Preparation method and device of pharmaceutical grade turpentine

Abstract

The invention discloses a preparation method of pharmaceutical grade turpentine, and belongs to the technical field of traditional Chinese medicine material preparation, and the pharmaceutical grade turpentine with high purity and stable quality can be prepared by using the method so as to meet the safety and treatment effect requirements of products. Comprising the following steps: S1, feeding raw material turpentine into a tower kettle of a rectifying tower for preheating, and feeding vaporized turpentine into the rectifying tower; and S2, cooling the vaporized turpentine entering the rectifying tower, sequentially feeding the cooled vaporized turpentine into a rectifying oil cooler and a rectifying oil distribution tank, and leading out finished oil from the rectifying oil distribution tank to a finished product temporary storage tank for storage, thereby obtaining the pharmaceutical grade turpentine. The invention also discloses a device for preparing the pharmaceutical-grade turpentine.

Description

Technical Field

[0001] The present invention relates to the technical field of preparation of traditional Chinese medicine materials, and more specifically, to a method for preparing pharmaceutical-grade turpentine oil. The present invention also discloses a device for realizing the preparation method. Background Art

[0002] Turpentine is a natural resin extracted from pine trees and has a wide range of applications. These include industrial and medical uses. Pharmaceutical-grade turpentine is mainly used in the pharmaceutical and health care industries. In the pharmaceutical field, it is used to make medicines, ointments, oral liquids, etc. In the field of health care products, it is used as a natural essential oil in the fields of physical and mental health, beauty and skin care. Pharmaceutical-grade turpentine has a high degree of refining requirements and has the following characteristics: First, its composition and purity are relatively high, which can meet the high-demand pharmaceutical and health care product production needs; second, its smell and color are also purer and will not affect the product; finally, its price is relatively high, suitable for high-end market sales.

[0003] There are great differences between industrial turpentine and pharmaceutical turpentine in terms of use and quality standards. The choice of which turpentine depends on the specific application needs and quality requirements. There are corresponding national standards for the production and sales of industrial turpentine, among which the quality standards are mainly reflected in the refining system, impurity content, etc., while pharmaceutical turpentine also needs to meet the pharmacopoeia standards and undergo strict quality control and testing to ensure its purity and harmlessness. The source and properties of pharmaceutical turpentine are specifically required as follows: it is an oleoresin exuded from several plants of the genus Pinus in the Pinaceae family, and is a volatile oil obtained by distillation or extraction; it is a colorless to slightly yellow clear liquid; it has a specific odor; when stored for a long time or exposed to the air, the odor gradually increases and the color gradually turns yellow; it is flammable and produces thick smoke when burned. It is easily soluble in ethanol, can be mixed with chloroform, ether or glacial acetic acid at will, and is insoluble in water. The relative density should be 0.850-0.870. According to the distillation range determination method, the amount distilled at 154-165°C shall not be less than 90.0% (ml / ml). The refractive index should be 1.466-1.477. The current preparation method for producing pharmaceutical-grade turpentine oil generally only takes the oleoresin exuded from several plants of the genus Pinus in the Pinaceae family, and obtains volatile oil after distillation or extraction. The quality of the prepared pharmaceutical-grade turpentine oil is unstable, and it even contains heavy oil or other harmful components, which cannot meet the product safety requirements. Therefore, it is urgent to design a method for large-scale preparation of pharmaceutical-grade turpentine oil to solve the above problems. Summary of the invention

[0004] The purpose of the present invention is to provide a method for preparing pharmaceutical-grade turpentine oil, by which pharmaceutical-grade turpentine oil with high purity and stable quality can be prepared to meet the requirements of product safety and therapeutic effect.

[0005] Another object of the present invention is to provide a device for implementing the preparation method.

[0006] The first technical solution adopted by the present invention is as follows:

[0007] A method for preparing pharmaceutical grade turpentine oil comprises the following steps:

[0008] S1, take the raw material turpentine and send it to the bottom of the distillation tower for preheating, and the vaporized turpentine enters the distillation tower;

[0009] S2. The vaporized turpentine oil entering the distillation tower is sent to the distillation oil cooler and the distillation oil distribution tank in sequence after being cooled. The finished oil is drawn out from the distillation oil distribution tank and stored in the finished product temporary storage tank to obtain pharmaceutical grade turpentine oil.

[0010] Furthermore, in the step S1, the raw material turpentine oil selected is gum turpentine oil, and the temperature of the heating oil in the kettle of the distillation tower is 154-165°C.

[0011] Furthermore, in step S2, the liquid phase temperature of the material in the distillation tower is controlled to be less than or equal to 165°C.

[0012] Furthermore, the preparation process is carried out under vacuum or normal pressure, and the vacuum degree in the vacuum state is -0.1Mpa.

[0013] Another technical solution adopted by the present invention is as follows:

[0014] A preparation device for pharmaceutical-grade turpentine comprises a distillation tower, a tower top condenser, a distillation oil cooler, a distillation oil distribution tank and a gas-liquid separator, wherein the feed inlet of the distillation tower is connected to an external turpentine storage tank, the vaporization outlet of the distillation tower is connected to the feed inlet of the tower top condenser, the discharge port of the tower top condenser is connected to the feed inlet of the distillation oil cooler, the discharge port of the distillation oil cooler is connected to the feed inlet of the distillation oil distribution tank, the liquid outlet of the distillation oil distribution tank is connected to a finished oil temporary storage tank, the steam outlet of the distillation oil distribution tank is connected to the steam inlet of the gas-liquid separator, the steam outlet of the gas-liquid separator is connected to a tail gas recovery tank, the liquid outlet of the gas-liquid separator is connected to the liquid inlet of the distillation oil distribution tank, and the distillation tower and the gas-liquid separator are both connected to a vacuum pressure stabilizing tank.

[0015] Furthermore, a vapor-liquid distributor is provided at the outlet of the tower top condenser, one of the outlets of the vapor-liquid distributor is connected to the tower section of the distillation tower, and the other outlet of the vapor-liquid distributor is connected to the inlet of the distillation oil cooler.

[0016] Furthermore, a flow meter and a sampling port are provided on the liquid outlet of the vapor-liquid distributor connected to the distillation oil cooler, and a valve is provided on the flow meter.

[0017] Furthermore, the bottom liquid outlet of the distillation tower is connected to the residual oil storage tank.

[0018] Compared with the prior art, the present invention has the following beneficial effects:

[0019] 1. A method for preparing pharmaceutical-grade turpentine oil of the present invention comprises preheating and distilling the raw material turpentine oil respectively to achieve refining and purification of the raw material turpentine oil, thereby preparing pharmaceutical-grade turpentine oil with high purity and stable quality. The refined turpentine oil can remove heavy oil and other harmful components, and its property indicators meet the requirements of the "Pharmacopoeia of the People's Republic of China" to meet the safety and therapeutic effect requirements of the product.

[0020] 2. A preparation device for pharmaceutical-grade turpentine of the present invention preheats and rectifies the raw material turpentine by setting a distillation tower. After the preheated vaporized raw material turpentine enters the distillation tower, the vaporized material is separated and cooled into condensed liquid through a tower top condenser through vapor-liquid contact, and then flows back to the vapor-liquid distributor. A part of the condensed liquid refluxes to the distillation tower, and another part of the condensed liquid enters the distillation oil cooler. At the same time, the part that enters the tower top condenser in vapor phase and is not condensed also enters the distillation oil cooler for further cooling, and then enters the distillation oil distribution tank. The finished oil obtained from the distillation oil distribution tank is the pharmaceutical-grade turpentine. The tail gas discharged from the distillation oil distribution tank and a small amount of finished turpentine are further separated into gas and liquid by a gas-liquid separator, and the tail gas is recovered, and the finished oil obtained by condensation in the gas-liquid separator is sent back to the distillation oil distribution tank for unified recovery, so that the purification rate is higher and the effect is better. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of this application. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0022] Figure 1 It is a structural schematic diagram of a device for preparing medical-grade turpentine oil of the present invention.

[0023] Explanation of the reference numerals: 1. distillation tower; 2. top condenser; 3. distillation oil cooler; 4. distillation oil distribution tank; 5. gas-liquid separator; 6. gas-liquid distributor; 7. flow meter; 8. sampling port; 9. valve; 10. vacuum pressure stabilizing tank; 11. tail gas recovery tank; 12. residual oil storage tank; 13. finished oil temporary storage tank. DETAILED DESCRIPTION

[0024] The technical solution of the present invention is further described in detail below in conjunction with specific implementation methods, but does not constitute any limitation to the present invention.

[0025] A method for preparing pharmaceutical-grade turpentine oil of the present invention comprises the following steps:

[0026] S1, take raw material turpentine oil and send it to the bottom of distillation tower 1 for preheating, and the vaporized turpentine oil enters distillation tower 1.

[0027] Among them, the raw material turpentine oil selected is gum turpentine oil, and the temperature of the heating oil in the bottom of the distillation tower 1 is 154-165°C. According to the boiling point difference in the gum turpentine oil components, the temperature of the heating oil in the bottom of the distillation tower 1 is controlled within this temperature range to preheat the raw material turpentine oil, which is beneficial to control its vaporization within this temperature range to achieve the effect of purifying it.

[0028] S2, the vaporized turpentine oil entering the distillation tower 1 is sent to the distillation oil cooler 3 and the distillation oil distribution tank 4 in sequence after being cooled, and the finished oil is drawn out from the distillation oil distribution tank 4 and stored in the finished product temporary storage tank to obtain pharmaceutical grade turpentine oil.

[0029] Among them, the liquid phase temperature of the material in the distillation tower is controlled to be less than or equal to 165°C. By controlling the liquid phase of the material in the distillation tower to remain within this temperature range, the substances with boiling points below this temperature in the vaporized material are condensed, while the substances with boiling points above this temperature remain in a vaporized state, thereby achieving precise distillation of each substance.

[0030] Furthermore, the preparation process is carried out under vacuum with a vacuum degree of -0.1Mpa, and the refining and purification effect in vacuum state is good.

[0031] The invention discloses a method for preparing pharmaceutical-grade turpentine oil. The raw material turpentine oil is preheated and distilled respectively to achieve the refining and purification of the raw material turpentine oil, thereby preparing pharmaceutical-grade turpentine oil with high purity and stable quality. Compared with the traditional process for preparing pharmaceutical-grade turpentine oil, the preparation method of the invention refines the raw material turpentine oil to achieve higher purity, and can also remove heavy oil and other harmful components in the raw material turpentine oil. The property index of the obtained finished product turpentine oil is more in line with the provisions of the "Pharmacopoeia of the People's Republic of China", so as to meet the safety and therapeutic effect requirements of the product.

[0032] A preparation device for pharmaceutical-grade turpentine comprises a distillation tower 1, a tower top condenser 2, a distillation oil cooler 3, a distillation oil distribution tank 4 and a gas-liquid separator 5, wherein the feed inlet of the distillation tower 1 is connected to an external turpentine storage tank, the vaporization outlet of the distillation tower 1 is connected to the feed inlet of the tower top condenser 2, the discharge port of the tower top condenser 2 is connected to the feed inlet of the distillation oil cooler 3, the discharge port of the distillation oil cooler 3 is connected to the feed inlet of the distillation oil distribution tank 4, the liquid outlet of the distillation oil distribution tank 4 is connected to a finished oil temporary storage tank 13, the steam outlet of the distillation oil distribution tank 4 is connected to the steam inlet of the gas-liquid separator 5, the steam outlet of the gas-liquid separator 5 is connected to a tail gas recovery tank 11, the liquid outlet of the gas-liquid separator 5 is connected to the liquid inlet of the distillation oil distribution tank 4, and the distillation tower 1 and the gas-liquid separator 5 are both connected to a vacuum pressure stabilizing tank 10. The invention discloses a preparation device for pharmaceutical-grade turpentine oil. The raw material turpentine oil is sent from a raw material tank in a tank area to a bottom of a distillation tower 1 for preheating after being metered and regulated by a raw material pump and a flow meter. The amount of hot oil entering the bottom of the distillation tower 1 is regulated by a regulating valve on the distillation tower 1. After the raw material turpentine oil is preheated to an operating temperature, vaporization is started to realize fractionation. The vaporized material steam enters the distillation tower 1 for rectification. The vaporized material after rectification enters a distillation oil cooler 3. The circulating water in the distillation oil cooler 3 is temperature-controlled by a regulating valve to realize condensation of the vaporized material. The pharmaceutical-grade turpentine oil is obtained and enters a distillation oil distribution tank 4. The condensed tail gas also enters the distillation oil distribution tank 4 at the same time. The tail gas discharged from the distillation oil distribution tank 4 and a small amount of finished turpentine oil are further separated into gas and liquid by a gas-liquid separator 5. The tail gas is then recovered. The finished turpentine oil obtained by condensation in the gas-liquid separator is returned to the distillation oil distribution tank for unified recovery. The purification rate is higher and the effect is better.

[0033] Furthermore, the (inlet) and outlet ports of the tower top condenser 2 are provided with a vapor-liquid distributor 6, one of the liquid outlets of the vapor-liquid distributor 6 is connected to the tower section of the distillation tower 1, and the other liquid outlet of the vapor-liquid distributor 6 is connected to the inlet port of the distillation oil cooler 3. The vapor-liquid distributor 6 is used to divert the condensed liquid in the tower top condenser 2 according to actual needs, a part of the condensed liquid flows back to the distillation tower 1, and the other part of the condensed liquid enters the refined oil cooler 3 for further cooling to obtain finished oil.

[0034] Furthermore, a flow meter 7 and a sampling port 8 are provided on the liquid outlet of the vapor-liquid distributor 6 connected to the distillation oil cooler 3. A valve 9 is provided on the flow meter 7. The sample of the condensed liquid obtained from the vapor-liquid distributor 6 can be obtained from the sampling port 8 through the sampling port 8, which is convenient for testing the distillation sample. The valve 9 on the flow meter 7 can be used to adjust the flow of the condensed liquid flowing to the refined oil cooler 3 according to the quality of the condensed liquid. If the quality of the condensed liquid is good, the valve 9 is adjusted to increase the flow to the distillation oil cooler 3, otherwise the valve 9 is adjusted to decrease the flow to the distillation oil cooler 3.

[0035] Furthermore, the liquid outlet of the distillation tower 1 is connected to the residual oil storage tank 12 to facilitate the discharge of the remaining oil after distillation from the distillation tower 1.

[0036] The invention discloses a preparation device for pharmaceutical-grade turpentine. The device preheats and rectifies raw material turpentine by setting a rectifying tower 1. After the preheated vaporized raw material turpentine enters the rectifying tower 1, the vaporized material is cooled into condensed liquid through a tower top condenser 2 through vapor-liquid contact, and then flows back to a vapor-liquid distributor 6. A part of the condensed liquid flows back to the rectifying tower 1, and another part of the condensed liquid enters a rectified oil cooler 3. Meanwhile, the uncondensed part that enters the tower top condenser 2 in vapor phase also enters the rectified oil cooler 3 for further cooling, and then enters a rectified oil distribution tank 4. The finished oil obtained by the rectified oil distribution tank 4 is the pharmaceutical-grade turpentine. The tail gas discharged from the rectified oil distribution tank 4 and a small amount of finished turpentine are further separated into gas and liquid by a gas-liquid separator 5. The tail gas is then recovered, and the finished oil obtained by condensation in the gas-liquid separator 5 is sent back to the rectified oil distribution tank 4 for unified recovery, so that the purification rate is higher and the effect is better.

[0037] The above description is only a preferred embodiment of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing pharmaceutical grade turpentine, characterized in that: The following steps are involved: S1, taking raw material turpentine oil and sending it to the bottom of the distillation tower (1) for preheating, and the vaporized turpentine oil enters the distillation tower (1); S2, the vaporized turpentine oil entering the distillation tower (1) is sent to the distillation oil cooler (3) and the distillation oil distribution tank (4) in sequence after being cooled, and the finished oil is drawn out from the distillation oil distribution tank (4) and stored in the finished product temporary storage tank to obtain pharmaceutical grade turpentine oil.

2. The method for preparing pharmaceutical grade turpentine according to claim 1, characterized in that: In the step S1, the raw material turpentine oil selected is gum turpentine oil, and the temperature of the heating oil in the kettle of the distillation tower (1) is 154-165°C.

3. A method for preparing pharmaceutical grade turpentine according to claim 1 or 2, characterized in that: In the step S2, the liquid phase temperature of the material in the distillation tower (1) is controlled to be less than or equal to 165°C.

4. The method for preparing pharmaceutical grade turpentine according to claim 1, characterized in that: The preparation process is carried out under vacuum, and the vacuum degree is -0.1Mpa.

5. A device for implementing the method for preparing pharmaceutical-grade turpentine oil according to claim 1, characterized in that: The invention comprises a distillation tower (1), a tower top condenser (2), a distillation oil cooler (3), a distillation oil distribution tank (4) and a gas-liquid separator (5), wherein the feed inlet of the distillation tower (1) is connected to an external turpentine oil storage tank, the vaporization outlet of the distillation tower (1) is connected to the feed inlet of the tower top condenser (2), the discharge outlet of the tower top condenser (2) is connected to the feed inlet of the distillation oil cooler (3), the discharge outlet of the distillation oil cooler (3) is connected to the discharge outlet of the distillation oil distribution tank (4), and the discharge outlet of the distillation oil cooler (3) is connected to the discharge outlet of the distillation oil distribution tank (4). The feed inlet is connected, the liquid outlet of the rectified oil distribution tank (4) is connected to the finished oil temporary storage tank (13), the steam outlet of the rectified oil distribution tank (4) is connected to the steam inlet of the gas-liquid separator (5), the steam outlet of the gas-liquid separator (5) is connected to the tail gas recovery tank (11), the liquid outlet of the gas-liquid separator (5) is connected to the liquid inlet of the rectified oil distribution tank (4), and the distillation tower (1) and the gas-liquid separator (5) are both connected to a vacuum pressure stabilizing tank (10).

6. The device for preparing pharmaceutical-grade turpentine according to claim 5, characterized in that: The outlet of the tower top condenser (2) is provided with a vapor-liquid distributor (6), one of the outlets of the vapor-liquid distributor (6) is connected to a tower section of the distillation tower (1), and the other outlet of the vapor-liquid distributor (6) is connected to an inlet of a distillation oil cooler (3).

7. The device for preparing pharmaceutical-grade turpentine according to claim 6, characterized in that: A flow meter (7) and a sampling port (8) are provided on the liquid outlet of the vapor-liquid distributor (6) connected to the distillation oil cooler (3), and a valve (9) is provided on the flow meter (7).

8. The device for preparing pharmaceutical-grade turpentine according to claim 5, characterized in that: The liquid outlet of the bottom of the distillation tower (1) is connected to the residual oil storage tank (12).

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