CN113604286A

CN113604286A - Supermolecule self-assembly of rose extract and method for preparing rose essential oil and nano material

Info

Publication number: CN113604286A
Application number: CN202110937569.0A
Authority: CN
Inventors: 许林兴; 孙勉; 梁丽; 曾秀娟; 黄珍
Original assignee: Zhongshan Yaohe Biotechnology Co ltd
Current assignee: Zhongshan Yaohe Biotechnology Co ltd
Priority date: 2021-08-16
Filing date: 2021-08-16
Publication date: 2021-11-05

Abstract

The invention discloses a supermolecule self-assembly method of rose extract and a method for preparing rose essential oil and nano materials, which mainly comprises the following steps: respectively pre-extracting rose liquid phase components and rose fruit liquid phase oil components, and uniformly mixing rose solid phase residues, rose fruit solid phase pomace, crushed rose leaves, rose branches and rose roots to obtain a solid phase mixture; extracting the solid phase mixture with aqueous enzymatic method to obtain liquid phase mixed component, and reserving the residual solid phase dregs for later use; homogenizing and mixing rose liquid phase component, rose fruit liquid phase oil component and liquid phase mixed component to obtain a rose full component mixture, and performing ultrasonic treatment and supermolecule self-assembly to obtain a fluid substance; purifying the rose essential oil from the fluid substance obtained by self-assembly of the supermolecule; preparing the nano biological medicine material by using the remainder after purifying the rose essential oil. The final product prepared by the invention is high-purity rose essential oil, a carbon nano material and a nano biomedical material, and has good market application prospect.

Description

Supermolecule self-assembly of rose extract and method for preparing rose essential oil and nano material

Technical Field

The invention belongs to the technical field of molecular biology, supermolecule chemistry and nano materials, and particularly relates to a method for supermolecule self-assembly of a rose extract and preparation of rose essential oil and a nano material.

Background

The rose essential oil is a group of safe, nontoxic and special fragrant volatile substances extracted from roses. At present, the extraction is mainly carried out by a steam distillation method and subcritical extraction, chemical components are extremely complex, main active substances are terpenes, alcohols, esters, ethers, aldehydes, alkanes and the like, and main aroma substances are citronellol, geraniol, phenethyl alcohol, linalool, eugenol, rose oxide and the like. The rose essential oil has stable property, good antioxidant, antidepressant and antibacterial activities, and can be used as a natural flavoring agent for medical care, beauty and cosmetics and high-grade daily chemical products.

Most of the enterprises in the rose industry in China concentrate near the rose planting areas such as Shandong Pingyin and Gansu Kushui, and are mostly distributed in low-end markets such as dried roses, fresh flowers and flower buds, and the like, and the added value of products is not large. Besides producing and processing products such as rose buds, rose essential oil and the like, most rose enterprises have fewer research and development of other deep-processed products and high-added-value products, and the added value of the products still needs to be improved.

In the domestic rose industry, rose fruits, rose leaves, pruned branches of roses, crude oil extracted from roses, purified residues and the like are not effectively utilized, so that a great deal of rose resource is wasted. In China, the extracted essential oil mainly comprises roses, the extraction yield is low, and the high-purity rose essential oil obtained after purification is lower; the extracted rose essential oil has unbalanced indexes, the fragrance is not outstanding, the rose essential oil is restricted by the rose variety, and part of the rose essential oil cannot be eaten. In the face of the requirements of the international standard of the rose essential oil, the pursuit of consumers for the international fragrance of the rose essential oil, the limitation of diversified technical indexes of the rose essential oil by food, medicine, daily chemicals and the like, innovation of extraction and purification of the rose essential oil and the comprehensive utilization technology of roses are urgently needed to meet the global market demand. Moreover, the rose plant contains various antibacterial and immunoregulatory active components and trace elements, and the rose plant residue after extracting essential oil is processed to be a natural medical material. Therefore, the advanced development and utilization of the multiple effects and multiple ways of the rose plants are the technical problems which are urgently needed to be solved by the rose industry in China at present.

Disclosure of Invention

The invention aims to: aiming at the problems of the prior art, provides a method for supermolecule self-assembly of rose extract and preparation of rose essential oil and nano materials. The invention takes the whole plant of the rose as the basic raw material to prepare the high-purity rose essential oil, the carbon nano material, the nano biomedical material and the like, realizes the development and utilization of multiple effects and multiple ways of the rose plant, has zero emission and zero pollution in the whole process, and has good market application prospect and economic and technical values.

In order to achieve the purpose, the invention adopts the following technical scheme:

a method for supermolecule self-assembly of rose extract and preparation of rose essential oil and nano materials comprises the following steps:

a. respectively pre-extracting rose liquid phase components and rose fruit liquid phase oil components, and uniformly mixing rose solid phase residues, rose fruit solid phase pomace, crushed rose leaves, rose branches and rose roots to obtain a solid phase mixture;

b. extracting the solid phase mixture with aqueous enzymatic method to obtain liquid phase mixed component, and reserving the residual solid phase dregs for later use;

c. homogenizing and mixing the rose liquid phase component, the rose fruit liquid phase oil component and the liquid phase mixed component obtained in the step b to obtain a rose whole plant component mixture, and performing ultrasonic treatment and supermolecule self-assembly to obtain a fluid substance;

d. purifying the fluid substance obtained by self-assembly of the supermolecule into rose essential oil;

e. preparing the nano biological medicine material by using the remainder after purifying the rose essential oil.

The rose extract is a mixture of rose whole plant components, and comprises rose components, rose hip components, rose leaves, rose branches and rose roots.

In the invention, the rose in the step a is clean and impurity-free fresh rose flowers or dry rose flowers, and the rose fruits are clean and impurity-free seeds of mature rose fruits.

And d, in the step a, the rose leaves, the rose branches and the rose roots are fresh or dried substances.

In the invention, the specific operation method of the step a is as follows:

firstly, obtaining a liquid-phase component and a solid-phase residue of rose by adopting a conventional water distillation extraction method, and separately storing for later use;

secondly, obtaining a rose fruit liquid phase oil component and residual solid phase pomace by adopting a squeezing method, and separately storing for later use;

thirdly, crushing the mixture of the rose leaves, the rose branches and the rose roots in advance, and storing for later use;

and fourthly, mixing the rose solid-phase residue and the rose fruit solid-phase pomace treated in the three steps and a pre-crushed mixture of rose leaves, rose branches and rose roots again, drying, and performing superfine crushing to 800-1200 meshes to be used as a raw material for water enzyme extraction for later use.

The first step adopts a conventional water distillation extraction method to obtain liquid-phase components and solid-phase residues of roses, and comprises the following specific steps:

feeding rose: putting the rose into a stirring and mixing high-pressure reaction kettle, and if dried rose flowers are used as a raw material, injecting deionized water into the stirring and mixing high-pressure reaction kettle, wherein the ratio of the dried rose flowers to the deionized water is 1: 2-3; if new fresh rose flowers are used as raw materials, water does not need to be added into the stirring and mixing high-pressure reaction kettle;

pretreatment of rose: after feeding of the roses is finished, adding an organic acid aqueous solution with the mass concentration of 2% into a stirring and mixing high-pressure reaction kettle, wherein the mass ratio of the roses to the organic acid aqueous solution is 1: 2-3, and after uniformly stirring and mixing, closing a feeding port of the stirring and mixing high-pressure reaction kettle; the organic acid is any one of malic acid, citric acid and acetic acid;

high-pressure treatment: after the pretreatment of the roses is finished, pressurizing in a stirring and mixing high-pressure reaction kettle, and carrying out high-pressure treatment on the roses, wherein the pressure of the high-pressure treatment is 500-550 MPa, the pressure maintaining time is 6-10 min, and the pressure maintaining temperature is 25-35 ℃;

and fourthly, distillation: and (3) sending the rose liquid after the high-pressure treatment into a steam distillation extraction device, and collecting distillate and rose dregs after the distillation is finished to obtain rose liquid-phase components and residual solid-phase dregs for later use.

The second step adopts a squeezing method to obtain the rose fruit liquid phase oil component and the residual solid phase pomace, and comprises the following specific steps:

oil extraction of rose fruits: sending the rose hips into an oil press by adopting a cold pressing method to press oil;

collecting: collecting oil and oil residue to obtain liquid phase oil component of fructus Rosae Davuricae and residual solid phase residue;

in the invention, the aqueous enzymatic extraction of the liquid phase mixed component in the step b comprises two steps of ultrasonic size mixing treatment and enzymatic hydrolysis. The ultrasonic size mixing treatment comprises the steps of mixing a rose liquid-phase component, a rose fruit liquid-phase oil component and a solid-phase mixture according to the weight ratio of 1: 8-9: 10-11, adding the mixture into an ultrasonic auxiliary stirring device, stirring and size mixing, wherein the ultrasonic size mixing temperature is 25-35 ℃, and the size mixing time is 30-45 min; and (3) after ultrasonic size mixing treatment, adding complex enzyme for hydrolysis, concentrating and separating out a liquid phase mixture after extraction is finished, and preparing the carbon nano material from the residual solid phase dregs.

Further, the mixing weight ratio of the rose liquid phase component, the rose fruit liquid phase oil component and the solid phase mixture is preferably 1:8: 10.

The compound enzyme is prepared by mixing 30-60: 20-30: 10-20: 5-10 weight ratio of cellulase, hemicellulase, pectinase, amylase and protease, and further preferably 60:20:10:5:5 weight ratio.

The separated liquid phase is a mixture component of oil and water.

In the invention, the homogeneous mixing in the step c is as follows: and mixing the remaining rose liquid phase component and the rose fruit liquid phase oil component for 20-30 min, then adding the liquid phase mixed component obtained by the aqueous enzymatic extraction, and continuously carrying out homogeneous mixing, wherein the average mixing time is 30-50 min, so as to obtain the rose whole plant component mixture.

The ultrasonic treatment comprises the following steps: and (3) conveying the whole rose plant component mixture into an ultrasonic treatment device, and carrying out ultrasonic treatment for 40-50 min.

The supramolecular self-assembly in the step c comprises two stages:

the first stage, after ultrasonic treatment is finished, feeding the whole plant component mixture of the roses into a fluid magnetizer for magnetization, adjusting the magnetic field intensity to 5500-6500 GS, continuing for 15-20 min, combining volatile compounds in the roses and sugar by glycosidic bonds to form glycoside molecules for breakage, splitting methyl eugenol molecules contained in the roses and having genotoxicity and carcinogenicity, eliminating toxicity, and instantly breaking hydrogen bonds in fluid substances;

in the second stage, the fluid after magnetization is sent into an ultrasonic processor, is processed for 40-45 min under the ultrasonic intensity of 15000-25000 Hz, is sent into a high-speed refrigerated centrifuge, is centrifugally processed for 3-5 min under the condition of 12000-23000 rpm, is then input into an ultra-high speed centrifuge, is processed for 1-2 min under the condition of 75000-85000 rpm, and is arranged into an ordered structure under the centrifugal force; and finally, sending the rose plant component mixture into a quick heating device, wherein the temperature in the quick heating device is increased to 100-110 ℃ within 3-5 s, so that the rose plant component mixture reaches a gas-liquid phase critical state and becomes a fluid substance.

Supramolecular assembly (supramollbular assembly) is defined as a group of molecules assembled by non-covalent bonds, which can be as simple as two molecules, with dimensions ranging from nanometers to micrometers.

The process of supramolecular assembly is called molecular self-assembly (Sdle-organization), which is a process that generates high order of supramolecules. Supramolecules generally refer to complex, organized aggregates of two or more molecules held together by intermolecular interactions and maintained in integrity to give them well-defined microscopic and macroscopic properties. From molecule to supramolecule and intermolecular interactions, just as from atom to molecule and covalent bonds.

In the invention, the method for purifying the rose essential oil is to extract and separate the high-purity rose essential oil by supercritical carbon dioxide extraction. The fluid substance is sent into supercritical carbon dioxide extraction separation equipment, and the high-purity rose essential oil is obtained by extraction separation, the yield of the rose essential oil reaches up to 0.35 percent, the components are balanced, the fragrance is unique and lasting, and the rose essential oil meets the best quality standard of the rose essential oil of the International Association for fragrance and flavor.

In the invention, the method for preparing the nano-biomedical material in the step e comprises the following steps: and (3) carrying out ultrasonic oscillation extraction, freeze concentration and low-temperature freeze drying on the remainder after extracting the rose essential oil.

The ultrasonic oscillation extraction-freeze concentration-low temperature freeze drying process comprises the following steps: and (3) carrying out ultrasonic oscillation extraction on the remainder after extracting the rose essential oil in an ultrasonic oscillation device for 55-60 min, wherein the ultrasonic frequency is 25-30 MHz, obtaining a solid concentrate by a freeze concentration method after the ultrasonic oscillation extraction is finished, and carrying out freeze drying on the solid concentrate at a low temperature of-70-60 ℃ to obtain the nano biomedical material.

In the invention, the method for preparing the carbon nano material comprises the following steps: and (3) pretreating the residual solid-phase slag in a steam explosion device, then carrying out high-temperature treatment in a high-temperature furnace, fully carbonizing, and collecting to obtain the carbon nano material with the size of 60-90 nm. The high-temperature treatment is carried out in a high-temperature furnace, the temperature setting range is 200-700 ℃, the initial temperature heating value is 200 ℃, the end point temperature is 700 ℃, the temperature is increased every 5 ℃/min, the temperature is kept for 1-2 h after the preset end point temperature is reached, and the carbonization is fully carried out.

The dregs after extraction and separation by the aqueous enzymatic method are pretreated in a steam explosion device, so that steam molecules permeating into plant tissues are instantaneously released, the internal energy of the steam is converted into mechanical energy and acts between cell layers of biomass tissues, and the raw materials are decomposed according to the purpose by using less energy. The principle is that the fiber in plant cell is bonded by lignin, under the action of high-temperature and high-pressure steam, the crystallinity of cellulose is increased, the polymerization degree is reduced, the hemicellulose is partially degraded, the lignin is softened, the transverse connection strength is reduced, even the lignin is softened and plastic, when the material filled with pressure steam is suddenly decompressed, the gas in the pores is expanded, the 'blasting' effect is generated, the lignin can be partially stripped, and the raw material is torn into fine fiber.

The following functions exist in the steam explosion process:

acid hydrolysis and thermal degradation, and in the steam explosion process, high-pressure hot steam enters the fiber raw material and permeates into gaps inside the fibers. Because the combined action of the water vapor and the heat generates the acid-like degradation and the thermal degradation of the fiber raw material, the low molecular substances are dissolved out, and the polymerization degree of the fiber is reduced.

The fiber is subjected to mechanical fracture action, when high-pressure steam is released, hot steam molecules which penetrate into the fiber are instantaneously released from a closed pore at a high speed in an air flow mode, and the hot steam inside and around the fiber instantly flows at a high speed to cause the fiber to be subjected to mechanical fracture to a certain extent, wherein the fracture is represented by bond fracture in cellulose macromolecules, increase of reduction end groups and damage of hydrogen bonds inside the cellulose, and is also represented by damage of an amorphous area and damage of a partial crystalline area.

And thirdly, hydrogen bond destruction effect, in the steam explosion process, water vapor permeates into each pore of the fiber and forms hydrogen bonds with partial hydroxyl on a cellulose molecular chain, and meanwhile, the destruction to the hydrogen bonds in the cellulose is aggravated under the conditions of high temperature, high pressure and water content, so that new hydroxyl is dissociated, and the adsorption capacity of the cellulose is improved. The instant pressure relief blasting enables water vapor among pores in the cellulose to be instantly removed to the air, and hydrogen bonds in the cellulose are broken. The hydrogen bonds in the molecules are broken and the cellulose is rapidly cooled to room temperature, so that the supermolecular structure of the cellulose is frozen, and only a small part of the hydrogen bonds are recombined. Thus, solvent molecules can easily enter between the layers, and the infiltrated solvent further performs solvation with the cellulose macromolecular chains and causes the destruction of residual intramolecular hydrogen bonds, accelerates the movement of glucose ring groups and finally causes the complete destruction of other crystal regions until complete dissolution.

And fourthly, structural rearrangement, under high temperature and high pressure, hydrogen bonds in cellulose molecules are damaged to a certain degree, and the mobility of cellulose chains is increased, thereby being beneficial to the change of cellulose to an ordered structure. At the same time, the cellulose molecular chains are broken, making the cellulose chains more easily rearrange.

The invention utilizes various intermolecular interactions such as electrostatic interaction, hydrogen bonds, coordination bonds, hydrophobic effects and synergistic effects thereof according to the principles of molecular self-assembly and molecular self-organization in the nature to assemble the rose essential oil and rose biological nano material assembly body with special physical and chemical properties and multifunctional integration, assembles a new assembly body for the interface molecules of the rose biological nano material, and constructs a three-dimensional layered assembly body with clear interface and stable structure and a new rose product with controllable two-dimensional shape of the molecular assembly body.

Compared with the prior art, the invention has the beneficial effects that:

1. the invention uses the fresh or dried rose plant to prepare high-purity rose essential oil, nano carbon material and nano biological medicine material, thus fully utilizing the whole plant of rose and improving the economic and technical value of rose.

2. The supermolecule self-assembly method is used for preparing the rose essential oil, and the yield of the extracted rose essential oil is up to 0.35%; the yield of the prepared carbon nano material is 0.01-0.02%; the yield of the nano-biomedical material is 0.001-0.003%; the economic and technical value of the method is 50-100 times of the income of independently extracting the rose essential oil by other methods.

3. The rose plant contains various antibacterial and immunity-regulating active components and trace elements, the rose plant residue after extracting essential oil contains rich carbon elements, and is a natural medicinal antibacterial nano material and a nano carbon material after being processed by a nano technology. The nano biological medicine material prepared by the invention can be used as polypeptide protein medicine and gene transfer carrier, biological detection, nano medicine controlled release, nano medicine and preparation carrier, molecular biological chip material and the like.

4. The final product prepared by the invention is high-purity rose essential oil, a carbon nano material and a nano biomedical material, has good market application prospect, and has zero emission and zero pollution in the whole process.

5. The technical method adopted by the invention is the foremost technology in the whole world at present, is suitable for extracting the rose plants to obtain products, and is also suitable for extracting all plants and comprehensively developing and utilizing the products.

Drawings

FIG. 1 shows the supermolecule self-assembly of rose extract and the process flow chart for preparing rose essential oil and nano material

Detailed Description

The present invention will be further described with reference to the following examples, but is not limited thereto.

Examples

As shown in fig. 1, a method for supermolecular self-assembly of rose extract and preparation of rose essential oil and nano material comprises the following steps:

firstly, obtaining rose liquid-phase components and residual solid-phase slag by adopting a water distillation conventional extraction method, and specifically comprising the following steps:

(1) selecting rose raw materials: the rose is fresh flower or dry flower, and is required to be clean and free of impurities;

(2) feeding rose: and (3) putting the rose into a stirring and mixing high-pressure reaction kettle. The method is characterized in that deionized water is injected into a stirring and mixing high-pressure reaction kettle by taking dried rose flowers as raw materials, and the ratio of the dried rose flowers to the water is 1: 2-3. When the fresh rose flowers are used as raw materials, water does not need to be added into the stirring and mixing high-pressure reaction kettle by utilizing the moisture of the fresh rose flowers;

(3) pretreatment of rose: after feeding of the roses is finished, adding an organic acid aqueous solution with the mass concentration of 2% into a stirring and mixing high-pressure reaction kettle, wherein the mass ratio of the roses to the organic acid aqueous solution is 1: 2-3, uniformly stirring and mixing, and then closing a feeding port of the stirring and mixing high-pressure reaction kettle. Wherein the organic acid can be one of malic acid, citric acid and acetic acid;

(4) high-pressure treatment: after the pretreatment of the roses is finished, pressurizing in a stirring and mixing high-pressure reaction kettle to carry out high-pressure treatment on the roses, and carrying out steam distillation after the high-pressure treatment is finished. Wherein the conditions of high-pressure treatment are set to be 500-550 MPa of pressure, 6-10 min of pressure maintaining time and 25-35 ℃ of pressure maintaining temperature;

(5) and (3) distillation: sending the rose liquid after the high-pressure treatment into a steam distillation and extraction device, and taking deionized water as a steam source; controlling the heating temperature to be 100-120 ℃ to ensure the continuous and stable output of the water vapor; setting the heat preservation temperature of a distillation device to be 90-100 ℃ so as to control the evaporation rate in the distillation flask; the distillation time is 2-3 h; the cooling water circulation device is used for controlling the flow rate and the temperature of the condensed water so as to control the condensation rate. After distillation, collecting distillate and rose dregs to obtain liquid phase rose components and residual solid phase dregs for later use.

The second step is that: a squeezing method is adopted to obtain a rose fruit liquid phase oil component and residual solid phase pomace, and the adopted specific method comprises the following steps:

(1) selecting rose fruit raw materials: the rose hip is seed of mature rose fruit, and is required to be clean and free of impurities;

(2) rose fruit oil pressing: sending the rose hips into an oil press by adopting a cold pressing method to press oil; obtaining the rose fruit liquid phase oil component and the residual solid phase pomace for later use.

The third step: ultrafine grinding rose flower dregs, rose pomace, rose leaves, branches and roots, mixing, extracting by a water enzymatic method to obtain a liquid-phase mixed component, and separating the rest solid phase substance, wherein the specific method comprises the following steps:

(1) crushing: ultrafine grinding rose dregs, rose pomace and rose leaves, branches and roots, mixing, feeding into a grinding device, performing coarse grinding, performing ultrafine grinding to 800-1200 meshes, and uniformly mixing in a mixing and stirring device to obtain a solid-phase mixture;

(2) ultrasonic size mixing treatment: mixing a rose liquid-phase component, a rose fruit liquid-phase oil component and a solid-phase mixture according to a weight ratio of 1: 8-9: 10-11, adding the mixture into an ultrasonic auxiliary stirring device, stirring and mixing slurry, wherein the ultrasonic slurry mixing temperature is 25-35 ℃, and the slurry mixing time is 30-45 min;

(3) and (3) enzymatic hydrolysis: and (4) adding enzyme for hydrolysis after the size mixing is finished, wherein the enzymolysis time is 20-24 h. And after the enzymolysis is finished, carrying out solid-liquid separation and concentration by using a solid-liquid separation device, and concentrating and separating out a liquid-phase mixture and solid-phase dregs for later use. The enzyme is a complex enzyme, wherein the weight ratio of cellulase to hemicellulase to pectinase to amylase to protease is 30-60: 20-30: 10-20: 5-10, and the preferable ratio is 60:20:10:5: 5. The separated solid-phase slag is prepared into carbon nano-materials.

The fourth step: and (3) homogenizing and mixing the rose liquid phase component and the rose fruit liquid phase oil component, and then adding the liquid phase mixed component obtained by the extraction with the aqueous enzymatic method for further homogenizing and mixing to obtain a rose whole plant component mixture. The method comprises the following specific steps: and (3) feeding the rose liquid-phase component prepared in the first step and the rose fruit liquid-phase oil component prepared in the second step into a homogenizer for homogenizing and mixing for 20-30 min, then adding the rose residue, the rose leaves, the branches and the roots liquid-phase mixed component into the homogenizer for homogenizing and mixing for 30-50 min, and obtaining a rose whole-plant component mixture for later use.

The fifth step: carrying out ultrasonic treatment on the rose whole-plant component mixture prepared in the fourth step, carrying out supermolecule self-assembly after ultrasonic treatment, extracting and separating by supercritical carbon dioxide to obtain high-purity rose essential oil, and preparing the remainder after extracting the rose essential oil into the nano biomedical material. The method comprises the following specific steps:

(1) sending the rose whole plant component mixture obtained in the fourth step into an ultrasonic treatment device, and carrying out ultrasonic treatment for 40-50 min;

(2) after the ultrasonic treatment is finished, feeding the rose whole plant component mixture into a fluid magnetizer, adjusting the magnetic field intensity to 5500-6500 GS, continuing for 15-20 min, and finishing the first stage of supermolecule self-assembly;

(3) and (3) conveying the magnetized fluid into an ultrasonic processor, conveying the fluid into a high-speed refrigerated centrifuge for centrifugal treatment for 3-5 min under the condition of 12000-23000 rpm, conveying the fluid into an ultrahigh-speed centrifugal machine for centrifugal treatment for 1-2 min under the condition of 75000-85000 rpm, and arranging the fluid into an ordered structure under centrifugal force, thus completing the supermolecule self-assembly in the second stage. Finally, the temperature is raised to 100-115 ℃ in 3-5 s in a quick heating device, and the rose whole plant component mixture is in a gas-liquid phase critical state to form a fluid substance;

(4) feeding the fluid substance into supercritical carbon dioxide extraction and separation equipment, and extracting and separating to obtain high-purity rose essential oil with a yield of 0.35%;

(5) and (3) carrying out ultrasonic oscillation extraction on the remainder after the rose essential oil is extracted in an ultrasonic oscillation device for 55-60 min, wherein the ultrasonic frequency is 25-30 MHz. After the ultrasonic oscillation extraction is finished, a solid concentrate is obtained by a freeze concentration method, and the nano biomedical material is obtained after the solid concentrate is freeze-dried at the low temperature of-70 to-60 ℃.

In the third step described in this embodiment, the solid-phase slag is prepared into the carbon nanomaterial mainly by using the abundant carbon element in the slag, and the specific preparation method includes the following steps:

(1) pretreating the slag after the extraction and separation by the aqueous enzymatic method in a steam explosion device;

(2) after the pretreatment of the slag extracted and separated by the aqueous enzymatic method in a steam explosion device is finished, the slag is subjected to high-temperature treatment in a high-temperature furnace, wherein the temperature setting range is 200-700 ℃, the initial temperature of heating is 200 ℃, and the final temperature is 700 ℃. And (3) heating at every 5 ℃/min, keeping the temperature for 1-2 h after the preset end point temperature is reached, fully carbonizing, and collecting to obtain the carbon nano material with the average size of 60-90 nm.

According to the preparation steps, 10kg of rose whole plants are weighed in the example 1, the example 2 and the example 3 respectively for experiments, and the specific experimental data and the process parameters are controlled as shown in the following table:

TABLE 1 Process parameters and Experimental data for examples 1-3

As can be seen from the above table, the yields of the rose essential oil extracted in this example were 0.355%, 0.358%, and 0.356%, respectively. By inquiry and comparison, the yield of the rose essential oil prepared by the traditional water distillation method is about 0.025 percent, and the yield of the rose essential oil prepared by the subcritical method is about 0.1 percent, so that the yield of the rose essential oil prepared by supermolecular self-assembly of the invention is as high as 0.35 percent, and the yield of the rose essential oil is obviously improved.

In the invention, the rose, the mixture of rose leaves, rose branches and rose roots in the whole plant of the rose is dry or fresh, and the influence on the yield of the extracted rose essential oil is little; the content ratio of the rose, the rose fruit, and the mixture of the rose leaves, the rose branches and the rose roots in the whole plant of the rose also has little influence on the yield of the extracted rose essential oil, and all the content ratios are in a controllable range.

The above-described preferred embodiments should be considered as illustrations of embodiments of the present invention, and it would be apparent to those skilled in the art that any insubstantial changes, modifications, technical derivations, substitutions and alterations can be made to these embodiments without departing from the principle and spirit of the present invention.

Claims

1. A method for supermolecule self-assembly of rose extract and preparation of rose essential oil and nano materials is characterized by comprising the following steps:

c. homogenizing and mixing the rose liquid phase component, the rose fruit liquid phase oil component and the liquid phase mixed component obtained in the step b to obtain a rose full-component mixture, and performing ultrasonic treatment and supermolecule self-assembly to obtain a fluid-like substance;

d. purifying the rose essential oil from the fluid substance obtained by self-assembly of the supermolecule;

2. The supramolecular self-assembly and preparation method of rose essential oil and nano-materials of claim 1, wherein the supramolecular self-assembly comprises the following steps: in the step a, the roses are clean and impurity-free fresh roses or dry roses; the rose hip is the seed of clean and impurity-free mature rose hip; the rose leaves, rose branches and rose roots are fresh or dried clean and free of impurities.

3. The supramolecular self-assembly and preparation method of rose essential oil and nanometer material of claim 1, wherein the specific operation method of step a is as follows:

and fourthly, mixing the rose solid-phase residue and the rose fruit solid-phase pomace treated in the three steps and a pre-crushed mixture of rose leaves, rose branches and rose roots again, drying, and performing superfine crushing to 800-1200 meshes to obtain a solid-phase mixture.

4. The supramolecular self-assembly and preparation method of rose essential oil and nano-materials of claim 1, wherein the supramolecular self-assembly comprises the following steps: the aqueous enzymatic extraction of the liquid phase mixed component comprises two steps of ultrasonic size mixing treatment and enzymatic hydrolysis.

5. The supramolecular self-assembly and preparation method of rose essential oil and nano-materials of claim 4, wherein the supramolecular self-assembly comprises the following steps: the ultrasonic size mixing treatment comprises the steps of adding a rose liquid-phase component, a rose fruit liquid-phase oil component and a solid-phase mixture into an ultrasonic auxiliary stirring device according to the proportion of 1: 8-9: 10-11, stirring and size mixing, wherein the ultrasonic size mixing temperature is 25-35 ℃, and the size mixing time is 30-45 min; and (3) after ultrasonic size mixing treatment, adding complex enzyme for hydrolysis, concentrating and separating out a liquid phase mixture after extraction is finished, and preparing the carbon nano material from the residual solid phase dregs.

6. The method for supermolecule self-assembly of rose extract and preparation of rose essential oil and nano material according to claim 5, wherein the complex enzyme is prepared by mixing cellulase, hemicellulase, pectinase, amylase and protease according to a weight ratio of 30-60: 20-30: 10-20: 5-10.

7. The supramolecular self-assembly of rose extract and method for preparing rose essential oil and nano material as claimed in claim 5, wherein the method for preparing carbon nano material is: and (3) pretreating the residual solid-phase slag in a steam explosion device, then carrying out high-temperature treatment in a high-temperature furnace, fully carbonizing, and collecting to obtain the carbon nano material with the size of 60-90 nm.

8. The supramolecular self-assembly of rose extract and method for preparing rose essential oil and nano material as claimed in claim 1, wherein the supramolecular self-assembly in step c comprises two stages:

9. The supramolecular self-assembly of rose extract and method for preparing rose essential oil and nano material as claimed in claim 1, wherein the method for purifying rose essential oil in step d is extracting high purity rose essential oil by supercritical carbon dioxide extraction separation.

10. The supramolecular self-assembly and preparation method of rose essential oil and nano-material of claim 1, wherein the method for preparing nano-biomedical material in step e comprises: and carrying out ultrasonic oscillation extraction, freeze concentration and low-temperature freeze drying on the remainder after extracting the rose essential oil to obtain the nano biomedical material.