Production process of water-fried realgar powder

Abstract

The invention discloses a production process of water-flying realgar powder. The production process comprises the following steps: selecting materials, cleaning with purified water, coarsely crushing, adding water and grinding, flying with water, dehydrating, dehumidifying and drying at low temperature under the protection of nitrogen, carrying out dry heat sterilization at 75 DEG C under the protection of nitrogen, grinding, sieving, totally mixing, packaging in vacuum, and warehousing a finished product. According to the realgar powder prepared by the production process disclosed by the invention, the total amount of trivalent arsenic and pentavalent arsenic which are toxic components is less than or equal to 1.0% in terms of arsenic (AS) and is far lower than 7.0% of a legal standard, and the cholate-resistant gram-negative bacteria is less than or equal to 102cfu / g and is lower than or equal to 104cfu / g of the legal standard; the effective component is greater than or equal to 95.0% in terms of arsenic disulfide (AS2S2), and is greater than or equal to 90.0% in terms of a legal standard.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine processing, and particularly relates to a production process of water-flying realgar powder. Background Art

[0002] In the traditional water-flying method, extremely fine powder of realgar is obtained through repeated grinding and static separation, which has problems such as low efficiency, long time consumption, high residue of toxic components (arsenic trioxide), and poor powder particle size uniformity. For example, the traditional process requires multiple grindings and static separations, with a production cycle of up to several days, and the content of disulfide diarsenic (active ingredient) only reaches more than 90%, and the content of arsenic trioxide is close to the pharmacopoeia limit of 7%.

[0003] For example, the invention patent with the patent number 2010101687111 discloses a method and device for preparing realgar powder. The method is as follows: injecting the realgar slurry obtained after grinding into a cylindrical container for continuous suspension sedimentation separation, and the injection direction is non-coplanar with the axis of the cylindrical container. The present invention utilizes the impact force of fluid injection to make the ground realgar slurry flow in a vortex state in the cylindrical container. The fine realgar particles in the realgar slurry form a realgar suspension on the upper layer of water under the action of the vortex flow, while the coarse realgar particles sink and concentrate at the center of the vortex under the action of the vortex flow. With the continuous injection of the realgar slurry, the realgar suspension on the upper layer of water continuously overflows into the centrifugal separation process, and the coarse realgar particles sinking at the center of the lower layer of water flow out under the action of gravity and return to the grinding process, realizing the continuity of realgar powder production, avoiding some unnecessary cumbersome steps, and greatly improving the production efficiency.

[0004] However, it does not solve the problems of long time consumption, high residue of toxic components (arsenic trioxide), and poor particle uniformity. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a production process of water-flying realgar powder to solve the problems raised in the background art.

[0006] To solve the above technical problems, the technical solution of the present invention is: a production process of water-flying realgar powder, including the following steps:

[0007] S1. Material selection: Select realgar medicinal materials;

[0008] S2. Cleaning with purified water: Put the realgar medicinal materials into a medicine-washing machine and spray them with purified water;

[0009] S3. Coarse crushing: After the spraying and washing are completed, put the realgar medicinal materials into a collision crusher for crushing and then into a disk mill for coarse crushing to obtain the coarsest realgar powder;

[0010] S4. Grinding with water: Put the coarsest realgar powder into a grinder and grind it with purified water, and put the ground slurry into a receiving cart to obtain realgar slurry;

[0011] S5. Levigation: Pump the realgar slurry into the levigation bucket, continuously add purified water into the levigation bucket for stirring and levigation, and pour out the realgar suspension;

[0012] S6. Dewatering: Pump the realgar suspension into a plate and frame filter press for dewatering to obtain realgar filter cake;

[0013] S7. Low-temperature dehumidifying drying under nitrogen protection: Take out the realgar filter cake, put it into a baking tray, place it on a baking rack, transfer it into a drying room and carry out low-temperature dehumidifying drying at a temperature below 25°C. At the same time, fill nitrogen until the volume of nitrogen reaches 6 times the total volume of the drying room, then close the nitrogen valve until the drying is completed;

[0014] S8. Dry heat sterilization at 75°C under nitrogen protection: After the low-temperature dehumidifying drying is completed, transfer it to a hot air circulation drying oven, fill nitrogen with a concentration of 99.9%. When the volume of the filled nitrogen is equivalent to 8 times the volume of the hot air circulation drying oven, adjust the nitrogen flow rate to 30 L / min, start heating, set the temperature to 75°C. After the temperature in the oven reaches the set temperature, start timing. The dry heat sterilization time is 36 hours. Nitrogen is filled throughout the dry heat sterilization process until the heating of the dry heat sterilization stops and the temperature drops to room temperature before the nitrogen valve can be closed.

[0015] S9. Pulverization: Take out the dried realgar filter cake and put it into a disk mill for pulverization to obtain realgar powder;

[0016] S10. Sieving: Place the pulverized realgar powder on an ultrasonic vibrating sieve and sieve it through a 250-mesh sieve;

[0017] S11. Total mixing: Put the sieved realgar powder into a mixer for mixing;

[0018] S12. Package the finished product and store it in the warehouse.

[0019] The specific steps of the step S2 are as follows: Use a medicinal herb washer to spray and wash online with purified water. The receiving vehicle at the discharge port is equipped with a filter plate to collect the washed realgar medicinal materials.

[0020] The specific steps of the step S4 are as follows: In a ball mill, put 200 kg of the coarsest realgar powder and 150 L of purified water, set the time to 2 h, set the rotation speed to 30 r / min, keep the rotation speed until the grinding is completed. After discharging the ground slurry, add purified water for washing three times, 150 L each time. After starting the equipment for 3 min each time, discharge the washing liquid and merge it into the receiving vehicle, and then a grinding operation is completed;

[0021] The suspension in the step S6 is pumped into a plate and frame filter press for dewatering. The filter cloth is made of polypropylene 750a with a mesh number of 1000, and the filter cake is taken out.

[0022] The specific steps of step S7 are as follows: Place the filter cake on the baking tray, place it on the baking cart frame, and move it into the drying room. After the baking carts loaded with realgar filter cake in the drying room reach the maximum allowable loading quantity of the drying room, close the drying room door and lock it with a double lock. Open the nitrogen valve, fill the drying room with nitrogen, record the initial reading of the nitrogen flowmeter. When the inflow volume of nitrogen reaches 6 times the volume of the drying room, close the nitrogen valve until the drying is completed.

[0023] The specific steps of step S8 are as follows: After the low-temperature dehumidification drying is completed, transfer it to a hot air circulation drying oven, fill it with nitrogen with a concentration of 99.9%. When the volume of the filled nitrogen is equivalent to 8 times the volume of the hot air circulation drying oven, adjust the nitrogen flow rate to 30 L / min, start heating, set the temperature to 75 °C. Start timing after the temperature in the oven reaches the set temperature. The dry heat sterilization time is 36 hours. Nitrogen is filled throughout the dry heat sterilization process until the heating of the dry heat sterilization stops and the temperature drops to room temperature before the nitrogen valve can be closed.

[0024] Step S10 includes: All realgar powder passes through a 250-mesh sieve to ensure that the realgar powder after sieving can meet the quality requirements of extremely fine powder during particle size detection (the quantity of realgar powder passing through a 150-mesh sieve and a 200-mesh sieve ≥ 95.0%).

[0025] The mixing time in step S11 is 30 min and the batch size is 1200 kg.

[0026] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0027] The total amount of its toxic components, trivalent arsenic and pentavalent arsenic, calculated as arsenic (A S ) is ≤ 1.0%, far lower than the legal standard of 7.0%. The bile salt-resistant Gram-negative bacteria are ≤ 10 2 cfu / g, lower than the legal standard of ≤ 10 4 cfu / g; the active ingredient, calculated as diarsenic disulfide (A S2 S2), is ≥ 95.0%, higher than the legal standard of ≥ 90.0%. Specific embodiments

[0028] The specific embodiments of the present invention will be further described below. It should be noted here that the description of these embodiments is for helping to understand the present invention, but does not constitute a limitation to the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0029] The present invention discloses a production process of levigated realgar powder, including the following steps:

[0030] S1. Select realgar medicinal materials;

[0031] S2. Purified water cleaning: Transfer the realgar placed in the turnover container into the medicinal herb washing room. Start the rotating drum of the medicinal herb washing machine and the purified water spraying pump. After the rotation speed is stable and the purified water spraying flow is stable, add the realgar to be cleaned into the feeding port of the medicinal herb washing machine. Place a receiving cart with a filter plate at the discharging port. Shovel the washed realgar collected on the filter plate of the receiving cart into the turnover vehicle for standby.

[0032] S3. Coarse crushing: Take the above-mentioned washed and water-filtered realgar, first crush it into pieces with a crusher, and then crush it into the finest powder with a disk mill for standby.

[0033] S4. Grinding with water: Take 200 kg of the coarsest powder of the above-mentioned realgar, add it into the cylinder of the ball mill, add 150 L of purified water, cover the sealing cover, set the vibration grinding time to 120 minutes, close the exhaust valve on the side wall of the cylinder, place the safety fence in front of the ball mill so that the front of the ball mill is completely surrounded by the fence, start the ball mill, set the rotation speed of the ball mill to 30 revolutions per minute, stop grinding after the grinding time reaches 120 minutes. After the machine stops rotating, press the manual button to rotate the ball mill so that the air release valve on its side is in the upper position, open the air release valve, release the gas generated by grinding heat in the cylinder, and then close the air release valve; press the manual button, adjust the sealing cover to the upper position, then loosen the fastening bolts of the sealing cover, remove the sealing cover and place it in a basin filled with purified water, replace it with a sealing cover with filter holes and a discharging ball valve, and tighten the bolts. Press the manual button, rotate the cylinder so that the discharging valve is downward within the range of the receiving cart, open the discharging ball valve and the air release valve, release the ground realgar grinding liquid, and then wash it with water three times, 150 L each time. Release the washing liquid into the receiving cart 3 minutes after starting the equipment each time, and thus complete one grinding operation.

[0034] S5. Levigation: Pump the grinding liquid in the receiving cart into the levigation bucket, continuously add purified water to the levigation bucket for stirring and levigation. When the liquid level reaches the position of the overflow pipe, the suspension flows out from the overflow pipe. Continuously add purified water for stirring and levigation to obtain the levigated realgar suspension.

[0035] S6. Dewatering: Pump the levigated suspension flowing out from the overflow pipe into a plate and frame filter press for dewatering. The filter cloth used for dewatering is made of polypropylene 750ab with a mesh number of about 1000 meshes.

[0036] S7. Low-temperature dehumidifying drying under nitrogen protection:

[0037] Low-temperature dehumidifying drying under nitrogen protection: Place the above-mentioned dewatered realgar filter cake on the drying cart, hang the identification plate, push it into the airing room, seal it, start the dehumidifier, set the temperature to 23 °C, open the nitrogen valve to fill nitrogen until the volume of the drying room is 6 times, and then close the nitrogen valve until the drying is completed.

[0038] S8. Dry heat sterilization at 75°C under nitrogen protection: After the low-temperature dehumidification drying is completed, transfer it to a hot air circulation drying oven, fill it with nitrogen with a concentration of 99.9%. When the volume of the filled nitrogen is equivalent to 8 times the volume of the hot air circulation drying oven, adjust the nitrogen flow rate to 30 L / min, start heating, set the temperature to 75°C, start timing after the temperature in the oven reaches the set temperature, and the dry heat sterilization time is 36 hours. During the dry heat sterilization process, nitrogen is filled throughout until the dry heat sterilization stops heating and the temperature drops to room temperature before the nitrogen valve can be closed.

[0039] S9. Pulverization: Collect the above-mentioned dried realgar filter cake and pulverize it with a disk mill.

[0040] S10. Sieving: Take the pulverized realgar powder above and sieve it with a 250-mesh ultrasonic vibrating sieve.

[0041] S11. Total mixing: Collect 1200 kg of realgar powder that has passed through a 250-mesh sieve, place it in a trough-shaped mixer, and mix for 30 minutes to obtain the realgar powder to be packaged.

[0042] S12. Package the finished product and store it in the warehouse.

[0043] After sampling the finished product, the Production Department issues the "Batch Packaging Instruction Sheet" and then the inner packaging of the finished product can be carried out.

[0044] Collect the qualified PE bags inspected from the warehouse according to the batch packaging instruction, place them in the packaging material temporary storage room, stack them neatly, and make good marks.

[0045] The realgar powder prepared by the invention of the present invention is inspected and the following table is obtained:

[0046]

[0047]

[0048] As can be seen from the above table, for the realgar powder prepared by the process of the present invention, the total amount of the toxic components trivalent arsenic and pentavalent arsenic, calculated as arsenic (A S ) is ≤ 1.0%, far lower than the legal standard of 7.0%, and the bile salt-tolerant Gram-negative bacteria are ≤ 10 2 cfu / g, lower than the legal standard of ≤ 10 4 cfu / g; the active ingredient, calculated as disulfide diarsenic (A S2 S2), is ≥ 95.0%, higher than the legal standard of ≥ 90.0%.

[0049] The above has described the embodiments of the present invention in detail, but the present invention is not limited to the described embodiments. For those skilled in the art, without departing from the principles and spirit of the present invention, various changes, modifications, substitutions, and variations made to these embodiments still fall within the protection scope of the present invention.

Claims

1. A production process of realgar powder by levigation, characterized in that, The following steps are involved: S1. Material selection: Select realgar medicinal material; S2, purified water washing: put the realgar medicinal material into the medicine washing machine and add purified water to spray and wash; S3, coarse crushing: after the spray washing, the realgar medicinal material is sequentially placed in a crusher for crushing and a grinding disc grinder for coarse crushing to obtain the coarsest realgar powder; S4, grinding with water: put the coarsest realgar powder into a grinder, add purified water and grind it, and put the ground slurry into a receiving vehicle to obtain realgar slurry; S5, water fly: pump the realgar slurry into the water fly bucket, continuously add purified water into the water fly bucket to stir and water fly, and pour out the realgar suspension; S6, dehydration: pumping the realgar suspension into a plate and frame filter press for dehydration to obtain a realgar filter cake; S7, low-temperature dehumidification and drying under nitrogen protection: take out the realgar filter cake and place it on a drying tray, place it on a drying rack, move it into the drying room, start the dehumidifier, set the temperature to 23°C, and ensure low-temperature dehumidification and drying below 25°C; at the same time, fill the nitrogen volume to 6 times the total volume of the drying room, and then close the nitrogen valve until the drying is completed; S8. Dry heat sterilization at 75°C under nitrogen protection: After the low-temperature dehumidification and drying is completed, transfer it to a hot air circulation drying oven and fill it with nitrogen with a concentration of 99.9%. When the volume of nitrogen filled is equivalent to 8 times the volume of the hot air circulation drying oven, adjust the nitrogen flow rate to 30L / min, start heating, set the temperature to 75°C, and start counting after the temperature in the oven reaches the set temperature. The dry heat sterilization time is 36 hours. During the dry heat sterilization process, nitrogen is filled throughout the process until the dry heat sterilization stops heating and the temperature drops to room temperature before the nitrogen valve can be closed. S9, grinding: taking out the dried realgar filter cake and putting it into a disc grinder to grind it to obtain realgar powder; S10, sieving: placing the ground realgar powder in an ultrasonic vibration sieve and passing it through a 250-mesh sieve; S11, total mixing: putting the sieved realgar powder into a mixer and mixing; S12. Finished products are packaged and put into storage.

2. The production process of the realgar powder by water separation according to claim 1, characterized in that, The specific steps of step S2 are: using a medicine washing machine to add purified water for online rolling spray washing, and the material receiving vehicle at the discharge port is provided with a filter plate to collect the washed realgar medicine.

3. The production process of the realgar powder by water separation according to claim 1, characterized in that, The specific steps of step S4 are as follows: put 200 kg of the coarsest realgar powder and 150 L of purified water into the ball mill, set the timer for 2 hours, and set the speed at 30 r / min. Maintain the speed until the grinding is completed. After releasing the ground slurry, add purified water for washing three times, 150 L each time. After starting the equipment for 3 minutes each time, release the washing liquid and put it into the receiving car to complete one grinding operation.

4. The production process of realgar powder by levigation according to claim 1, characterized in that: The suspension in step S6 is pumped into a plate-and-frame filter press for dehydration. The filter bag is made of polypropylene 750a with a mesh size of 1000 mesh, and the filter cake is taken out.

5. The production process of realgar powder by levigation according to claim 1, characterized in that, The specific steps of step S7 are: the filter cake is placed on a drying tray, placed on a drying cart frame, and moved into a drying room. When the number of drying carts loaded with realgar filter cakes in the drying room reaches the maximum allowable loading number of the drying room, the drying room door is closed, the nitrogen valve is opened, nitrogen is filled into the drying room, and the bottom number of the nitrogen flow meter is recorded. When the volume of nitrogen inflow reaches 6 times the volume of the drying room, the nitrogen valve can be closed until the drying is completed.

6. The production process of the realgar powder by water flying according to claim 1, characterized in that, The batch size of step S10 is 1200 kg and the mixing time is 30 min.

7. The production process of the calcined realgar powder according to claim 1, characterized in that, The step S9 includes: all realgar powder passes through a 250-mesh sieve to ensure that the realgar powder after sieving can meet the quality requirements of ultra-fine powder when performing particle size detection (the quantity of realgar powder that all passes through a 150-mesh sieve and passes through a 200-mesh sieve ≥ 95.0%).

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