Room-temperature reactive fluorine-containing silicone bright semi-permanent release agent and preparation method thereof

Abstract

The application relates to a room-temperature-reactive fluorine-containing silicon bright semi-permanent release agent and a preparation method thereof. The application aims to solve the problems of the existing release agent, such as one-mold coating, high-temperature curing, low production efficiency and cost increase. The room-temperature-reactive fluorine-containing silicon bright semi-permanent release agent is prepared from 30-80% solvent, 10-30% auxiliary film forming agent, 10-20% spreading promoter, 1-10% film forming agent and 0.1-2% catalyst according to mass fraction; the film forming agent is methoxy-terminated organic silicon resin and fluorine silicon resin. The fast volatilization of the solvent is utilized, and under the synergistic action of the auxiliary film forming agent and the spreading promoter, the film forming agent is used to form a uniform and dense polymer film layer with low surface energy on the surface of the mold under the action of the catalyst, so that the one-time coating and multiple demolding are realized. The application improves the production efficiency and saves the cost.

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 mold release agents, which require one application per mold and high-temperature curing, resulting in low production efficiency and increased costs. The invention provides a room-temperature reactive fluorinated silicone glossy semi-permanent mold release agent and its preparation method.

[0006] A room-temperature reactive fluorinated silicone glossy 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 agent is a methoxy-terminated organosilicon resin and a fluorosilicone resin.

[0008] A method for preparing a room-temperature reactive fluorinated silicone glossy semi-permanent release agent is specifically carried out according to the following steps:

[0009] 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;

[0010] The film-forming agent mentioned in step one is a methoxy-terminated organosilicon resin and a fluorosilicone resin;

[0011] 2. Add methoxy-terminated organosilicon resin and fluorosilicone resin to a solvent and stir until completely dissolved to obtain solution A;

[0012] 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;

[0013] 4. Add the catalyst to solution B and shake it under sealed conditions to obtain a room temperature reactive fluorinated silicone glossy semi-permanent release agent. Store it in a sealed container.

[0014] The principle of this invention:

[0015] This invention utilizes the rapid volatility of the solvent, and with the synergistic effect of the film-forming agent and the spreading agent, the film-forming agent forms a uniform, dense, low-surface-energy polymer film layer on the mold surface under the action of a catalyst. 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".

[0016] Advantages of this invention:

[0017] I. This invention uses methoxy-terminated organosilicon resin and fluorosilicone resin as film-forming agents, and prepares a room-temperature reactive fluorosilicone bright semi-permanent release agent with a mass fraction of 30%~80% solvent, 10%~30% film-forming aid, 10%~20% spreading accelerator, 1%~10% film-forming agent and 0.1%~2% catalyst. 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.

[0018] 2. After applying the room-temperature reactive fluorinated silicon glossy 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 6 times, which improves production efficiency and saves costs. Attached Figure Description

[0019] Figure 1 The image shows the demolded product obtained after successfully demolding 6 times using the room-temperature reactive fluorinated silicone glossy semi-permanent release agent prepared in Example 1. Detailed Implementation

[0020] 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.

[0021] Specific Implementation Method 1: This implementation method is a room temperature reactive fluorinated silicone glossy 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;

[0022] The film-forming agent is a methoxy-terminated organosilicon resin and a fluorosilicone resin.

[0023] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that the mass fraction of methoxy-terminated silicone resin and the mass fraction of fluorosilicone resin in the room-temperature reactive fluorinated silicone glossy semi-permanent release agent are 0.5%~10%. The other steps are the same as in Specific Implementation Method One.

[0024] Specific Implementation Method 3: This implementation method differs from Specific Implementation Method 1 or 2 in that: the film-forming agent is n-nonane and 2,6-dimethyloctane; the mass fraction of n-nonane in the room-temperature reactive fluorinated silicone glossy 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.

[0025] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that: the spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane; the mass fraction of 1-ethyl-4-methylcyclohexane in the room-temperature reactive fluorinated silicone glossy 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.

[0026] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that the catalyst used is triethylamine. The other steps are the same as in Specific Implementation Methods One to Four.

[0027] Specific Implementation Method Six: This implementation method differs from Specific Implementation Methods One to Five in that: the methoxy-terminated silicone resin (CAS No.: 67763-03-5) has a methoxy content of 18% to 40% in its structure; and the fluorosilicone resin (CAS No.: 38891-59-7) has a molecular weight of 4000 to 15000. Other steps are the same as in Specific Implementation Methods One to Five.

[0028] Specific Implementation Method Seven: This implementation method is a preparation method for a room temperature reactive fluorinated silicone glossy semi-permanent release agent, specifically completed according to the following steps:

[0029] 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;

[0030] The film-forming agent mentioned in step one is a methoxy-terminated organosilicon resin and a fluorosilicone resin;

[0031] The film-forming aids mentioned in step one are n-nonane and 2,6-dimethyloctane;

[0032] The spreading agent mentioned in step one is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane;

[0033] 2. Add methoxy-terminated organosilicon resin and fluorosilicone resin to a solvent and stir until completely dissolved to obtain solution A;

[0034] 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;

[0035] 4. Add the catalyst to solution B and shake it under sealed conditions to obtain a room temperature reactive fluorinated silicone glossy semi-permanent release agent. Store it in a sealed container.

[0036] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Methods One to Seven in that: the solvent mentioned in step one is dibutyl ether; the catalyst mentioned in step one is triethylamine. The other steps are the same as in Specific Implementation Methods One to Seven.

[0037] Specific Implementation Method Nine: This implementation method differs from Specific Implementation Methods One to Eight in that: the stirring speed in step two is 40 r / min to 60 r / min; the oscillation treatment time in step four is 5 min to 10 min. Other steps are the same as in Specific Implementation Methods One to Eight.

[0038] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in that: in step four, the mass fraction of methoxy-terminated silicone resin in the room-temperature reactive fluorinated silicone glossy semi-permanent release agent is 0.5% to 10%, the mass fraction of fluorosilicone resin is 0.5% to 10%, the mass fraction of n-nonane is 2% to 20%, the mass fraction of 2,6-dimethyloctane is 5% to 25%, the mass fraction of 1-ethyl-4-methylcyclohexane is 5% to 10%, and the mass fraction of 1,2,4-trimethylcyclohexane is 5% to 15%. The other steps are the same as in Specific Implementation Methods One to Nine.

[0039] The beneficial effects of the present invention are verified using the following embodiments:

[0040] Example 1: A method for preparing a room-temperature reactive fluorinated silicone glossy semi-permanent release agent with a film-forming agent content of 2%, specifically completed according to the following steps:

[0041] 1. Weigh out 47% dibutyl ether, 1% methoxy-terminated silicone resin, and 1% fluorosilicone resin by mass fraction.

[0042] 16% n-nonane, 14% 2,6-dimethyloctane, 6% 1-ethyl-4-methylcyclohexane, 14% 1,2,4-trimethylcyclohexane and 1% triethylamine;

[0043] The methoxy-terminated silicone resin (CAS No.: 67763-03-5) mentioned in step one has a methoxy content of 30% in its structure;

[0044] The fluorosilicone resin mentioned in step one has the CAS number 38891-59-7 and a molecular weight of 9000~12000.

[0045] 2. Add methoxy-terminated organosilicon resin and fluorosilicone resin to dibutyl ether and stir at a stirring speed of 60 r / min until completely dissolved to obtain solution A;

[0046] 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;

[0047] 4. Add triethylamine to solution B and shake for 10 minutes under sealed conditions to obtain a 2% room temperature reactive fluorinated silicone glossy semi-permanent release agent. Store in a sealed container.

[0048] Performance Testing: First, at room temperature, a clean, lint-free cloth was used to apply release agent evenly to the surface of a flat metal 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. Once the mold surface was visually dry, it was allowed to stand at room temperature for another 20 minutes. Then, two layers of triaxial fabric (glass fiber 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 laminate production process was repeated without reapplying the release agent. The test results showed that with a single application of release agent, the laminate (demolded product) could be successfully demolded 6 times.

[0049] Figure 1 The image shows the demolded product obtained after successfully demolding 6 times using the room-temperature reactive fluorinated silicone glossy semi-permanent release agent prepared in Example 1.

[0050] from Figure 1 It can be seen that the room temperature reactive fluorinated silicone glossy semi-permanent mold release agent prepared by the present invention can be molded at room temperature, can be applied once and used multiple times, the mold surface is glossy before and after demolding, multiple demoldings are smooth, and the product is transparent and has no internal turbidity.

Claims

1. A room-temperature reactive fluorinated silicone glossy semi-permanent release agent, characterized in that... The room-temperature reactive fluorinated silicone glossy 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 agent is a methoxy-terminated organosilicon resin and a fluorosilicone resin.

2. The room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 1, characterized in that... The room-temperature reactive fluorinated silicone glossy semi-permanent release agent contains 0.5% to 10% methoxy-terminated silicone resin and 0.5% to 10% fluorosilicone resin by mass.

3. The room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 1, characterized in that... The film-forming agent is n-nonane and 2,6-dimethyloctane; the room-temperature reactive fluorinated silicone glossy semi-permanent release agent contains n-nonane at a mass fraction of 2%~20% and 2,6-dimethyloctane at a mass fraction of 5%~25%.

4. The room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 1, characterized in that... The spreading agent is 1-ethyl-4-methylcyclohexane and 1,2,4-trimethylcyclohexane; the mass fraction of 1-ethyl-4-methylcyclohexane in the room temperature reactive fluorinated silicone glossy semi-permanent release agent is 5%~10%, and the mass fraction of 1,2,4-trimethylcyclohexane is 5%~15%.

5. The room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 1, characterized in that... The catalyst is triethylamine.

6. The room-temperature reactive fluorinated silicone glossy 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 fluorosilicone resin has a molecular weight of 4000 to 15000.

7. The preparation method of a room-temperature reactive fluorinated silicone glossy 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 agent mentioned in step one is a methoxy-terminated organosilicon resin and a fluorosilicone resin; 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; 2. Add methoxy-terminated organosilicon resin and fluorosilicone resin to a 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 catalyst to solution B and shake it under sealed conditions to obtain a room temperature reactive fluorinated silicone glossy semi-permanent release agent. Store it in a sealed container.

8. The preparation method of a room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 7, characterized in that... The solvent mentioned in step one is dibutyl ether; the catalyst mentioned in step one is triethylamine.

9. The preparation method of a room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 7, characterized in that... The stirring speed in step two is 40 r / min to 60 r / min; the oscillation treatment time in step four is 5 min to 10 min.

10. The method for preparing a room-temperature reactive fluorinated silicone glossy semi-permanent release agent according to claim 7, characterized in that... In step four, the room-temperature reactive fluorinated silicone glossy semi-permanent release agent contains 0.5%~10% methoxy-terminated silicone resin, 0.5%~10% fluorosilicone resin, 2%~20% n-nonane, 5%~25% 2,6-dimethyloctane, 5%~10% 1-ethyl-4-methylcyclohexane, and 5%~15% 1,2,4-trimethylcyclohexane.

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