Preparation process of iodophor disinfectant

Abstract

The invention discloses a preparation process of an iodophor disinfectant, and belongs to the technical field of disinfectants. The preparation method comprises the following steps: uniformly mixing elemental iodine, polyvinylpyrrolidone, poloxamer and deionized water to obtain an iodine-carrier compound solution; uniformly mixing the folium artemisiae argyi carbonized superfine powder, the garden burnet leaf carbonized superfine powder, glycerol, sodium hyaluronate and propylene glycol to obtain plant charcoal synergistic slurry; transferring the iodine-carrier compound solution into a reaction kettle, dropwise adding the plant charcoal synergistic slurry while stirring at a low speed, and stirring at a high speed until the mixture is uniform to obtain a primary liquid medicine; the primary liquid medicine is subjected to high-speed shearing emulsification, vacuum degassing is performed, the pH is adjusted to 5.5-6.5, and finally standing and curing are performed. According to the invention, the product stability is excellent, and the industrial problem that iodine is easy to volatilize and precipitate is fundamentally solved; the product provided by the invention can significantly promote wound healing while maintaining efficient sterilization, and meets the requirements of the market on high-end wound nursing products.

Description

Technical Field

[0001] This invention belongs to the field of disinfectant technology, specifically relating to a preparation process for iodine tincture disinfectant. Background Technology

[0002] Iodine tincture is an amorphous complex formed by the complexation of elemental iodine with a surfactant as a carrier. Due to its advantages such as broad-spectrum bactericidal activity, long-lasting effect, and low irritation to skin and mucous membranes, it has become one of the most widely used topical disinfectants in clinical practice. However, in the long-term production and use process, the existing preparation process of iodine tincture and its products still have several technical defects that urgently need to be addressed.

[0003] First, the chemical instability of iodine is a core challenge restricting product quality. Current technologies generally use single polymers such as polyvinylpyrrolidone (PVP) as iodine carriers. However, this traditional complex structure is relatively loose. Especially under fluctuating storage temperatures or light exposure, iodine molecules easily dissociate from the complex and volatilize, causing a significant decrease in the effective iodine content over time, directly affecting the reliability of disinfection. Simultaneously, the precipitation of free iodine easily leads to sedimentation, reducing solution clarity, affecting not only product appearance but also potentially causing inaccurate dosage during use.

[0004] Secondly, existing products have significant limitations in terms of user experience and additional functions. To maintain disinfection effectiveness, some products tend to use higher concentrations of iodine, which often exacerbates skin irritation, causing dryness, tightness, and even allergic reactions. This is particularly unfriendly to children, people with sensitive skin, or users who need to use the product long-term. Furthermore, traditional povidone-iodine has a single function, focusing solely on disinfection and lacking the ability to promote wound healing, making it difficult to meet the market's growing demand for multifunctional nursing products.

[0005] Secondly, there is room for improvement in traditional preparation processes. Many existing production processes are not precise enough in mixing, stirring, and grinding, which can easily lead to uneven dispersion of solid raw materials and affect product uniformity. More importantly, some processes fail to effectively control temperature during preparation, especially in the complexation and mixing stages involving iodine. Higher ambient temperatures or heat generated by mechanical friction can accelerate the volatilization of iodine, not only wasting raw materials but also further exacerbating the aforementioned stability problems.

[0006] Therefore, there is an urgent need in this field for an innovative preparation process for iodine disinfectant, aiming to fundamentally improve the stability of iodine, extend the product's shelf life, enhance user comfort, and provide it with richer wound care functions. This is the key technical problem that the technical solution of this invention aims to solve. Summary of the Invention

[0007] In view of this, the purpose of this invention is to provide a preparation process for iodine disinfectant. This invention has excellent product stability and fundamentally solves the industry problem of iodine's volatility and precipitation. While maintaining high-efficiency sterilization, the product of this invention can significantly promote wound healing, meeting the market demand for high-end wound care products.

[0008] To achieve the above objectives, the present invention provides the following technical solution: This invention provides a preparation process for iodine disinfectant, comprising the following preparation steps: S1. Mix elemental iodine, polyvinylpyrrolidone, poloxamer, and deionized water to obtain an iodine-carrier complex solution; S2. Mix the carbonized ultrafine powder of Artemisia argyi, carbonized ultrafine powder of Sanguisorba officinalis, glycerin, sodium hyaluronate, and propylene glycol evenly to obtain a plant charcoal synergistic slurry. S3. The iodine-carrier complex solution was transferred to a reaction vessel and plant charcoal synergist slurry was added dropwise under low-speed stirring. After the addition was completed, the mixture was stirred at high speed until homogeneous to obtain the primary drug solution. S4. The primary drug solution is emulsified by high-speed shearing, then degassed under vacuum, and the pH is adjusted to 5.5~6.5. Finally, it is allowed to stand for aging.

[0009] Preferably, the mass ratio of elemental iodine, polyvinylpyrrolidone, poloxamer, and deionized water in S1 is (1-3):(5-15):(1-3):(70-85).

[0010] Preferably, the polyvinylpyrrolidone is of type PVP-K30 or PVP-S630.

[0011] Preferably, the mixing temperature in S1 is 25-35℃, the mixing speed is 300-500 rpm, and the mixing time is 2-4h.

[0012] This invention, by employing the above-mentioned technical solution, forms a stable disinfection substrate, yielding a uniform and clear brownish-red iodine base solution, reducing evaporation waste. Through a dual-locking mechanism of "PVP complexation" and "poloxam micelle encapsulation," coupled with a low-temperature process, the loss rate of raw iodine is reduced to an extremely low level, lowering production costs. The carbonyl oxygen atom in the PVP molecule possesses a lone pair of electrons, which can form a loose, reversible charge-transfer complex (PVP-I2) with iodine molecules. This reaction transforms unstable, volatile elemental iodine into a stable, slow-release state. Poloxamer 407 is a triblock copolymer nonionic surfactant. Above its critical micelle concentration, it self-assembles in water to form tiny micelles. These micelles can encapsulate the already formed PVP-I2 complex within a hydrophobic core, or adsorb onto the micelle surface through hydrogen bonding, forming a physical barrier that greatly inhibits iodine volatilization and the precipitation of free iodine, solving the precipitation problem. The evaporation rate of iodine increases sharply with increasing temperature. Keeping the temperature below 35℃ throughout the process is an effective way to minimize iodine loss during production from a thermodynamic perspective.

[0013] Preferably, the mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate and propylene glycol in S2 is (1-5):(0.5-2):(3-8):(0.5-1.5):(2-5).

[0014] Preferably, the particle size D90 of the charred ultrafine powder of Artemisia argyi and charred ultrafine powder of Sanguisorba officinalis in S2 is less than 10 μm. The charred powders from these specific plants possess traditional astringent, adsorbent, and wound-healing properties, which synergistically enhance the bactericidal effect of iodine. The ultrafine powder morphology allows it to be evenly dispersed in the liquid, forming a protective film on the wound surface and aiding in scab formation.

[0015] Preferably, the stirring rate in step S2 is 2000-4000 rpm and the stirring time is 10-20 min.

[0016] Carbon powder is highly hydrophobic; direct addition to the aqueous phase results in severe agglomeration and floating. Glycerin and propylene glycol, as polyols, preferentially penetrate the gaps between carbon powder particles, replacing surface air and achieving thorough wetting. High shear force breaks down the original powder aggregates, ensuring each carbon powder particle is coated with humectants and co-solvents, forming a stable, free-flowing slurry. Simultaneous homogenization and vacuuming remove air bubbles carried by the powder and entangled in the mixing process, preventing these bubbles from affecting product quality or causing oxidation reactions in subsequent steps.

[0017] Preferably, the mass ratio of the iodine-carrier complex solution and the plant charcoal synergistic slurry in S3 is 9:1.

[0018] Preferably, the low-speed stirring frequency in S3 is 100-200 rpm; the high-speed stirring frequency is 400-600 rpm.

[0019] Preferably, the high-speed shear emulsification temperature in S4 is 25~30℃, the high-speed shear emulsification speed is 8000-12000 rpm, and the time is 5-10 min.

[0020] Preferably, the conditions for static ripening in S4 are as follows: Avoid light; Temperature 20-25℃; The settling time is 24-48 hours.

[0021] It contains at least the following beneficial technical effects: This invention boasts exceptional product stability, fundamentally solving the industry-wide problem of iodine's volatility and precipitation. By scientifically compounding highly effective moisturizing ingredients such as glycerin and sodium hyaluronate in the formula, a moisturizing film is formed on the skin surface, effectively combating the dryness and tightness caused by iodine. The invention incorporates ultrafine powders of Artemisia argyi charcoal and Sanguisorba officinalis charcoal, combining their traditional Chinese medicine properties of "adsorption, astringency, tissue regeneration, and hemostasis" with modern disinfection technology. Experiments have demonstrated that this product, while maintaining highly effective sterilization, significantly promotes wound healing, achieving a functional leap from simple disinfection to a four-in-one approach of "disinfection, adsorption, astringency, and repair," meeting the market demand for high-end wound care products. The entire process is carried out at low temperatures, reducing the thermodynamic volatilization of iodine at the source, improving raw material utilization, lowering production costs, and making it suitable for industrial production. Attached Figure Description

[0022] Figure 1 A bar chart comparing the wound healing rates of rats at different time points. Detailed Implementation

[0023] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0024] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that each intermediate value between the upper and lower limits of the range is also specifically disclosed. Every smaller range between any stated value or intermediate value within a stated range, and any other stated value or intermediate value within said range, is also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0025] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or testing of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0026] Various modifications and variations can be made to the specific embodiments described in this specification without departing from the scope or spirit of the invention, as will be apparent to those skilled in the art. Other embodiments derived from this specification will also be obvious to those skilled in the art. This application specification and embodiments are merely exemplary.

[0027] The terms “include,” “including,” “have,” “contain,” etc., used in this article are all open-ended terms, meaning that they include but are not limited to.

[0028] Unless otherwise specified, "room temperature" and "normal temperature" in this invention refer to 25±2℃.

[0029] Unless otherwise specified, all raw materials or instruments used in the following embodiments of the present invention are commercially available.

[0030] Raw material description: The carbonized ultrafine powder of Artemisia argyi leaves and the carbonized ultrafine powder of Sanguisorba officinalis leaves with a particle size D90 of less than 10μm are both sourced from commercially available products.

[0031] Example 1: A preparation process for iodine disinfectant, comprising the following preparation steps: S1. Mix elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water at 30°C and a stirring rate of 400 rpm for 3 hours to obtain an iodine-carrier complex solution; wherein the mass ratio of elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water is 2:10:2:80.

[0032] S2. Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol are stirred at a stirring speed of 3000 rpm for 15 min to obtain plant charcoal slurry; wherein the mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol is 3:1:5:1:3.

[0033] S3. The iodine-carrier complex solution was transferred to a reaction vessel, and plant charcoal synergistic slurry was added dropwise at a stirring rate of 150 rpm. After the addition was completed, the mixture was stirred evenly at a stirring rate of 500 rpm to obtain the primary drug solution. The mass ratio of the iodine-carrier complex solution to the plant charcoal synergistic slurry was 9:1.

[0034] S4. The primary drug solution is emulsified at 28℃ and 10000 rpm for 8 minutes, then degassed under vacuum and the pH is adjusted to 6. Finally, it is allowed to stand for aging. The aging conditions are: protection from light; temperature 23℃; aging time 30 hours.

[0035] Example 2, a preparation process for iodine disinfectant, includes the following preparation steps: S1. Mix elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water at 25°C and a stirring rate of 300 rpm for 2 hours to obtain an iodine-carrier complex solution; wherein the mass ratio of elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water is 1:1:1:70.

[0036] S2. Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol are stirred at a stirring speed of 2000 rpm for 10 min to obtain plant charcoal slurry; wherein the mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol is 1:(0.5-2):3:0.5:2.

[0037] S3. The iodine-carrier complex solution was transferred to a reaction vessel, and plant charcoal synergistic slurry was added dropwise at a stirring rate of 100 rpm. After the addition was completed, the mixture was stirred evenly at a stirring rate of 400 rpm to obtain the primary drug solution. The mass ratio of the iodine-carrier complex solution to the plant charcoal synergistic slurry was 9:1.

[0038] S4. The primary drug solution is emulsified at 25℃ and 8000 rpm for 5 minutes, then degassed under vacuum and the pH is adjusted to 5.5. Finally, it is allowed to stand for aging. The aging conditions are: protection from light; temperature 20℃; aging time 24 hours.

[0039] Example 3: A preparation process for iodine disinfectant, comprising the following preparation steps: S1. Mix elemental iodine, polyvinylpyrrolidone (PVP-K30), poloxamer, and deionized water at 35°C and a stirring rate of 500 rpm for 4 hours to obtain an iodine-carrier complex solution; wherein the mass ratio of elemental iodine, polyvinylpyrrolidone (PVP-K30), poloxamer, and deionized water is 3:15:3:85.

[0040] S2. Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol are stirred at a stirring speed of 4000 rpm for 20 min to obtain plant charcoal slurry; wherein the mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol is 5:2:8:1.5:5.

[0041] S3. The iodine-carrier complex solution was transferred to a reaction vessel, and plant charcoal synergistic slurry was added dropwise at a stirring rate of 200 rpm. After the addition was completed, the mixture was stirred evenly at a stirring rate of 600 rpm to obtain the primary drug solution. The mass ratio of the iodine-carrier complex solution to the plant charcoal synergistic slurry was 9:1.

[0042] S4. The primary drug solution is emulsified at 30℃ and 12000 rpm for 10 minutes, then degassed under vacuum and the pH is adjusted to 6.5. Finally, it is allowed to stand for aging. The aging conditions are: protection from light; temperature 25℃; aging time 48 hours.

[0043] Comparative Example 1 The preparation method of this comparative example is the same as that of Example 1, except that S1 does not contain polyvinylpyrrolidone.

[0044] Comparative Example 2 The preparation method of this comparative example is the same as that of Example 1, except that S1 does not contain poloxamer.

[0045] Comparative Example 3 A preparation process for an iodine disinfectant includes the following steps: S1. Mix elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water at 30°C and a stirring rate of 400 rpm for 3 hours to obtain an iodine-carrier complex solution; wherein the mass ratio of elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water is 2:10:2:80.

[0046] S2. Adjust the pH of the iodine-carrier complex solution to 6, and then allow it to stand for aging. The aging conditions are: protection from light; temperature 23℃; aging time 30h.

[0047] Comparative Example 4 A preparation process for an iodine disinfectant includes the following steps: S1. Mix elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water at 30°C and a stirring rate of 400 rpm for 3 hours to obtain an iodine-carrier complex solution; wherein the mass ratio of elemental iodine, polyvinylpyrrolidone (PVP-S630), poloxamer, and deionized water is 2:10:2:80.

[0048] S2. Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, and water are stirred at a stirring speed of 3000 rpm for 15 min to obtain plant charcoal slurry; wherein the mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, and water is 3:1:9.

[0049] S3. The iodine-carrier complex solution was transferred to a reaction vessel, and plant charcoal synergistic slurry was added dropwise at a stirring rate of 150 rpm. After the addition was completed, the mixture was stirred evenly at a stirring rate of 500 rpm to obtain the primary drug solution. The mass ratio of the iodine-carrier complex solution to the plant charcoal synergistic slurry was 9:1.

[0050] S4. The primary drug solution is emulsified at 28℃ and 10000 rpm for 8 minutes, then degassed under vacuum and the pH is adjusted to 6. Finally, it is allowed to stand for aging. The aging conditions are: protection from light; temperature 23℃; aging time 30 hours.

[0051] Experimental Example 1 Product stability test Accelerated stability tests were conducted on the products obtained in Examples 1-3 and Comparative Examples 1-4 of this invention, in accordance with the "Disinfection Technical Specifications" and the drug stability guidelines in the "Chinese Pharmacopoeia".

[0052] Experimental conditions: Each sample was placed in a constant temperature and humidity chamber at 40±2°C and 75%±5% relative humidity, and samples were taken and tested at 0 days, 30 days, 60 days and 90 days respectively.

[0053] Testing indicators: Effective iodine content: determined by sodium thiosulfate titration.

[0054] pH value: Measured using a precision pH meter.

[0055] Sedimentation: Visually observe and record whether sedimentation or stratification occurs.

[0056] The rate of change in effective iodine content during accelerated stability testing is shown in Table 1.

[0057] Table 1

[0058] The appearance and precipitation records of the accelerated stability test (90 days) are shown in Table 2.

[0059] Table 2

[0060] Experimental conclusion: After the 90-day accelerated test of Examples 1-3 of the present invention, the decline rate of the available iodine content was lower than 5%, and no precipitation occurred, showing excellent chemical stability and physical stability.

[0061] In Comparative Example 1 and Comparative Example 2, the available iodine content decreased sharply and precipitation occurred, which proved the crucial importance of the dual stability mechanism of "PVP complexation" and "poloxamer micelle encapsulation", and neither can be missing.

[0062] The iodine stability of Comparative Example 3 was acceptable, but it also decreased compared with the examples, indicating that the use of carbon powder would also increase the stability to a certain extent.

[0063] In Comparative Example 4, severe precipitation occurred without glycerol, sodium hyaluronate, etc. in the slurry, which proved the key role of the pretreatment step of forming the synergistic slurry in ensuring the stable dispersion of carbon powder and preventing aggregation.

[0064] Experimental Example 2 Antibacterial experiment 1. Experimental method: Experimental strains: Staphylococcus aureus (ATCC 6538), Escherichia coli (ATCC 8099), Pseudomonas aeruginosa (ATCC 15442).

[0065] Test samples: the product of Example 1, the product of Comparative Example 3, negative control (normal saline).

[0066] Experimental steps: Mix the bacterial suspension and the disinfectant in a certain ratio, act for a predetermined time (2 minutes), immediately terminate the reaction, and culture and count the number of surviving colonies.

[0067] Results of suspension quantitative bactericidal test: Table 3

[0068] If the logarithm of killing > 3.00 (i.e., the bactericidal rate > 99.9%), it can be determined that the disinfection is qualified; > 5.00 indicates that the bactericidal rate > 99.999% Experimental conclusion: Both Example 1 of the product of the present invention and Comparative Example 3 of the traditional iodine tincture without plant carbon showed extremely strong instantaneous broad-spectrum bactericidal ability, fully meeting the disinfectant standard. This indicates that the addition of the plant carbon synergistic component did not affect the core bactericidal efficacy of iodine tincture, and the two can coexist well.

[0069] Experimental Example 3 Wound healing promotion effect test 1. Experimental method: Experimental animals: 30 SD rats, and a full-thickness skin defect model was established.

[0070] Experimental grouping: Experimental group: Apply the product from Example 1 to the wound.

[0071] Control group: The wound was treated with product 3 (comparison ratio 3).

[0072] Blank group: No treatment was given to the wound.

[0073] Observation indicators: The wound healing rate was measured on postoperative days 3, 7, and 14, and wound tissue was taken for pathological analysis.

[0074] The results of the comparative experiment on wound healing rate (%) in rats are shown in the figure. Figure 1 .

[0075] On days 7 and 14 of wound healing, the wound healing rate in the experimental group was significantly higher than that in the control group and the blank group. Pathological sections showed that the experimental group had more vigorous granulation tissue growth and a milder inflammatory response. This indicates that the charred Artemisia argyi and carbonized Sanguisorba officinalis leaves added in this invention do indeed exert a synergistic effect of adsorbing exudate, astringing the wound, and promoting granulation tissue growth, achieving an integrated "disinfection-repair" technical effect.

[0076] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A preparation process for iodine disinfectant, characterized in that, The preparation steps include the following: S1. Mix elemental iodine, polyvinylpyrrolidone, poloxamer, and deionized water to obtain an iodine-carrier complex solution; S2. Mix the carbonized ultrafine powder of Artemisia argyi, carbonized ultrafine powder of Sanguisorba officinalis, glycerin, sodium hyaluronate, and propylene glycol evenly to obtain a plant charcoal synergistic slurry. S3. The iodine-carrier complex solution was transferred to a reaction vessel and plant charcoal synergist slurry was added dropwise under low-speed stirring. After the addition was completed, the mixture was stirred at high speed until homogeneous to obtain the primary drug solution. S4. The primary drug solution is emulsified by high-speed shearing, then degassed under vacuum, and the pH is adjusted to 5.5~6.

5. Finally, it is allowed to stand for aging.

2. The preparation process according to claim 1, characterized in that, The mass ratio of elemental iodine, polyvinylpyrrolidone, poloxamer, and deionized water in S1 is (1-3):(5-15):(1-3):(70-85).

3. The preparation process according to claim 2, characterized in that, The polyvinylpyrrolidone is designated as PVP-K30 or PVP-S630.

4. The preparation process according to claim 1, characterized in that, The mixing temperature in S1 is 25-35℃, the mixing speed is 300-500 rpm, and the mixing time is 2-4h.

5. The preparation process according to claim 1, characterized in that, The mass ratio of Artemisia argyi carbonized ultrafine powder, Sanguisorba officinalis carbonized ultrafine powder, glycerin, sodium hyaluronate, and propylene glycol in S2 is (1-5):(0.5-2):(3-8):(0.5-1.5):(2-5).

6. The preparation process according to claim 5, characterized in that, The particle size D90 of the carbonized ultrafine powder of Artemisia argyi and the carbonized ultrafine powder of Sanguisorba officinalis are both less than 10 μm.

7. The preparation process according to claim 1, characterized in that, The stirring rate in S2 is 2000-4000 rpm, and the stirring time is 10-20 min.

8. The preparation process according to claim 1, characterized in that, The mass ratio of the iodine-carrier complex solution and the plant charcoal synergistic slurry in S3 is 9:

1.

9. The preparation process according to claim 1, characterized in that, The low-speed stirring frequency in S3 is 100-200 rpm; the high-speed stirring frequency is 400-600 rpm.

10. The preparation process according to claim 1, characterized in that, The high-speed shear emulsification temperature in S4 is 25~30℃, the high-speed shear emulsification speed is 8000-12000 rpm, and the time is 5-10 min.

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