A sublimed sulfur drug substance and a method of preparing the same

Abstract

The application provides a sublimed sulfur raw material medicine and a preparation method thereof, and belongs to the technical field of chemical medicines, and comprises the following steps: S1, industrial sulfur is added into a sublimation instrument, a vacuum is started, and then the temperature is gradually increased to 160-180 DEG C, the sulfur is heated and sublimated by controlling different temperatures in different temperature zones; S2, after the sublimation is completed, the furnace cavity is opened, and the sublimed sulfur solid material is collected, and the sublimed sulfur solid material is obtained.The sublimed sulfur solid material is prepared by the simple sublimation method, the preparation method is simple, the prepared product is high in purity and good in quality.

Description

Technical Field

[0001] This invention relates to the field of chemical pharmaceutical technology, specifically to a sublimed sulfur raw material and its preparation method. Background Technology

[0002] Sulfur vaporizes into a gas at high temperatures, a process known as sublimation. If the vaporized sulfur is carried away before it can burn, it cannot continue to burn below its ignition temperature (approximately 250°C) and will re-condense into a solid upon cooling. This solid, containing at least 98.0% sulfur (S), is called sublimed sulfur. Sublimed sulfur is a yellow crystalline powder with a slight odor and is practically insoluble in water or ethanol.

[0003] Insoluble sublimed sulfur presents numerous problems, including poor dispersibility, high cost, poor high-temperature stability, and the use of large amounts of highly volatile organic solvents in the extraction process, which restricts the development of insoluble sublimed sulfur. Summary of the Invention

[0004] The purpose of this invention is to provide a sublimed sulfur raw material and its preparation method. After ball milling, the sublimed sulfur raw material is dispersed in edible oil and then encapsulated with sodium alginate to obtain microcapsule-type sublimed sulfur raw material. This solves the problem of easy agglomeration of sublimed sulfur. The obtained sublimed sulfur raw material has good dispersibility, good high temperature resistance, and the preparation method is simple and low in cost, and has broad application prospects.

[0005] The technical solution of this invention is implemented as follows:

[0006] This invention provides a method for preparing sublimed sulfur raw material, comprising the following steps:

[0007] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 160-180℃, controlling different temperatures in different temperature zones to sublimate the sulfur.

[0008] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material.

[0009] As a further improvement of the present invention, the temperature is raised to 170°C.

[0010] As a further improvement of the present invention, step S3 is also included: encapsulating the sublimed sulfur solid material obtained in step S2 in microcapsules.

[0011] As a further improvement of the present invention, step S3 specifically includes the following steps: ball milling the sublimed sulfur solid material and dispersing it in edible oil to obtain an oil phase; dissolving sodium alginate in water and adding an emulsifier to obtain an aqueous phase; adding the oil phase to the aqueous phase, emulsifying, adding a metal ion solution dropwise, solidifying at room temperature, filtering, washing, and drying to obtain sublimed sulfur microcapsules.

[0012] As a further improvement of the present invention, the emulsifier is selected from at least one of sodium dodecylbenzenesulfonate, sodium dodecyl sulfonate, sodium dodecyl sulfate, sodium tetradecyl sulfide, sodium tetradecyl sulfonate, sodium tetradecylbenzenesulfonate, sodium hexadecylbenzenesulfonate, sodium hexadecyl sulfonate, sodium hexadecyl sulfate, sodium octadecyl sulfonate, sodium octadecylbenzenesulfonate, and sodium octadecyl sulfate.

[0013] As a further improvement of the present invention, the edible oil is selected from at least one of peanut oil, rapeseed oil, corn oil, soybean oil, sunflower seed oil, flaxseed oil, and olive oil.

[0014] As a further improvement of the present invention, the mass ratio of the sublimed sulfur solid material to the edible oil is 7-12:50; the mass ratio of sodium alginate, water, and emulsifier is 22-25:100:1-2.

[0015] As a further improvement of the present invention, the mass ratio of the oil phase, aqueous phase, and metal ion solution is 30-50:70-90:12-15; the metal ion solution is a 3-5 wt% calcium chloride or aluminum chloride solution; the ball milling time is 2-4 hours; the room temperature curing time is 30-50 minutes; and the emulsification speed is 12000-15000 r / min for 3-5 minutes.

[0016] As a further improvement to the present invention, the specific steps include:

[0017] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 160-180℃, controlling different temperatures in different temperature zones to sublimate the sulfur.

[0018] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material;

[0019] S3. After ball milling 7-12 parts by weight of sublimed sulfur solid material for 2-4 hours, disperse it in 50 parts by weight of edible oil to obtain an oil phase; dissolve 22-25 parts by weight of sodium alginate in 100 parts by weight of water, add 1-2 parts by weight of emulsifier to obtain an aqueous phase; add 30-50 parts by weight of the oil phase to 70-90 parts by weight of the aqueous phase, emulsify at 12000-15000 r / min for 3-5 min, add 12-15 parts by weight of 3-5 wt% calcium chloride or aluminum chloride solution, solidify at room temperature for 30-50 min, filter, wash, and dry to obtain sublimed sulfur raw material.

[0020] This invention further protects a sublimed sulfur raw material prepared by the above-described preparation method.

[0021] The present invention has the following beneficial effects: The present invention prepares sublimated sulfur solid material through a simple sublimation method. The preparation method is simple and the product obtained has high purity and good quality.

[0022] Furthermore, this invention disperses the obtained sublimed sulfur solid material in edible oil after ball milling, and then encapsulates it with sodium alginate to obtain microcapsule-type sublimed sulfur raw material. This solves the problem of easy agglomeration of sublimed sulfur. The obtained sublimed sulfur raw material has good dispersibility, good high temperature resistance, and the preparation method is simple and low in cost, with broad application prospects. Attached Figure Description

[0023] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0024] Figure 1 This is a SEM image of the sublimed sulfur raw material prepared in Example 4. Implementation

[0025] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example

[0026] This embodiment provides a method for preparing sublimed sulfur raw material, including the following steps:

[0027] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 170°C. Control different temperatures in different temperature zones to sublimate the sulfur.

[0028] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material. Example

[0029] This embodiment provides a method for preparing sublimed sulfur raw material, including the following steps:

[0030] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 160°C, controlling different temperatures in different temperature zones to sublimate the sulfur.

[0031] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material;

[0032] S3. After ball milling 7 parts by weight of sublimed sulfur solid material for 2 hours, disperse it in 50 parts by weight of corn oil to obtain an oil phase; dissolve 22 parts by weight of sodium alginate in 100 parts by weight of water, add 1 part by weight of sodium dodecylbenzenesulfonate to obtain an aqueous phase; add 30 parts by weight of the oil phase to 70 parts by weight of the aqueous phase, emulsify at 12000 r / min for 3 min, add 12 parts by weight of 3wt% calcium chloride solution, solidify at room temperature for 30 min, filter, wash, and dry to obtain sublimed sulfur raw material. Example

[0033] This embodiment provides a method for preparing sublimed sulfur raw material, including the following steps:

[0034] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 180°C, controlling different temperatures in different temperature zones to sublimate the sulfur.

[0035] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material;

[0036] S3. After ball milling 12 parts by weight of sublimed sulfur solid material for 4 hours, disperse it in 50 parts by weight of sunflower seed oil to obtain an oil phase; dissolve 25 parts by weight of sodium alginate in 100 parts by weight of water, add 2 parts by weight of sodium octadecyl sulfonate to obtain an aqueous phase; add 50 parts by weight of the oil phase to 90 parts by weight of the aqueous phase, emulsify at 15000 r / min for 5 min, add 15 parts by weight of 5 wt% aluminum chloride solution, solidify at room temperature for 50 min, filter, wash, and dry to obtain sublimed sulfur raw material. Example

[0037] This embodiment provides a method for preparing sublimed sulfur raw material, including the following steps:

[0038] S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 170°C. Control different temperatures in different temperature zones to sublimate the sulfur.

[0039] S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material;

[0040] S3. After ball milling 10 parts by weight of sublimed sulfur solid material for 3 hours, disperse it in 50 parts by weight of rapeseed oil to obtain an oil phase; dissolve 23.5 parts by weight of sodium alginate in 100 parts by weight of water, add 1.5 parts by weight of sodium tetradecylbenzenesulfonate to obtain an aqueous phase; add 40 parts by weight of the oil phase to 80 parts by weight of the aqueous phase, emulsify at 13500 r / min for 4 min, add 13.5 parts by weight of 4 wt% calcium chloride solution dropwise, solidify at room temperature for 40 min, filter, wash, and dry to obtain sublimed sulfur raw material. Figure 1The image shows a SEM image of the sublimed sulfur raw material. As can be seen from the image, the particle size of the sublimed sulfur raw material is between 0.5 and 2 micrometers.

[0041] Test Example 1

[0042] The sublimed sulfur raw materials prepared in Examples 2-4 of this invention were subjected to encapsulation rate tests, and the results are shown in Table 1.

[0043] Table 1

[0044]

[0045] As shown in the table above, the sublimed sulfur raw materials prepared in Examples 2-4 of this invention have a high encapsulation rate, which solves the problem of easy agglomeration of sublimed sulfur. The sublimed sulfur raw materials prepared have good dispersibility, good high temperature resistance, and the preparation method is simple and low in cost, and has broad application prospects.

[0046] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A method for preparing a sublimed sulfur raw material, characterized in that, Includes the following steps: S1. Add industrial-grade sulfur to the sublimation apparatus, turn on the vacuum, and then gradually raise the temperature to 160-180℃, controlling different temperatures in different temperature zones to sublimate the sulfur. S2. After sublimation is complete, open the furnace chamber and collect the sublimated sulfur solid material; S3. After ball milling 7-12 parts by weight of sublimed sulfur solid material for 2-4 hours, disperse it in 50 parts by weight of edible oil to obtain an oil phase; dissolve 22-25 parts by weight of sodium alginate in 100 parts by weight of water, add 1-2 parts by weight of emulsifier to obtain an aqueous phase; add 30-50 parts by weight of the oil phase to 70-90 parts by weight of the aqueous phase, emulsify at 12000-15000 r / min for 3-5 min, add 12-15 parts by weight of 3-5 wt% calcium chloride or aluminum chloride solution, solidify at room temperature for 30-50 min, filter, wash, and dry to obtain sublimed sulfur raw material.

2. The preparation method according to claim 1, characterized in that, The temperature is raised to 170°C.

3. The preparation method according to claim 1, characterized in that, The emulsifier is selected from at least one of sodium dodecylbenzenesulfonate, sodium dodecyl sulfonate, sodium dodecyl sulfate, sodium tetradecyl sulfide, sodium tetradecyl sulfonate, sodium tetradecylbenzenesulfonate, sodium hexadecylbenzenesulfonate, sodium hexadecyl sulfonate, sodium hexadecyl sulfate, sodium octadecyl sulfonate, sodium octadecylbenzenesulfonate, and sodium octadecyl sulfate.

4. The preparation method according to claim 1, characterized in that, The edible oil is selected from at least one of peanut oil, rapeseed oil, corn oil, soybean oil, sunflower seed oil, flaxseed oil, and olive oil.

5. A sublimed sulfur raw material prepared by the preparation method according to any one of claims 1-4.

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