阅读说明：本技术 一种龙脑樟天然冰片分离工艺 (Process for separating natural borneol of borneol camphor ) 是由 李靖 杨翔顺 于 2021-10-28 设计创作，主要内容包括：本发明涉及天然冰片制造技术领域,具体为一种龙脑樟天然冰片分离工艺,包括以下步骤：S1、选取原料,将龙脑樟各部位进行区分,原料选取龙脑樟的树叶；S2、将龙脑樟树叶放入粉碎机粉碎,将粉碎过的龙脑樟树叶放入加入汽油的水中浸泡；S3、将浸泡的龙脑樟树叶碎末倒入萃取罐中煮沸,萃取罐顶部安装有导管,导管另一端连接有结晶室；S4、结晶室内壁顶端安装有若干棉绳,结晶室外安装有冷凝机,往结晶室输入氩气；本发明通过设置棉绳和增加结晶室内的压强,可以使天然冰片更快速的在棉绳表面进行结晶,加速了天然冰片的结晶,缩短了天然冰片的成型时间,也减少了收取天然冰片结晶的时间。(The invention relates to the technical field of natural borneol preparation, in particular to a borneol camphor natural borneol separation process, which comprises the following steps: s1, selecting raw materials, distinguishing all parts of the cinnamomum camphora, and selecting leaves of the cinnamomum camphora as the raw materials; s2, putting the borneol camphor tree leaves into a grinder to be ground, and putting the ground borneol camphor tree leaves into water added with gasoline to be soaked; s3, pouring the soaked borneol camphor tree leaf powder into an extraction tank to be boiled, wherein the top of the extraction tank is provided with a conduit, and the other end of the conduit is connected with a crystallization chamber; s4, installing a plurality of cotton ropes at the top end of the inner wall of the crystallization chamber, installing a condenser outside the crystallization chamber, and inputting argon into the crystallization chamber; according to the invention, the cotton rope is arranged and the pressure in the crystallization chamber is increased, so that the natural borneol can be crystallized on the surface of the cotton rope more quickly, the crystallization of the natural borneol is accelerated, the forming time of the natural borneol is shortened, and the time for collecting the natural borneol crystals is also reduced.)

1. A process for separating natural borneol from borneol camphor is characterized by comprising the following steps: the method comprises the following steps:

s1, selecting raw materials, distinguishing all parts of the cinnamomum camphora, and selecting leaves of the cinnamomum camphora as the raw materials;

s2, putting the borneol camphor tree leaves into a grinder to be ground, and putting the ground borneol camphor tree leaves into water added with gasoline to be soaked;

s3, pouring the soaked borneol camphor tree leaf powder into an extraction tank to be boiled, wherein the top of the extraction tank is provided with a conduit, and the other end of the conduit is connected with a crystallization chamber;

s4, a plurality of cotton ropes are arranged at the top end of the inner wall of the crystallization chamber, a condensing machine is arranged outside the crystallization chamber, and argon is input into the crystallization chamber.

2. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: the method comprises the steps of selecting borneol camphor tree leaves as raw materials, selecting 200-300 g of the borneol camphor tree leaves, removing petioles of the borneol camphor tree leaves, and then cleaning with clear water.

3. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: and putting the borneol camphor leaf with the leaf stalk removed and cleaned into a grinder, and stirring and grinding for 5-15 minutes.

4. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: preparing a soaking solvent: mixing 400-500 g of water and 300-390 g of gasoline in parts by weight, and stirring for 10-20 minutes.

5. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: and pouring the crushed borneol camphor leaf particles into a soaking solvent to be soaked for 20-24 h, wherein the size of the crushed borneol camphor leaf particles is less than 1 mm.

6. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: after the borneol camphor leaf particles are soaked, the borneol camphor leaf particles and a soaking solvent are poured into an extraction tank together for heating, and the heating temperature is kept at 95-110 ℃.

7. The process for separating the natural borneol from the borneol camphor according to claim 1, which is characterized in that: in the heating process, steam in the extraction tank enters the crystallization chamber through the guide pipe, the temperature of the crystallization chamber is 10-20 ℃, the length of a cotton rope in the crystallization chamber is 10-20 cm, the diameter of the cotton rope is 1-2.5 mm, the crystallization chamber is sealed when the steam is crystallized, argon is input into the crystallization chamber at the flow rate of 0.05-0.6 MPa for 10-15 times in the crystallization period, the input time is 5-10 minutes each time, and the crystallization time is 2-3 days.

Technical Field

The invention relates to the technical field of natural borneol preparation, in particular to a process for separating borneol and camphor natural borneol.

Background

The borneol camphor tree is a rare medicinal material, is a high-grade spice and is an important chemical raw material, the borneol camphor tree is also a raw material for preparing natural borneol, the natural borneol is a traditional Chinese medicine name and is prepared by extracting and processing fresh branches and leaves of Lauraceae plants, the natural borneol is white crystalline powder or flaky crystal, the smell is fragrant, the taste is pungent and cool, the borneol is volatile, dense smoke exists when the borneol is ignited, and the flame is yellow.

At present, the natural borneol is mostly prepared by a steam distillation method, the operation is simple, the investment is low, the purity of the produced natural borneol is high, but the production needs long time, the production efficiency is low, and the improvement is needed.

Disclosure of Invention

The invention aims to provide a process for separating natural borneol from borneol camphor, which comprises the following steps:

s1, selecting raw materials, distinguishing all parts of the cinnamomum camphora, and selecting leaves of the cinnamomum camphora as the raw materials;

s2, putting the borneol camphor tree leaves into a grinder to be ground, and putting the ground borneol camphor tree leaves into water added with gasoline to be soaked;

s3, pouring the soaked borneol camphor tree leaf powder into an extraction tank to be boiled, wherein the top of the extraction tank is provided with a conduit, and the other end of the conduit is connected with a crystallization chamber;

s4, a plurality of cotton ropes are arranged at the top end of the inner wall of the crystallization chamber, a condensing machine is arranged outside the crystallization chamber, and argon is input into the crystallization chamber.

Optionally, the raw materials are selected from camphor tree leaves, 200-300 g of camphor tree leaves are selected, petioles of the camphor tree leaves are removed, and then the camphor tree leaves are cleaned by clear water.

Optionally, the borneol camphor leaves after the cleaning of the leaf stalks are put into a pulverizer to be stirred and pulverized for 5-15 minutes.

Optionally, preparing a soaking solvent: mixing 400-500 g of water and 300-390 g of gasoline in parts by weight, and stirring for 10-20 minutes.

Optionally, the crushed borneol camphor leaf particles are poured into a soaking solvent to be soaked for 20-24 hours, and the size of the crushed borneol camphor leaf particles is smaller than 1 mm.

Optionally, after the borneol camphor leaf particles are soaked, the borneol camphor leaf particles and the soaking solvent are poured into an extraction tank together for heating, and the heating temperature is kept at 95-110 ℃.

Optionally, in the heating process, steam in the extraction tank enters the crystallization chamber through the guide pipe, the temperature of the crystallization chamber is 10-20 ℃, the length of a cotton rope in the crystallization chamber is 10-20 cm, the diameter of the cotton rope is 1-2.5 mm, the crystallization chamber is sealed when steam is crystallized, argon is input into the crystallization chamber at the flow rate of 0.05-0.6 MPa, the argon is input for 10-15 times in the crystallization period, the input time is 5-10 minutes each time, and the crystallization time is 2-3 days.

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

according to the invention, the cotton rope is arranged and the pressure in the crystallization chamber is increased, so that the natural borneol can be crystallized on the surface of the cotton rope more quickly, the crystallization of the natural borneol is accelerated, the forming time of the natural borneol is shortened, and the time for collecting the natural borneol crystals is also reduced.

Drawings

FIG. 1 is a process flow diagram of the present invention.

The objects, features, and advantages of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The invention provides a process for separating natural borneol from borneol camphor, which comprises the following steps:

s1, selecting raw materials, distinguishing all parts of the cinnamomum camphora, and selecting leaves of the cinnamomum camphora as the raw materials;

selecting borneol camphor tree leaves as raw materials, selecting 270g of the borneol camphor tree leaves, removing petioles of the borneol camphor tree leaves, and then cleaning with clear water; the natural borneol content in the borneol camphor tree leaves is the most, dried branches and leaves of the borneol camphor tree are divided into branch bark, branch xylem, tail end branches and leaves, then coarse extraction is carried out, and the extracted natural borneol mass fractions are respectively: 50.2%, 24.3%, 47.6% and 71.5%, knowing that the content of natural borneol in the camphor tree leaves is the most, selecting the camphor tree leaves as the raw material can easily improve the content of natural borneol and can also obtain more yield;

s2, putting the borneol camphor tree leaves into a grinder to be ground, and putting the ground borneol camphor tree leaves into water added with gasoline to be soaked;

the borneol camphor leaf after the cleaning of the leaf stalk is removed is put into a pulverizer to be stirred and pulverized for 10 minutes, and a soaking solvent is prepared: mixing 400g of water and 300g of gasoline, stirring for 15 minutes, pouring the crushed borneol camphor leaf particles into a soaking solvent, soaking for 22 hours, wherein the size of the crushed borneol camphor leaf particles is less than 1mm, the gasoline has strong penetrating power to plant cells, lipophilic components such as starch, polysaccharide and the like in the borneol camphor leaf have high solubility in the gasoline, the components in the crushed borneol camphor leaf particles can be purified, the distillation temperature of the gasoline is matched with the borneol camphor leaf particles, the water is used as a common extraction solution, the bottom of an extraction tank can be well prevented from being burnt, and the steam and the gasoline steam carry natural borneol components to upwards enter a conduit, so that the natural borneol oil can be better separated during further purification, and the subsequent crystallization treatment is facilitated;

s3, pouring the soaked borneol camphor tree leaf powder into an extraction tank to be boiled, wherein the top of the extraction tank is provided with a conduit, and the other end of the conduit is connected with a crystallization chamber;

after the borneol camphor leaf particles are soaked, pouring the borneol camphor leaf particles and a soaking solvent into an extraction tank for heating, and keeping the heating temperature at 110 ℃; during heating, the borneol camphor leaf particles in the extraction tank need to be stirred to prevent the borneol camphor leaf particles from being burnt, natural borneol essential oil in the borneol camphor leaf particles rises along with steam in the extraction tank to enter the guide pipe, and the guide pipe is arranged to guide and convey the steam;

s4, installing a plurality of cotton ropes at the top end of the inner wall of the crystallization chamber, installing a condenser outside the crystallization chamber, and inputting argon into the crystallization chamber;

during heating, steam in the extraction tank enters a crystallization chamber through a guide pipe, the temperature of the crystallization chamber is 13 ℃, the length of a cotton rope in the crystallization chamber is 20cm, the diameter of the cotton rope is 2mm, the crystallization chamber is closed during steam crystallization, argon is input into the crystallization chamber, the flow rate is 0.45MPa, the argon is input for 12 times in the crystallization period, each time is input for 5 minutes, and the crystallization time is 3 days; the vapor is guided to the crystallization chamber through the guide pipe, a plurality of cotton ropes are arranged at the top end of the crystallization chamber, more fibers are arranged on the cotton ropes, the natural borneol can be more easily attached to the cotton ropes when being crystallized, the crystallization process of the natural borneol is accelerated, the cotton ropes can also absorb the moisture in the vapor and guide the moisture to flow downwards, the problem that the crystal part of the natural borneol is dissolved in the water again and flows downwards to influence the output of the natural borneol is avoided, when the vapor in the extraction tank partially enters the crystallization chamber, the crystallization chamber is closed, argon is input into the crystallization chamber to increase the air pressure in the crystallization chamber, the natural borneol can be crystallized faster, the argon is inert gas, the property is more stable, the reaction between the argon and the natural borneol crystal can be avoided, a water pool is arranged at the lower end of the crystallization chamber and is used for storing condensed moisture, and the natural borneol can be crystallized on the surface more rapidly by arranging the cotton ropes and increasing the pressure in the crystallization chamber, accelerates the crystallization of the natural borneol, shortens the forming time of the natural borneol and reduces the time for collecting the natural borneol crystals.

The following table shows the effect of distillation time on the yield of natural borneol product:

example 2

The invention provides a process for separating natural borneol from borneol camphor, which comprises the following steps:

s1, selecting raw materials, distinguishing all parts of the cinnamomum camphora, and selecting leaves of the cinnamomum camphora as the raw materials;

selecting borneol camphor tree leaves as raw materials, selecting 260g of the borneol camphor tree leaves, removing petioles of the borneol camphor tree leaves, and then cleaning with clear water; the natural borneol content in the borneol camphor tree leaves is the most, dried branches and leaves of the borneol camphor tree are divided into branch bark, branch xylem, tail end branches and leaves, then coarse extraction is carried out, and the extracted natural borneol mass fractions are respectively: 50.2%, 24.3%, 47.6% and 71.5%, knowing that the content of natural borneol in the camphor tree leaves is the most, selecting the camphor tree leaves as the raw material can easily improve the content of natural borneol and can also obtain more yield;

s2, putting the borneol camphor tree leaves into a grinder to be ground, and putting the ground borneol camphor tree leaves into water added with ethanol to be soaked;

the borneol camphor leaf after the cleaning of the leaf stalk is removed is put into a pulverizer to be stirred and pulverized for 15 minutes, and a soaking solvent is prepared: mixing 460g of water and 320g of ethanol, stirring for 20 minutes, pouring the crushed borneol camphor leaf particles into a soaking solvent, soaking for 21 hours, wherein the size of the crushed borneol camphor leaf particles is less than 1mm, the ethanol has strong penetrating power on plant cells, lipophilic components such as mucoid, pectin and the like in the borneol camphor leaf particles also have high solubility in the ethanol, the components in the crushed borneol camphor leaf particles can be purified, the water is used as a common extraction solution, the bottom of an extraction tank can be well prevented from being burnt, and water vapor and ethanol vapor carry natural borneol components to upwards enter a conduit, so that the natural borneol oil can be better separated during further purification, the subsequent crystallization treatment is facilitated, and the ethanol is used as the extraction solvent to facilitate the environmental protection;

s3, pouring the soaked borneol camphor tree leaf powder into an extraction tank to be boiled, wherein the top of the extraction tank is provided with a conduit, and the other end of the conduit is connected with a crystallization chamber;

after the borneol camphor leaf particles are soaked, pouring the borneol camphor leaf particles and a soaking solvent into an extraction tank for heating, and keeping the heating temperature at 100 ℃; during heating, the borneol camphor leaf particles in the extraction tank need to be stirred to prevent the borneol camphor leaf particles from being burnt, natural borneol essential oil in the borneol camphor leaf particles rises along with steam in the extraction tank to enter the guide pipe, and the guide pipe is arranged to guide and convey the steam;

s4, installing a plurality of cotton ropes at the top end of the inner wall of the crystallization chamber, installing a condenser outside the crystallization chamber, and inputting argon into the crystallization chamber;

during heating, steam in the extraction tank enters a crystallization chamber through a guide pipe, the temperature of the crystallization chamber is 10 ℃, the length of a cotton rope in the crystallization chamber is 15cm, the diameter of the cotton rope is 1.5mm, the crystallization chamber is closed when steam is crystallized, argon is input into the crystallization chamber, the flow rate is 0.6MPa, the argon is input for 10 times in the crystallization period, each time, the input time is 7 minutes, and the crystallization time is 2.5 days; the vapor is guided to the crystallization chamber through the guide pipe, a plurality of cotton ropes are arranged at the top end of the crystallization chamber, more fibers are arranged on the cotton ropes, the natural borneol can be more easily attached to the cotton ropes when being crystallized, the crystallization process of the natural borneol is accelerated, the cotton ropes can also absorb the moisture in the vapor and guide the moisture to flow downwards, the problem that the crystal part of the natural borneol is dissolved in the water again and flows downwards to influence the output of the natural borneol is avoided, when the vapor in the extraction tank partially enters the crystallization chamber, the crystallization chamber is closed, argon is input into the crystallization chamber to increase the air pressure in the crystallization chamber, the natural borneol can be crystallized faster, the argon is inert gas, the property is more stable, the reaction between the argon and the natural borneol crystal can be avoided, a water pool is arranged at the lower end of the crystallization chamber and is used for storing condensed moisture, and the natural borneol can be crystallized on the surface more rapidly by arranging the cotton ropes and increasing the pressure in the crystallization chamber, accelerates the crystallization of the natural borneol, shortens the forming time of the natural borneol and reduces the time for collecting the natural borneol crystals.

The following table shows the effect of distillation time on the yield of natural borneol product:

according to the embodiment, compared with the method using ethanol as the extraction solvent, the extraction efficiency of the natural borneol is higher, the crystallization time of the natural borneol is shortened by 20-25% by arranging cotton ropes in the crystallization chamber and increasing the pressure, and the production efficiency of the natural borneol is greatly improved.

While the invention has been described in further detail in connection with specific embodiments thereof, it will be understood that the invention is not limited thereto, and that various other modifications and substitutions may be made by those skilled in the art without departing from the spirit of the invention, which should be considered to be within the scope of the invention as defined by the appended claims.