Polydimethylsiloxane nano-film solubilizer and preparation method thereof
By reacting with distilled water on the inner wall of the glass cup through the drainage method, the ring-shaped refrigerator absorbs heat and inhibits the activity of hydrogen chloride gas, the problem of corrosion and preparation time of hydrogen chloride gas in the preparation of polydimethylsiloxane nano-film solubilizer is solved, and the problem of corrosion and preparation time of hydrogen chloride gas in the preparation of polydimethylsiloxane nano-film solubilizer is achieved. More efficient preparation process.
Patent Information
- Application Number
- CN202411396651.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-09
- Publication Date
- 2024-12-06
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Corrosive hydrogen chloride gas is generated during the preparation process of existing polydimethylsiloxane nanofilm solubilizers, and the preparation time of the dropping method is long and the efficiency is slow.
The drainage method is used to react dimethyldichlorosilane with distilled water along the inner wall of the glass cup, and the ring-shaped refrigerator absorbs heat and inhibits the activity of hydrogen chloride gas, and combines the continuous addition of raw materials to shorten the reaction time and improve efficiency.
The preparation time is significantly shortened by the drainage method, improved preparation efficiency, prevented high temperature from affecting nanomembrane activity and inhibited the dispersion of hydrogen chloride gas, and formed hydrochloric acid faster.
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Figure CN119081118A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of polydimethylsiloxane nanofilm solubilizing agent, and more specifically to a polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof. Background Art
[0002] Polydimethylsiloxane nanofilm solubilizer is widely used in cosmetics and personal care products, often in skin care products, hair care products and makeup. It can promote the dissolution of water and oil and ensure the solubility of the product. When the product containing this solubilizer is used, it can form a layer of nano oil film, which can better protect the skin while having a soft and smooth touch, making the product easier to apply and spread, improving the use experience.
[0003] During the preparation process of polydimethylsiloxane nanofilm solubilizer, a large amount of hydrogen chloride gas will be generated. The hydrogen chloride gas is corrosive and can cause harm to the respiratory mucosa and skin of people. However, when the hydrogen chloride gas contacts with the aqueous solution again, hydrochloric acid will be generated. Therefore, the existing polydimethylsiloxane nanofilm solubilizer is often prepared by the dripping method. A small amount of the preparation raw material is added each time, which can give the hydrogen chloride gas and the aqueous solution sufficient reaction time to produce hydrochloric acid. However, this method takes a long time to prepare and is inefficient. Summary of the invention
[0004] 1. Technical issues to be solved
[0005] In view of the problems existing in the prior art, the purpose of the present invention is to provide a polydimethylsiloxane nanofilm solubilizer and a preparation method thereof, which can realize the addition of the preparation raw material dimethyldichlorosilane into distilled water along a glass cup by a drainage method, and the hydrolysis reaction of dimethyldichlorosilane and distilled water will be carried out near the inner wall of the glass cup. Since the inner wall of the glass cup is very close to the annular refrigerator, the heat generated during the hydrolysis reaction will be quickly absorbed to prevent the high temperature during the hydrolysis process from affecting the activity of the polydimethylsiloxane nanofilm solubilizer. In addition, under the action of the annular refrigerator, the temperature near the inner wall of the glass cup is relatively low, which can well inhibit the activity of hydrogen chloride gas molecules, making it difficult to disperse, and can react with distilled water again to form hydrochloric acid faster, shortening the reaction time. Combined with the drainage method, the preparation raw materials can be continuously added, which can greatly shorten the preparation time and improve the preparation efficiency.
[0006] 2. Technical solution
[0007] To solve the above problems, the present invention adopts the following technical solutions.
[0008] A polydimethylsiloxane nanofilm solubilizer and a preparation method thereof, characterized in that it comprises the following steps:
[0009] S1. First, prepare a tray with a refrigerator;
[0010] S2, placing the glass on the tray, and placing a cooler on the outer circumference of the lower end of the glass; then inserting a thermometer into the glass;
[0011] S3, then insert a temperature agent into the glass and pour distilled water into the glass;
[0012] S4. Place a pressure equalizing funnel on the top of the glass cup, pour dimethyldichlorosilane into the pressure equalizing funnel, and finally seal the pressure equalizing funnel with a leather stopper;
[0013] S5, opening the control valve on the pressure equalizing funnel, controlling the flow rate so that the dimethyldichlorosilane in the pressure equalizing funnel slowly flows into the glass cup, and undergoes a hydrolysis reaction with distilled water along the inner wall of the glass cup, thereby generating polysiloxane and hydrogen chloride gas, wherein the hydrogen chloride gas reacts with the distilled water again to generate hydrochloric acid, and finally the products in the glass cup are polydimethylsiloxane nanofilm solubilizing agent and hydrochloric acid;
[0014] S6, transfer the product in S5 into a separatory bottle, add MTBE extractant, shake and extract to separate the products, and discharge the bottom hydrochloric acid product;
[0015] S7, adding sodium bicarbonate solution to the remaining product in S6, shaking the product to separate into layers again, draining the bottom layer of water, adding anhydrous sodium sulfate to absorb the remaining water in the remaining product, and shaking the separatory bottle to accelerate the absorption of water, thereby obtaining a mixture of polydimethylsiloxane nanofilm solubilizer and MTBE extractant;
[0016] S7, distilling the mixture of the polydimethylsiloxane nanofilm solubilizer and MTBE extractant prepared in S7 to finally prepare the polydimethylsiloxane nanofilm solubilizer.
[0017] Furthermore, the added amounts of the distilled water, dimethyldichlorosilane, MTBE extractant, sodium bicarbonate solution and anhydrous sodium sulfate are 300 ml, 100 ml, 140 ml, 70 ml and 10 mg respectively, wherein 140 ml of MTBE extractant is added in excess.
[0018] Furthermore, the thermometer is used to monitor the temperature of the product in the glass in real time, and the temperature is preferably maintained at 5 degrees Celsius.
[0019] Furthermore, a monitoring port is provided at the upper end of the glass, and a small sealing plug is provided on the outer circumferential surface of the thermometer, and the small sealing plug is embedded in the monitoring port.
[0020] Furthermore, a refrigerator is provided at the upper end of the tray, and the refrigerator is made of a plurality of semiconductor refrigeration sheets spliced in a ring shape.
[0021] Furthermore, the upper end of the tray is fixedly connected to a limiting frame, and the limiting frame is sleeved on the outer circumferential surface of the glass.
[0022] Furthermore, a main drainage rod is arranged in the glass, and six branch drainage rods are arranged at the lower end of the main drainage rod. The lower ends of the six branch drainage rods are all fixed to the inner wall of the glass, and the main drainage rod corresponds to the lower end of the pressure equalizing funnel.
[0023] Furthermore, the outer circumferential surface of the pressure equalizing funnel is fixedly connected to a support frame, and the support frame is connected to the bottle mouth of the glass cup.
[0024] Furthermore, a connecting plug is fixedly connected to the outer circumferential surface of the pressure equalizing funnel, and the connecting plug is embedded in the bottle mouth of the glass.
[0025] 3. Beneficial effects
[0026] Compared with the prior art, the advantages of the present invention are:
[0027] In this scheme, the preparation raw material dimethyldichlorosilane is added to the distilled water along the glass by the drainage method. The hydrolysis reaction of dimethyldichlorosilane and distilled water will be carried out near the inner wall of the glass. Since the inner wall of the glass is very close to the annular refrigerator, the heat generated during the hydrolysis reaction will be quickly absorbed to prevent the high temperature during the hydrolysis process from affecting the activity of the polydimethylsiloxane nanofilm solubilizer. In addition, under the action of the annular refrigerator, the temperature near the inner wall of the glass is relatively low, which can well suppress the activity of the hydrogen chloride gas molecules, making it difficult to disperse, and can react with the distilled water again to form hydrochloric acid faster, shortening the reaction time. Combined with the drainage method, the preparation raw materials are continuously added, which can greatly shorten the preparation time and improve the preparation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS
[0028] Figure 1 It is a schematic diagram of the overall steps of the present invention;
[0029] Figure 2 It is a schematic diagram of the structure of the glass cup and the pressure equalizing funnel of the present invention;
[0030] Figure 3 This is a schematic diagram of the split structure of the glass cup and the pressure equalizing funnel of the present invention;
[0031] Figure 4 It is a schematic diagram of the cross-sectional structure of the glass cup of the present invention.
[0032] Description of the numbers in the figure:
[0033] 1. Tray; 11. Limit rack; 2. Refrigerator; 3. Glass; 31. Monitoring port; 4. Thermometer; 41. Small sealing plug; 5. Pressure equalizing funnel; 51. Support frame; 52. Connecting plug; 6. Leather plug; 7. Control valve; 8. Main drainage rod; 81. Branch drainage rod. DETAILED DESCRIPTION
[0034] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments, and all other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making creative work are within the scope of protection of the present invention.
[0035] In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top / bottom" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific position, be constructed and operated in a specific position, and therefore cannot be understood as limiting the present invention. In addition, the terms "first" and "second" are used for descriptive purposes only and cannot be understood as indicating or implying relative importance.
[0036] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "installed", "provided with", "mounted / connected", "connected", etc. should be understood in a broad sense. For example, "connected" can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0037] Example:
[0038] See also Figure 1 , a polydimethylsiloxane nanofilm solubilizer and a preparation method thereof, comprising the following steps:
[0039] S1, first prepare a tray 1 with a refrigerator 2;
[0040] S2, placing the glass 3 on the tray 1, and the refrigerator 2 is sleeved on the outer circumference of the lower end of the glass 3; then inserting the thermometer 4 into the glass 3;
[0041] S3, then insert the temperature agent 4 into the glass 3, and pour distilled water into the glass 3;
[0042] S4, placing a pressure equalizing funnel 5 on the upper end of the glass cup 3, and pouring dimethyldichlorosilane into the pressure equalizing funnel 5, and finally sealing the pressure equalizing funnel 5 with a leather stopper 6;
[0043] S5, opening the control valve 7 on the pressure equalizing funnel 5, controlling the flow rate so that the dimethyldichlorosilane in the pressure equalizing funnel 5 slowly flows into the glass 3, and undergoes a hydrolysis reaction with distilled water along the inner wall of the glass 3, thereby generating polysiloxane and hydrogen chloride gas, wherein the hydrogen chloride gas reacts with the distilled water again to generate hydrochloric acid, and finally the products in the glass 3 are polydimethylsiloxane nanofilm solubilizing agent and hydrochloric acid;
[0044] S6, transfer the product in S5 into a separatory bottle, add MTBE extractant, shake and extract to separate the products, and discharge the bottom hydrochloric acid product;
[0045] S7, adding sodium bicarbonate solution to the remaining product in S6, shaking the product to separate into layers again, draining the bottom layer of water, adding anhydrous sodium sulfate to absorb the remaining water in the remaining product, and shaking the separatory bottle to accelerate the absorption of water, thereby obtaining a mixture of polydimethylsiloxane nanofilm solubilizer and MTBE extractant;
[0046] S7, distilling the mixture of the polydimethylsiloxane nanofilm solubilizer and MTBE extractant prepared in S7 to finally prepare the polydimethylsiloxane nanofilm solubilizer.
[0047] In the present method, the preparation raw material dimethyldichlorosilane is added into the distilled water along the glass 3 by the drainage method, and the hydrolysis reaction of dimethyldichlorosilane and distilled water will be carried out near the inner wall of the glass 3. Since the inner wall of the glass 3 is very close to the annular refrigerator 2, the heat generated during the hydrolysis reaction will be quickly absorbed to prevent the high temperature during the hydrolysis process from affecting the activity of the polydimethylsiloxane nanofilm solubilizer. In addition, under the action of the annular refrigerator 2, the temperature near the inner wall of the glass 3 is relatively low, which can well suppress the activity of the hydrogen chloride gas molecules, making it difficult to disperse, and can react with the distilled water again to form hydrochloric acid faster, shortening the reaction time. Combined with the drainage method, the preparation raw materials are continuously added, which can greatly shorten the preparation time and improve the preparation efficiency.
[0048] The added amounts of distilled water, dimethyldichlorosilane, MTBE extractant, sodium bicarbonate solution and anhydrous sodium sulfate are 300 ml, 100 ml, 140 ml, 70 ml and 10 mg respectively, of which 140 ml of MTBE extractant is added in excess.
[0049] Preparation of raw materials Addition amount Distilled water 300ml Dimethyldichlorosilane 100ml MTBE Extraction Agent 140ml Sodium bicarbonate solution 70ml Anhydrous sodium sulfate 10mg
[0050] In the present invention, by adding 140 ml of MTBE extractant in excess, the hydrochloric acid in the product can be fully reacted to avoid residual hydrochloric acid in the product.
[0051] See also Figure 1-2 The thermometer 4 is used to monitor the temperature of the product in the glass 3 in real time, and it is best to keep the temperature at 5 degrees Celsius.
[0052] In the present invention, the temperature of the product in the glass 3 is maintained at 5 degrees Celsius by the refrigerator 2, firstly, to prevent the hydrolysis reaction from causing the product temperature to be too high, thereby affecting the activity of the polydimethylsiloxane nanofilm solubilizer, and secondly, to suppress the activity of the hydrogen chloride gas molecules, making it difficult to disperse.
[0053] See also Figure 2-3 A monitoring port 31 is provided at the upper end of the glass 3, and a small sealing plug 41 is provided on the outer circumference of the thermometer 4, and the small sealing plug 41 is embedded with the monitoring port 31;
[0054] In the present invention, after the thermometer 4 extends to the interior of the glass 3 through the monitoring port 31 , the small sealing plug 41 can seal the monitoring port 31 to prevent leakage of hydrogen chloride gas.
[0055] See also Figure 2-3 A refrigerator 2 is arranged at the upper end of the tray 1, and the refrigerator 2 is made of a plurality of semiconductor refrigeration sheets spliced in a ring shape.
[0056] In the present invention, the annular refrigerator 2 can better contact the outer circumferential surface of the glass cup 3, and the refrigeration effect can be improved under full contact.
[0057] See also Figure 2-3 The upper end of the tray 1 is fixedly connected to a limiting frame 11, and the limiting frame 11 is sleeved on the outer circumference of the glass 3.
[0058] In the present invention, the positioning stability of the glass 3 can be further improved by means of the limiting frame 11 .
[0059] See also Figure 2-4 A main drainage rod 8 is arranged in the glass 3 , and six branch drainage rods 81 are arranged at the lower end of the main drainage rod 8 . The lower ends of the six branch drainage rods 81 are all fixed to the inner wall of the glass 3 , and the main drainage rod 8 corresponds to the lower end of the pressure equalizing funnel 5 .
[0060] In the present invention, the raw material dimethyldichlorosilane is added into the distilled water along the glass cup 3 through the main drainage rod 8 and the branch drainage rod 81, and the hydrolysis reaction of dimethyldichlorosilane and distilled water will be carried out near the inner wall of the glass cup 3, and the reaction area is closer to the annular refrigerator 2, thereby improving the refrigeration effect on the product.
[0061] See also Figure 2-3The outer circumferential surface of the pressure equalizing funnel 5 is fixedly connected to the support frame 51, and the support frame 51 is connected to the bottle mouth of the glass cup 3.
[0062] In the present invention, when the pressure equalizing funnel 5 is placed at the mouth of the glass 3 , the support frame 51 can improve the stability of the placement of the pressure equalizing funnel 5 .
[0063] See also Figure 2-3 The outer circumferential surface of the pressure equalizing funnel 5 is fixedly connected with a connecting plug 52 , and the connecting plug 52 is embedded with the bottle mouth of the glass cup 3 .
[0064] In the present invention, when the pressure equalizing funnel 5 is placed at the mouth of the glass 3, the connecting plug 52 can block the mouth of the glass 3 to further prevent the leakage of hydrogen chloride gas.
[0065] The present invention adds the preparation raw material dimethyldichlorosilane into distilled water along the glass 3 by the drainage method, and the hydrolysis reaction of dimethyldichlorosilane and distilled water is carried out near the inner wall of the glass 3. Since the inner wall of the glass 3 is very close to the annular refrigerator 2, the heat generated during the hydrolysis reaction will be quickly absorbed to prevent the high temperature during the hydrolysis process from affecting the activity of the polydimethylsiloxane nanofilm solubilizing agent. Moreover, under the action of the annular refrigerator 2, the temperature near the inner wall of the glass 3 is relatively low, which can well inhibit the activity of the hydrogen chloride gas molecules, making it difficult to disperse, and can react with the distilled water again to form hydrochloric acid faster, shortening the reaction time. In combination with the drainage method, the preparation raw material can be continuously added, which can greatly shorten the preparation time and improve the preparation efficiency.
[0066] The above is only a preferred specific implementation of the present invention; however, the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solution and its improved conception within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.
Claims
1. A polydimethylsiloxane nanofilm solubilizer and a preparation method thereof, characterized in that: The following steps are involved: S1. First, prepare a tray (1) with a refrigerator (2); S2, placing the glass (3) on the tray (1), and placing the refrigerator (2) on the outer circumference of the lower end of the glass (3); then inserting a thermometer (4) into the glass (3); S3, then inserting a temperature agent (4) into the glass (3), and pouring distilled water into the glass (3); S4, placing a pressure equalizing funnel (5) on the top of the glass cup (3), pouring dimethyldichlorosilane into the pressure equalizing funnel (5), and finally sealing the pressure equalizing funnel (5) with a leather stopper (6); S5, opening the control valve (7) on the pressure equalizing funnel (5), controlling the flow rate so that the dimethyldichlorosilane in the pressure equalizing funnel (5) slowly flows into the glass cup (3), and undergoes a hydrolysis reaction with the distilled water along the inner wall of the glass cup (3), thereby generating polysiloxane and hydrogen chloride gas, wherein the hydrogen chloride gas reacts with the distilled water again to generate hydrochloric acid, and finally the products in the glass cup (3) are polydimethylsiloxane nanofilm solubilizing agent and hydrochloric acid; S6, transfer the product in S5 into a separatory bottle, add MTBE extractant, shake and extract to separate the products, and discharge the bottom hydrochloric acid product; S7, adding sodium bicarbonate solution to the remaining product in S6, shaking the product to separate into layers again, draining the bottom layer of water, adding anhydrous sodium sulfate to absorb the remaining water in the remaining product, and shaking the separatory bottle to accelerate the absorption of water, thereby obtaining a mixture of polydimethylsiloxane nanofilm solubilizer and MTBE extractant; S7, distilling the mixture of the polydimethylsiloxane nanofilm solubilizer and MTBE extractant prepared in S7 to finally prepare the polydimethylsiloxane nanofilm solubilizer.
2. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: The added amounts of the distilled water, dimethyldichlorosilane, MTBE extractant, sodium bicarbonate solution and anhydrous sodium sulfate are 300 ml, 100 ml, 140 ml, 70 ml and 10 mg respectively, wherein 140 ml of MTBE extractant is added in excess.
3. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: The thermometer (4) is used to monitor the temperature of the product in the glass (3) in real time, and the temperature is preferably maintained at 5 degrees Celsius.
4. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 3, characterized in that: A monitoring port (31) is provided at the upper end of the glass cup (3), and a small sealing plug (41) is provided on the outer circumferential surface of the thermometer (4), wherein the small sealing plug (41) is engaged with the monitoring port (31).
5. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: A refrigerator (2) is provided at the upper end of the tray (1), and the refrigerator (2) is made by splicing a plurality of semiconductor refrigeration sheets in a ring shape.
6. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: The upper end of the tray (1) is fixedly connected to a limiting frame (11), and the limiting frame (11) is sleeved on the outer circumferential surface of the glass (3).
7. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: A main drainage rod (8) is arranged in the glass (3), and six branch drainage rods (81) are arranged at the lower end of the main drainage rod (8), and the lower ends of the six branch drainage rods (81) are fixed to the inner wall of the glass (3), and the main drainage rod (8) corresponds to the lower end of the pressure equalizing funnel (5).
8. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: The outer circumferential surface of the pressure equalizing funnel (5) is fixedly connected to a support frame (51), and the support frame (51) is connected to the mouth of the glass (3).
9. A polydimethylsiloxane nanofilm solubilizing agent and a preparation method thereof according to claim 1, characterized in that: A connecting plug (52) is fixedly connected to the outer circumferential surface of the pressure equalizing funnel (5), and the connecting plug (52) is engaged with the mouth of the glass (3).
