Heterogeneous nucleating agent toughening-modified phenolic resin foam and preparation method thereof

Abstract

The invention discloses heterogeneous nucleating agent toughening-modified phenolic resin foam and a preparation method thereof. The preparation method of the foam comprises the following steps of preparing a heterogeneous nucleating agent and preparing the modified phenolic resin foam. According to the method, silane coupling agent modified graphene is added for regulating the foam pore structure; meanwhile, the synergistic effect of graphene nanoparticles is exerted, the defects that phenolic foam is poor in mechanical property, high in brittleness and prone to disengagement are effectively overcome, and wide application of the phenolic foam in the engineering field is promoted.

Description

technical field

[0001] The invention relates to a polymer / nano particle foam composite material, in particular to a preparation method of graphene toughened phenolic foam modified by a silane coupling agent. Background technique

[0002] Phenolic foam is currently the fastest growing new type of green thermal insulation material, widely used in civil construction, oil pipelines, military industry, aerospace and other fields. However, after the phenolic resin is cured, the benzene rings are connected by a single methylene group, which lacks flexible groups. This structure leads to excessive density of rigid groups and small rotational freedom of chain links, resulting in high brittleness, and its foam products are fragile, It is easy to pulverize, which seriously restricts the application range and service life of phenolic foam. Therefore, it is of great theoretical and practical significance to study the toughening modification of it, prepare high-performance phenolic foam ...

Examples

Embodiment 1

[0028] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0029] (1) Preparation of heterogeneous nucleating agent:

[0030] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0031] ② Ultrasonic dispersion of 100mg graphene oxide and 100mg calcium oxide in anhydrous tetrahydrofuran for 1 hour, then under the protection of nitrogen, add 2.5mg KH550 dropwise, and stir for 10 hours at 50°C to obtain a black product;

[0032] ③ The black product obtained in step ② is centrifugally washed, dried in a 60°C oven, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0033] (2) Preparation of modified phenolic resin foam:

[0034] ① Weigh 100 parts of expandable phenolic resin, 3 ...

Embodiment 2

[0039] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0040] (1) Preparation of heterogeneous nucleating agent:

[0041] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0042] ② Ultrasonic dispersion of 100mg graphene oxide and 250mg DCC in anhydrous tetrahydrofuran for 1.5h, then under the protection of nitrogen, add 1mg KH560 dropwise, and stir at 70°C for 30h to obtain a black product;

[0043] ③The black product obtained in step ② is centrifugally washed, dried in an oven at 90°C, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0044] (2) Preparation of modified phenolic resin foam:

[0045] ① Weigh 100 parts of expandable phenolic resin, 5 parts of ethylen...

Embodiment 3

[0049] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0050] (1) Preparation of heterogeneous nucleating agent:

[0051] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0052] ② Ultrasonic dispersion of 80mg graphene oxide and 160mg calcium chloride in anhydrous tetrahydrofuran for 1 hour, then under the protection of nitrogen, add 5.6mg KH560 dropwise, and stir for 15 hours at 70°C to obtain a black product;

[0053] ③ The black product obtained in step ② is centrifugally washed, dried in an oven at 65°C, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0054] (2) Preparation of modified phenolic resin foam:

[0055] ①Weigh 100 parts of expandable phenolic resin,...

technical field

[0001] The invention relates to a polymer / nano particle foam composite material, in particular to a preparation method of graphene toughened phenolic foam modified by a silane coupling agent. Background technique

[0002] Phenolic foam is currently the fastest growing new type of green thermal insulation material, widely used in civil construction, oil pipelines, military industry, aerospace and other fields. However, after the phenolic resin is cured, the benzene rings are connected by a single methylene group, which lacks flexible groups. This structure leads to excessive density of rigid groups and small rotational freedom of chain links, resulting in high brittleness, and its foam products are fragile, It is easy to pulverize, which seriously restricts the application range and service life of phenolic foam. Therefore, it is of great theoretical and practical significance to study the toughening modification of it, prepare high-performance phenolic foam ...

Examples

Embodiment 1

[0028] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0029] (1) Preparation of heterogeneous nucleating agent:

[0030] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0031] ② Ultrasonic dispersion of 100mg graphene oxide and 100mg calcium oxide in anhydrous tetrahydrofuran for 1 hour, then under the protection of nitrogen, add 2.5mg KH550 dropwise, and stir for 10 hours at 50°C to obtain a black product;

[0032] ③ The black product obtained in step ② is centrifugally washed, dried in a 60°C oven, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0033] (2) Preparation of modified phenolic resin foam:

[0034] ① Weigh 100 parts of expandable phenolic resin, 3 ...

Embodiment 2

[0039] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0040] (1) Preparation of heterogeneous nucleating agent:

[0041] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0042] ② Ultrasonic dispersion of 100mg graphene oxide and 250mg DCC in anhydrous tetrahydrofuran for 1.5h, then under the protection of nitrogen, add 1mg KH560 dropwise, and stir at 70°C for 30h to obtain a black product;

[0043] ③The black product obtained in step ② is centrifugally washed, dried in an oven at 90°C, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0044] (2) Preparation of modified phenolic resin foam:

[0045] ① Weigh 100 parts of expandable phenolic resin, 5 parts of ethylen...

Embodiment 3

[0049] A heterogeneous nucleating agent toughened modified phenolic resin foam, the preparation method of the foam comprises the steps:

[0050] (1) Preparation of heterogeneous nucleating agent:

[0051] 1. graphene is oxidized into graphene oxide according to the ratio of 1:1 volume ratio of concentrated sulfuric acid (mass concentration is 98%) and concentrated nitric acid (mass concentration is 68%);

[0052] ② Ultrasonic dispersion of 80mg graphene oxide and 160mg calcium chloride in anhydrous tetrahydrofuran for 1 hour, then under the protection of nitrogen, add 5.6mg KH560 dropwise, and stir for 15 hours at 70°C to obtain a black product;

[0053] ③ The black product obtained in step ② is centrifugally washed, dried in an oven at 65°C, and fully ground to obtain graphene oxide grafted with a silane coupling agent, which is the heterogeneous nucleating agent;

[0054] (2) Preparation of modified phenolic resin foam:

[0055] ①Weigh 100 parts of expandable phenolic resin,...

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