CN110643432A

CN110643432A - Method for preparing cedar essential oil by using old roots of cedar as raw materials

Info

Publication number: CN110643432A
Application number: CN201910835320.1A
Authority: CN
Inventors: 卞奎友
Original assignee: Individual
Current assignee: Individual
Priority date: 2019-09-05
Filing date: 2019-09-05
Publication date: 2020-01-03

Abstract

The invention discloses a method for preparing cedar essential oil by taking old cedar roots as raw materials, which is characterized in that the old tree roots left in forest land for many years are subjected to fine processing to extract biological essential oil, and then are prepared into active carbon, thereby not only improving the economic benefit of enterprises, but also reducing the emission of harmful gas in the forest land and in the distillation process and protecting the ecological environment.

Description

Method for preparing cedar essential oil by using old roots of cedar as raw materials

Technical Field

The invention relates to a preparation technology of fir essential oil, in particular to a method for extracting biological essential oil by taking old fir roots as raw materials.

Background

The plant extract is a product formed by taking plants as raw materials, directionally obtaining and concentrating one or more active ingredients in the plants through a physical or chemical separation and extraction process according to the application requirements of the extracted final product, and not changing the structures of the active ingredients.

The biological extract, namely the 'essential oil', is a general name of oily substances existing in plants and capable of being separated out along with distillation and dry distillation, has unique physiological functions, and has important effects in the aspects of food, medicine, health care, beauty treatment and the like.

The cedar essential oil is colorless or yellowish oily liquid with fragrance similar to ambergris and musk, has unique physiological activity and wide application, and is a natural bactericide and preservative for storing grains, fruits and vegetables; the extracted essential oil is natural perfume, has unique fragrance which cannot be replaced by synthetic perfume, has no toxic or side effect, and is favored by the market; thirdly, the product is used as a raw material of human health care, beauty treatment and cosmetics; fourthly, has certain medicinal value. After further separation, the fir essential oil can also produce the medicine with the functions of relieving asthma, resisting inflammation, diminishing inflammation, resisting fungi, relieving pain and preventing corrosion.

China fir, commonly called as redcore China fir and cedar, is a main tree species used in China, and the afforestation area and the forest stock amount of the China fir are the first places of artificial forests in China. According to the fourth national forest resource clearing statistics, the area of the artificial Chinese fir forest reaches 911 million hectares, which accounts for 30.4 percent of the area of the artificial forest in China, and the total accumulation is 3.4 billion cubic meters. Plays an important role in national economy. Particularly, Jiangxi province is the main distribution area and producing area of China fir, the area of the fir in the whole province is about 140 million hectares, the area accounts for 30 percent of the total forest area of the whole province, and the storage amount of mature forest is about 5500 million cubic meters. During the wood cutting process, a large amount of lignocellulose waste such as China fir sawdust and the like is generated and is used as a raw material for extracting China fir essential oil and producing activated carbon. Although the fir harvested in the overground part is fully utilized, the roots of the fir buried in the soil are a huge resource and are never effectively utilized after the woods are harvested in the past year. Old tree roots left in the forest land not only affect artificial forestation, but also volatilize volatile organic compounds such as VOS4 and the like in rotting and pollute the environment. The method has the advantages that the aged root resources of the cedars are developed, the cedar essential oil is extracted, the pressure caused by the increasing demand of natural plant essential oil in China can be relieved, cedar oil which is widely applied in the past is replaced, the cedar planting in artificial forestation can be facilitated, and the economic development of forest regions in China is promoted. After the fir tree roots are treated by the process to extract the fir essential oil, the rest substances can be extruded at high temperature to form, and then the fir tree roots are prepared into the granular active carbon. The active carbon can be widely applied to deep purification of domestic water, industrial wastewater treatment, air purification and industrial waste gas treatment.

Disclosure of Invention

The invention aims to solve and recover the problem that the old fir tree root resources left in the forest land for years in the long-term timber production and felling are processed to prepare the essential oil and then are prepared into the activated carbon to achieve the purpose of full utilization. The inventor successfully researches a method for preparing the cedar essential oil by taking the aged roots of the cedar as the raw material through repeated research experiments, thereby completing the invention.

The method has the advantages of high utilization rate, and not only realizes the characteristics of completely squeezing the dried Chinese fir roots, but also obtains higher economic benefit and green and environment-friendly ecological benefit.

The method comprises the steps of washing most of collected half-rotten whole tree roots by using a high-pressure water gun to remove mud and rotten materials, rotary-cutting a washed old tree root skeleton into 5cm thick pieces, carrying out coarse crushing to obtain coarse materials, carrying out secondary crushing on the coarse materials, sieving by using a sieve with 10-60 meshes, and drying to obtain crushed powder materials.

Through repeated test screening, the invention finally determines that 100 kg of crushed powder materials after crushing and screening are added with 1 kg to 2 kg of urea containing 46 percent of nitrogen (N) and used as a catalyst to be stirred uniformly. If the outer skin of the fir wood root is rotten and the wood appearance is fresh, adding urea containing 46 percent of nitrogen (N) according to 2 percent of the weight of the crushed powder; if the outer wood of Chinese fir root is rotted to form skeleton, urea containing 46% of nitrogen (N) is added according to 1% of the weight of the crushed powder. Urea has protein denaturation, particularly proteins that can effectively break non-covalent bonds. This feature may improve the solubility of certain proteins. Therefore, the urea is added into the crushed material of the root of the old fir and the distillation process is improved, and the effect is shown in two aspects: firstly, the oil yield is increased, the fresh cedar chips are distilled according to the conventional process, the oil yield is about 5 percent, and the oil yield of the cedar roots added with the urea can reach more than 7 to 8 percent. That is, compared with the conventional process that one ton of fir essential oil consumes 18-20 tons of raw materials, the new process of the invention with the added urea reduces the consumption of one ton of fir essential oil from 18-20 tons of raw materials of the conventional process to 13-15 tons of raw materials. Secondly, the contents of cedrol and cedrene in the root distillate oil are increased, the contents of cedrol and cedrene in the cedar chip essential oil prepared by the conventional process are only 55-56%, and the selling price per ton is 2-3 ten thousand yuan. And because urea is added into the roots of the aged cedar trees with the same water content and the same weight as the aged cedar trees, the contents of cedar brain and cedar alkene in the essential oil can be improved to 58-60 percent, the selling price per ton is also improved to 4-4.2 ten thousand yuan, and the increased economic benefit is obvious.

The scheme of the invention is that firstly, the well stirred root material of the aged fir is put into a vertical distillation retort, boiler steam is introduced from the bottom, essential oil is distilled out from an oil outlet pipe at the upper part along with the steam through three-stage distillation, and is introduced into a condenser, and oil-water separation is realized through cooling, so as to obtain the fir essential oil.

According to the invention, old tree roots left in the forest land for many years are subjected to fine processing to extract the biological essential oil and then are prepared into the active carbon, so that the economic benefit of enterprises is improved, the pollution caused by the rot of the tree roots in the forest land for many years and the emission of harmful gas in the distillation process are reduced, and the ecological environment is protected.

Detailed Description

The preparation method of the aged cedar root essential oil comprises the following steps:

1. washing collected fir tree roots under high pressure, removing soil and rotten sundries, rotary cutting the washed fir tree roots into 5cm wood chips, crushing to obtain coarse materials, crushing the coarse materials for the second time, sieving by a sieve of 10-60 meshes to obtain powder materials, and drying to control the water content to be 20-25%;

2. adding 1 kg-2 kg of nitrogen (N) -containing 46% urea into 100 kg of crushed powder material after crushing and drying, and stirring into a uniform mixture; if the outer skin of the fir wood root is rotten and the wood appearance is fresh, adding urea containing 46 percent of nitrogen (N) according to 2 percent of the weight of the crushed powder; if the outer wood of the fir wood root is rotted to form a skeleton, adding urea containing 46 percent of nitrogen (N) according to 1 percent of the weight of the crushed powder;

3. adding the uniformly stirred mixture into a distillation tank by using a conveyor, reserving a space of 30 cm at the upper part of the distillation tank, and closing an upper cover of the distillation tank;

4. and (3) distillation: the invention adopts a three-stage sectional type pressurizing and heating distillation method which is developed by self test and is different from the traditional conventional distillation method:

(1) first-stage distillation, closing the valve of the oil outlet pipe at the upper part of the distillation tank, introducing steam, adjusting the pressure of the steam in a boiler to 5-7 Mpa (MPa), keeping the flow rate of the steam at 94ml/min, and keeping the temperature in the distillation tank for 20-30min when the temperature rises to 120 ℃; under the action of pressure, water vapor enters cells of lignin and cellulose, so that essential oil solidified in cell walls is diluted, and urea is used for dissolving protein, thereby laying the foundation for distilling the essential oil. On the other hand, the temperature and pressure from the steam force the cell cavity to expand and open a channel for the essential oil to be distilled out;

(2) continuously pressurizing the secondary distillation, opening an oil outlet pipe valve at the upper part of the distillation tank when the temperature in the tank rises to 135 ℃, distilling off a large amount of essential oil in the mixture from an oil outlet pipeline at the upper part of the tank body along with water vapor to enter a condenser, and rapidly increasing the oil yield of the essential oil along with the increase of the steam flow when the temperature in the tank rises to 150 ℃ and the pressure of boiler gas rises to 7-8 Mpa, wherein the control time is 60-65 min;

(3) continuously pressurizing the three-stage distillation, distilling for 40min when the temperature in the tank rises to 160 ℃, and distilling for 20min when the oil yield is not increased when the steam flow reaches 100 ml/min;

5. introducing all the oil-water mixture obtained by the third-stage distillation into a condenser, condensing to normal temperature, filtering out white mucus with a fine filter screen to obtain fir root distillation essential oil, filling into a barrel, and warehousing;

6. and (5) after deslagging. Then new materials are filled into the distillation tank, and the circulation production is carried out in sequence.

7. Collecting the distilled waste residue, and then preparing the wood activated carbon by a physical method.

Claims

1. A method for preparing fir essential oil by taking old fir roots as a raw material is characterized by comprising the following steps: the traditional Chinese medicine is prepared from the following raw materials in parts by weight:

100 kg of crushed and dried old fir root powder material is added with 1 kg-2 kg of nitrogen (N) containing 46% urea.

2. The method for preparing fir essential oil according to claim 1, wherein: it comprises the following steps:

(1) washing collected fir tree roots under high pressure, removing soil and rotten sundries, rotary cutting the washed fir tree roots into 5cm wood chips, crushing to obtain coarse materials, crushing the coarse materials for the second time, sieving by a sieve of 10-60 meshes to obtain powder materials, and drying to control the water content to be 20-25%;

(2) adding 1 kg-2 kg of nitrogen (N) -containing 46% urea catalyst into 100 kg of crushed powder material after crushing and drying, and stirring into a uniform mixture; if the outer skin of the fir wood root is rotten and the wood appearance is fresh, adding urea containing 46 percent of nitrogen (N) according to 2 percent of the weight of the crushed powder; if the outer wood of the fir wood root is rotted to form a skeleton, adding urea containing 46 percent of nitrogen (N) according to 1 percent of the weight of the crushed powder;

(3) adding the uniformly stirred mixture into a distillation tank by using a conveyor, reserving a space of 30 cm at the upper part of the distillation tank, and closing an upper cover of the distillation tank;

(4) and (3) distillation: a three-stage sectional type pressurizing and heating distillation method is adopted:

firstly, first-stage distillation, closing a distillation tube valve at the upper part of a distillation tank, introducing steam, adjusting the pressure of the steam in a boiler to 5-7 Mpa (megapascal), enabling the flow rate of the steam to be 94ml/min, and keeping for 20-30min when the temperature in the distillation tank rises to 120 ℃; under the action of pressure, water vapor enters cells of lignin and cellulose, so that essential oil solidified in cell walls is diluted and protein is dissolved by urea on one hand, a foundation is laid for distillation of the essential oil, and on the other hand, the temperature and the pressure of the steam force cell cavities to be enlarged to open a channel for distillation of the essential oil;

secondly, continuously pressurizing the secondary distillation, opening an oil outlet pipe valve at the upper part of the distillation tank when the temperature in the tank rises to 135 ℃, distilling the essential oil in the mixture from an oil outlet pipeline at the upper part of the tank body along with water vapor to enter a condenser, and rapidly increasing the oil yield of the essential oil along with the increase of the steam flow when the temperature in the tank rises to 150 ℃ and the pressure of boiler gas rises to 7-8 Mpa, wherein the control time is 60-65 min;

thirdly, continuously increasing the pressure by the three-stage distillation, distilling for 40min when the temperature in the tank rises to 160 ℃, and distilling for 20min after the oil yield is not increased when the steam flow reaches 100 ml/min;

(5) introducing all the oil-water mixture obtained by the third-stage distillation into a condenser, condensing to normal temperature, filtering out white mucus with a fine filter screen to obtain fir root distillation essential oil, filling into a barrel, and warehousing.