CN112263851A - Preparation method of simethicone defoaming composition - Google Patents
Preparation method of simethicone defoaming composition Download PDFInfo
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- CN112263851A CN112263851A CN202011055926.2A CN202011055926A CN112263851A CN 112263851 A CN112263851 A CN 112263851A CN 202011055926 A CN202011055926 A CN 202011055926A CN 112263851 A CN112263851 A CN 112263851A
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- simethicone
- silicon dioxide
- defoaming
- stirring
- colloidal silicon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Colloid Chemistry (AREA)
- Degasification And Air Bubble Elimination (AREA)
Abstract
The invention discloses a preparation method of a simethicone defoaming composition, which comprises the steps of mixing simethicone and colloidal silicon dioxide in a mass ratio of 94-97: 3-6, stirring at 150-200 ℃ for a constant temperature of more than 1h, treating the obtained material with a colloid mill for not less than 30min, and stirring the material subjected to the colloid mill at 150-200 ℃ for a constant temperature of more than 2 h. The colloidal silicon dioxide in the prepared product is uniformly dispersed, and has excellent defoaming capability and stable quality.
Description
Technical Field
The invention relates to a preparation method of a simethicone defoaming composition, and belongs to the field of medicine synthesis.
Background
Dimethicone (Dimethicone), chemical name polydimethylsiloxane, is a medical antifoaming agent commonly used in clinic and is commonly used for preoperative antifoaming in digestive endoscopy or abdominal imaging examination. Simethicone breaks up the accumulation of air bubbles by changing the surface tension of the air bubbles in the digestive tract, and the released gas is absorbed by the intestinal wall or expelled by peristalsis. The defoaming effect of the simethicone is weaker when the simethicone is used alone, and the defoaming effect of the simethicone can be enhanced by adding the silicon dioxide. The composition is used as a compound of dimeticone and silicon dioxide, and the defoaming performance of the composition is far better than that of dimeticone or silicon dioxide alone. The dimeticone belongs to pharmacological and physiological inert substances, and toxicological experiments show that the dimeticone has no toxic effect. Simethicone is a classic defoamer containing simethicone and silicon dioxide, and is a mixture of 4-7% of silicon dioxide and 90.5-99.0% of simethicone with the viscosity of 20-400 cps, and is off-white to milky viscous liquid.
The silicon dioxide is used as the defoaming synergist of the dimeticone, and whether the silicon dioxide is uniformly dispersed in the dimeticone directly determines the strength and stability of the defoaming capability of the defoaming composition.
The invention provides a method for improving the dispersion degree of colloidal silicon dioxide in dimeticone, which can prepare the dimeticone defoaming composition with excellent defoaming capability, and has simple and convenient operation and good stability.
Disclosure of Invention
The invention mainly solves the technical problem of providing a preparation method of the simethicone defoaming composition, which can produce and obtain a product with uniform dispersion of colloidal silicon dioxide and excellent defoaming capability.
In order to solve the technical problems, the invention adopts a technical scheme that: a preparation method of the simethicone defoaming composition is provided, which comprises the following steps:
(1) mixing dimeticone and colloidal silicon dioxide, stirring and keeping the temperature for more than 1 h;
(2) treating the material obtained in the step (1) by a colloid mill for not less than 30 minutes;
(3) and (3) stirring the material obtained in the step (2) for more than 2 hours at constant temperature.
The viscosity of the dimeticone is 500-600 mPa & s.
In the step (1), the colloidal silicon dioxide has an average particle diameter of 16nm or less and a bulk density of 0.029 to 0.042g/cm3A specific surface area of 200 to 300m2/g。
In the step (1), the stirring constant temperature is 150-200 ℃.
In the step (1), the mass ratio of the colloidal silicon dioxide to the dimeticone is 3-6: 94-97.
In the step (3), the stirring constant temperature is 150-200 ℃.
The invention has the beneficial effects that: the preparation method of the simethicone defoaming composition comprises the steps of firstly mixing simethicone and colloidal silicon dioxide, then stirring and keeping the temperature, reducing the viscosity of the mixture to facilitate the mixture to pass through a colloid mill, then treating the mixture by using the colloid mill to disperse the aggregated colloidal silicon dioxide, and finally stirring and keeping the temperature of the mixture of the simethicone and the colloidal silicon dioxide again to obtain a product with uniformly dispersed colloidal silicon dioxide and excellent defoaming capability.
Detailed Description
Example 1:
mixing dimeticone (A) with certain viscosity with colloidal silicon dioxide according to a certain proportion (B), stirring at a certain temperature (C) for a certain time (D), and reducing the viscosity to facilitate passing through a colloid mill.
Four-factor three-level
Orthogonal table design and experimental results
| Test No | Design of experiments | Kinematic viscosity (mP.s) | Degree of difficulty in grinding through colloid |
| 1 | A1B1C1D1 | 878 | Is easy to pass through |
| 2 | A1B2C2D2 | 1114 | Is easy to pass through |
| 3 | A1B3C3D3 | 1675 | Is easy to pass through |
| 4 | A2B1C2D3 | 2265 | Is easy to pass through |
| 5 | A2B2C3D1 | 4896 | Can pass through |
| 6 | A2B3C1D2 | 7105 | Is difficult to pass through |
| 7 | A3B1C3D2 | 4232 | Can pass through |
| 8 | A3B2C1D3 | 9871 | Is difficult to pass through |
| 9 | A3B3C2D1 | 16084 | Is difficult to pass through |
From the results of the orthogonal test, the degree of difficulty in colloid milling is most affected by the viscosity of the dimethicone. Thus, the viscosity of the simethicone is 550mm/s2Keeping the temperature for more than 1h, keeping the temperature at 150-200 ℃, and mixing the dimethyl silicone oil: the colloidal silicon dioxide is 94-98: 2 to 6.
Example 2
550mm/s2Mixing the dimeticone with viscosity and the colloidal silicon dioxide according to a certain proportion (A), stirring at 175 ℃ and keeping the temperature for 1h, processing for a certain time (B) by a colloid mill, collecting materials, stirring at a certain temperature (C) and keeping the temperature for a certain time (D), and obtaining the product. And (4) carrying out n-hexane dispersion test and defoaming capability detection on the product.
N-hexane dispersion test: taking 2g of the simethicone defoaming composition, adding 10ml of n-hexane, fully mixing and dispersing uniformly, observing the properties of the dispersion liquid, and obtaining an off-white uniform suspension without large particles.
And (3) defoaming capability detection: according to the detection method under the item of USP simethicone quality standard defoaming capability, the foam is completely eliminated within 15 s.
Four-factor three-level
Orthogonal table design and experimental results
| Test No | Design of experiments | Result of n-hexane dispersion | Defoaming capability |
| 1 | A1B1C1D1 | Off-white suspension with large particles precipitated | 20s |
| 2 | A1B2C2D2 | Off-white homogeneous suspension | 18s |
| 3 | A1B3C3D3 | Off-white homogeneous suspension | 16s |
| 4 | A2B1C2D3 | Off-white suspension with large particles precipitated | 10s |
| 5 | A2B2C3D1 | Off-white homogeneous suspension | 17s |
| 6 | A2B3C1D2 | Off-white homogeneous suspension | 8s |
| 7 | A3B1C3D2 | Off-white suspension with large particles precipitated | 5s |
| 8 | A3B2C1D3 | Off-white homogeneous suspension | 6s |
| 9 | A3B3C2D1 | Off-white homogeneous suspension | 15s |
According to the orthogonal test result, the colloid mill treatment time is more than 30min, the constant temperature time is more than 2h, the constant temperature is 150-200 ℃, and the dimeticone: the colloidal silicon dioxide is 94-96: 4-6, the dimeticone defoaming composition with high dispersity and excellent defoaming capability can be prepared.
Example 3
(1) Will be 600mm/s2Mixing the dimeticone with viscosity and the colloidal silicon dioxide according to the proportion of 97:3, stirring at 150 ℃, and keeping the temperature for 1 h;
(2) treating the product obtained in the step (1) for 30min by a colloid mill, wherein the product is easier to pass through the colloid mill;
(3) stirring the product obtained in the step (2) at 150 ℃ and keeping the temperature for 2 hours to obtain the simethicone defoaming composition;
(4) taking 2g of the simethicone defoaming composition, and dispersing with 10ml of n-hexane to obtain an off-white uniform suspension, wherein no precipitated particles are found;
(5) taking the simethicone defoaming composition, and detecting the defoaming capability according to the method carried under the quality standard defoaming capability test item of USP simethicone, wherein the defoaming time is 7s, and the specification is met.
(6) Samples are respectively taken from the upper layer, the middle layer and the lower layer of the reaction container, and the content of the silicon dioxide is detected, so that the content is 3.05 percent, 3.08 percent and 3.01 percent, and is relatively uniform.
Example 4
The sample of example 3 was filled in colorless glass bottles, placed in a constant temperature stable box with an open mouth, examined for 6 months at 40 ℃. + -. 2 ℃ and RH 75%. + -. 5%, sampled for 1, 2, 3, 6 months, and tested for properties, n-hexane dispersion, defoaming ability, and silica content.
Stability survey results
After the sample of example 3 prepared according to the proposed conditions is tested and investigated for 6 months in an accelerated test, all the investigation indexes still meet the regulations, and the preparation method of the simethicone defoaming composition is feasible.
Claims (5)
1. The preparation method of the simethicone defoaming composition is characterized by comprising the following steps:
1) mixing dimeticone and colloidal silicon dioxide, stirring and keeping the temperature for more than 1 h;
2) processing the material obtained in the step 1) by a colloid mill for not less than 30 minutes;
3) stirring the materials obtained in the step 2) and keeping the temperature for more than 2 hours.
2. The method of preparing the simethicone antifoam composition of claim 1 wherein: in the step 1), the stirring constant temperature is 150-200 ℃.
3. The method of preparing the simethicone antifoam composition of claim 1 wherein: in the step 1), the mass ratio of the colloidal silicon dioxide to the dimeticone is 3-6: 94-97.
4. The method of preparing the simethicone antifoam composition of claim 1 wherein: in the step 1), the colloidal silicon dioxide has an average particle size of less than 16nm and a bulk density of 0.029-0.042 g/cm3A specific surface area of 200 to 300m2/g。
5. The method of preparing the simethicone antifoam composition of claim 1 wherein: in the step 1), the viscosity of the dimeticone is 500-600 mm/s2。
The method of preparing the simethicone antifoam composition of claim 1 wherein: in the step 3), the stirring constant temperature is 150-200 ℃.
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5073384A (en) * | 1989-10-19 | 1991-12-17 | Valentine Enterprises, Inc. | Maltodextrin/defoaming composition combinate |
| CN102307978A (en) * | 2009-02-04 | 2012-01-04 | 陶氏康宁公司 | Foam control composition |
| CN102532901A (en) * | 2010-12-21 | 2012-07-04 | 重庆北碚现代应用药物研究所 | Method for preparing simethicone |
| CN103250926A (en) * | 2012-02-17 | 2013-08-21 | 重庆北碚现代应用药物研究所 | Complex antifoaming agent and preparation method thereof |
| CN104610745A (en) * | 2015-01-13 | 2015-05-13 | 山东大学 | Preparation method for simethicone |
| WO2016021427A1 (en) * | 2014-08-05 | 2016-02-11 | 信越化学工業株式会社 | Defoamer oil compound, production method therefor, and defoamer composition |
| CN106422427A (en) * | 2016-09-28 | 2017-02-22 | 佛山慧创正元新材料科技有限公司 | 1-cyclohexene ethylamine/nanometer silicon dioxide compound de-foaming agent and preparation method thereof |
| CN107469414A (en) * | 2017-10-10 | 2017-12-15 | 优美特（北京）环境材料科技股份公司 | A kind of defoamer containing poly-organosilicon and preparation method thereof |
-
2020
- 2020-09-30 CN CN202011055926.2A patent/CN112263851A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5073384A (en) * | 1989-10-19 | 1991-12-17 | Valentine Enterprises, Inc. | Maltodextrin/defoaming composition combinate |
| CN102307978A (en) * | 2009-02-04 | 2012-01-04 | 陶氏康宁公司 | Foam control composition |
| CN102532901A (en) * | 2010-12-21 | 2012-07-04 | 重庆北碚现代应用药物研究所 | Method for preparing simethicone |
| CN103250926A (en) * | 2012-02-17 | 2013-08-21 | 重庆北碚现代应用药物研究所 | Complex antifoaming agent and preparation method thereof |
| WO2016021427A1 (en) * | 2014-08-05 | 2016-02-11 | 信越化学工業株式会社 | Defoamer oil compound, production method therefor, and defoamer composition |
| CN104610745A (en) * | 2015-01-13 | 2015-05-13 | 山东大学 | Preparation method for simethicone |
| CN106422427A (en) * | 2016-09-28 | 2017-02-22 | 佛山慧创正元新材料科技有限公司 | 1-cyclohexene ethylamine/nanometer silicon dioxide compound de-foaming agent and preparation method thereof |
| CN107469414A (en) * | 2017-10-10 | 2017-12-15 | 优美特（北京）环境材料科技股份公司 | A kind of defoamer containing poly-organosilicon and preparation method thereof |
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| 黄文润: "《硅油及其应用》", 31 July 2018, 成都：四川科学技术出版社 * |
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