water bath, stirring for reacting for 4 hours, and discharging to obtain a lignin modified solution;
(4) adding sodium acrylate into the lignin modified solution, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 60 ℃, adding the ammonium persulfate and the expanded perlite, keeping the temperature and stirring for 2.5 hours, filtering, washing the precipitate with water, and drying at the temperature of 50 ℃ for 110 minutes in vacuum to obtain the intercalated perlite;
(5) mixing 2-mercaptobenzimidazole and dicumyl peroxide, adding the mixture into absolute ethyl alcohol with the weight 40 times that of the mixture, and uniformly stirring to obtain an alcohol dispersion liquid;
(6) mixing the intercalated perlite, the alcohol dispersion liquid and caprolactam, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65 ℃, keeping the temperature and stirring for 3.5 hours, discharging, filtering, washing precipitate with water, drying at normal temperature, mixing with aluminum stearate, uniformly stirring, feeding into an extruder, carrying out melt extrusion, and cooling to obtain the intercalated reinforced polyamide material.
Mechanical property test (GB/T1040-92):
the tensile strength of the intercalated reinforced polyamide material in the embodiment 1 of the invention is as follows: 89.1 Mpa;
the tensile strength of the intercalated reinforced polyamide material in the embodiment 2 of the invention is as follows: 79.7 Mpa;
the tensile strength of the intercalated reinforced polyamide material in the embodiment 3 of the invention is as follows: 84.4 Mpa;
commercial nylon 6: 55-65 Mpa;
and (3) testing the flame retardant property:
UL-94 of the pure nylon 6 particles is V-2 grade, the limiting oxygen index value is 22-25, the maximum heat release rate is 570-600KW/m2；
The intercalated reinforcing polyamide material particles of example 1 of the present invention were measured to have a UL-94 rating of V-1, a limiting oxygen index value of 29 and a maximum heat release rate of 460KW/m2；
The intercalated reinforced polyamide material particles of example 2 of the present invention were measured to have a UL-94 rating of V-1, a limiting oxygen index value of 31, and a maximum heat release rate of 407KW/m2；
The intercalated reinforced polyamide material particles obtained in example 2 of the present invention were measured to have a UL-94 rating of V-1, a limiting oxygen index value of 30 and a maximum heat release rate of 421KW/m2。
Claims (2)
1. The intercalation reinforced polyamide material is characterized by comprising the following raw materials in parts by weight:
10-16 parts of lignin, 40-50 parts of expanded perlite, 30-40 parts of sodium acrylate, 0.9-1 part of ammonium persulfate, 300 parts of caprolactam 200-sodium silicate, 1-2 parts of 2-mercaptobenzimidazole, 20-30 parts of thionyl chloride, 8-11 parts of stearic acid, 4-5 parts of antimony trioxide, 0.1-0.2 part of triethylamine, 4-6 parts of aluminum stearate and 3-5 parts of dicumyl peroxide.
2. A process for the preparation of the intercalated reinforced polyamide material according to claim 1, comprising the steps of:
(1) adding ammonium persulfate into deionized water with the weight of 20-30 times of that of the ammonium persulfate, and uniformly stirring;
(2) adding antimony trioxide into thionyl chloride, stirring uniformly, adding stearic acid, raising the temperature to 50-55 ℃, keeping the temperature and stirring for 1-2 hours, and distilling to remove the thionyl chloride to obtain antimony oxychloride;
(3) adding lignin into deionized water which is 35-40 times of the weight of the mixture, adding antimony oxychloride, uniformly stirring, adding triethylamine, feeding into an ice water bath, stirring for reacting for 3-5 hours, and discharging to obtain a lignin modified solution;
(4) adding sodium acrylate into the lignin modified solution, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to be 60-75 ℃, adding the ammonium persulfate and the expanded perlite, keeping the temperature and stirring for 2-3 hours, filtering, washing the precipitate with water, and drying at the temperature of 50-60 ℃ for 100-3 minutes in vacuum to obtain the intercalated perlite;
(5) mixing 2-mercaptobenzimidazole and dicumyl peroxide, adding the mixture into anhydrous ethanol with the weight 37-40 times of that of the mixture, and uniformly stirring to obtain an alcohol dispersion liquid;
(6) mixing the intercalated perlite, the alcohol dispersion liquid and caprolactam, uniformly stirring, feeding into a reaction kettle, introducing nitrogen, adjusting the temperature of the reaction kettle to 65-75 ℃, preserving heat, stirring for 3-4 hours, discharging, filtering, washing precipitate with water, drying at normal temperature, mixing with aluminum stearate, uniformly stirring, feeding into an extruder, carrying out melt extrusion, and cooling to obtain the intercalated reinforced polyamide material.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113604908A (en) * | 2021-09-07 | 2021-11-05 | 宁波瑞耐复合材料有限公司 | Preparation method of carbon nanofiber and nylon composite material reinforced by carbon nanofiber |
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