Preparation method of high-flexibility and high-adhesiveness rosin gel

Abstract

The invention discloses a preparation method of high-flexibility and high-adhesiveness rosin gel, which comprises the following steps of: performing ring-opening reaction on epoxy chloropropane by using rosin as a nucleophilic reagent, and promoting cross-linking by using urushiol as a cross-linking agent, so that the rosin, the epoxy chloropropane and the urushiol form a firm gel network through hydrogen bonds and covalent bonds; the existence of rosin and urushiol in the gel system endows the gel system with excellent adhesion performance, and the formation of a supramolecular network endows the gel system with excellent flexibility. The method disclosed by the invention is simple in steps, and the prepared rosin gel system is high in stability, good in flexibility and strong in adhesive capacity and has a good application prospect.

Description

Technical Field

[0001] The invention belongs to the field of natural polymer materials, and in particular relates to a method for preparing a high-flexibility and high-adhesion rosin gel. Background Art

[0002] The main materials that make up the gel are polyethylene glycol, polyvinyl alcohol, polyacrylic acid and its derivatives, polyethylene oxide, polyacrylamide, polyhydroxyethyl methacrylate, polyacrylic acid, polymethacrylic acid, etc. So far, synthetic gels with controllable composition and structure and adjustable mechanical properties have been developed, which are widely used in adsorbents, biomedicine, cosmetics, food, catalysts, energy storage, etc. However, most gels lack unique biological properties, such as non-toxicity, biocompatibility and biodegradability. While doing a good job in the recycling and utilization of gels, green raw materials should also be developed to replace petroleum-based raw materials. Rosin is a gel synthesized from rosin as a raw material, which contains a large sterically hindered rigid ring structure. It has the advantages of being green and environmentally friendly and having good biocompatibility, and has great potential in the preparation of functional gel materials. Based on this, the present invention provides a method for preparing a highly flexible and highly adhesive rosin gel. Summary of the invention

[0003] The object of the present invention is to provide a method for preparing a rosin gel with high flexibility and high adhesion.

[0004] To achieve the above object, the present invention adopts the following technical solution: A highly flexible and highly adhesive rosin gel, the preparation method of which comprises the following steps: (1) dissolving rosin in anhydrous ethanol to obtain a rosin solution; (2) adding rosin solution and urushiol to epichlorohydrin in sequence, stirring and reacting to obtain a reaction solution; (3) Pour the reaction solution obtained in step (2) into a mold, cool it to room temperature and then take it out to obtain rosin gel.

[0005] Furthermore, the rosin in step (1) is any one of hydrogenated rosin, disproportionated rosin and polymerized rosin.

[0006] Furthermore, the rosin used in step (1) is pre-crushed to a particle size of 40-200 mesh.

[0007] Furthermore, the concentration of the rosin solution obtained in step (1) is 0.1-1 g / mL.

[0008] Furthermore, the amount of the rosin solution used in step (2) is converted according to the mass ratio of rosin to epichlorohydrin and urushiol of 1:1:1-4:1:1.

[0009] Furthermore, the reaction in step (2) is carried out under condensation reflux at 70°C-100°C for 6-8h.

[0010] The significant advantages of the present invention are: (1) The present invention uses rosin as a nucleophilic reagent to open the ring of epichlorohydrin, and uses urushiol to provide cohesive force through self-crosslinking, so that the three are interconnected through hydrogen bonds and covalent bonds to form a gel with a supramolecular network structure, and endow it with high flexibility and high adhesion.

[0011] (2) The method of the present invention is simple to operate, and the constructed rosin-based gel system has high stability, strong adhesion ability and good tensile properties. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 This is a reaction mechanism diagram of the rosin gel prepared in the present invention.

[0013] Figure 2 Schematic diagram of the tensile properties of the rosin gel prepared in Example 2.

[0014] Figure 3 This is the SEM image of the rosin gel prepared in Example 2. DETAILED DESCRIPTION

[0015] A highly flexible and highly adhesive rosin gel, the preparation method of which comprises the following steps: (1) Pre-crushing rosin to 40-200 mesh, and then dissolving it in anhydrous ethanol to obtain a rosin solution with a concentration of 0.1-1 g / mL; (2) adding rosin solution and urushiol to epichlorohydrin in a mass ratio of rosin to epichlorohydrin and urushiol of 1:1:1-4:1:1, heating and stirring to 70°C-100°C, condensing and refluxing for 6-8h, and obtaining a reaction solution; (3) Pour the reaction solution obtained in step (2) into a mold, cool it to room temperature and then take it out to obtain rosin gel.

[0016] The rosin used is any one of hydrogenated rosin, disproportionated rosin and polymerized rosin.

[0017] In order to make the contents of the present invention easier to understand, the technical solution of the present invention is further described below in conjunction with specific implementation methods, but the present invention is not limited thereto.

[0018] Example 1 (1) Grind the hydrogenated rosin with a grinder, pass it through a 100-mesh sieve, and then weigh 30 g and dissolve it in 30 mL of anhydrous ethanol to form a rosin solution with a concentration of 1 g / mL; (2) The rosin solution obtained in step (1) and 10 g of urushiol were added to 10 g of epichlorohydrin in sequence, and the mixture was heated at 90° C. with stirring and condensing under reflux for 6 h. After the reaction was completed, the reaction solution was poured into a mold and cooled to room temperature to obtain a rosin gel.

[0019] Example 2 (1) Grind the hydrogenated rosin with a grinder, pass it through a 100-mesh sieve, and then weigh 20 g and dissolve it in 30 mL of anhydrous ethanol to form a rosin solution with a concentration of 0.67 g / mL; (2) The rosin solution obtained in step (1) and 10 g of urushiol were added to 10 g of epichlorohydrin in sequence, and the mixture was heated at 90° C. with stirring and condensing under reflux for 6 h. After the reaction was completed, the reaction solution was poured into a mold and cooled to room temperature to obtain a rosin gel.

[0020] Figure 2 The tensile properties of the obtained gel are shown in Figure 2. As can be seen from the figure, the obtained gel has good tensile properties.

[0021] Figure 3 The SEM image of the obtained gel shows that a cross-linked network with a supramolecular network structure is formed inside the obtained gel.

[0022] Example 3 (1) Grind the hydrogenated rosin with a grinder, pass it through a 100-mesh sieve, and then weigh 10 g and dissolve it in 30 mL of anhydrous ethanol to form a rosin solution with a concentration of 0.33 g / mL; (2) The rosin solution obtained in step (1) and 10 g of urushiol were added to 10 g of epichlorohydrin in sequence, and the mixture was heated at 90° C. with stirring and condensing under reflux for 6 h. After the reaction was completed, the reaction solution was poured into a mold and cooled to room temperature to obtain a rosin gel.

[0023] Comparative Example 1 (1) Grind the hydrogenated rosin with a grinder, pass it through a 100-mesh sieve, and then weigh 20 g and dissolve it in 30 mL of anhydrous ethanol to form a rosin solution with a concentration of 0.67 g / mL; (2) Add the rosin solution obtained in step (1) to 10 g of epichlorohydrin, heat at 90° C., stir, condense and reflux for 6 h, and after the reaction is completed, pour the reaction solution into a mold and cool to room temperature.

[0024] Comparative Example 2 (1) Grind the hydrogenated rosin with a grinder, pass it through a 100-mesh sieve, and then weigh 20 g and dissolve it in 30 mL of anhydrous ethanol to form a rosin solution with a concentration of 0.67 g / mL; (2) The rosin solution obtained in step (1) and 10 g of catechol were added to 10 g of epichlorohydrin in sequence, and the mixture was heated at 90° C. with stirring and condensing under reflux for 6 h. After the reaction was completed, the reaction solution was poured into a mold and cooled to room temperature.

[0025] The performance of the samples prepared in the embodiments and comparative examples was tested, and the results are shown in Table 1.

[0026] Table 1 Performance test results of samples obtained in the examples and comparative examples

[0027] As shown in Table 1, the tensile strain of the rosin gel obtained in the examples can reach more than 3300%, and has good adhesion to the interfaces of various materials, among which Example 2 has the best effect. This is because the rosin in the examples can cause the ring-opening polymerization of epichlorohydrin, and the urushiol can provide cohesive force through self-crosslinking, so that the obtained gel has a supramolecular network structure and gives it high flexibility and high adhesion. Compared with the examples, the network structure of the gel in Comparative Example 1 is poor due to the lack of crosslinking of urushiol, and the mechanical properties and adhesion properties are poor; although the catechol used in Comparative Example 2 can give the gel certain adhesion properties, it does not have self-crosslinking ability and cannot increase the crosslinking degree of the gel system, so the tensile strain of the gel is poor.

[0028] The above description is only a preferred embodiment of the present invention. All equivalent changes and modifications made according to the scope of the patent application of the present invention should fall within the scope of the present invention.

Claims

1. A high flexibility and high adhesion rosin gel preparation method, characterized in that: The following steps are involved: (1) Dissolve rosin in anhydrous ethanol to obtain a rosin solution; (2) Add rosin solution and uluol to epoxychlorohydrin in turn, stirring and obtaining the reaction solution; (3) Pour the reaction liquid obtained in step (2) into the mold, cool to room temperature and remove it to obtain a rosin gel.

2. The preparation method of a high flexibility and high adhesion rosin gel according to claim 1, characterized in that: The rosin described in step (1) is any one of hydrogenated rosin, disproportionated rosin, and polymerized rosin.

3. The preparation method of a high flexibility and high adhesion rosin gel according to claim 1, characterized in that: The rosin used in step (1) is pre-pulverized to a particle size of 40-200 mesh.

4. The preparation method of a high flexibility and high adhesion rosin gel according to claim 1, characterized in that: The concentration of the obtained rosin solution in step (1) is 0.1-1 g / mL.

5. The preparation method of a high flexibility and high adhesion rosin gel according to claim 1, characterized in that: The amount of rosin solution used in step (2) is converted according to the mass ratio of rosin to epoxychlorohydrin and uruophenol in the range of 1:1:1-4:1:

1.

6. The preparation method of a high flexibility and high adhesion rosin gel according to claim 1, characterized in that: Step (2) The reaction is condensed and refluxed at 70°C-100°C for 6-8 hours.

7. A highly flexible, highly adhesion rosin gel prepared according to any one of claims 1-6.

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