Preparation method for organic silicon composition
By introducing small molecule hydroxy silicone oil and α-olefin reactions into the silicone composition, an alkyl-modified polysiloxane is formed and silicone resin filler is added, the problem of attenuation of foam suppression performance of existing silicone compositions is solved, and a longer-lasting foam suppression effect and better compatibility is achieved.
Patent Information
- Application Number
- PCT/CN2024/136728
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-10-31
- Filing Date
- 2024-12-04
- Publication Date
- 2025-05-08
AI Technical Summary
The foam suppression properties of the existing silicone compositions are prone to attenuation in the later stage and are difficult to effectively emulsify and disperse in water.
By introducing small molecule hydroxy silicone oil and hydrogen-containing silicone oil to produce a spatial network structure of T-link connected polysiloxane, and react with α-olefin under the action of an acid catalyst to form an alkyl-modified polysiloxane, and finally add silicone resin filler to prepare a silicone composition with an MDT structure.
This method not only improves the rapid defoaming performance of the silicone composition, but also enhances its high and low temperature resistance and shear resistance, has a longer-lasting foam suppression ability, and alkyl modification improves compatibility with the foaming system.
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Figure PCTCN2024136728-FTAPPB-I100001 
Figure PCTCN2024136728-FTAPPB-I100002
Abstract
Description
A method for preparing an organosilicon composition Technical Field
[0001] The present invention relates to a method for preparing an organosilicon composition. The organosilicon defoaming composition belongs to fine chemicals, so the present invention belongs to the technical field of fine chemical preparations. Background Art
[0002] Foaming is a common phenomenon in daily life and production, especially in large-scale industrial production. The generation of large amounts of foam seriously affects the progress of production, such as reducing the efficiency of production equipment, delaying the working time of production personnel, and affecting the quality of products. Methods for eliminating harmful foam can be divided into physical methods and chemical methods. The use of defoaming agents is one of the chemical methods. With the significant increase in industrial production scale and production efficiency, defoaming agents have been more widely promoted and applied. At present, defoaming agents have been widely used in industries such as papermaking, textile printing and dyeing, oil extraction and refining, coatings, emulsion polymerization, sewage treatment, metal cleaning, solid and liquid detergents, etc. Defoaming agents have become an indispensable functional additive in the production process.
[0003] Currently, defoamers on the market are classified by active ingredient into polyethers, silicones, mineral oils, fatty alcohols, and other polymers. Among them, silicone defoamers are widely favored by consumers due to their stable chemical properties, minimal side effects, and strong anti-foaming properties.
[0004] The silicone composition is the core component of silicone defoamers. Its defoaming speed and antifoaming performance directly affect the performance of the final product. The original silicone composition was prepared by polydimethylsiloxane and silicon dioxide through a specific processing technology. For example, the defoamer composition introduced in GB1051687A was prepared by heating polydimethylsiloxane and hydrophilic silicon dioxide, but its antifoaming performance was poor. Therefore, researchers at home and abroad have conducted large-scale research on its performance. For example, DE-OS2925722 uses hydrophobic silicon dioxide instead of hydrophilic silicon dioxide; US-A4145308 introduces (CH3)3SiO 1 / 2and SiO2 units; US4395352 describes an antifoaming agent composition containing a high-viscosity polydimethylsiloxane fluid and finely dispersed hydrophobic particles, which can be used as a defoaming agent by itself or in the form of an emulsion; US3691091 discloses an organosilicon emulsion of an aqueous liquid defoaming agent, wherein the organosilicon is composed of a polydimethylsiloxane fluid, silicon dioxide, and an organosilicon compound or oligomer containing alkoxy and / or silanol groups; EP0163541 discloses a method for preparing an organosilicon defoaming agent by reacting a mixture of components including a preformed polyorganosiloxane polymer with one or more hydroxyl and / or hydrocarbonoxy groups, an organosilicon resin, a filler, and a catalyst to promote the reaction; EP-A-578424 prepares a foam control agent using a polydiorganosiloxane having some side chains with long-chain alkyl groups, each alkyl side chain containing 9 to 35 carbon atoms. The above patents all mention non-crosslinked silicone polymers. Such compositions have poor foam suppression performance in the later stage and are easily attenuated.
[0005] To improve the late-stage antifoaming properties of silicone compositions, EP163541B1, CN102698475A, and CN104274998A describe the reaction of a polysiloxane containing terminal hydroxyl groups with a polysiloxane containing other reactive functional groups under the action of a catalyst to form a branched polysiloxane. This branched polysiloxane is then used in place of standard polysiloxane and mixed with hydrophilic silica. The resulting silicone antifoaming composition exhibits high viscosity and good antifoaming properties, but is difficult to emulsify and disperse in water. US5153258 describes the introduction of lightly crosslinked polysiloxanes to enhance the composition's antifoaming properties. For example, vinyl polysiloxanes crosslink with hydrogen-containing polysiloxanes, or hydroxyl-containing polysiloxanes crosslink with alkyl silicates under the action of a catalyst, but the degree of crosslinking is difficult to control. US5486306 describes a defoamer synthesized directly by reacting hydrogenated polyorganosiloxane with α-olefins. This process is simple to synthesize, but the resulting defoamer has poor defoaming properties and is only suitable for use in laundry detergents. It is prone to silicon spots on fabrics when in contact with it. WO2007137948A1 describes a method of reacting hydrogenated polyorganosiloxane with vinyl polyorganosiloxane and then adding trimethylsiloxy-terminated polydimethylsiloxane for dilution. However, the diluent's contribution to defoaming performance is minimal. Furthermore, the reaction between hydrogenated polyorganosiloxane and vinyl polyorganosiloxane produces high viscosity, making it difficult to control, resulting in a defoamer composition with poor defoaming and anti-foaming properties. Summary of the Invention
[0006] The invention relates to a method for preparing an organosilicon composition. During the preparation process, small-molecule hydroxy silicone oil is introduced to react with some Si-H bonds in hydrogen-containing silicone oil to remove hydrogen, thereby obtaining a polysiloxane with a spatial network structure connected by T-linked segments. The polysiloxane is then reacted with alpha-olefin under the action of an acidic catalyst to obtain an alkyl-modified polysiloxane. Finally, a silicone resin filler dissolved in a solvent is added, and the mixture is kept warm to obtain an alkyl-modified organosilicon composition with an MDT structure. The organosilicon composition not only has low surface tension and chain flexibility, but also can spread rapidly, thereby achieving a rapid defoaming effect. At the same time, the structure has good high and low temperature resistance and shear resistance, and has a more lasting foam suppression ability. At the same time, the introduction of the alkyl group imparts a certain compatibility between the composition and a foaming system, thereby achieving the effect of not affecting the foaming system itself.
[0007] The organosilicon composition of the present invention is composed of the following substances:
[0008] A. Small molecule hydroxy silicone oil
[0009] At least one of the following general structural formulas:
[0010] HO[(CH3)2SiO] m H
[0011] The subscript m is an integer of 20-80, and the amount of the small molecule hydroxy silicone oil is 10-20% of the total mass of the organosilicon composition;
[0012] B. Hydrogen-containing polysiloxane
[0013] At least one of the following general structural formulas:
[0014] Me3SiO(R 1 HSiO) b (R 1 2SiO) c SiMe3
[0015] In the formula, the substituent R 1 The same or different, is an alkyl group with 1 to 4 carbon atoms, specifically selected from methyl, ethyl, n-propyl, n-butyl, isobutyl; preferably R 1 is a methyl group; subscript b is an integer of 10 to 100; subscript c is an integer of 10 to 200; the amount of hydrogen-containing polyorganosiloxane is 30-60% of the total mass of the organosilicon composition;
[0016] C.α-olefins
[0017] The α-olefin is a mixture of any one or more of linear α-olefins, α-aromatic olefins or branched α-olefins, selected from α-octene, α-decene, α-dodecene, α-tetradecene, α-hexadecene, α-octadecene, α-eicosene, a C20-C24 linear α-olefin mixture, a C24-C28 linear α-olefin mixture, α-triacontene, α-methylstyrene, and α-styrene, and can be used alone or in any proportion. The amount of the α-olefin is 20-50% of the total mass of the organosilicon composition.
[0018] D.MQ silicone resin
[0019] The MQ silicone resin is composed of chain segments (CH3)3SiO l / 2 (M unit) and chain SiO 4 / 2 The MQ resin (Q unit) is composed of the following: the molar ratio between the two is (0.4-1.2):1.0, and the amount used accounts for 2-10% of the total mass of the organosilicon composition;
[0020] E. Solvent
[0021] The solvent is used to dissolve the MQ silicone resin in advance and is selected from one or more of dioctyl phthalate, dimethyl phthalate, dibutyl phthalate, tributyl phosphate, dioctyl adipate, dioctyl azelate, and dioctyl sebacate; the amount used accounts for 2-10% of the total mass of the organosilicon composition;
[0022] F. Catalyst 1
[0023] The catalyst 1 is selected from a platinum-alcohol complex, a platinum-olefin complex, a platinum-alkoxide complex, a platinum-ether complex, a platinum-ketone complex, a chloroplatinic acid isopropanol solution, and a platinum-vinyl complex, preferably a chloroplatinic acid isopropanol solution; the amount of the catalyst 1 is 3 to 20 ppm (calculated as platinum) of the total mass of the small molecule hydroxy silicone oil A, the hydrogen-containing polyorganosiloxane B, and the α-olefin C;
[0024] G. Catalyst 2
[0025] The catalyst 2 is selected from sodium hydroxide, potassium hydroxide, cesium hydroxide, tetramethylammonium hydroxide, sodium ethoxide, diethanolamine, triethanolamine, and potassium organosiloxane, preferably potassium hydroxide. The amount of the catalyst 2 is 0.1% to 2% of the total mass of the small molecule hydroxy silicone oil A and the hydrogen-containing polyorganosiloxane B.
[0026] The preparation method of the organosilicon composition of the present invention is as follows:
[0027] (1) Weigh a specified amount of MQ silicone resin and solvent, dissolve and stir evenly to form a mixture M for later use;
[0028] (2) adding small molecule hydroxy silicone oil, hydrogen-containing polyorganosiloxane, and catalyst 2 into a reactor, mixing and heating, and then reacting at 60-120° C. for 2-4 hours to form polysiloxane N;
[0029] (3) adding α-olefin and catalyst 1 to the polysiloxane N obtained in step (2) to continue the reaction, raising the temperature to 60-140° C. and keeping the temperature for 0.5-1.5 hours to obtain terminal alkyl polysiloxane Y;
[0030] (4) The mixture M is further added to the terminal alkyl polysiloxane Y obtained in step (3), and the mixture is kept at 100-160° C. for 1-5 hours, and then cooled to room temperature to obtain the organosilicon composition.
[0031] A method for preparing an organic silicone emulsion using the above-mentioned organic silicone composition is implemented by: mixing the organic silicone composition and an emulsifier, and gradually adding water and a thickener. After mixing evenly, the mixture is passed through mechanical equipment such as a colloid mill and a homogenizer to prepare an oil-in-water organic silicone emulsion.
[0032] The emulsifier is a nonionic surfactant selected from nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, lauric acid polyoxyethylene ether, oleic acid polyoxyethylene ether, sorbitan monostearate, sorbitan monooleate, sorbitan tristearate, sorbitan trioleate, sorbitan monostearate polyoxyethylene ether ester, sorbitan monooleate polyoxyethylene ether ester, sorbitan tristearate polyoxyethylene ether ester, and castor oil polyoxyethylene ether. DETAILED DESCRIPTION
[0033] Example 1
[0034] (1) Weigh 10 g of MQ silicone resin (the molar ratio of M to Q is 0.4:1.0) and 10 g of dioctyl phthalate, dissolve and stir evenly to form a mixture M1 for later use;
[0035] (2) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 20 H, 30g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 10 [(CH3)2SiO] 100 SiMe3 and 0.6 g of potassium hydroxide were added to the reactor, mixed, and heated, and then kept at 60°C for 4 h to form polysiloxane N1.
[0036] (3) adding 40 g of α-hexadecene and 3 ppm of chloroplatinic acid isopropanol solution to the polysiloxane N1 obtained in step (2) to continue the reaction, heating to 100° C. and keeping the temperature for 1.5 h to obtain terminal alkyl polyorganosiloxane Y1;
[0037] (4) The mixture M1 was further added to the terminal alkyl polysiloxane Y1 obtained in step (3), and the mixture was kept at 100° C. for 5 h and cooled to room temperature to obtain the organosilicon composition.
[0038] Example 2
[0039] (1) Weigh 2 g of MQ silicone resin (the molar ratio of M to Q is 0.6:1.0), 8 g of a mixture of dimethyl phthalate and dibutyl phthalate, dissolve and stir them evenly to form a mixture M2 for later use;
[0040] (2) 20g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 40 H, 40g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 50 [(CH3)(C2H5)SiO] 50 SiMe3 and 0.06 g of sodium hydroxide were added to the reactor, mixed and heated, and kept at 80°C for 3 h to form polysiloxane N2;
[0041] (3) adding 30 g of a mixture of α-dodecene and α-tetradecene and 5 ppm of a platinum-alcohol complex to the polysiloxane N2 obtained in step (2) and continuing the reaction, heating to 60° C. and keeping the temperature for 1 h to obtain an alkyl-terminated polyorganosiloxane Y2;
[0042] (4) The mixture M2 is further added to the terminal alkyl polysiloxane Y2 obtained in step (3), and the mixture is kept at 140° C. for 4 h and cooled to room temperature to obtain the organosilicon composition.
[0043] Example 3
[0044] (1) Weigh 2 g of MQ silicone resin (the molar ratio of M to Q is 0.8:1.0) and 8 g of tributyl phosphate, dissolve and stir evenly to form a mixture M3 for later use;
[0045] (2) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 60 H, 60g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 80 [(CH3)(C4H9)SiO] 200 SiMe3 and 0.7 g of diethanolamine were added to the reactor, mixed, and heated, and then kept at 100°C for 3 h to form polysiloxane N3;
[0046] (3) adding 20 g of a mixture of α-octene and α-decene and 10 ppm of a platinum-olefin complex to the polysiloxane N3 obtained in step (2) and continuing the reaction, heating to 80° C. and keeping the temperature for 1.5 h to obtain an alkyl-terminated polyorganosiloxane Y3;
[0047] (4) The mixture M3 was further added to the terminal alkyl polysiloxane Y3 obtained in step (3), and the mixture was kept at 130° C. for 2 h, and then cooled to room temperature to obtain the organosilicon composition.
[0048] Example 4
[0049] (1) Weigh 7 g of MQ silicone resin (the molar ratio of M to Q is 1.0:1.0), 8 g of a mixture of dioctyl adipate and dioctyl azelate, dissolve and stir evenly to form a mixture M4 for later use;
[0050] (2) 15g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 80 H, 40g hydrogen-containing polyorganosiloxane Me3SiO[(C2H5)HSiO] 20 [(CH3)2SiO] 10 SiMe3 and 0.3 g of potassium organosiloxane were added to the reactor, mixed and heated, and kept at 120°C for 2 h to form polysiloxane N4;
[0051] (3) adding 30 g of a mixture of α-methylstyrene and α-styrene and 15 ppm of a platinum-alkoxide complex to the polysiloxane N4 obtained in step (2) and continuing the reaction, heating to 100° C. and keeping the temperature for 1.5 h to obtain an alkyl-terminated polyorganosiloxane Y4;
[0052] (4) The mixture M4 was further added to the terminal alkyl polysiloxane Y4 obtained in step (3), and the mixture was kept at 160° C. for 1 h and cooled to room temperature to obtain the organosilicon composition.
[0053] Example 5
[0054] (1) Weigh 5 g of MQ silicone resin (the molar ratio of M to Q is 1.2:1.0) and 5 g of dioctyl sebacate, dissolve and stir evenly to form a mixture M5 for later use;
[0055] (2) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 30 H, 50g hydrogen-containing polysiloxane Me3SiO[(C2H5)HSiO] 50 [(C2H5)2SiO] 100 SiMe3 and 0.6 g of tetramethylammonium hydroxide were added to the reactor, mixed and heated, and kept at 110°C for 3 h to form polysiloxane N5;
[0056] (3) adding 30 g of a C24-C28 linear α-olefin mixture and 20 ppm of a platinum-vinyl complex to the polysiloxane N5 obtained in step (2) and continuing the reaction, heating to 120° C. and keeping the temperature for 1 hour to obtain an alkyl-terminated polyorganosiloxane Y5;
[0057] (4) The mixture M5 was further added to the terminal alkyl polysiloxane Y5 obtained in step (3), and the mixture was kept at 150° C. for 3 h and cooled to room temperature to obtain the organosilicon composition.
[0058] Example 6
[0059] (1) Weigh 4 g of MQ silicone resin (the molar ratio of M to Q is 0.5:1.0) and 6 g of dioctyl adipate, dissolve and stir evenly to form a mixture M6 for later use;
[0060] (2) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 50 H, 30g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 100 [(CH3)2SiO] 30 SiMe3 and 0.6 g of cesium hydroxide were added to the reactor, mixed and heated, and kept at 90°C for 3 h to form polysiloxane N6;
[0061] (3) adding 50 g of α-triacontene and 6 ppm of platinum-ketone complex to the polysiloxane N6 obtained in step (2) and continuing the reaction, heating to 140° C. and keeping the temperature for 0.5 h to obtain terminal alkyl polyorganosiloxane Y6;
[0062] (4) The mixture M6 was further added to the terminal alkyl polysiloxane Y6 obtained in step (3), and the mixture was kept at 130° C. for 2 h and cooled to room temperature to obtain the organosilicon composition.
[0063] Comparative Example 1 - MQ silicone resin not pre-dissolved
[0064] (1) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 20 H, 30g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 10 [(CH3)2SiO] 100 SiMe3 and 0.6 g of potassium hydroxide were added to the reactor, mixed, and heated, and then kept at 60°C for 4 h to form polysiloxane N1.
[0065] (2) adding 40 g of α-hexadecene and 3 ppm of chloroplatinic acid isopropanol solution to the polysiloxane N1 obtained in step (1) to continue the reaction, heating to 100° C. and keeping the temperature for 1.5 h to obtain terminal alkyl polyorganosiloxane Y1;
[0066] (3) 10 g of MQ silicone resin (the molar ratio of M to Q is 0.4:1.0) and 10 g of diisooctyl phthalate were added to the terminal alkyl polysiloxane Y1 obtained in step (2), and the mixture was kept at 100° C. for 5 h and cooled to room temperature to obtain an organosilicon composition.
[0067] Comparative Example 2 - Solvent Removal
[0068] (1) 20g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 40 H, 40g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 50 [(CH3)(C2H5)SiO] 50 SiMe3 and 0.06 g of sodium hydroxide were added to the reactor, mixed and heated, and kept at 80°C for 3 h to form polysiloxane N2;
[0069] (2) adding 30 g of a mixture of α-dodecene and α-tetradecene and 5 ppm of a platinum-alcohol complex to the polysiloxane N2 obtained in step (1) and continuing the reaction, heating to 60° C. and keeping the temperature for 1 hour to obtain an alkyl-terminated polyorganosiloxane Y2;
[0070] (3) 10 g of MQ silicone resin (the molar ratio of M to Q is 0.6:1.0) was further added to the terminal alkyl polysiloxane Y2 obtained in step (2), and the mixture was kept at 140° C. for 4 h and cooled to room temperature to obtain an organosilicon composition.
[0071] Comparative Example 3-Polymer Hydroxyl Silicone Oil
[0072] (1) Weigh 2 g of MQ silicone resin (the molar ratio of M to Q is 0.8:1.0) and 8 g of tributyl phosphate, dissolve and stir evenly to form a mixture M3 for later use;
[0073] (2) 10g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 200 H, 60g hydrogen-containing polysiloxane Me3SiO[(CH3)HSiO] 80 [(CH3)(C4H9)SiO] 200 SiMe3 and 0.7 g of diethanolamine were added to the reactor, mixed, and heated, and then kept at 100°C for 3 h to form polysiloxane N7;
[0074] (3) adding 20 g of a mixture of α-octene and α-decene and 10 ppm of a platinum-olefin complex to the polysiloxane N7 obtained in step (2) and continuing the reaction, heating to 80° C. and keeping the temperature for 1.5 h to obtain an alkyl-terminated polyorganosiloxane Y7;
[0075] (4) The mixture M3 was further added to the terminal alkyl polysiloxane Y7 obtained in step (3), and the mixture was kept at 130° C. for 2 h and cooled to room temperature to obtain the organosilicon composition.
[0076] Comparative Example 4-hydroxy silicone oil excess
[0077] (1) Weigh 2 g of MQ silicone resin (the molar ratio of M to Q is 0.8:1.0) and 8 g of tributyl phosphate, dissolve and stir evenly to form a mixture M3 for later use;
[0078] (2) 60g of small molecule hydroxy silicone oil HO[(CH3)2SiO] 200 H, 10g hydrogen-containing polyorganosiloxane Me3SiO[(CH3)HSiO] 10 [(CH3)(C4H9)SiO] 200 SiMe3 and 0.7 g of diethanolamine were added to the reactor, mixed, and heated, and then kept at 100°C for 3 h to form polysiloxane N8;
[0079] (3) adding 20 g of a mixture of α-octene and α-decene and 10 ppm of a platinum-olefin complex to the polysiloxane N8 obtained in step (2) and continuing the reaction, heating to 80° C. and keeping the temperature for 1.5 h to obtain an alkyl-terminated polyorganosiloxane Y8;
[0080] (4) The mixture M3 was further added to the terminal alkyl polysiloxane Y8 obtained in step (3), and the mixture was kept at 130° C. for 2 h and cooled to room temperature to obtain the organosilicon composition.
[0081] Examples 7 to 16
[0082] According to the well-known emulsion defoamer preparation technology in the technical field, the silicone compositions of Examples 1 to 6 and Comparative Examples 1 to 4 were used to prepare emulsion defoamers K1 to K6 and L1 to L4, respectively. The preparation methods are as follows:
[0083] 100 g of a silicone defoaming composition, 30 g of sorbitan monostearate (Span 60), and 20 g of polyoxyethylene (20) sorbitan monostearate were mixed at 70° C. for 10 minutes, and 500 g of water were added in batches. 2 g of polyacrylic acid was then added to the mixture, and the pH was adjusted to 6-7 with 10% NaOH, followed by the addition of 345 g of water. Finally, the emulsion was homogenized with a high-pressure homogenizer, and the pH was again adjusted to 6-7 with 10% NaOH, followed by the addition of 3 g of an isothiazolinone-based preservative, thereby obtaining emulsion defoamers K1-K6 and L1-L4.
[0084] Defoamer performance test
[0085] Textile Slurry Testing
[0086] Test method: Add 160ml of prepared textile pulp to a 250ml stoppered graduated cylinder, then add 0.05g of emulsion defoamer. Shake the flask up and down at a speed of 2 seconds per shake. Shake each flask 10 times and record the defoaming time for each group. The shorter the defoaming time in each group, the better the defoaming and antifoaming performance of the defoamer sample.
[0087] Table 3 Slurry system test
[0088] It can be seen that in the textile slurry test, the shake flask defoaming times of the emulsion defoamers K1-K6 prepared using Examples 1-6 were all shorter than those of the emulsion defoamers L1-L5 prepared using Comparative Examples 1-4. Therefore, the organosilicon composition has excellent defoaming and anti-foaming properties in the textile slurry system, as well as late-stage anti-fading performance.
[0089] Table 3 Slurry system test
[0090] As can be seen from Table 3, the liquid defoamers G1 to G7 prepared using the organosilicon defoaming compositions prepared in Examples 7 to 13 have better defoaming and anti-foaming performance in textile slurry than the liquid defoamers YG1 to YG5 prepared using the organosilicon defoaming compositions of Comparative Examples 5 to 9, and have good anti-attenuation performance in the later stage.
Claims
1. A method for preparing an organosilicon composition, characterized in that: It is composed of the following components: A. Small molecule hydroxy silicone oil At least one of the general structural formulas is as follows: HO[(CH3)2SiO] m H The subscript m is an integer of 20-80, and the amount of the small molecule hydroxy silicone oil is 10-20% of the total mass of the organic silicon composition; B. Hydrogen-containing polysiloxane At least one of the following general structural formulas: Me3SiO(R 1 HSiO) b (R 1 2SiO) c SiMe3 In the formula, the substituent R 1 The same or different, is an alkyl group with 1 to 4 carbon atoms, specifically selected from methyl, ethyl, n-propyl, n-butyl, isobutyl; subscript b is an integer of 10 to 100; subscript c is an integer of 10 to 200; the amount of hydrogen-containing polysiloxane is 30-60% of the total mass of the silicone composition; C. α-olefins The α-olefin is a mixture of any one or more of linear α-olefins, α-aromatic olefins or branched α-olefins, selected from α-octene, α-decene, α-dodecene, α-tetradecene, α-hexadecene, α-octadecene, α-eicosene, a C20-C24 linear α-olefin mixture, a C24-C28 linear α-olefin mixture, α-triacontene, α-methylstyrene, α-styrene, and can be used alone or in any proportion; the amount of the α-olefin is 20-50% of the total mass of the organosilicon composition; D. MQ silicone resin The MQ silicone resin is composed of chain segments (CH3)3SiO l / 2 (M unit) and chain SiO 4 / 2 The MQ resin composed of (Q unit) and the molar ratio between the two is (0.4-1.2):1.0, and the amount used accounts for 2-10% of the total mass of the organosilicon composition; E. Solvent The solvent is used to dissolve the MQ silicone resin in advance, and is selected from one or more of diisooctyl phthalate, dimethyl phthalate, dibutyl phthalate, tributyl phosphate, dioctyl adipate, dioctyl azelate, and dioctyl sebacate; the amount used accounts for 2-10% of the total mass of the organosilicon composition; F. Catalyst 1 The catalyst 1 is selected from platinum-alcohol complex, platinum-olefin complex, platinum-alkoxide complex, platinum-ether complex, platinum-ketone complex, chloroplatinic acid isopropanol solution, platinum-vinyl complex; the amount of the catalyst 1 is 3-20 ppm (in terms of platinum) of the total mass of small molecule hydroxy silicone oil A, hydrogen-containing polyorganosiloxane B, and α-olefin C; G. Catalyst 2 The catalyst 2 is selected from sodium hydroxide, potassium hydroxide, cesium hydroxide, tetramethylammonium hydroxide, sodium ethoxide, diethanolamine, triethanolamine, potassium organosiloxane; the amount of the catalyst 2 is 0.1%-2% of the total mass of the small molecule hydroxy silicone oil A and the hydrogen-containing polyorganosiloxane B; The preparation method of the organosilicon composition is as follows: (1) Weighing a specified amount of MQ silicone resin and solvent, dissolving and stirring them evenly to form a mixture M for later use; (2) adding small molecule hydroxy silicone oil, hydrogen-containing polyorganosiloxane, and catalyst 2 into a reactor, mixing and heating, and reacting at 60-120° C. for 2-4 hours to form polysiloxane N; (3) adding α-olefin and catalyst 1 to the polysiloxane N obtained in step (2) to continue the reaction, raising the temperature to 60-140° C., and keeping the temperature for 0.5-1.5 h to obtain terminal alkyl polysiloxane Y; (4) Add the mixture M to the terminal alkyl polysiloxane Y obtained in step (3), keep the mixture at 100-160° C. for 1-5 hours, and cool to room temperature to obtain the organosilicon composition.
2. The method for preparing a silicone composition according to claim 1, characterized in that: R 1 It is methyl.
3. The method for preparing a silicone composition according to claim 1, characterized in that: The catalyst 1 is a chloroplatinic acid isopropanol solution.
4. The method for preparing a silicone composition according to claim 1, characterized in that: The catalyst 2 is potassium hydroxide.
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