Method for producing epoxy composite materials based on modified hydrated cellulose technical threads
By modifying hydrated cellulose technical threads with epoxy binders and forming physicochemical bonds, the method enhances the mechanical properties of polymer composite materials, addressing the limitations of existing methods.
Patent Information
- Authority / Receiving Office
- RU · RU
- Patent Type
- Patents
- Current Assignee / Owner
- FEDERALNOE GOSUDARSTVENNOE AVTONOMNOE OBRAZOVATELNOE UCHREZHDENIE VYSSHEGO OBRAZOVANIYA NATSIONALNYJ ISSLEDOVATELSKIJ YADERNYJ UNIV MIFI (NIYAU MIFI)
- Filing Date
- 2026-03-12
- Publication Date
- 2026-07-07
AI Technical Summary
Existing methods for producing polymer composite materials using epoxy resins and viscose technical threads result in insufficient bending strength, impact toughness, and hardness.
The method involves impregnating hydrated cellulose technical threads (GCTN) with an epoxy binder modified by 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, or 3-methacryloxypropyltrimethoxysilane, followed by pressing and heating under specific conditions to form physicochemical bonds, enhancing the interaction between epoxy groups and organofunctional groups.
This approach significantly increases the bending strength, impact toughness, and hardness of the composite materials, achieving improved mechanical properties.
Smart Images
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Abstract
Description
[0001] The invention relates to the production of polymer composite materials and can be used in the technology of producing epoxy plastics reinforced with hydrated cellulose technical threads (GCTN) to increase their bending strength, impact toughness and hardness.
[0002] A known technology includes a method (patent 1616930 IPC C08G 8 / 28, C08L 61 / 10, published 30.12.90) for producing composite materials based on chemical fibers, which consists of impregnating a fibrous filler based on viscose technical thread with a mixture containing phenol, formaldehyde, caustic soda and an epoxy resin with an epoxy group content of 22 wt. % at a component weight ratio of 1: 0.36-0.416: 0.02-0.025: 0.05-0.2 and a filling degree of 50.5 wt. %. The polycondensation process is carried out in a heat chamber at a temperature of 100 ° C for 25 minutes. The resulting press material is dried at a temperature of 120 ° C for 15 minutes. The disadvantage of this method is the insufficiently high strength characteristics of composite materials.
[0003] The closest to the claimed invention is the method for producing a reinforced polymer composite material, adopted as a prototype, given in patent 2324709 IPC C08J 5 / 24, C08J 5 / 06, C08L 63 / 02, C08G 59 / 56, B29C 35 / 08, published. 05 / 20 / 2008. The production method consists in impregnating viscose technical thread with a mixture of ED-20 epoxy resin and polyethylenepolyamine hardener at a mass ratio of components of 9:1 and forming a bundle of separately impregnated threads with a thread count of 100, heat treatment at a temperature of 30-70 ° C. At the same time, the formed bundle is subjected to ultraviolet radiation with a power of 0.70-0.80 W / m 3 at a wavelength of λ = 253.7 nm for 8-12 minutes and cured at a temperature of 20-25°C for 24 hours. The disadvantage of this method is the length of the process of obtaining the epoxy composite material and insufficiently high values of bending stress (133 MPa), impact strength (74 kJ / m 2) and Brinell hardness (171 MPa).
[0004] The technical result is aimed at increasing the strength of composite materials based on modified GCTN due to the physicochemical interaction between the epoxy groups of the binder and the organofunctional groups of GCTN modified with 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and 3-methacrylokispropyltrimethoxysilane with the formation of physicochemical bonds.
[0005] The technical result is achieved due to the fact that in the proposed method, composite materials are obtained based on modified GCTN by pressing a composition obtained by impregnation with an epoxy binder GCTN modified with a solution containing 5 wt. % 3-aminopropyltriethoxysilane, or GCTN modified with a solution containing 5 wt. % 3-glycidoxypropyltrimethoxysilane, or GCTN modified with a solution containing 5 wt. % 3-methacrylokispropyltrimethoxysilane, under the following conditions:
[0006] temperature, °C, 18-22
[0007] content of modified GCTN in the composition, wt. %, 49-51
[0008] content of epoxy binder in the composition, wt. %, 49-51,
[0009] obtained by mixing epoxy oligomer ED-20 with polyethylene polyamine hardener to a homogeneous state under the following conditions:
[0010] temperature, °C, 18-22
[0011] content of ED-20 epoxy oligomer in the binder, wt. %, 89-91
[0012] content of polyethylenepolyamine hardener in the binder, wt. %, 9-11,
[0013] followed by maintaining the composition consisting of 3-aminopropyltriethoxysilane-modified GCTN, or 3-glycidoxypropyltrimethoxysilane-modified GCTN, or 3-methacryloxypropyltrimethoxysilane-modified GCTN impregnated with an epoxy binder in a closed form under a pressure of 4.5-5.5 MPa when heated to a temperature of 105-115°C at a heating rate of 10°C per minute for 55-65 minutes in a laboratory thermal furnace.
[0014] Below are examples of implementation of the proposed method.
[0015] The process of modifying GCTN with a solution containing (by weight) 5% 3-glycidoxypropyltrimethoxysilane is described in patent 2816360 IPC D01F 11 / 02, published 03 / 28 / 2024.
[0016] Example 1
[0017] The GCTNs, modified with a solution containing 5 wt.% 3-aminopropyltriethoxysilane, are impregnated in the form of unidirectional continuous threads with an epoxy binder obtained by mixing 90 wt.% ED-20 epoxy oligomer with 10 wt.% polyethylenepolyamine hardener until a homogeneous state is obtained. The resulting composition, containing 50 wt.% modified GCTNs and 50 wt.% epoxy binder, is maintained in a closed mold under a pressure of 5.0 MPa while heating to a temperature of 110°C for 60 minutes in a laboratory heating furnace.
[0018] Example 2
[0019] GCTNs modified with a solution containing 5 wt.% 3-glycidoxypropyltrimethoxysilane are impregnated in the form of unidirectional continuous threads with an epoxy binder obtained by mixing 90 wt.% ED-20 epoxy oligomer with 10 wt.% polyethylenepolyamine hardener until a homogeneous state is obtained. The resulting composition, containing 50 wt.% modified GCTNs and 50 wt.% epoxy binder, is maintained in a closed mold under a pressure of 5.0 MPa while heating to a temperature of 110°C for 60 minutes in a laboratory heating furnace.
[0020] Example 3
[0021] The GCTNs, modified with a solution containing 5 wt.% 3-methacryloxypropyltrimethoxysilane, are impregnated in the form of unidirectional continuous threads with an epoxy binder obtained by mixing 90 wt.% ED-20 epoxy oligomer with 10 wt.% polyethylenepolyamine hardener until a homogeneous state is obtained. The resulting composition, containing 50 wt.% modified GCTNs and 50 wt.% epoxy binder, is maintained in a closed mold under a pressure of 5.0 MPa while heating to a temperature of 110°C for 60 minutes in a laboratory heating furnace.
[0022] The properties of composite materials based on modified GTsTN were studied using an IR 5046-5 tensile testing machine, a KM-5 pendulum impact tester, and a TM-2M hardness tester. Table 1 (see graphic section) presents the properties of composite materials based on modified GTsTN.
[0023] As a result of the experiments, the limits for obtaining composite materials based on modified GCTN by the proposed method were selected, which made it possible to increase the bending stress - 223-317 MPa, impact strength - 119-218 kJ / m 2 and Brinell hardness of 228-260 MPa of composite materials based on modified GCTN (example 1-3) compared to the prototype, which was a composite material obtained by impregnating viscose technical thread with a mixture of ED-20 epoxy resin and polyethylene polyamine hardener at a mass ratio of components of 9:1.
[0024] When obtaining composite materials based on modified GCTN by pressing a composition containing 50 wt. % GCTN modified with 3-aminopropyltriethoxysilane or 50 wt. % GCTN modified with 3-glycidoxypropyltrimethoxysilane or 50 wt. % GCTN modified with 3-methacryloxypropyltrimethoxysilane and 50 wt. % of epoxy binder, followed by maintaining the composition in a closed form under a pressure of 4.5-5.5 MPa while heating to a temperature of 105-115°C at a heating rate of 10°C per minute for 55-65 minutes in a laboratory thermal furnace, an increase in the strength of composite materials is achieved as a result of the physicochemical interaction between the epoxy groups of the binder and the organofunctional groups of GCTN modified with 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane and 3-methacrylokispropyltrimethoxysilane with the formation of physicochemical bonds.
[0025] Thus, the invention makes it possible to increase the bending strength, impact toughness and hardness of composite materials based on hydrated cellulose technical threads and can find application in the technology of producing polymer composite materials.
Claims
A method for producing composite materials based on modified hydrated cellulose technical threads (GCTN), comprising pressing a composition containing modified GCTN impregnated with an epoxy binder, characterized in that the process for producing composite materials is carried out by pressing a composition obtained by impregnating GCTN with an epoxy binder, modified with a solution containing 5 wt.% 3-aminopropyltriethoxysilane, or GCTN modified with a solution containing 5 wt.% 3-glycidoxypropyltrimethoxysilane, or GCTN modified with a solution containing 5 wt.% 3-methacrylokispropyltrimethoxysilane, under the following conditions: temperature, °C, 18-22 content of modified GCTN in the composition, wt.%, 49-51 content of epoxy binder in the composition, wt.%, 49-51, obtained by mixing epoxy oligomer ED-20 with polyethylene polyamine hardener until a homogeneous state is achieved under the following conditions: temperature, °C, 18-22 content of epoxy oligomer ED-20 in the binder, wt.%, 89-91 content of polyethylene polyamine hardener in the binder, wt.%, 9-11, followed by maintaining the composition consisting of 3-aminopropyltriethoxysilane-modified GCTN, or 3-glycidoxypropyltrimethoxysilane-modified GCTN, or 3-methacryloxypropyltrimethoxysilane-modified GCTN impregnated with an epoxy binder in a closed form under a pressure of 4.5-5.5 MPa when heated to a temperature of 105-115 °C at a heating rate of 10 °C per minute for 55-65 minutes in a laboratory thermal furnace.