阅读说明：本技术 一种天然龙脑的提取精制工艺 (Extraction and refining process of natural borneol ) 是由 熊华民 于 2020-10-31 设计创作，主要内容包括：本发明涉及天然龙脑制备领域,具体为一种天然龙脑的提取精制工艺,包括以下步骤：1)取粗脑原料清洗,脱水干燥；2)将步骤1)中清洗后的原料置入真空罐,真空罐抽真空,使真空罐处于真空状态；3)对步骤2)中的真空罐充入惰性气体,控制真空罐内的压力,范围值在0.005至0.02MPa；4)电脑控制真空罐内温度,使真空罐内的罐顶温度维持在50-90℃,罐内气压控制在0.15MPa以内,时间控制为1-3h；5)降温冷却,温度维持在40-50℃最佳,真空罐内进气,达到正常气压,开罐,提取成品。本发明提纯度高,工艺步骤简单,操作方便,生产成本低,并且采用食品级或药品级的工业提纯工艺,产品能够达到医用标准。(The invention relates to the field of natural borneol preparation, in particular to a process for extracting and refining natural borneol, which comprises the following steps: 1) cleaning raw brain, dehydrating and drying; 2) putting the cleaned raw materials in the step 1) into a vacuum tank, and vacuumizing the vacuum tank to enable the vacuum tank to be in a vacuum state; 3) filling inert gas into the vacuum tank in the step 2), and controlling the pressure in the vacuum tank to be in a range of 0.005-0.02 MPa; 4) controlling the temperature in the vacuum tank by a computer, keeping the temperature of the tank top in the vacuum tank at 50-90 ℃, controlling the pressure in the tank within 0.15MPa, and controlling the time to be 1-3 h; 5) cooling, maintaining the temperature at 40-50 deg.C, introducing air to normal pressure, opening the tank, and extracting. The invention has the advantages of high purification degree, simple process steps, convenient operation and low production cost, and the product can reach the medical standard by adopting a food-grade or pharmaceutical-grade industrial purification process.)

1. The extraction and refining process of natural borneol is characterized by comprising the following steps:

1) cleaning raw brain, dehydrating and drying;

2) putting the cleaned raw materials in the step 1) into a vacuum tank, and vacuumizing the vacuum tank to enable the vacuum tank to be in a vacuum state;

3) filling inert gas into the vacuum tank in the step 2), and controlling the pressure in the vacuum tank to be in a range of 0.005-0.02 MPa;

4) controlling the temperature in the vacuum tank by a computer, keeping the temperature of the tank top in the vacuum tank at 50-90 ℃, controlling the pressure in the tank within 0.15MPa, and controlling the time to be 1-3 h;

5) cooling, maintaining the temperature at 40-50 deg.C, introducing air into the vacuum tank to reach normal pressure, opening the tank, and extracting to obtain the final product.

2. The extraction and refining process of natural borneol according to claim 1, which is characterized in that: the water content in the step 1) is controlled to be less than 1%.

3. The extraction and refining process of natural borneol according to claim 1, which is characterized in that: the temperature in the step 1) is controlled to be below 50 ℃.

4. The extraction and refining process of natural borneol according to claim 1, which is characterized in that: and in the step 1), dewatering and drying are carried out by adopting methods such as a cold dryer, a vacuum dryer, a dehydrator, drying, natural drying and the like.

5. The extraction and refining process of natural borneol is characterized by comprising the following steps:

1) cleaning raw brain, dehydrating and drying;

2) selecting 65-95% alcohol, and proportioning the alcohol and the cleaned raw materials in the step 1), wherein the proportion is 1: 0.5-3, heating and dissolving the proportioned solution in water bath, wherein the temperature range is 80-100 ℃;

3) quickly filtering after dissolving, and standing to normal temperature;

4) cooling the normal-temperature solution obtained in the step 3);

5) crystallizing, crystallizing the product obtained in the step 4), and filtering again;

6) and (3) drying at low temperature, namely drying the product filtered in the step 5) at low temperature, and controlling the temperature to be below 50 ℃ to obtain a finished product.

6. The extraction and refining process of natural borneol according to claim 5, which is characterized in that: and in the step 3), a filter of 1000 meshes to 10000 meshes or 0.3 micron is adopted for filtering.

7. The extraction and refining process of natural borneol according to claim 5, which is characterized in that: the temperature reduction and cooling in the step 4) adopt a sectional type temperature reduction method, the optimal temperature is gradually adjusted from 0 ℃ to-40 ℃, and the time is 12-48 h.

8. The extraction and refining process of natural borneol according to claim 5, which is characterized in that: the temperature reduction and cooling in the step 4) adopt a constant temperature cooling method, the optimal temperature range is from minus 10 ℃ to minus 30 ℃, and the time is 24-48 h.

9. The extraction and refining process of natural borneol according to claim 5, which is characterized in that: and in the step 5), a filter with 300-1000 meshes is adopted for filtering.

10. The extraction and refining process of natural borneol according to any one of claims 1 to 9, characterized by comprising the following steps: extracting according to the extraction and refinement process of the natural borneol of the claims 1 to 4, further refining according to the extraction and refinement process of the natural borneol of the claims 5 to 9 after extraction, and obtaining a high-purity product by repeated refining according to the extraction and refinement process of the natural borneol of the claims 5 to 9.

Technical Field

The invention relates to the field of borneol preparation, in particular to a process for extracting and refining natural borneol.

Background

Borneol is commonly called borneol, and natural borneol is borneol extracted and processed from plants. The source of the camphor is different from that of the camphor, the isoborneol and trace other volatile oil components. The borneol used as medicine and high-grade spice is hopeful to have the content of non-borneol as low as possible, and the content of levo-borneol in blumea balsamifera borneol is required to be more than 85% at least by the pharmacopoeia of the 2015 version of the people's republic of China, but the existing extraction process is difficult to stably reach the standard requirement at present. The natural borneol obtained from borneol camphor requires 96% of dextroborneol, and is more difficult to meet by the traditional process, in the traditional preparation means, an industrial purification process is adopted, the borneol possibly has industrial additives or solvent residues, and the food and medicine level effect is difficult to achieve, so the extraction and refining process of the natural borneol is provided.

Disclosure of Invention

The invention provides an extraction and refining process of natural borneol, which aims to solve the problems of low purity, complex process, high extraction cost and the like of the purification process in the prior art, and has the advantages of simple process, large-scale production and low cost.

The invention is realized by the following technical scheme:

technical scheme one

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

cleaning and impurity removal are carried out to remove large-particle impurities in the raw materials;

2) putting the cleaned raw materials in the step 1) into a vacuum tank, and vacuumizing the vacuum tank to enable the vacuum tank to be in a vacuum state;

3) filling inert gas into the vacuum tank in the step 2), and controlling the pressure in the vacuum tank to be within the range of 0.005-0.02 MPa; the inert gas adopts nitrogen or carbon dioxide or argon;

4) controlling the temperature in the vacuum tank by a computer, keeping the temperature of the tank top in the vacuum tank at 50-90 ℃, controlling the pressure in the tank within 0.15MPa, and controlling the time to be 1-3 h;

5) cooling, maintaining the temperature at 40-50 deg.C, introducing air into the vacuum tank to reach normal pressure, opening the tank, and extracting to obtain the final product.

Further, the moisture content in the step 1) is controlled to be less than 1%.

Further, the temperature in the step 1) is controlled to be below 50 ℃.

Further, the dehydration drying is carried out in the step 1) by adopting methods such as a cold dryer, a vacuum dryer, a dehydrator, drying, natural drying and the like.

In the scheme, the purity of the levorotatory borneol (borneol) and the purity of the dextrorotatory borneol (borneol) can reach more than 95 percent, and finished products can be crushed according to actual conditions and are crushed into blocky products.

Technical scheme two

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

cleaning and impurity removal are carried out to remove large-particle impurities in the raw materials;

2) selecting 65-95% alcohol, and matching the alcohol with the cleaned raw materials in the step 1), wherein the optimal proportion is 1: 0.5-3, heating and dissolving the proportioned solution in water bath, wherein the temperature range is 80-100 ℃; the alcohol concentration is in direct proportion to the solubility and in inverse proportion to the yield, the preferred alcohol concentration is selected within the range of 65-95%, the yield is 60-80%, the alcohol concentration is lower than 65%, the final yield may be higher, but the absolute value may be lower; alcohol concentrations above 95% may have lower final yields but higher absolute values;

3) quickly filtering after dissolving, and standing to normal temperature;

4) cooling the normal-temperature solution obtained in the step 3);

5) crystallizing, crystallizing the product obtained in the step 4), and filtering again;

6) and (3) drying at low temperature, namely drying the product filtered in the step 5) at low temperature, and controlling the temperature to be below 50 ℃ to obtain a finished product.

Further, a filter of 1000 meshes to 10000 meshes or 0.3 micron is adopted for filtering in the step 3).

Further, the temperature reduction and cooling in the step 4) adopt a sectional type temperature reduction method, the optimal temperature is gradually adjusted from 0 ℃ to-40 ℃, and the time is 12-48 h.

Further, the temperature reduction and cooling in the step 4) adopt a constant temperature cooling method, the optimal temperature range is from-10 ℃ to-30 ℃, and the time is 24-48 h.

Further, a filter with 300 and 1000 meshes is adopted for filtering in the step 5).

The selection of the filter is selected according to actual requirements.

In the scheme, the purity of the levo-borneol (borneol) and the dextro-borneol (natural borneol) can reach more than 98 percent, and the finished product is a small tablet or a powdery product.

Technical scheme three

An extraction and refining process of natural borneol comprises the following steps: firstly, extracting according to the extraction and refining process of the natural borneol in the technical scheme I, and then further refining according to the extraction and refining process of the natural borneol in the technical scheme II after extraction, or repeatedly extracting by using the scheme II to obtain a product with higher purity.

In the scheme, the purity of the levo-borneol (borneol) and the dextro-borneol (natural borneol) can reach more than 99 percent, and the product can be crushed into powder and prepared into powder, solvent or medicament according to actual requirements.

Compared with the prior art, the invention has the following advantages and beneficial effects:

the invention has the advantages of high purification degree, simple process steps, convenient operation and low production cost, and the product can reach the medical standard by adopting a food-grade or pharmaceutical-grade industrial purification process.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.

Example one

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

2) putting the cleaned raw materials in the step 1) into a vacuum tank, and vacuumizing the vacuum tank to enable the vacuum tank to be in a vacuum state;

3) filling inert gas into the vacuum tank in the step 2), and controlling the pressure in the vacuum tank to be within the range of 0.005-0.01 MPa;

4) controlling the temperature in the vacuum tank by a computer, keeping the temperature of the tank top in the vacuum tank at 50-90 ℃, controlling the pressure in the tank within 0.1MPa, and controlling the time to be 1-2 h;

5) cooling, maintaining the temperature at 35-40 deg.C, introducing air into the vacuum tank to reach normal pressure, opening the tank, and extracting to obtain the final product.

Preferably, the water content in step 1) is controlled to 1%.

Preferably, the temperature in step 1) above is controlled at 50 ℃.

Preferably, the dehydration drying is performed in the step 1) by using a method such as a freeze dryer, a vacuum dryer, a dehydrator, drying, natural drying, and the like.

Example two

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

2) putting the cleaned raw materials in the step 1) into a vacuum tank, and vacuumizing the vacuum tank to enable the vacuum tank to be in a vacuum state;

3) filling inert gas into the vacuum tank in the step 2), and controlling the pressure in the vacuum tank to be within the range of 0.01-0.015 MPa;

4) controlling the temperature in the vacuum tank by a computer, keeping the temperature of the tank top in the vacuum tank at 50-90 ℃, controlling the pressure in the tank within 0.12MPa, and controlling the time to be 2-3 h;

5) cooling, maintaining the temperature at 40-50 deg.C, introducing air into the vacuum tank to reach normal pressure, opening the tank, and extracting to obtain the final product.

Preferably, the water content in step 1) is controlled to 1%.

Preferably, the temperature in step 1) above is controlled at 50 ℃.

Preferably, the dehydration drying is performed in the step 1) by using a method such as a freeze dryer, a vacuum dryer, a dehydrator, drying, natural drying, and the like.

EXAMPLE III

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

2) selecting 65% alcohol, and matching the alcohol with the cleaned raw materials in the step 1), wherein the proportion is 1: 0.5, heating and dissolving the solution after proportioning in water bath, wherein the temperature value range is 80-100 ℃, and the yield is 75-85%;

3) quickly filtering after dissolving, and standing to normal temperature;

4) cooling the normal-temperature solution obtained in the step 3);

5) crystallizing, crystallizing the product obtained in the step 4), and filtering again;

6) and (3) drying at low temperature, namely drying the product filtered in the step 5) at low temperature, and controlling the temperature to be 50 ℃ to obtain a finished product.

Preferably, the step 3) is performed by filtering with a filter of 1000 mesh to 10000 mesh or 0.3 micron.

Preferably, the temperature reduction and cooling in the step 4) adopt a constant temperature cooling method, the temperature is between 18 ℃ below zero and 20 ℃ below zero, and the time is 24 hours.

Preferably, the step 5) is performed by filtering with a filter of 300 and 1000 meshes.

Example four

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

2) selecting 75% alcohol, and proportioning the alcohol and the cleaned raw materials in the step 1), wherein the proportion is 1: 1.5, heating and dissolving the solution after proportioning in water bath, wherein the temperature value range is 80-100 ℃, and the yield is 70-80%;

3) quickly filtering after dissolving, and standing to normal temperature;

4) cooling the normal-temperature solution obtained in the step 3);

5) crystallizing, crystallizing the product obtained in the step 4), and filtering again;

6) and (3) drying at low temperature, namely drying the product filtered in the step 5) at low temperature, and controlling the temperature to be 50 ℃ to obtain a finished product.

Preferably, the step 3) is performed by filtering with a filter of 1000 mesh to 10000 mesh or 0.3 micron.

Preferably, the temperature reduction and cooling in the step 4) adopt a constant temperature cooling method, the temperature range is from-18 ℃ to-20 ℃, and the time is 24 hours.

Preferably, the step 5) is performed by filtering with a filter of 300 and 1000 meshes.

EXAMPLE five

An extraction and refining process of natural borneol comprises the following steps:

1) cleaning raw brain, dehydrating and drying;

2) selecting 95% alcohol, and matching the alcohol with the cleaned raw materials in the step 1), wherein the proportion is 1: 2, heating and dissolving the proportioned solution in water bath, wherein the temperature range is 80-100 ℃, and the yield is 60-70%;

3) quickly filtering after dissolving, and standing to normal temperature;

4) cooling the normal-temperature solution obtained in the step 3);

5) crystallizing, crystallizing the product obtained in the step 4), and filtering again;

6) and (3) drying at low temperature, namely drying the product filtered in the step 5) at low temperature, and controlling the temperature to be 50 ℃ to obtain a finished product.

Preferably, the step 3) is performed by filtering with a filter of 1000 mesh to 10000 mesh or 0.3 micron.

Preferably, the temperature reduction and cooling in the step 4) adopt a sectional type temperature reduction method, the temperature is gradually adjusted from 0 ℃ to-40 ℃, and the time is 24 hours.

Preferably, the step 5) is performed by filtering with a filter of 300 and 1000 meshes.

EXAMPLE six

An extraction and refining process of natural borneol comprises the following steps: firstly, extracting according to the extraction and refining process of the natural borneol in the first technical scheme, and then further refining according to the extraction and refining process of the natural borneol in the second technical scheme to obtain a product or repeatedly refining according to the second technical scheme to obtain a product with higher purity.

The above-mentioned embodiments, objects, technical solutions and advantages of the present invention are further described in detail, it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.