A kind of fluorine-containing silicone polymer modified furfural acetone epoxy grouting material and preparation method thereof
A technology of acetone epoxy and grouting materials, which is applied in the field of building materials, can solve problems such as poor compatibility and low-temperature toughness, and achieve the effects of good bonding strength, good low-temperature performance, and avoiding phase separation
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Embodiment 1
[0041] Preparation of Fluorinated Silicone Polymer PMSF1
[0042] Add 350g of γ-trifluoropropylmethylcyclotrisiloxane, 50g of octamethylcyclotetrasiloxane, 1,3-bis(3-aminopropyl base)-1,1,3,3-Tetramethyldisiloxane 50g (the mass ratio of the three is 100:14.3:14.3), aminosilane coupling agent N-β-aminoethyl-γ-aminopropyl 12g of methyldiethoxysilane (the total mass of the aforementioned materials is 2.64wt%) and 0.27g of tetramethylammonium hydroxide (the total mass of the aforementioned materials is 0.06wt%), the temperature is raised to 100°C under nitrogen protection, and the reaction is carried out for 6h; Low boilers and solvents are used to obtain amino-terminated and side-amino fluorine-containing silicone polymers, denoted as PMSF1. The weight-average molecular weight of the prepared fluorine-containing silicone polymer was detected by gel permeation chromatography, and the result was 4834g / mol; the amino group content of the fluorine-containing silicone polymer was mea...
Embodiment 2
[0048] Preparation of Fluorinated Silicone Polymer PMSF2
[0049] Add 280g of γ-trifluoropropylmethylcyclotrisiloxane, 120g of octamethylcyclotetrasiloxane, 1,3-bis(3-aminopropyl base)-1,1,3,3-tetramethyldisiloxane 10g (the mass ratio of the three is 100:42.9:6.7), aminosilane coupling agent γ-aminopropylmethyldiethoxysilane 10g (2.3wt% of the total mass of the aforementioned materials) and 0.64g of tetramethylammonium hydroxide (0.15wt% of the total mass of the aforementioned materials), the temperature was raised to 90°C under nitrogen protection, and the reaction was carried out for 8h; Amino and pendant amino fluorine-containing silicone polymers, denoted as PMSF2, have a weight-average molecular weight of 9876 g / mol and an amino content of 0.81 wt%. Through the detection and analysis of proton nuclear magnetic spectrum, the structure of the product is:
[0050]
[0051] The H NMR spectrum data are as follows:
[0052] 1 H NMR (300MHz, CDCl 3 )δ0~0.21ppm(-CH 3 ),0...
Embodiment 3
[0055] Preparation of Fluorinated Silicone Polymer PMSF3
[0056] Add 150g of γ-trifluoropropylmethylcyclotrisiloxane, 250g of octamethylcyclotetrasiloxane, 1,3-bis(3-aminopropyl base)-1,1,3,3-tetramethyldisiloxane 25g (the mass ratio of the three is 100:167:8.9), tetramethylammonium hydroxide 1.0g (the total mass of the aforementioned materials is 0.24wt%), The temperature was raised to 110°C under the protection of nitrogen, and the reaction was carried out for 4 hours; the low boilers and solvents were removed by distillation under reduced pressure, and the fluorine-containing silicone polymer with terminal and side amino groups was obtained, which was denoted as PMSF3, with a weight average molecular weight of 6484g / mol and an amino group content of 0.58 wt%.
[0057] Through the detection and analysis of proton nuclear magnetic spectrum, the structure of the product is:
[0058]
[0059] The H NMR spectrum data are as follows:
[0060] 1 H NMR (300MHz, CDCl 3 )δ0~...
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