A highly active moisture-curing organosilicon polymer component and its preparation process
By preparing highly reactive moisture-curing silicone polymer components, the safety hazards and slow curing speed of using organotin catalysts in existing silane-terminated polyether resins are solved, and a fast and environmentally friendly bonding and sealing effect is achieved.
Patent Information
- Application Number
- CN202411654769.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-19
- Publication Date
- 2025-07-22
- Estimated Expiration
- 2044-11-19
AI Technical Summary
The existing silane-capped polyether resins use organic tin catalysts that can cause potential human damage and cure speed is slow, making it difficult to meet the fast bonding and sealing needs of home decoration and industrial assembly.
Highly active α-silane is used as a moisture curing agent, and the polyether polyol is reacted with organic polyisocyanate, and the moisture curing silane blocking agent is added to prepare high-active moisture curing silicone polymer components, avoid the use of metal tin catalysts, and optimize the crosslinking and adhesion of the polyether resin.
It realizes rapid deep curing without metal tin catalyzed, releases small molecule alcohols, is environmentally friendly and pollution-free, has strong adhesiveness, and is brushable, suitable for home decoration and industrial assembly.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of silane-modified polyether resins, and specifically discloses a highly active moisture-curable organosilicon polymer component and its preparation process. Background Art
[0002] Silane-capped polyether resin is a technical product obtained by capping polyether with a silane capping agent containing active groups. It combines the dual advantages of organosilicon and polyurethane, has good weather resistance and colloid strength, and the small molecule alcohols released after its curing are safe and environmentally friendly.
[0003] Silane-capped polyether resin is often used to prepare silane-capped polyether sealants. Compared with silicone sealants, silane-capped polyether sealants do not produce pungent odors during curing and can be painted on the surface; compared with polyurethane sealants, silane-capped polyether sealants have better weather resistance, do not contain free isocyanates, and do not contain organic solvents. This kind of silane-capped polyether sealant maximally combines the advantages of silicone sealants and polyurethane sealants, while avoiding the disadvantages of silicone sealants and polyurethane sealants, so it has a wide range of applications.
[0004] The silane used in conventional silane-capped polyether resins is γ-silane, and organic tin catalysts are required for curing, which may cause harm to the human body. While the highly active moisture-curable organosilicon polymer component uses highly active α-silane and does not require the use of metal tin for catalytic curing. It has the advantages of strong adhesion, paintable, no pollutant volatilization during curing, and good deep curing, and is especially suitable for the fields of bonding and sealing of structural parts such as home decoration, construction, and industrial assembly. Therefore, it is of great significance to develop a highly active moisture-curable organosilicon polymer component with better performance and faster curing speed and its preparation method. Summary of the Invention
[0005] The purpose of the present invention is to provide a highly active moisture-curable organosilicon polymer component and its preparation process to solve the problems raised in the prior art.
[0006] To achieve the above purpose, the present invention provides the following technical solution: A preparation process of a highly active moisture-curable organosilicon polymer component, comprising the following steps: S1: Dehydrating and degassing polyether polyol, cooling it to 30-50°C, adding organic polyisocyanate, and stirring and reacting at 40-80°C for 2-4 hours to obtain a hydroxyl-terminated prepolymer;
[0007] S2: Adding a moisture-curable silane capping agent and reacting at 40-60°C for 2-4 hours under the protection of an inert atmosphere to obtain the highly active moisture-curable organosilicon polymer component.
[0008] More preferably, the specific process of the dehydration and degassing treatment comprises the following steps: Treating at a temperature of 100-120°C for 1-3 hours.
[0009] Preferably, the organic polyisocyanate includes one or more of toluene diisocyanate, diphenylmethane diisocyanate, hexamethylene diisocyanate, and isophorone diisocyanate.
[0010] Preferably, the organic polyisocyanate is hexamethylene diisocyanate (HDI), BASF.
[0011] Preferably, in the highly active moisture-curable organosilicon polymer component, the addition amount of the organic polyisocyanate is 0.4-1.5% of the mass of the polyether polyol; the addition amount of the moisture-curable silane end-capping agent is 2-5% of the mass of the hydroxyl-terminated prepolymer.
[0012] Preferably, the preparation of the moisture-curable silane end-capping agent includes the following steps: Mix chloromethyltriethoxysilane, potassium cyanate, ethanol, DMF, and 18-crown-6 ether evenly, heat up to 120-125 °C and react for 11-12 h, filter, and the distillate after rectification is the moisture-curable silane end-capping agent.
[0013] Preferably, the moisture-curable silane end-capping agent includes the following raw materials, by mass: 100-120 parts of chloromethyltriethoxysilane, 50-60 parts of potassium cyanate, 6-8 parts of ethanol, 50-60 parts of DMF, and 1-2 parts of 18-crown-6 ether.
[0014] Preferably, the functionality of the polyether polyol is 2, and the number average molecular weight is 4000-20000.
[0015] Preferably, the polyether polyol is DL-8000 with a functionality of 2, provided by Shandong Bluestar Dongda Co., Ltd., and the number average molecular weight is 8000.
[0016] Preferably, the polyether polyol includes DL-8000, four-arm polyethylene glycol epoxy, and modified polyethylene glycol in a mass ratio of (8-9):(0.5-0.8):(0.8-1). The preparation of the modified polyethylene glycol includes the following steps: Take four-arm polyethylene glycol epoxy and dimethyl 3-aminophthalate, add them to a solvent and mix evenly, heat up to 60-70 °C, stir for 5-8 h, and remove the solvent to obtain the modified polyethylene glycol.
[0017] Preferably, in the modified polyethylene glycol, the molar ratio of four-arm polyethylene glycol epoxy to dimethyl 3-aminophthalate is 1:(1.8-2).
[0018] Preferably, in the highly active moisture-curable organosilicon polymer component, a catalyst N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is also added, accounting for 0.5-1% of the total mass of the highly active moisture-curable organosilicon polymer component.
[0019] Preferably, after adding the catalyst N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and mixing evenly, and curing and maintaining in the moisture in the air for one week, the modulus of the obtained gel is 0.4 mPa to 1 mPa.
[0020] Compared with the prior art, the beneficial effects achieved by the present invention are as follows: (1) The highly active moisture-curing organosilicon polymer component does not contain free isocyanate, can be cured without metal tin catalysis, and has fast deep curing; after the resin is cured, small molecule alcohols are released, with low VOC emissions, environmental protection and no pollution, strong adhesion to the substrate, can be painted, and has good mechanical properties.
[0021] (2) In the scheme, DL-8000 is replaced by DL-8000, tetra-arm polyethylene glycol-epoxy group, and modified polyethylene glycol with a mass ratio of (8-9):(0.5-0.8):(0.8-1); its advantages are as follows: The tetra-arm polyethylene glycol-epoxy group contains multiple functional groups that can participate in the reaction, which can improve the crosslinking degree of the polyether resin, thereby improving its mechanical properties; the modified polyethylene glycol is prepared from tetra-arm polyethylene glycol-epoxy group and dimethyl phthalate-3-amine with a molar ratio of 1:(1.8-2), which plays a toughening role; and polyethylene glycol has strong hydrophilicity, which can accelerate the curing of the polyether resin;
[0022] The addition amounts of the above substances in the polyether resin need to be strictly controlled. Excessive addition of the tetra-arm polyethylene glycol-epoxy group leads to a large degree of branching, obvious viscosity change and may lead to a decrease in mechanical properties. At the same time, excessive crosslinking degree leads to a decrease in water absorption rate and a decrease in curing speed; when the addition amount of the modified polyethylene glycol is large, the mechanical properties may decrease due to steric hindrance. Specific Embodiments
[0023] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0024] Unless otherwise specified, the following parts are all parts by mass;
[0025] Example 1: S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane end-capping agent;
[0026] S2: Charge 1000 parts of polyether polyol DL-8000 into a reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 5.32 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0027] S3: Under nitrogen protection, add 28.12 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 50 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0028] Example 2: S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 ether evenly, heat up to 120 °C and react for 12 h, filter, and the rectified distillate is a moisture-curing silane-terminated agent;
[0029] S2: Charge 1000 parts of polyether polyol DL-8000 into a reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 5.3 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 70 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0030] S3: Under nitrogen protection, add 42.06 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 50 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0031] Example 3: S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 ether evenly, heat up to 120 °C and react for 12 h, filter, and the rectified distillate is a moisture-curing silane-terminated agent;
[0032] S2: Charge 1000 parts of polyether polyol DL-8000 into a reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 9.05 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 70 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0033] S3: Under nitrogen protection, add 30.11 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0034] Example 4: S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 ether evenly, heat up to 120 °C and react for 12 h, filter, and the rectified distillate is a moisture-curing silane-terminated agent;
[0035] S2: Put 1000 parts of polyether polyol DL-8000 into the reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0036] S3: Under nitrogen protection, add 36.08 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0037] Example 5: S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane-terminated agent;
[0038] S2: Take tetra-arm-polyethylene glycol-epoxy group and dimethyl phthalate-3-amino with a molar ratio of 1:2, and mix them evenly in DMF with a mass 10 times that of the tetra-arm-polyethylene glycol-epoxy group, heat up to 65 °C and stir for 6 h, remove the solvent to obtain modified polyethylene glycol; Mix DL-8000, tetra-arm-polyethylene glycol-epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:0.6:0.8 to obtain polyether polyol;
[0039] S3: Put 1000 parts of polyether polyol into the reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0040] S4: Under nitrogen protection, add 36.08 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0041] Comparative Example 1 (changing the mass ratio of DL-8000, tetra-arm-polyethylene glycol-epoxy group, and modified polyethylene glycol, and the remaining method steps are the same as those in Example 5): S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane-terminated agent;
[0042] S2: Take tetra-arm polyethylene glycol epoxy group and dimethyl 3-aminophthalate with a molar ratio of 1:2, mix them evenly in DMF which is 10 times the mass of tetra-arm polyethylene glycol epoxy group, heat up to 65 °C and stir for 6 h, remove the solvent to obtain modified polyethylene glycol; Mix DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:1:0.5 to obtain polyether polyol;
[0043] S3: Put 1000 parts of polyether polyol into a reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0044] S4: Under nitrogen protection, add 36.08 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0045] Comparative Example 2 (changing the mass ratio of DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol, and the other method steps are the same as those in Example 5): S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane-terminated agent;
[0046] S2: Take tetra-arm polyethylene glycol epoxy group and dimethyl 3-aminophthalate with a molar ratio of 1:2, mix them evenly in DMF which is 10 times the mass of tetra-arm polyethylene glycol epoxy group, heat up to 65 °C and stir for 6 h, remove the solvent to obtain modified polyethylene glycol; Mix DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:0.3:1.2 to obtain polyether polyol;
[0047] S3: Put 1000 parts of polyether polyol into a reaction kettle, heat up to 110 °C, stir, evacuate to dehydrate and degas for 3 hours, cool down to 40 °C, then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0048] S4: Under nitrogen protection, add 36.08 parts of a moisture-curing silane-terminated agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0049] Comparative Example 3 (changing the mass ratio of DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol, and the remaining method steps are the same as those in Example 5): S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 ether evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane end-capping agent;
[0050] S2: Take tetra-arm polyethylene glycol epoxy group and dimethyl phthalate-3-amine in a molar ratio of 1:2, mix them evenly in DMF which is 10 times the mass of tetra-arm polyethylene glycol epoxy group, heat up to 65 °C and stir for 6 h, remove the solvent to obtain modified polyethylene glycol; Mix DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of 7.5:1:1 to obtain polyether polyol;
[0051] S3: Put 1000 parts of polyether polyol into the reaction kettle, heat up to 110 °C, stir, evacuate to remove water and gas for 3 hours, cool down to 40 °C and then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0052] S4: Under nitrogen protection, add 36.08 parts of the moisture-curing silane end-capping agent to the hydroxyl-terminated prepolymer prepared in step S2, and react at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0053] Comparative Example 4 (changing the mass ratio of tetra-arm polyethylene glycol epoxy group and dimethyl phthalate-3-amine in the modified polyethylene glycol, and the remaining method steps are the same as those in Example 5): S1: Mix 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 ether evenly, heat up to 120 °C and react for 12 h, filter, and the distillate after rectification is the moisture-curing silane end-capping agent;
[0054] S2: Take tetra-arm polyethylene glycol epoxy group and dimethyl phthalate-3-amine in a molar ratio of 1:1, mix them evenly in DMF which is 10 times the mass of tetra-arm polyethylene glycol epoxy group, heat up to 65 °C and stir for 6 h, remove the solvent to obtain modified polyethylene glycol; Mix DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:0.6:0.8 to obtain polyether polyol;
[0055] S3: Put 1000 parts of polyether polyol into the reaction kettle, heat up to 110 °C, stir, evacuate to remove water and gas for 3 hours, cool down to 40 °C and then add 9.01 parts of hexamethylene diisocyanate, and react and polymerize at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0056] S4: Under nitrogen protection, 36.08 parts of a moisture-curing silane end-capping agent were added to the hydroxyl-terminated prepolymer prepared in step S2, and the mixture was reacted at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0057] Comparative Example 5 (changing the mass ratio of tetra-arm polyethylene glycol-epoxy group and dimethyl 3-aminophthalate in the modified polyethylene glycol, and the remaining method steps are the same as those in Example 5): S1: 100 parts of chloromethyltriethoxysilane, 50 parts of potassium cyanate, 6 parts of ethanol, 50 parts of DMF, and 1 part of 18-crown-6 were mixed evenly, heated to 120 °C and reacted for 12 h, filtered, and the distillate after rectification was the moisture-curing silane end-capping agent;
[0058] S2: Tetra-arm polyethylene glycol-epoxy group and dimethyl 3-aminophthalate with a molar ratio of 1:3 were taken, mixed evenly in DMF with a mass 10 times that of the tetra-arm polyethylene glycol-epoxy group, heated to 65 °C and stirred for 6 h, the solvent was removed to obtain modified polyethylene glycol; DL-8000, tetra-arm polyethylene glycol-epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:0.6:0.8 were mixed to obtain a polyether polyol;
[0059] S3: 1000 parts of the polyether polyol were put into a reaction kettle, heated to 110 °C, stirred, evacuated to remove water and gas for 3 hours, cooled to 40 °C, and then 9.01 parts of hexamethylene diisocyanate were added, and the reaction was polymerized at a reaction temperature of 75 °C for 3 hours to obtain a hydroxyl-terminated prepolymer;
[0060] S4: Under nitrogen protection, 36.08 parts of a moisture-curing silane end-capping agent were added to the hydroxyl-terminated prepolymer prepared in step S2, and the mixture was reacted at 55 °C for 3 hours to obtain a highly active moisture-curing organosilicon polymer component.
[0061] In the above examples, the test methods used were all conventional methods without special instructions; the raw materials used were all commercially available without special instructions, and the raw material sources were as follows: chloromethyltriethoxysilane (CAS: 15267-95-5); potassium cyanate (CAS: 590-28-3); ethanol (CAS: 64-17-5); DMF (CAS: 68-12-2); 18-crown-6 (CAS: 17455-13-9); tetra-arm polyethylene glycol-epoxy group (molecular weight 2k, Xi'an Kaixin Biotechnology Co., Ltd.); dimethyl 3-aminophthalate (S98852, Shanghai Yuanye).
[0062] Experiment (1): The highly active moisture-curing organosilicon polymer components prepared in Examples 1 to 4 were taken, 0.6% of the total mass of a catalyst was added and mixed evenly, and at 25 °C, the viscosity, surface dry time, hardness, and tensile strength of the gel obtained after moisture-curing and curing in air for one week were measured respectively, and the test results are shown in Table 1;
[0063] Table 1:
[0064]
[0065] (2) Based on Example 4, replace DL-8000 with DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of 8.5:0.6:0.8 to obtain Example 5; Take the highly active moisture-curing organosilicon polymer components prepared in Example 5 and Comparative Examples 1-5, add a catalyst accounting for 0.6% of the total mass, mix evenly, cure and maintain in the air at 25°C for one week, and test the surface drying time and tensile strength. The test results are shown in Table 2;
[0066] Table 2:
[0067]
[0068] Conclusion: Changing the mass ratio of DL-8000, tetra-arm polyethylene glycol epoxy group, and modified polyethylene glycol in Comparative Examples 1-3 results in performance inferior to that of the examples. It can be seen that the ratio of each substance in the polyether polyol is of great significance; Changing the mass ratio of tetra-arm polyethylene glycol epoxy group and dimethyl 3-aminophthalate in the modified polyethylene glycol in Comparative Examples 4-5 leads to a decrease in performance due to the structural change. It can be seen that controlling the ratio is important; In summary, the highly active moisture-curing organosilicon polymer component prepared by the present invention has good mechanical properties, fast curing speed, good viscosity and meets environmental protection requirements.
[0069] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, it is intended to embrace all changes falling within the meaning and scope of the equivalent elements of the claims in the present invention.
Claims
1. A preparation process of a highly active moisture-curing organosilicon polymer component, characterized in that: It includes the following steps: S1: Perform dehydration and degassing treatment on the polyether polyol, cool it down to 30 - 50 °C, add organic polyisocyanate, and stir and react at 40 - 80 °C for 2 - 4 h to obtain a hydroxyl-terminated prepolymer; S2: Add a moisture-curing silane end-capping agent, and react at 40 - 60 °C for 2 - 4 h under the protection of an inert atmosphere to obtain the high-activity moisture-curing organosilicon polymer component; The polyether polyol includes DL-8000, four-arm polyethylene glycol epoxy group, and modified polyethylene glycol with a mass ratio of (8 - 9):(0.5 - 0.8):(0.8 - 1). The preparation of the modified polyethylene glycol includes the following steps: Take the four-arm polyethylene glycol epoxy group and dimethyl 3-aminophthalate, add them to a solvent and mix evenly, heat up to 60 - 70 °C, stir for 5 - 8 h, remove the solvent to obtain the modified polyethylene glycol; In the high-activity moisture-curing organosilicon polymer component, a catalyst N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is also added, accounting for 0.5 - 1% of the total mass of the high-activity moisture-curing organosilicon polymer component.
2. The preparation process of a highly active moisture-curable organosilicon polymer component according to claim 1, characterized in that: In the high-activity moisture-curing organosilicon polymer component, the addition amount of the organic polyisocyanate is 0.4 - 1.5% of the mass of the polyether polyol; the addition amount of the moisture-curing silane end-capping agent is 2 - 5% of the mass of the hydroxyl-terminated prepolymer.
3. The preparation process of a highly active moisture-curable organosilicon polymer component according to claim 1, characterized in that: The preparation of the moisture-curing silane end-capping agent includes the following steps: Mix chloromethyltriethoxysilane, potassium cyanate, ethanol, DMF, and 18-crown-6 evenly, heat up to 120 - 125 °C and react for 11 - 12 h, filter, and the rectified fraction is the moisture-curing silane end-capping agent.
4. The preparation process of a highly active moisture-curable organosilicon polymer component according to claim 3, characterized in that: The moisture-curing silane end-capping agent includes the following raw materials, by mass: 100 - 120 parts of chloromethyltriethoxysilane, 50 - 60 parts of potassium cyanate, 6 - 8 parts of ethanol, 50 - 60 parts of DMF, and 1 - 2 parts of 18-crown-6.
5. The preparation process of a highly active moisture-curable organosilicon polymer component according to claim 1, characterized in that: In the modified polyethylene glycol, the molar ratio of the four-arm polyethylene glycol epoxy group to dimethyl 3-aminophthalate is 1:(1.8 - 2).
6. A high-activity moisture-curing organosilicon polymer component prepared by the preparation process of a high-activity moisture-curing organosilicon polymer component according to any one of claims 1 - 5.
Citation Information
Patent Citations
Preparation method of 3-isocyanate propyltriethoxysilane
CN110437273A
Process for producing prepolymers which cure to improved sealants, and products formed thereby
CN1229804A
Alkoxysilane-terminated prepolymers
CN1813014A
Silicon-terminated polyurethane polymer
US4345053A
Moisture-curable resin composition
US5068304A