Room-temperature reactive silicon-containing matte semi-permanent release agent and preparation method thereof

Abstract

This invention relates to a room-temperature reactive silicone-containing matte semi-permanent release agent and its preparation method. The purpose of this invention is to solve the problems of existing release agents requiring one application per mold and high-temperature curing. The room-temperature reactive silicone-containing matte semi-permanent release agent is prepared by mass fraction of 30%–80% solvent, 10%–30% film-forming aid, 10%–20% spreading agent, 1%–10% film-forming agent, and 0.1%–2% catalyst. The film-forming aid is n-nonane and 2,6-dimethyloctane; the spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane; and the film-forming agent is methoxy-terminated silicone resin and hydroxyl-terminated polymethylphenylsiloxane. The release agent prepared by this invention adheres firmly to the mold surface based on chemical bonding, exhibiting a low transfer rate during repeated demolding of the product, thus achieving "one-time coating, multiple demoldings".

Description

Technical Field

[0001] This invention relates to a room-temperature reactive release agent and its preparation method. Background Technology

[0002] Resin-based composite materials and plastic products are widely used in aerospace, automotive, and other industries due to their lightweight properties. In the molding process of composite materials and plastics, demolding is a crucial step that determines the surface quality of the product and production efficiency. As a core auxiliary agent for separating the product from the mold, the performance of the mold release agent directly affects the success or failure of the molding process.

[0003] Currently, the most widely used release agents in the production of resin-based composite materials and plastic products mainly include ready-to-use release agents and wax-based release agents. While these release agents can perform basic demolding functions, their mechanism of action results in a common drawback—a single application can only support one product demolding. That is, after demolding, the effective components of the release agent are essentially transferred with the product or fail structurally. This "one mold, one coating" production model brings several problems: on the one hand, production efficiency is severely limited; on the other hand, the release agent adheres to the product surface after being transferred with the product, seriously affecting subsequent painting or gluing processes. Furthermore, a significant portion of existing release agents require high-temperature treatment after application to form a film, increasing additional energy consumption, time, and cost.

[0004] In summary, existing mold release agents are insufficient to meet the demands of modern manufacturing for high efficiency, high quality, and low cost. Therefore, there is an urgent need to develop a semi-permanent mold release agent that allows for repeated demolding of multiple products with a single application, thereby improving production efficiency and product surface quality. Simultaneously, it should possess the process characteristic of forming a film at room temperature without requiring high-temperature curing, thus shortening the process and reducing energy consumption. Summary of the Invention

[0005] The purpose of this invention is to solve the problems of existing release agents that require one application per mold and high-temperature curing, and to provide a room-temperature reactive silicone-containing matte semi-permanent release agent and its preparation method.

[0006] A room-temperature reactive silicone-containing matte semi-permanent release agent is prepared by mass fraction of 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst;

[0007] The film-forming aids are n-nonane and 2,6-dimethyloctane;

[0008] The spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane;

[0009] The film-forming agent is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane.

[0010] A method for preparing a room-temperature reactive silicone-containing matte semi-permanent mold release agent is specifically carried out according to the following steps:

[0011] 1. Weigh out 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst by mass fraction;

[0012] The film-forming aids mentioned in step one are n-nonane and 2,6-dimethyloctane;

[0013] The spreading agent mentioned in step one is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane;

[0014] The film-forming agent mentioned in step one is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane.

[0015] 2. Add the methoxy-terminated organosilicon resin to the solvent and stir until completely dissolved to obtain solution A;

[0016] 3. Add n-nonane, 2,6-dimethyloctane, 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane to solution A in sequence, and stir until completely dissolved to obtain solution B;

[0017] 4. Add the hydroxyl-terminated polymethylphenylsiloxane to solution B and stir until completely dissolved to obtain solution C;

[0018] 5. Add the catalyst to solution C and shake it under sealed conditions to obtain a room temperature reactive silicone-containing matte semi-permanent release agent. Store it in a sealed container.

[0019] The principle of this invention:

[0020] Utilizing the rapid volatility of the solvent, and with the synergistic effect of film-forming agents and spreading agents, the film-forming agent, under the action of a catalyst, forms a uniform, dense, and low-surface-energy polymer film layer on the mold surface. Simultaneously, this film layer adheres firmly to the mold surface based on chemical bonding, exhibiting a low transfer rate during product cyclic demolding, thus achieving "one-time coating, multiple demoldings".

[0021] Advantages of this invention:

[0022] I. This invention uses 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst to prepare a room temperature reactive silicone-containing matte semi-permanent release agent. This release agent can be applied at room temperature without high temperature heat treatment, and can achieve the purpose of multiple demoldings with one application.

[0023] 2. After applying the room-temperature reactive silicone-containing matte semi-permanent release agent prepared in this invention once to the surface of the flat fiberglass mold, the laminate can be repeatedly made. The laminate can be successfully demolded up to 5 times, which improves production efficiency and saves costs. Attached Figure Description

[0024] Figure 1 The image shows the composite board product obtained after successfully demolding five times using the room-temperature reactive silicone-containing matte semi-permanent release agent prepared in Example 1. Detailed Implementation

[0025] The following embodiments further illustrate the content of the present invention, but should not be construed as limiting the present invention. Any modifications and substitutions made to the methods, steps, or conditions of the present invention without departing from the essence of the invention are within the scope of the present invention.

[0026] Specific Implementation Method 1: This implementation method is a room temperature reactive silicone-containing matte semi-permanent release agent, which is prepared by mass fraction of 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst;

[0027] The film-forming aids are n-nonane and 2,6-dimethyloctane;

[0028] The spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane;

[0029] The film-forming agent is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane.

[0030] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the solvent used is dibutyl ether. All other steps are the same as in Specific Implementation Method One.

[0031] Specific Implementation Method 3: This implementation method differs from Specific Implementation Method 1 or 2 in that the mass fraction of n-nonane in the room-temperature reactive silicone-containing matte semi-permanent release agent is 2%~20%, and the mass fraction of 2,6-dimethyloctane is 5%~25%. Other steps are the same as in Specific Implementation Method 1 or 2.

[0032] Specific Implementation Method Four: The difference between this implementation method and Specific Implementation Methods One to Three is that the mass fraction of 1-ethyl-4-methylcyclohexane in the room temperature reactive silicone-containing matte semi-permanent release agent is 5%~10%, and the mass fraction of 1,2,4-trimethylcyclohexane is 5%~15%. Other steps are the same as in Specific Implementation Methods One to Three.

[0033] Specific Embodiment Five: This embodiment differs from Specific Embodiments One to Four in that: the methoxy-terminated silicone resin (CAS No.: 67763-03-5) has a methoxy content of 18% to 40%; and the hydroxyl-terminated polymethylphenylsiloxane (CAS No.: 80801-30-5) has a molecular weight of 2000 to 8000. Other steps are the same as in Specific Embodiments One to Four.

[0034] Specific Implementation Method Six: The difference between this implementation method and Specific Implementation Methods One to Five is that the mass fraction of methoxy-terminated silicone resin in the room temperature reactive silicone-containing matte semi-permanent release agent is 0.5% to 10%, and the mass fraction of hydroxyl-terminated polymethylphenylsiloxane is 0.25% to 5%. The other steps are the same as in Specific Implementation Methods One to Five.

[0035] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Methods One to Six in that the catalyst used is triethylamine. The other steps are the same as in Specific Implementation Methods One to Six.

[0036] Specific Implementation Method Eight: This implementation method is a preparation method for a room temperature reactive silicone-containing matte semi-permanent release agent, specifically completed according to the following steps:

[0037] 1. Weigh out 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst by mass fraction;

[0038] The film-forming aids mentioned in step one are n-nonane and 2,6-dimethyloctane;

[0039] The spreading agent mentioned in step one is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane;

[0040] The film-forming agent mentioned in step one is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane.

[0041] 2. Add the methoxy-terminated organosilicon resin to the solvent and stir until completely dissolved to obtain solution A;

[0042] 3. Add n-nonane, 2,6-dimethyloctane, 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane to solution A in sequence, and stir until completely dissolved to obtain solution B;

[0043] 4. Add the hydroxyl-terminated polymethylphenylsiloxane to solution B and stir until completely dissolved to obtain solution C;

[0044] 5. Add the catalyst to solution C and shake it under sealed conditions to obtain a room temperature reactive silicone-containing matte semi-permanent release agent. Store it in a sealed container.

[0045] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Methods One to Eight in the following ways: the solvent in step one is dibutyl ether; the catalyst in step one is triethylamine; the stirring speed in step two is 40 r / min to 60 r / min; and the oscillation treatment time in step five is 5 min to 10 min. The other steps are the same as in Specific Implementation Methods One to Eight.

[0046] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in that: in step five, the mass fraction of n-nonane in the room-temperature reactive silicone-containing matte semi-permanent release agent is 2%~20%, the mass fraction of 2,6-dimethyloctane is 5%~25%, the mass fraction of 1-ethyl-4-methylcyclohexane is 5%~10%, the mass fraction of 1,2,4-trimethylcyclohexane is 5%~15%, the mass fraction of methoxy-terminated silicone resin is 0.5%~10%, and the mass fraction of hydroxyl-terminated polymethylphenylsiloxane is 0.25%~5%. Other steps are the same as in Specific Implementation Methods One to Nine.

[0047] The beneficial effects of the present invention are verified using the following embodiments:

[0048] Example 1: A method for preparing a room-temperature reactive silicone-containing matte semi-permanent release agent with a film-forming agent content of 2%, specifically completed according to the following steps:

[0049] 1. Weigh out the following components by mass fraction: 47% dibutyl ether, 1% methoxy-terminated silicone resin, 16% n-nonane, 14% 2,6-dimethyloctane, 6% 1-ethyl-4-methylcyclohexane, 14% 1,2,4-trimethylcyclohexane, 1% hydroxyl-terminated polymethylphenylsiloxane, and 1% triethylamine.

[0050] The methoxy-terminated silicone resin (CAS No.: 67763-03-5) mentioned in step one has a methoxy content of 30% in its structure;

[0051] The hydroxyl-terminated polymethylphenylsiloxane (CAS No.: 80801-30-5) mentioned in step one has a molecular weight of 3500~5000;

[0052] 2. Add the methoxy-terminated silicone resin to dibutyl ether and stir at a stirring speed of 60 r / min until completely dissolved to obtain solution A;

[0053] 3. Add n-nonane, 2,6-dimethyloctane, 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane to solution A in sequence, and stir until completely dissolved to obtain solution B;

[0054] 4. Add the hydroxyl-terminated polymethylphenylsiloxane to solution B and stir until completely dissolved to obtain solution C;

[0055] 5. Add triethylamine to solution C and shake for 10 minutes under sealed conditions to obtain a room temperature reactive silicone-containing matte semi-permanent release agent with a film-forming agent content of 2%. Store in a sealed container.

[0056] Performance Testing: First, at room temperature, a clean, lint-free cloth was used to apply release agent evenly to the surface of the flat fiberglass mold, ensuring the release agent adhered uniformly and completely to the entire mold. After application, the mold was allowed to stand for 15 minutes to allow the release agent to cure. After visually inspecting the mold surface for dryness, it was allowed to stand at room temperature for another 20 minutes. Then, two layers of triaxial fabric (fiberglass cloth + epoxy resin system) were continuously hand-laid to prepare a composite laminate. After the laminate product cured and solidified, it was removed. Then, the process of making the laminate was repeated without reapplying the release agent. The test results showed that with only one application of release agent, the laminate (composite board product) could be successfully demolded 5 times.

[0057] Figure 1 The image shows the composite board product obtained after successfully demolding five times using the room-temperature reactive silicone-containing matte semi-permanent release agent prepared in Example 1.

[0058] from Figure 1 It can be seen that the room temperature reactive silicone-containing matte semi-permanent release agent prepared by the present invention can be molded at room temperature, can be applied once and used multiple times, leaves no residue on the mold surface after demolding, and the resulting composite board product is complete, transparent and free of internal turbidity.

Claims

1. A room-temperature reactive silicone-containing matte semi-permanent release agent, characterized in that... The room-temperature reactive silicone-containing matte semi-permanent release agent is prepared by mass fraction of 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst; The film-forming aids are n-nonane and 2,6-dimethyloctane; The spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane; The film-forming agent is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane.

2. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The solvent is dibutyl ether.

3. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The room-temperature reactive silicone-containing matte semi-permanent release agent contains 2% to 20% nonane and 5% to 25% 2,6-dimethyloctane by mass.

4. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The room-temperature reactive silicone-containing matte semi-permanent release agent contains 5% to 10% by mass of 1-ethyl-4-methylcyclohexane and 5% to 15% by mass of 1,2,4-trimethylcyclohexane.

5. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The methoxy-terminated organosilicon resin has a methoxy content of 18% to 40%; the hydroxyl-terminated polymethylphenylsiloxane has a molecular weight of 2000 to 8000.

6. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The room-temperature reactive silicone-containing matte semi-permanent release agent contains 0.5% to 10% methoxy-terminated silicone resin and 0.25% to 5% hydroxyl-terminated polymethylphenylsiloxane.

7. The room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 1, characterized in that... The catalyst is triethylamine.

8. The method for preparing a room-temperature reactive silicone-containing matte semi-permanent release agent as described in claim 1, characterized in that... The preparation method is specifically carried out according to the following steps:

1. Weigh out 30%~80% solvent, 10%~30% film-forming agent, 10%~20% spreading agent, 1%~10% film-forming agent and 0.1%~2% catalyst by mass fraction; The film-forming aids mentioned in step one are n-nonane and 2,6-dimethyloctane; The spreading agent mentioned in step one is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane; The film-forming agent mentioned in step one is a methoxy-terminated organosilicon resin and a hydroxyl-terminated polymethylphenylsiloxane; 2. Add the methoxy-terminated organosilicon resin to the solvent and stir until completely dissolved to obtain solution A; 3. Add n-nonane, 2,6-dimethyloctane, 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane to solution A in sequence, and stir until completely dissolved to obtain solution B; 4. Add the hydroxyl-terminated polymethylphenylsiloxane to solution B and stir until completely dissolved to obtain solution C; 5. Add the catalyst to solution C and shake it under sealed conditions to obtain a room temperature reactive silicone-containing matte semi-permanent release agent. Store it in a sealed container.

9. The preparation method of the room temperature reactive silicone-containing matte semi-permanent release agent according to claim 8, characterized in that... The solvent mentioned in step one is dibutyl ether; the catalyst mentioned in step one is triethylamine; the stirring speed mentioned in step two is 40 r / min to 60 r / min; and the shaking treatment time mentioned in step five is 5 min to 10 min.

10. The method for preparing the room-temperature reactive silicone-containing matte semi-permanent release agent according to claim 8, characterized in that... In step five, the room-temperature reactive silicone-containing matte semi-permanent release agent contains n-nonane at a mass fraction of 2%–20%, 2,6-dimethyloctane at a mass fraction of 5%–25%, 1-ethyl-4-methylcyclohexane at a mass fraction of 5%–10%, 1,2,4-trimethylcyclohexane at a mass fraction of 5%–15%, methoxy-terminated silicone resin at a mass fraction of 0.5%–10%, and hydroxyl-terminated polymethylphenylsiloxane at a mass fraction of 0.25%–5%.

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