Diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant as well as preparation method and application thereof

Abstract

The invention relates to the field of flame-retardant substances, in particular to a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant as well as a preparation method and application thereof. The preparation method comprises the following steps: melting diisobutyl aluminum hypophosphite in a high-temperature internal mixer, and adding montmorillonite for internal mixing and blending; performing high-speed stirring on the kneaded powder subjected to internal mixing in a high-speed mixer, and performing spray grafting on a silane coupling agent; grinding the silane coupling agent grafted diisobutyl aluminum hypophosphite intercalated montmorillonite into powder by using an airflow mill, and controlling the particle size to be 10-20 microns; polyimide (PI is a polymer containing an imide ring (-CO-NCO-1) repetitive group, is a faint yellow solid or powder in appearance, and has good flame retardance and low smoke formation without adding other auxiliaries, LOI can reach up to 47%, and the combustion grade is UL94-V-0 grade.

Description

Technical Field

[0001] The invention relates to the field of flame retardant materials, in particular to a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant and a preparation method and application thereof. Background Art

[0002] Diisobutyl aluminum hypophosphite (AHP) is a new type of organic halogen-free, green and environmentally friendly flame retardant. The product is insoluble in water and organic solvents, but easily soluble in strong alkaline solutions. It is an organic hypophosphite with high flame retardant efficiency, high thermal stability, non-toxicity, low smoke, low specific gravity, low melting point, and good dispersibility. However, diisobutyl aluminum hypophosphite has the risk of precipitation.

[0003] On December 10, 2024, with "diisobutyl aluminum hypophosphite and flame retardant and montmorillonite" as the abstract keywords, and the option to allow synonym expansion, a search was conducted in the China Patent Publication Database, and the "Study on the Microstructure, Dynamic Rheological Behavior and Flame Retardant Properties of Halogen-free Flame Retardant Nylon / Montmorillonite Composites" was found; this paper explores and compares the effects of the interaction between different montmorillonites and polymers on the structure, rheological behavior and flame retardant properties of flame-retardant nanocomposites. Studies have shown that the interfacial tension between CMMT and polymers is the smallest, the interaction is the strongest, and the dispersion of montmorillonite in polymers is good. For flame-retardant polymer nanocomposites, the strong interaction between CMMT and polymers can significantly improve the dispersion of CMMT in the system, help CMMT sheets form a particle network structure in space, restrict the movement of molecular chains, and improve melt stability, thereby effectively improving the combustion behavior of the material.

[0004] On December 10, 2024, an abstract search for "diisobutyl aluminum hypophosphite and flame retardant and montmorillonite" was conducted on China National Knowledge Infrastructure, and no relevant literature was found.

[0005] On December 10, 2024, a search was conducted on the website of the United States Patent and Trademark Office for "Diisobutyl aluminum phosphate with flame retardantwithmontmorillonite", and no relevant literature was found; the search URL was https: / / ppubs.uspto.gov / pubwebapp / .

[0006] On December 10, 2024, a search was conducted on the Korean Patent Office for "Diisobutyl aluminum phosphate and flame retardant and montmorillonite", but no relevant literature was found; the search URL was http: / / eng.kipris.or.kr / enghome / main.jsp.

[0007] On December 10, 2024, a search was conducted on WIPO's https: / / patentscope2.wipo.int / for "Diisobutyl aluminum phosphate and flame retardanttand montmorillonite", and no relevant documents were found.

[0008] On December 10, 2024, a search was conducted on the Japan Patent Office website https: / / www.j-platpat.inpit.go.jp / for "Diisobutyl aluminum phosphate and flame retardanttandmontmorillonite", but no relevant literature was found.

[0009] Completely different from the concept of this patent. Summary of the invention

[0010] Purpose of the invention: To provide a better diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant and its preparation method and use. The specific purpose can be seen in the multiple substantial technical effects of the specific implementation part.

[0011] In order to achieve the above purpose, the present invention adopts the following technical solutions: The invention discloses a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that diisobutyl aluminum hypophosphite is intercalated into montmorillonite to avoid precipitation of diisobutyl aluminum hypophosphite.

[0012] The invention discloses a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that the diisobutyl aluminum hypophosphite grafted with a silane coupling agent is intercalated into montmorillonite to avoid the precipitation of the diisobutyl aluminum hypophosphite.

[0013] The preparation method of diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant is characterized in that the lamellar structure of montmorillonite is utilized, diisobutyl aluminum hypophosphite is melted at high temperature, and mixed and intercalated into montmorillonite to improve precipitation.

[0014] A further technical solution of the present invention is to include the following steps: The diisobutyl aluminum hypophosphite is melted in a high-temperature internal mixer, and montmorillonite is added to perform internal mixing; The kneaded powder after internal mixing is stirred at high speed in a high-speed mixer, and the silane coupling agent is sprayed for grafting; The diisobutyl aluminum hypophosphite intercalated montmorillonite grafted with a silane coupling agent is ground by a jet mill to control the particle size to 10-20 um.

[0015] The present invention adopting the above technical solution has the following beneficial effects compared with the prior art: We have found through a large number of experiments that thermosetting polyimide can be used as a good flame retardant carbon-forming agent. Therefore, we invented a polymer flame retardant using thermosetting polyimide as a carbon-forming agent, which is applied to the flame retardancy of polymers. Polyimide (PI refers to a polymer containing imide ring (-CO-NCO-) repeating groups, with a light yellow solid or powder appearance. It has good flame retardancy and low smoke without the addition of other additives, LOI can be as high as 47%, and the combustion grade is UL94-V-0. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] In order to further illustrate the present invention, the following is further described in conjunction with the accompanying drawings: Figure 1 A diagram of the steps of the invention. DETAILED DESCRIPTION

[0017] The present invention is further explained below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In the description of the present invention, it should be noted that the orientation or position relationship indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", "top", "bottom", etc. is based on the orientation or position relationship shown in the accompanying drawings, which is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation of the present invention. In addition, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be directly connected, or indirectly connected through an intermediate medium, or it can be the internal connection of two elements. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood in specific circumstances.

[0018] The invention discloses a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that the diisobutyl aluminum hypophosphite grafted with a silane coupling agent is intercalated into montmorillonite to avoid the precipitation of the diisobutyl aluminum hypophosphite.

[0019] The preparation method of diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant is characterized in that the lamellar structure of montmorillonite is utilized, diisobutyl aluminum hypophosphite is melted at high temperature, and mixed and intercalated into montmorillonite to improve precipitation.

[0020] The following steps are included: The diisobutyl aluminum hypophosphite is melted in a high-temperature internal mixer, and montmorillonite is added to perform internal mixing; The kneaded powder after internal mixing is stirred at high speed in a high-speed mixer, and the silane coupling agent is sprayed for grafting; The diisobutyl aluminum hypophosphite intercalated montmorillonite grafted with a silane coupling agent is ground by a jet mill to control the particle size to 10-20 um.

[0021] Thermosetting polyimide waste is mechanically ground, and the recycled polyimide scraps are cut into pieces and then crushed. Use the following crushers for crushing: extrusion crusher, turbine crusher, air flow crusher, etc. You can also use a combination of multiple different crushers. In order to prevent polyimide degradation, the raw polyimide film can be immersed in liquid nitrogen before crushing; After cutting with a slitter, it was immersed in liquid nitrogen for 1 minute and then crushed in an extrusion mill. The obtained powder was observed by scanning electron microscope to be flat particles with an average particle size of 10-20μm. APP (ammonium polyphosphate) and PI powder are compounded in a ratio of 1:1-5:1 and added to polyolefin resin at a percentage of 20-30 to achieve UL94 1.6mm-V0 flame retardancy. AHP (aluminum hypophosphite) and PI powder are compounded in a ratio of 1:1-3:1 and added to TPE / TPU at a percentage of 25-30 to achieve UL94 1.6mm-V0 flame retardancy. By compounding ADP (diethylaluminum hypophosphite) and PI powder in a ratio of 1:1-3:1 and adding 15-25% to PA, UL94 1.6mm-V0 flame retardancy can be achieved.

[0022] It should be noted that the multiple solutions provided by this patent include the basic solution itself, which are independent of each other and do not restrict each other, but they can also be combined with each other without conflict to achieve multiple effects together.

[0023] The basic principle, main features and advantages of the present invention are shown and described above. Those skilled in the art should understand that the present invention is not limited to the above embodiments, and the above embodiments and descriptions are only for explaining the principles of the present invention. Without departing from the spirit and scope of the present invention, the present invention may have various changes and improvements, and these changes and improvements all fall within the scope of the protection required.

Claims

1. Diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that: Diisobutyl aluminum hypophosphite was intercalated into montmorillonite to avoid the precipitation of diisobutyl aluminum hypophosphite.

2. Diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that: Silane coupling agent grafted diisobutyl aluminum hypophosphite was intercalated into montmorillonite to avoid the precipitation of diisobutyl aluminum hypophosphite.

3. A method for preparing a diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant, characterized in that: By utilizing the lamellar structure of montmorillonite, diisobutyl aluminum hypophosphite is intercalated into montmorillonite by means of high temperature melting, mixing and blending to improve precipitation.

4. The method for preparing the diisobutyl aluminum hypophosphite intercalated montmorillonite flame retardant according to claim 3, characterized in that: The following steps are included: The diisobutyl aluminum hypophosphite is melted in a high-temperature internal mixer, and montmorillonite is added to perform internal mixing; The kneaded powder after internal mixing is stirred at high speed in a high-speed mixer, and the silane coupling agent is sprayed for grafting; The diisobutyl aluminum hypophosphite intercalated montmorillonite grafted with a silane coupling agent is ground by a jet mill to control the particle size to 10-20 um.

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