CN111808298A - Method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis - Google Patents
Method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis Download PDFInfo
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- CN111808298A CN111808298A CN202010669601.7A CN202010669601A CN111808298A CN 111808298 A CN111808298 A CN 111808298A CN 202010669601 A CN202010669601 A CN 202010669601A CN 111808298 A CN111808298 A CN 111808298A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
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Abstract
The invention discloses a method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis. The method comprises the following steps: extracting eucommia ulmoides with ethanol to obtain ethanol solution containing chlorogenic acid and extraction residue; adding a certain amount of dilute acid solution into the extraction residue, carrying out hydrolysis reaction for 0.5-6 h at 100-180 ℃, and carrying out solid-liquid separation on the product to obtain a sugar-containing hydrolysate and hydrolysis residue; and adding the hydrolysis residues into a nonpolar organic solvent, refluxing for 6-24 h at 50-80 ℃, filtering while hot, cooling the filtrate, and precipitating to obtain the gutta-percha. Compared with the traditional gutta-percha extraction process, the invention adopts dilute acid hydrolysis to extract the gutta-percha from the eucommia, and greatly improves the yield of the gutta-percha by controlling the degree of the acid hydrolysis. Besides the gutta-percha, the method can also simultaneously harvest chlorogenic acid and sugar-containing hydrolysate, and has the characteristics of high comprehensive utilization rate, simple and convenient operation, good economic benefit and the like.
Description
Technical Field
The invention belongs to the technical field of high-valued utilization of eucommia ulmoides, and particularly relates to a method for extracting gutta-percha from eucommia ulmoides by adopting dilute acid hydrolysis.
Background
China is a country with large rubber consumption, and rubber resources mainly depend on import. The research and production of eucommia bark, a special industry capable of replacing natural rubber, are of great practical significance due to the requirement of national security strategy. Eucommia ulmoides is a single-genus plant of the family Eucommiaceae, and is a unique and precious economic tree species in China. The leaves, bark, fruits and seeds of eucommia ulmoides Oliver contain different amounts of gutta percha. The gutta-percha is a natural polymer material, belongs to an isomer with natural rubber, and has a molecular structure of trans-1, 4-polyisoprene (TPI). Gutta-percha is widely used as a raw material for elastomer materials, shape memory materials, antenna sealing materials, medical materials, high-temperature damping materials, and the like.
The gutta-percha content in the gutta-percha cells of the eucommia ulmoides tree is low, and the viscosity is high, so that the gutta-percha cannot be directly collected by tapping like natural rubber, and the extraction process of the gutta-percha is special. Generally, the extraction of gutta-percha is divided into 3 steps: breaking cell walls, extracting gutta-percha, and separating and purifying the gutta-percha. The common extraction methods mainly comprise: mechanization, alkaline leaching, fermentation (microbiological method), solvent method or a combination of the methods. As a kind of lignocellulose, eucommia ulmoides contains a large amount of cellulose, hemicellulose and lignin in addition to gutta percha. Most of these substances are lost as waste materials during the gutta percha improving process, causing a great waste of resources. Therefore, the invention provides a new eucommia ulmoides gum extraction method, and has important practical significance for realizing the utilization of the whole components of eucommia ulmoides.
Disclosure of Invention
The invention aims to provide a method for extracting gutta-percha from eucommia ulmoides by adopting dilute acid hydrolysis. Besides the gutta-percha, the method can also simultaneously harvest chlorogenic acid and sugar-containing hydrolysate, and has the characteristics of high comprehensive utilization rate, simple and convenient operation, good economic benefit and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis comprises the following steps: extracting eucommia ulmoides with ethanol to obtain ethanol solution containing chlorogenic acid and extraction residue; adding a certain amount of dilute acid solution into the extraction residue, carrying out hydrolysis reaction for 0.5-6 h at 100-180 ℃, and carrying out solid-liquid separation on the product to obtain a sugar-containing hydrolysate and hydrolysis residue; and adding the hydrolysis residues into a nonpolar organic solvent, refluxing for 6-24 h at 50-80 ℃, filtering while hot, cooling the filtrate, and precipitating to obtain the gutta-percha.
Preferably, the mass ratio of the ethanol to the eucommia ulmoides is 2-10: 1.
Preferably, the mass fraction of the dilute acid solution is 0.01-10%; the acid is at least one of sulfuric acid, hydrochloric acid and nitric acid.
Preferably, in the hydrolysis reaction, the mass fraction of the eucommia ulmoides extraction residue is 5-40%.
Preferably, the nonpolar organic solvent is at least one selected from petroleum ether, cyclohexane, dichloromethane and toluene; the mass ratio of the nonpolar organic solvent to the hydrolysis residues is 5-10: 1.
Preferably, the eucommia ulmoides is at least one selected from eucommia ulmoides leaves, eucommia ulmoides bark and eucommia ulmoides fruits.
The invention has the technical effects that:
1) while extracting gutta-percha, cellulose and hemicellulose in eucommia can be converted into sugar-containing hydrolysate, and the sugar-containing hydrolysate can be used for producing chemicals such as bioethanol and biobutanol by fermentation.
2) While extracting the gutta-percha, the chlorogenic acid can be obtained, and the economic benefit of the extraction process is further improved.
3) Compared with the traditional gutta-percha extraction process, the invention adopts dilute acid hydrolysis to extract the gutta-percha from the eucommia, and greatly improves the yield of the gutta-percha by controlling the degree of the acid hydrolysis.
Detailed Description
In order to make the above objects of the present invention more comprehensible, embodiments of the present invention are described in detail below with reference to specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
A method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis comprises the following steps:
(1) placing 100 parts of dry eucommia ulmoides leaves in a Soxhlet extractor, extracting the eucommia ulmoides leaves with 200 parts of ethanol, keeping refluxing for 12 hours, then filtering to obtain ethanol filtrate containing chlorogenic acid and extraction residues, and air-drying the extraction residues for later use.
(2) Adding 50 parts of extraction slag into 950 parts of sulfuric acid solution with the mass fraction of 0.01%, carrying out hydrolysis reaction for 3 hours at 160 ℃, filtering after the reaction is finished to obtain sugar-containing hydrolysis liquid and hydrolysis slag, washing the hydrolysis slag to be neutral, and drying for later use.
(3) And (2) adding 200 parts of petroleum ether into 20 parts of hydrolysis residues, refluxing for 12 hours at 80 ℃, filtering while hot after the reflux is finished, transferring the filtrate into a refrigerator for freeze-out treatment, then centrifugally collecting solids, washing separated solid precipitates with acetone and water in sequence, and air-drying to obtain the gutta percha, wherein the yield of the gutta percha is 3.4%.
Example 2
A method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis comprises the following steps:
(1) placing 100 parts of dry eucommia bark in a Soxhlet extractor, extracting the eucommia bark with 1000 parts of ethanol, keeping refluxing for 12 hours, then filtering to obtain ethanol filtrate containing chlorogenic acid and extraction residues, and air-drying the extraction residues for later use.
(2) Adding 50 parts of extraction residues into 75 parts of mixed acid solution with the mass fraction of 10% (the mass ratio of hydrochloric acid to sulfuric acid is 1: 1), carrying out hydrolysis reaction for 0.5h at 180 ℃, filtering after the reaction is finished to obtain sugar-containing hydrolysis liquid and hydrolysis residues, washing the hydrolysis residues to be neutral, and drying for later use.
(3) And (2) adding 250 parts of toluene into 50 parts of hydrolysis residues, refluxing for 24 hours at 50 ℃, filtering while hot after the reflux is finished, transferring the filtrate into a refrigerator for freeze-out treatment, then centrifugally collecting solids, washing the precipitated solid precipitates with acetone and water in sequence, and air-drying to obtain the gutta percha, wherein the yield of the gutta percha is 2.9%.
Example 3
A method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis comprises the following steps:
(1) placing 100 parts of dry eucommia ulmoides fruit in a Soxhlet extractor, extracting the eucommia ulmoides fruit with 500 parts of ethanol, keeping refluxing for 12 hours, then filtering to obtain ethanol filtrate containing chlorogenic acid and extraction residues, and air-drying the extraction residues for later use.
(2) Adding 100 parts of extraction residues into 400 parts of hydrochloric acid solution with the mass fraction of 5%, carrying out hydrolysis reaction for 1h at 160 ℃, filtering after the reaction is finished to obtain sugar-containing hydrolysis liquid and hydrolysis residues, washing the hydrolysis residues to be neutral, and drying for later use.
(3) And (2) adding 160 parts of cyclohexane into 20 parts of hydrolysis residues, refluxing for 18 hours at 70 ℃, filtering while hot after refluxing is finished, transferring the filtrate into a refrigerator for freeze-out treatment, then centrifugally collecting solids, washing the precipitated solid precipitates with acetone and water in sequence, and air-drying to obtain the gutta percha, wherein the yield of the gutta percha is 2.84%.
The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.
Claims (6)
1. A method for extracting gutta-percha from eucommia ulmoides by dilute acid hydrolysis is characterized by comprising the following steps: extracting eucommia ulmoides with ethanol to obtain ethanol solution containing chlorogenic acid and extraction residue; adding a certain amount of dilute acid solution into the extraction residue, carrying out hydrolysis reaction for 0.5-6 h at 100-180 ℃, and carrying out solid-liquid separation on the product to obtain a sugar-containing hydrolysate and hydrolysis residue; and adding the hydrolysis residues into a nonpolar organic solvent, refluxing for 6-24 h at 50-80 ℃, filtering while hot, cooling the filtrate, and precipitating to obtain the gutta-percha.
2. The method for extracting gutta-percha from eucommia ulmoides oliv by dilute acid hydrolysis according to claim 1, wherein the mass ratio of the ethanol to the eucommia ulmoides oliv is 2-10: 1.
3. The method for extracting gutta percha from eucommia ulmoides oliv by dilute acid hydrolysis according to claim 1, wherein the mass fraction of the dilute acid solution is 0.01-10%; the acid is at least one of sulfuric acid, hydrochloric acid and nitric acid.
4. The method for extracting gutta-percha from eucommia ulmoides oliv by dilute acid hydrolysis according to claim 1 or 3, wherein the mass fraction of eucommia ulmoides oliv extract residue in the hydrolysis reaction is 5-40%.
5. The method of claim 1, wherein the non-polar organic solvent is at least one selected from the group consisting of petroleum ether, cyclohexane, dichloromethane, and toluene; the mass ratio of the nonpolar organic solvent to the hydrolysis residues is 5-10: 1.
6. The method of claim 1, wherein the eucommia ulmoides is selected from at least one of eucommia ulmoides leaves, eucommia ulmoides bark, and eucommia ulmoides fruit.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870130A (en) * | 2021-03-30 | 2021-06-01 | 中国科学院合肥物质科学研究院 | Preparation method of eucommia pollen fermentation liquor and application of eucommia pollen fermentation liquor in cosmetics |
| CN113881066A (en) * | 2021-10-25 | 2022-01-04 | 中国科学院广州能源研究所 | Method for extracting gutta-percha from eucommia ulmoides by adopting ultrasonic wave and acid hydrolysis |
| CN114561437A (en) * | 2022-03-24 | 2022-05-31 | 中国科学院广州能源研究所 | Method for preparing functional bacterial cellulose by in-situ fermentation of eucommia ulmoides hydrolysate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112870130A (en) * | 2021-03-30 | 2021-06-01 | 中国科学院合肥物质科学研究院 | Preparation method of eucommia pollen fermentation liquor and application of eucommia pollen fermentation liquor in cosmetics |
| CN113881066A (en) * | 2021-10-25 | 2022-01-04 | 中国科学院广州能源研究所 | Method for extracting gutta-percha from eucommia ulmoides by adopting ultrasonic wave and acid hydrolysis |
| CN113881066B (en) * | 2021-10-25 | 2023-10-10 | 中国科学院广州能源研究所 | Method for extracting gutta-percha from eucommia ulmoides by ultrasonic wave and acid hydrolysis |
| CN114561437A (en) * | 2022-03-24 | 2022-05-31 | 中国科学院广州能源研究所 | Method for preparing functional bacterial cellulose by in-situ fermentation of eucommia ulmoides hydrolysate |
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