CN117247346A - MS gel, MS gel additive and preparation method thereof - Google Patents

Abstract

The invention discloses a MS glue, an MS glue additive and a preparation method thereof. The preparation method of the MS glue additive includes the following steps: dissolving pentamethylpiperidinol in an organic solvent, raising the temperature, and stirring; adding octadecacarbon Dienoic acid dimer, stir; add diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate, stir; raise the temperature, and extract the solvent under reduced pressure to obtain the product. In this technical solution, the MS glue additive can effectively capture free radicals in the polymer degradation chain reaction, thereby inhibiting the photooxidation process and achieving photostability. After evaluation, this additive can significantly reduce the performance attenuation and yellowing of MS glue due to photoaging.

Description

MS glue, MS glue additive and preparation method thereof

Technical field

The invention belongs to the technical field of MS glue additives, and in particular relates to a kind of MS glue, MS glue additives and preparation methods thereof.

Background technique

MS glue is the abbreviation of silane modified polyether glue. It is mainly an elastic sealant made of MS polymer as the base polymer, combined with fillers, plasticizers and other functional additives. It is divided into single-component and two-component It has two combination forms; it is a new generation of building sealant developed after silicone glue (SR) and polyurethane glue (PU). Mainly used in bonding, caulking, joints, sealing, waterproofing, reinforcement and other fields of construction engineering and decoration.

In the existing technology, MS glue is prone to performance attenuation and yellowing after photoaging under the influence of the environment after use. For this reason, we propose a MS glue, an MS glue additive and a preparation method thereof.

Contents of the invention

The main purpose of the present invention is to propose a MS glue, an MS glue additive and a preparation method thereof, aiming to solve the technical problem that the existing MS glue is prone to performance attenuation and yellowing after photoaging after use.

In order to achieve the above object, the present invention proposes a MS glue additive. The structural formula of the MS glue additive is as follows:

.

The present invention also proposes a preparation method of the above-mentioned MS glue additive, which preparation method includes the following steps:

Dissolve pentamethylpiperidinol in the organic solvent, heat up, and stir;

Add octadecadienoic acid dimer and stir;

Add diisopropyl bis (dioctyl pyrophosphate acyloxy) titanate and stir.

Raise the temperature and extract the solvent under reduced pressure to obtain the product.

Optionally, in the steps of dissolving pentamethylpiperidinol in an organic solvent, raising the temperature, and stirring, the organic solvent is toluene or xylene.

Optionally, in the steps of dissolving pentamethylpiperidinol in an organic solvent, raising the temperature, and stirring, the temperature is raised to 75°C to 85°C, and then stirred until the system is transparent.

Optionally, in the step of adding octadecadienoic acid dimer and stirring, the stirring time is 10 to 30 minutes.

Optionally, in the step of adding diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate and stirring, the stirring time is 3 to 5 hours.

Optionally, in the steps of raising the temperature and extracting the solvent under reduced pressure to obtain the product, the temperature is raised to 100°C to 120°C, vacuuming is carried out, and the solvent is extracted under reduced pressure to obtain the product.

Optionally, in the step of adding the octadecadienoic acid dimer and stirring, the weight ratio of the alcohol-soluble pentamethylpiperidine and the octadecadienoic acid dimer is (0.6~0.7): 1 .

Optionally, in the step of adding diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate and stirring, octadecadienoic acid dimer and diisopropyl bis(dioctyl pyrophosphate) The weight ratio of pyrophosphate acyloxy) titanate is 1: (0.007~0.009).

Optionally, the entire preparation process is protected with nitrogen.

The present invention also proposes a MS glue, which includes the above-mentioned MS glue additive.

In the technical solution of the present invention, the MS glue additive can effectively capture free radicals in the polymer degradation chain reaction, thereby inhibiting the photooxidation process and achieving photostability. After evaluation, this additive can significantly reduce the performance attenuation and yellowing of MS glue after light aging.

Description of drawings

In order to explain the embodiments of the present invention or the technical solutions in the prior art more clearly, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings in the following description are only For some embodiments of the present invention, those of ordinary skill in the art can also obtain other related drawings based on these drawings without exerting creative efforts.

Figure 1 is a schematic flow diagram of an embodiment of the MS glue additive and its preparation method provided by the present invention.

The realization of the purpose, functional features and advantages of the present invention will be further described with reference to the embodiments and the accompanying drawings.

Detailed ways

In order to make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are only some of the embodiments of the present invention, but not all of the embodiments.

It should be noted that if specific conditions are not specified in the examples, the conditions should be carried out in accordance with conventional conditions or conditions recommended by the manufacturer. If the manufacturer of the reagents or instruments used is not indicated, they are all conventional products that can be purchased commercially. In addition, the meaning of "and/or" appearing in the entire text includes three parallel solutions. Taking "A and/or B" as an example, it includes solution A, or solution B, or a solution that satisfies both A and B at the same time. In addition, the technical solutions in the various embodiments can be combined with each other, but it must be based on what a person of ordinary skill in the art can implement. When the combination of technical solutions is contradictory or cannot be realized, it should be considered that such a combination of technical solutions does not exist. , nor within the protection scope required by the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts fall within the scope of protection of the present invention.

In the existing technology, MS glue is prone to photoaging and yellowing under the influence of the environment after use. In view of this, the present invention provides a MS glue, MS glue additive and a preparation method thereof, wherein the structural formula of the MS glue additive is as follows:

.

The present invention also proposes a preparation method of the above-mentioned MS glue additive. Combined with the flow diagram provided in Figure 1, the preparation method includes the following steps.

Step S10: Dissolve pentamethylpiperidinol in an organic solvent, raise the temperature, and stir.

It should be noted that pentamethylpiperidinol is a hindered amine light stabilizer intermediate, and its structural formula is . In this embodiment, the organic solvent is toluene or xylene, and pentamethylpiperidinol is first dissolved in toluene or xylene, where the weight ratio of pentamethylpiperidinol to toluene or xylene is 1 : (2.5~3), the concentration of the reaction system is conducive to the reaction. Then, heat the solution to 75°C to 85°C and stir until the system is transparent.

Step S20: Add octadecadienoic acid dimer and stir;

It should be noted that the structural formula of octadecadienoic acid dimer is . During specific implementation, octadecadienoic acid dimer is added to the solution obtained in the previous step and stirred for 10 to 30 minutes. Among them, the weight ratio of pentamethylpiperidinol and octadecadienoic acid dimer is (0.6~0.7):1. It should be understood that this reaction is an esterification reaction, and the molar ratio of the reaction is 2:1. In order to prevent excessive acid from causing hydrolysis, excess pentamethylpiperidinol must be added.

Step S30: Add diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate and stir.

It should be noted that diisopropyl bis (dioctyl pyrophosphate acyloxy) titanate is a titanate coupling agent, which has the function of absorbing free water and dissolves in pentamethylpiperidine alcohol and ten The eight-carbon dienoic acid dimer acts as a catalyst when reacting. During the specific implementation, the weight ratio of octadecadienoic acid dimer and diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate is 1: (0.007~0.009), which is added to the previous step. After the solution obtained in this step is stirred, the reaction is carried out for 3 to 5 hours.

Step S40: Raise the temperature, extract the solvent under reduced pressure, and obtain the product.

In specific implementation, after the reaction in the previous step is completed, the system is heated to 100°C to 120°C, vacuumed, and the solvent is evaporated under reduced pressure through equipment such as a rotary evaporator to finally obtain the product, which is MS glue additive.

It should be understood that nitrogen is used to protect the entire preparation process, which can be used to provide inert protection and prevent oxidation.

The technical solution of the present invention will be further described in detail below with reference to specific examples. It should be understood that the following examples are only used to explain the present invention and are not intended to limit the present invention.

Example 1

The entire preparation process is protected by nitrogen. Dissolve 336.55 parts (gravimetric method, the same below) of pentamethylpiperidinol in 841.37 parts of toluene. After raising the temperature to 75°C, stir until the system is transparent; add 560.91 parts of octadecane. Dienoic acid dimer, stir for 10 minutes; add 3.93 parts of diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate, stir for 3 hours; raise the temperature to 100°C, evacuate, and remove the solvent under reduced pressure , get the product.

Example 2

The entire preparation process was protected with nitrogen. Dissolve 392.64 parts of pentamethylpiperidinol in 1177.91 parts of xylene. After raising the temperature to 85°C, stir until the system is transparent; add 560.91 parts of octadecadienoic acid dimer. , stir for 30 minutes; add 5.05 parts of diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate, stir for 5 hours; raise the temperature to 120°C, evacuate, and extract the solvent under reduced pressure to obtain the product.

Example 3

The entire preparation process was protected with nitrogen. Dissolve 342.56 parts of pentamethylpiperidinol in 903.47 parts of toluene. After raising the temperature to 75°C, stir until the system is transparent; add 560.91 parts of octadecadienoic acid dimer. Stir for 10 minutes; add 4.52 parts of diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate, stir for 3 hours; raise the temperature to 100°C, evacuate, and extract the solvent under reduced pressure to obtain the product.

Example 4

The entire preparation process was protected with nitrogen. Dissolve 342.56 parts of pentamethylpiperidinol in 903.47 parts of xylene. After raising the temperature to 85°C, stir until the system is transparent; add 560.91 parts of octadecadienoic acid dimer. , stir for 30 minutes; add 4.52 parts of diisopropyl bis(dioctyl pyrophosphate acyloxy) titanate, stir for 5 hours; raise the temperature to 120°C, evacuate, and extract the solvent under reduced pressure to obtain the product.

Example 5

The entire preparation process was protected by nitrogen. Dissolve 342.56 parts of pentamethylpiperidinol in 903.47 parts of toluene. After raising the temperature to 80°C, stir until the system is transparent; add 560.91 parts of octadecadienoic acid dimer. Stir for 20 minutes; add 4.52 parts of diisopropyl bis(dioctylpyrophosphate acyloxy) titanate, stir for 4 hours; raise the temperature to 110°C, evacuate, and extract the solvent under reduced pressure to obtain the product.

Comparative example 1

The entire preparation process was protected by nitrogen. Dissolve 342.56 parts of pentamethylpiperidinol in 903.47 parts of toluene. After raising the temperature to 80°C, stir until the system is transparent; add 560.91 parts of octadecadienoic acid dimer. Stir for 4 hours; raise the temperature to 110°C, vacuum, and extract the solvent under reduced pressure to obtain the product.

After sampling, sample pretreatment, and sample measurement, the yields of each embodiment were calculated as follows:

Example 1 Example 2 Example 3 Example 4 Example 5 Comparative example 1 Yield 50.7% 54% 49.1% 49.8% 50% 26.3%

It can be concluded from the above control experiment that the product yield is better improved in the reaction with the addition of catalyst.

【Performance evaluation】

The MS glue additive prepared in Example 5 was made into a transparent MS glue. Compared with the MS glue without the MS glue additive, the test was carried out according to "GB/T 14522-2008 Artificial climate aging test of plastics, coatings and rubber materials for mechanical industrial products". Method: The standard ultraviolet light of fluorescent ultraviolet lamp was irradiated for 1000 hours, the appearance was compared and observed, and the body strength was tested. See table below:

Exterior Body tensile strength change rate MS glue (with additives) slightly yellowish transparent -8.5% MS glue (no additives) dark yellow opaque -91%

In the absence of light stabilizer for transparent MS glue, ultraviolet light has a huge impact on it, causing the surface to deteriorate and the strength to drop seriously. The addition of the MS additive and light stabilizer in Example 5 will effectively inhibit the damage of ultraviolet light to the MS glue and improve the weather resistance of the MS glue.

The technical features of the above-described embodiments can be combined in any way. To simplify the description, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, All should be considered to be within the scope of this manual.

The above-described embodiments only express several implementation modes of the present application, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that, for those of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all fall within the protection scope of the present application. Therefore, the protection scope of this patent application should be determined by the appended claims.

Claims (10)

1. The MS glue additive is characterized by comprising the following structural formula:

。

2. a method of preparing an MS glue additive according to claim 1, comprising the steps of:

dissolving pentamethylpiperidinol in an organic solvent, heating and stirring;

adding octadecadienoic acid dimer, and stirring;

adding diisopropyl bis (dioctyl pyrophosphoryloxy) titanate, and stirring;

heating, decompressing and extracting the solvent to obtain the product.

3. The method for preparing MS glue additive as defined in claim 2, wherein the steps of dissolving pentamethylpiperidinol in an organic solvent, heating and stirring, wherein the organic solvent is toluene or xylene.

4. The method for preparing the MS glue additive according to claim 2, wherein the steps of dissolving pentamethylpiperidinol in an organic solvent, heating and stirring are performed, and after the temperature is raised to 75-85 ℃, the system is stirred until the system is transparent.

5. The method for preparing an MS glue additive according to claim 2, wherein in the step of adding octadecadienoic acid dimer and stirring, the stirring time is 10-30 minutes.

6. The method for preparing an MS glue additive according to claim 2, wherein the step of adding diisopropyl bis (dioctyl pyrophosphoryloxy) titanate and stirring is performed for 3-5 hours.

7. The method for preparing an MS glue additive according to claim 2, wherein in the step of heating and decompressing to extract the solvent, the temperature is raised to 100 ℃ to 120 ℃, and the solvent is vacuumized and decompressed to extract the solvent, thereby obtaining the product.

8. The method for preparing an MS glue additive according to claim 2, wherein in the step of adding octadecadienoic acid dimer and stirring, the weight ratio of pentamethylpiperidine alcohol to octadecadienoic acid dimer is (0.6-0.7): 1.

9. the method for preparing an MS glue additive according to claim 2, wherein the step of adding diisopropyl bis (dioctyl pyrophosphoryl oxy) titanate and stirring comprises the steps of: (0.007 to 0.009).

10. An MS glue, characterized in that it comprises an MS glue additive according to claim 1.