阅读说明：本技术 一种插层补强聚酰胺材料及其制备方法 (Intercalation reinforced polyamide material and preparation method thereof ) 是由 李俊 鲍俊瑶 开金文 汪汉雄 方振兴 张文强 于 2019-11-13 设计创作，主要内容包括：本发明公开了一种插层补强聚酰胺材料及其制备方法,所述的插层补强聚酰胺材料由下述重量份的原料组成的：木质素10-16、膨胀珍珠岩40-50、丙烯酸钠30-40、过硫酸铵0.9-1、己内酰胺200-300、2-巯基苯并咪唑1-2、氯化亚砜20-30、硬脂酸8-11、三氧化二锑4-5、三乙胺0.1-0.2、硬脂酸铝4-6、过氧化二异丙苯3-5。本发明的材料具有很好的阻燃和力学稳定性,在遇火燃烧时,木质素燃烧成的碳层可以均匀分布在珍珠岩的层间,形成膨胀碳层,起到隔热防火的效果,从而提高了防火性能。(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.)

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.

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