Method for extracting gutta-percha

Abstract

The invention provides a method for extracting gutta-percha, which comprises the following steps: mixing a eucommia ulmoides raw material with a supramolecular solution, extracting, separating and drying to obtain crude gutta-percha; wherein the supramolecular solution is obtained by reacting a component A and a component B; the component A is cyclodextrin; the component B is at least one of crown ether, organic acid, organic alcohol and pillararene; according to the method, the specific supramolecular solution is used as the extracting agent to extract the eucommia ulmoides raw material to obtain the crude eucommia ulmoides gum, the extraction process is simple, and the extraction efficiency of the eucommia ulmoides gum can be effectively improved; in addition, the method provided by the invention can effectively reduce the extraction cost and reagent consumption, has small environmental pollution, and is suitable for industrial application.

Description

Technical Field

[0001] The present invention relates to the technical field of plant extraction, and more specifically, to a method for extracting Eucommia ulmoides gum. Background Art

[0002] Eucommia ulmoides is a precious economic tree species unique to China and also an important collagen plant with the widest application range in the world. The leaves, bark and pericarp of Eucommia ulmoides are all rich in a white filamentous substance - Eucommia ulmoides gum.

[0003] Eucommia ulmoides gum, also known as Eucommia ulmoides Gum (abbreviated as EUgum), is an excellent natural polymer material with both rubber and plastic properties and is trans - polyisoprene. Eucommia ulmoides gum can be used to develop thermoplastic functional materials and thermo - elastic shape - memory materials, and can be used for the development of tires in the aviation and related industries. The bark and leaves of Eucommia ulmoides are rich in Eucommia ulmoides gum. Eucommia ulmoides has simple growth conditions, is a high - quality gum - source tree species with great development potential, and is a recyclable resource.

[0004] Common methods for extracting Eucommia ulmoides gum from Eucommia ulmoides are as follows: (1) extracting crude gum with organic solvents such as toluene, benzene, dichloroethane, and petroleum ether, and then purifying with common organic solvents such as alcohols, ketones, ethers, and aldehydes, esters to complete the extraction of white filamentous Eucommia ulmoides gum; (2) boiling with acid or alkali solution, then crushing the raw materials to free the Eucommia ulmoides filaments, and then extracting with organic solvents; or hydrolyzing with cellulose enzyme after alkali boiling, and finally refluxing and extracting with organic solvents; (3) Soxhlet extraction with organic solvents.

[0005] However, in the existing publicly disclosed methods, the extraction rate of Eucommia ulmoides gum is generally low, and a large amount of reagents are required, resulting in high extraction costs and environmental pollution problems. Summary of the Invention

[0006] Based on the above - mentioned technical problems existing in the prior art, the present invention provides a method for extracting Eucommia ulmoides gum. Through this method, the extraction efficiency of Eucommia ulmoides gum can be effectively improved, and the extraction cost and reagent consumption can be reduced, and the environmental pollution is small.

[0007] To achieve the above object, the technical solution of the present invention is as follows:

[0008] A method for extracting Eucommia ulmoides gum, comprising the following steps: mixing Eucommia ulmoides raw materials and a supramolecular solution, then performing extraction, separation, and drying to obtain crude Eucommia ulmoides gum;

[0009] Among them, the supramolecular solution is obtained by reacting component A and component B; component A is cyclodextrin; component B is at least one of crown ether, organic acid, organic alcohol, and pillararene.

[0010] In some embodiments, the solid-liquid ratio of the Eucommia ulmoides raw material to the supramolecular solution is 1 g: 20-40 mL; preferably, it is 1 g: 30-40 mL.

[0011] In some embodiments, the extraction temperature is 50-90 °C; preferably, it is 80-90 °C.

[0012] In some embodiments, the extraction time is 30-120 min; preferably, it is 70-110 min.

[0013] In some embodiments, the separation method is as follows: after the extraction is completed, filter while it is hot, and collect the filtrate; place the filtrate at a temperature below -20 °C to precipitate, then separate, collect the precipitate, and obtain crude Eucommia ulmoides gum.

[0014] In some embodiments, the preparation of the polymer solution includes the following steps:

[0015] Mix component A and component B, raise the temperature to 40-90 °C, stir and react until the solution is homogeneous and transparent to obtain a supramolecular solution.

[0016] In some embodiments, the molar ratio of component A to component B is 1: 1-2.

[0017] In some embodiments, the organic acid includes at least one of citric acid, tartaric acid, and gallic acid; the organic alcohol includes at least one of mannitol, xylitol, octanol, and glucose.

[0018] In some embodiments, the Eucommia ulmoides raw material is at least one of Eucommia ulmoides leaves, Eucommia ulmoides roots, Eucommia ulmoides bark, and Eucommia ulmoides seeds; further, before mixing the Eucommia ulmoides raw material with the supramolecular solution, it is first dried and pulverized.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0020] The extraction method provided by the present invention uses a specific supramolecular solution as an extractant to extract Eucommia ulmoides gum, which can effectively improve the extraction rate of Eucommia ulmoides gum, and the extraction process is simple, and the extraction time is greatly shortened. It effectively avoids the problems of long extraction time, large solvent consumption, long process flow, long extraction time, and high cost existing in the existing extraction methods, and Eucommia ulmoides gum is easier to precipitate and separate, with strong controllability, suitable for industrial application, and provides a new process technology for the extraction of Eucommia ulmoides gum. Description of the Drawings

[0021] Figure 1 It is the NMR characterization result of the supramolecular solution prepared in Example 1;

[0022] Figure 2Infrared characterization results of the supramolecular solution prepared in Example 1;

[0023] Figure 3 This is a physical picture of the crude Eucommia ulmoides gum prepared in the embodiment of the present invention. Detailed implementation manners

[0024] Many specific details are set forth in the following description in order to provide a thorough understanding of the present invention. However, the present invention can be implemented in many other ways different from those described herein, and those skilled in the art can make similar improvements without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific implementations disclosed below.

[0025] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which this invention belongs. The terms used in the description of the present invention herein are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

[0026] Example 1

[0027] The preparation of a supramolecular solution includes the following steps:

[0028] Mix component A and component B in a molar ratio of 1:1, heat up to 80 °C, and stir to react until the solution becomes transparent to obtain a supramolecular solution; wherein, component A and component B are specifically shown in Table 1.

[0029] Table 1 Raw materials and ratios of the supramolecular solution

[0030]

[0031] Characterize the supramolecular solution 1 obtained in this example, and the characterization results are as Figure 1 and Figure 2 shown.

[0032] Example 2

[0033] A method for extracting Eucommia ulmoides gum includes the following steps:

[0034] S1. Crush dry Eucommia ulmoides leaves and pass through a 60-mesh sieve, and take the Eucommia ulmoides leaf powder obtained under the sieve;

[0035] S2. Add the Eucommia ulmoides leaf powder and the extractant into a centrifuge tube at a solid-liquid ratio of 1 g:30 mL, mix, heat up to 70 °C for extraction for 70 min; after the extraction is completed, filter while it is hot to remove the filter residue, and collect the filtrate; place the filtrate at a temperature of -20 °C to precipitate, then separate, and collect the precipitate; place the precipitate in a vacuum drying oven and dry at 60 °C to obtain crude Eucommia ulmoides gum.

[0036] Specifically, the types and extraction rates of the extractant are shown in Table 2.

[0037] After drying, the crude Eucommia ulmoides gum is obtained as Figure 3 shown.

[0038] Table 2 Types of extractants and extraction rates

[0039] Serial number Extractor Extraction rate of gutta-percha (mg / g) 1 Supramolecular solution 1 15.85 2 Supramolecular solution 2 15.51 3 Supramolecular solution 3 14.14 4 Supramolecular solution 4 15.54 5 Supramolecular solution 5 15.24 6 Acetone 12.57

[0040] Example 3 examines the influence of different solid-liquid ratios on the extraction rate

[0041] The extraction method in this example is the same as that in Example 2, except that the extractant used in this example is supramolecular solution 1, and the solid-liquid ratio of Eucommia ulmoides leaf powder to the extractant is different. The specific solid-liquid ratios and extraction rates are shown in Table 3.

[0042] Table 3 Influence of solid-liquid ratio on extraction rate

[0043] Serial number Solid-liquid ratio (g / ml) Extraction rate of gutta-percha (mg / g) 1 1:20 15.78 2 1:25 15.24 3 1:30 16.57 4 1:35 16.91 5 1:40 16.54

[0044] Example 3 Influence of different extraction temperatures on extraction rate

[0045] The extraction method in this example is the same as that in Example 2, except that the extractant used in this example is supramolecular solution 3, the solid-liquid ratio is 1 g: 30 mL, and the extraction is carried out at different temperatures. The specific extraction temperatures and extraction rates are shown in Table 4.

[0046] Table 4 Influence of extraction temperature on extraction rate

[0047] Serial number Temperature (°C) Extraction rate of gutta-percha (mg / g) 1 50 16.57 2 60 16.37 3 70 16.21 4 80 17.65 5 90 17.72

[0048] Example 4 Influence of extraction time on extraction rate

[0049] The extraction method in this example is the same as that in Example 2, except that the extractant used in this example is supramolecular solution 3, the extraction temperature is 80 °C, and the extraction time is different. The specific extraction times and extraction rates are shown in Table 5.

[0050] Table 5 Influence of extraction time on extraction rate

[0051] Serial number Time (min) Extraction rate of gutta-percha (mg / g) 1 30 16.95 2 50 16.80 3 70 17.16 4 90 17.76 5 110 17.02

[0052] In summary, through experiments, the optimal scheme of the extraction method of the present invention includes the following steps:

[0053] S1. After pulverizing Eucommia ulmoides leaves, sieve them through a 60-mesh sieve, and take the powder obtained under the sieve;

[0054] S2. Add the powder and the supramolecular solution 1 into a centrifuge tube at a solid-liquid ratio of 1 g: 35 mL, mix them, and heat up to 90 °C for extraction for 90 min. After the extraction is completed, filter while it is hot to remove the residue, and collect the filtrate. Place the filtrate at a temperature of -20 °C to precipitate, then separate, collect the precipitate, and dry it to obtain crude gutta-percha.

[0055] After testing, by extracting Eucommia ulmoides leaves through this preferred scheme, the extraction rate of gutta-percha is 17.76 mg / g.

[0056] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of 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, it should be considered as the scope recorded in this specification.

[0057] The above-described embodiments only represent several implementation manners of the present invention. The description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the invention. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several deformations and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention should be subject to the appended claims.

Claims

1. A method for extracting eucommia gum, characterized in that, It includes the following steps: After mixing Eucommia ulmoides raw materials and a supramolecular solution, carry out extraction, separation, and drying to obtain crude Eucommia ulmoides gum; Among them, the supramolecular solution is obtained by reacting component A and component B; component A is cyclodextrin; component B is at least one of crown ether, organic acid, organic alcohol, and pillararene.

2. The method for extracting gutta-percha according to claim 1, wherein The solid-liquid ratio of the Eucommia ulmoides raw materials and the supramolecular solution is 1 g: 20 - 40 mL.

3. The method for extracting gutta-percha according to claim 2, characterized in that, The solid-liquid ratio of the Eucommia ulmoides raw materials and the supramolecular solution is 1 g: 30 - 40 mL.

4. The method for extracting eucommia gum according to claim 1, characterized in that, The extraction temperature is 40 - 90 °C.

5. The method for extracting gutta-percha according to claim 4, characterized in that, The extraction temperature is 80 - 90 °C.

6. The method for extracting eucommia gum according to claim 1, characterized in that, The extraction time is 30 - 120 min.

7. The method for extracting eucommia gum according to claim 1, characterized in that, The specific steps of separation are: after the extraction is completed, filter while it is hot, collect the filtrate; place the filtrate below -20 °C to precipitate, then carry out separation, collect the precipitate, and obtain crude Eucommia ulmoides gum.

8. The method for extracting gutta-percha according to any one of claims 1-7, characterized in that, The molar ratio of component A and component B is 1: 1 - 2.

9. The method for extracting eucommia gum according to any one of claims 1-7, characterized in that, The organic acid includes at least one of citric acid, tartaric acid, and gallic acid; the organic alcohol includes at least one of mannitol, xylitol, octanol, and glucose.

10. The method for extracting gutta-percha according to any one of claims 1-7, characterized in that, The preparation of the supramolecular solution includes the following steps: Mix component A and component B, heat up to 40 - 90 °C and stir for reaction until the solution is homogeneous and transparent to obtain a supramolecular solution.

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