An organosilicon composition and a preparation method thereof

Abstract

The present invention provides a silicone composition and a preparation method thereof. A reaction is carried out on a hydrogen-containing polyorganosiloxane, a fluorinated acrylate and a hydroxyalkyl acrylate under the action of a chloroplatinic acid catalyst to obtain a mixture. The introduction of the fluorinated acrylate improves the defoaming and antifoaming performance, and the introduction of the hydroxyalkyl acrylate improves the compatibility of the composition; further, the mixture is reacted with a coupling agent and silica under the action of a base catalyst to form a network structure. The active groups in the silane coupling agent react with the surface hydroxyl groups of the silica and the surface hydroxyl groups of the mixture, which not only improves the dispersibility of the silica in the system, but also can disperse and fix the silica in the system, avoiding the problem of attenuation of the defoaming and antifoaming performance caused by the agglomeration of the silica in the later stage of defoaming; finally, MQ silicone resin and silicone polyether are added to further improve the defoaming and antifoaming performance and at the same time improve the dispersibility of the silicone composition, which is helpful for the later emulsification process. The finally formed silicone composition has a very fast defoaming rate and good antifoaming performance in anionic and nonionic systems, and can be widely used to eliminate harmful foams in industrial production.

Description

Technical Field

[0001] The present invention relates to a silicone composition and a preparation method thereof. Since the silicone composition belongs to fine chemicals, the present invention belongs to the technical field of fine chemical preparations. Background Art

[0002] Foams are common phenomena in life and work. However, in industrial production, foams sometimes cause great harm, such as reducing the working efficiency of machines, delaying labor time, and affecting the quality of products. The methods for eliminating harmful foams mainly include physical methods and chemical methods. Defoaming with defoamers is one of the chemical methods. With the substantial increase in the production scale and production efficiency of industrial enterprises, defoaming with defoamers has been more widely applied. At present, various defoamers are widely used in industries such as the paper industry, textile printing and dyeing, oil exploration and refining, coatings, emulsion polymerization, sewage treatment, and metal cleaning.

[0003] According to different defoaming active substances, defoamers are divided into several main types such as mineral oil type, polyether type, and silicone type. Compared with other defoamers, silicone defoamers have stable chemical properties and small side effects. At the same time, they also have good defoaming ability and long-lasting foam suppression ability even at very low dosages, so they are highly favored. The silicone composition is the core of the silicone defoamer, and its defoaming speed and foam suppression performance directly affect the performance of the final product.

[0004] For silicone defoamers, improving the defoaming and antifoaming performance of defoaming active substances is the main direction of improving silicone defoamers. EP163541B1 introduced that polysiloxanes with terminal hydroxyl groups react with polyorganosiloxanes containing other active functional groups under the action of a catalyst to form branched polyorganosiloxanes, but their viscosity is relatively high and it is difficult to emulsify and disperse them later; US5153258 introduced that introducing lightly crosslinked polyorganosiloxanes into the system can improve the defoaming and antifoaming performance of the composition. For example, vinyl-containing polyorganosiloxanes and hydrogen-containing polyorganosiloxanes, hydroxyl-containing polyorganosiloxanes and alkyl silicate esters undergo crosslinking reactions under the action of a catalyst, but the degree of crosslinking is difficult to control; in CN102337031B, after polysiloxanes react with coupling agents under an alkaline catalyst, a part of silica is added to adjust the crosslinking degree of polysiloxanes and coupling agents; then silicone resin is added and the reaction continues; then the remaining silica and polyether-modified polysiloxanes are added to obtain a silicone composition with low viscosity; the above patents all obtain defoaming active substances through the reaction of different types of polysiloxanes. In order to further improve the defoaming and antifoaming performance, other patents began to introduce fluorine-containing substances to improve the defoaming and antifoaming performance. CN115477758 mixed and reacted hydrogen-containing silicone oil with two ends, polyether terminated with diallyl, multifunctional monomers and a catalyst to obtain a branched silicon-containing precursor capped with hydrogen-containing silicone oil with two ends, and then continued to add fluorine-containing vinyl monomers, allyl alcohol polyether and a catalyst to obtain a branched fluorine-containing defoamer. Due to the introduction of fluorine-containing monomers, the defoaming and antifoaming performance has been significantly improved, but the structure of the fluorine-containing defoamer is complex and the synthesis process is relatively difficult to control; CN107840962A grafted alkyl acrylate, fluorine-containing acrylate and allyl-terminated polyether onto hydrogen-containing silicone oil in sequence to prepare a silicone defoamer for water-based color paste with better defoaming and antifoaming performance, but its compatibility needs to be improved. Summary of the Invention

[0005] The present invention provides a silicone composition and a preparation method thereof. A hydrogen-containing polyorganosiloxane, a fluorinated acrylate, and a hydroxyalkyl acrylate are reacted under the action of a chloroplatinic acid catalyst to obtain a mixture. The introduction of the fluorinated acrylate improves the defoaming and antifoaming performance, and the introduction of the hydroxyalkyl acrylate improves the compatibility of the composition. Further, the mixture is reacted with a coupling agent and silica under the action of a base catalyst to form a network structure. The active groups in the silane coupling agent react with the surface hydroxyl groups of silica and the surface hydroxyl groups of the mixture, which not only improves the dispersion of silica in the system, but also can disperse and fix silica in the system, avoiding the problem of attenuation of defoaming and antifoaming performance caused by silica agglomeration in the later stage of defoaming. Finally, MQ silicone resin and silicone polyether are added to further improve the defoaming and antifoaming performance and the dispersion of the silicone composition, which is helpful for later emulsification processing. The finally formed silicone composition has a very fast defoaming speed and good antifoaming performance in anionic and nonionic systems, and can be widely used to eliminate harmful foams in industrial production.

[0006] Technical solution

[0007] A silicone composition, characterized in that it is composed of the following substances:

[0008] A. Hydrogen-containing polyorganosiloxane

[0009] A hydrogen-containing polyorganosiloxane with the following general structural formula:

[0010] H a Me 3-a SiO(SiMeHO) b (SiMe2O) c SiMe 3-a H a

[0011] Wherein Me is methyl, subscript a is 1 or 2, subscript b is an integer from 1 to 40, subscript c is an integer from 20 to 200, and the dosage is 20 - 50% of the total mass of the silicone composition.

[0012] B. Hydroxyalkyl acrylate

[0013] A hydroxyalkyl acrylate with the following general structural formula:

[0014] In the molecular structure, R is hydrogen; R 0 is selected from 1-hydroxyethyl, 2-hydroxyethyl, 1-hydroxypropyl, 2-hydroxypropyl, 3-hydroxypropyl, 1-hydroxyisopropyl, 2-hydroxyisopropyl, 3-hydroxyisopropyl, 1-hydroxybutyl, 2-hydroxybutyl, 3-hydroxybutyl or 4-hydroxybutyl, and the dosage is 15 - 25% of the total mass of the silicone composition.

[0015] C. Fluoroacrylate

[0016] The fluoroacrylate is selected from trifluoroethyl acrylate, trifluoroethyl methacrylate, hexafluorobutyl acrylate, hexafluorobutyl methacrylate, octafluoropentyl acrylate, octafluoropentyl methacrylate, and the dosage is 15 - 25% of the total mass of the silicone composition.

[0017] D. Catalyst I

[0018] Catalyst I is an isopropanol solution of chloroplatinic acid, and the dosage is 0.01% - 0.2% of the total mass of the silicone composition.

[0019] E. Coupling agent

[0020] The structural formula of the coupling agent is

[0021] (Y(CH2) n ) P Si(OR 1 ) q

[0022] Among them, R 1 is selected from methyl, ethyl, propyl, butyl; p is 0 or 1, q is an integer from 1 to 4, p + q = 4, n is an integer from 0 to 16; Y is selected from methyl, amino, methacryloyloxy, epoxy, vinyl, mercapto, cyano; specifically selected from: 3 - methacryloxypropyltrimethoxysilane, vinyltriethoxysilane, 3 - aminopropyltrimethoxysilane, 12 - aminododecyltrimethoxysilane, 3 - glycidoxypropyltrimethoxysilane, dimethyldiethoxysilane, methyltriethoxysilane, methyltriacetoxysilane, tetraethyl orthosilicate, dimethyldiethoxysiloxane, ethyltriethoxysilane, propyltrimethoxysilane. The dosage is 1 - 4% of the total mass of the silicone composition.

[0023] F. Silicon dioxide

[0024] The silicon dioxide is hydrophobic silicon dioxide, and the dosage is 2 - 10% of the total mass of the silicone composition.

[0025] H. MQ silicone resin

[0026] The MQ silicone resin is an MQ resin composed of the link (CH3)3SiO l / 2 (M unit) and the link SiO 4 / 2 (Q unit), and the molar ratio between the two is (0.4 - 1.2):1.0, and the dosage is 3 - 10% of the total mass of the silicone composition.

[0027] I. Catalyst II

[0028] Catalyst II is a basic catalyst and is selected from NaOH, KOH, potassium silanolate, sodium silanolate, sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, b-hydroxyethyltrimethylamine, and tetramethylammonium hydroxide. The dosage is 0.5-2% of the total mass of the organosilicon composition.

[0029] J. Polyether-modified polysiloxane

[0030] The structural formula of the polyether-modified polysiloxane is as follows:

[0031] MD x (CH3GSiO) y M

[0032] Among them, M is the link (CH3)3SiO l / 2 , D is the link (CH3)2SiO 2 / 2 ; G is a polyether group, represented by the following structural general formula: –(CH2) z (EO) g (PO) h R 2 , where R 2 is -H or -CH3 or -COCH3; the subscripts x , y , z , g , h are the degrees of polymerization, x is an integer from 10 to 500; y is an integer from 1 to 50; z is an integer from 3 to 6; g is an integer from 1 to 40; h is an integer from 0 to 60. The dosage is 2-10% of the total mass of the organosilicon composition.

[0033] The preparation method of the organosilicon composition of the present invention is as follows:

[0034] Step 1: Add the hydrogen-containing polyorganosiloxane, fluorinated acrylate, and hydroxyalkyl acrylate to a reaction vessel, dropwise add Catalyst I, and react at 80-130°C for 1-4 h to obtain a mixture M;

[0035] Step 2: After the reaction is completed, continue to add the coupling agent and silica to the reaction vessel for mixing, dropwise add the basic catalyst, and react at 80-150°C for 1-4 h to obtain a mixture N;

[0036] Step 3: Finally, add the MQ resin and the polyether-modified polysiloxane, and keep warm at 80-150°C for 1-4 h to obtain the organosilicon composition. Specific implementation method

[0037] Example 1

[0038] Step 1: Add 20 g of HMe2SiO(HSiMeO)(SiMe2O)SiMe2H, 25 g of trifluoroethyl acrylate, and 25 g of 2-hydroxyethyl acrylate into a reaction vessel, dropwise add 0.2 g of isopropyl alcohol solution of chloroplatinic acid, and react at 80 °C for 4 h to obtain mixture M1; 200 SiMe2H, 25 g of trifluoroethyl acrylate and 25 g of 2-hydroxyethyl acrylate are added to the reaction vessel, 0.2 g of isopropyl alcohol solution of chloroplatinic acid is added dropwise, and the reaction is carried out at 80 °C for 4 h to obtain mixture M1;

[0039] Step 2: After the reaction is completed, continue to add 4 g of 3-methacryloxypropyltrimethoxysilane and 10 g of hydrophobic silica into the reaction vessel for mixing, dropwise add 1 g of NaOH, and react at 80 °C for 4 h to obtain mixture N1;

[0040] Step 3: Finally, add 10 g of MQ silicone resin (molar ratio of M to Q is 0.4:1.0) and 4.8 g of polyether-modified polysiloxane (R2 is H; x is 10, y is 50, z is 3, g is 1, h is 0), and keep the temperature at 80 °C for 4 h to obtain the silicone composition.

[0041] Example 2

[0042] Step 1: Add 35 g of H2MeSiO(HSiMeO)(SiMe2O)SiMeH2, 20 g of methyltrifluoroethyl acrylate, and 20 g of 2-hydroxypropyl acrylate into a reaction vessel, dropwise add 0.01 g of isopropyl alcohol solution of chloroplatinic acid, and react at 90 °C for 3 h to obtain mixture M2; 40 (SiMe2O) 20 SiMeH2, 20 g of methyltrifluoroethyl acrylate and 20 g of 2-hydroxypropyl acrylate are added to the reaction vessel, 0.01 g of isopropyl alcohol solution of chloroplatinic acid is added dropwise, and the reaction is carried out at 90 °C for 3 h to obtain mixture M2;

[0043] Step 2: After the reaction is completed, continue to add 2 g of vinyltriethoxysilane and 8 g of hydrophobic silica into the reaction vessel for mixing, dropwise add 2 g of KOH, and react at 90 °C for 3 h to obtain mixture N2;

[0044] Step 3: Finally, add 8 g of MQ silicone resin (molar ratio of M to Q is 0.5:1.0) and 4.99 g of polyether-modified polysiloxane (R2 is CH3; x is 50, y is 40, z is 4, g is 5, h is 6), and keep the temperature at 90 °C for 3 h to obtain the silicone composition.

[0045] Example 3

[0046] Step 1: Add 45 g of H2MeSiO(HSiMeO)5(SiMe2O)SiMeH2, 15 g of hexafluorobutyl acrylate, and 15 g of 2-hydroxybutyl acrylate into a reaction vessel, dropwise add 0.1 g of isopropyl alcohol solution of chloroplatinic acid, and react at 100 °C for 2 h to obtain mixture M3; 50 SiMeH2, 15 g of hexafluorobutyl acrylate and 15 g of 2-hydroxybutyl acrylate are added to the reaction vessel, 0.1 g of isopropyl alcohol solution of chloroplatinic acid is added dropwise, and the reaction is carried out at 100 °C for 2 h to obtain mixture M3;

[0047] Step 2: After the reaction is completed, continue to add 1 g of 3-aminopropyltrimethoxysilane and 2 g of hydrophobic silica into the reaction vessel for mixing, then dropwise add 2 g of potassium silanolate, and react at 100 °C for 2 h to obtain mixture N3;

[0048] Step 3: Finally, add 10 g of MQ silicone resin (the molar ratio of M to Q is 0.6:1.0) and 9.9 g of polyether-modified polysiloxane (R2 is COCH3; x is 100, y is 30, z is 5, g is 10, h is 12), and keep the temperature at 100 °C for 2 h to obtain the silicone composition.

[0049] Example 4

[0050] Step 1: Add 50 g of HMe2SiO(HSiMeO) 10 (SiMe2O) 100 SiMeH2, 17.4 g of hexafluorobutyl methacrylate and 19 g of hydroxyisopropyl acrylate into the reaction vessel, dropwise add 0.1 g of isopropyl alcohol solution of chloroplatinic acid, and react at 110 °C for 1 h to obtain mixture M4;

[0051] Step 2: After the reaction is completed, continue to add 3 g of dimethyldiethoxysilane and 5 g of hydrophobic silica into the reaction vessel for mixing, then dropwise add 0.5 g of sodium ethoxide, and react at 110 °C for 2 h to obtain mixture N4;

[0052] Step 3: Finally, add 3 g of MQ silicone resin (the molar ratio of M to Q is 0.8:1.0) and 2 g of polyether-modified polysiloxane (R2 is H; x is 200, y is 20, z is 6, g is 20, h is 20), and keep the temperature at 110 °C for 2 h to obtain the silicone composition.

[0053] Example 5

[0054] Step 1: Add 25 g of H2MeSiO(HSiMeO) 20 (SiMe2O) 150 SiMe2H, 23.35 g of octafluoropentyl acrylate and 24 g of hydroxypropyl acrylate into the reaction vessel, dropwise add 0.15 g of isopropyl alcohol solution of chloroplatinic acid, and react at 120 °C for 1 h to obtain mixture M5;

[0055] Step 2: After the reaction is completed, continue to add 3.5 g of tetraethyl orthosilicate and 8 g of hydrophobic silica into the reaction vessel for mixing, then dropwise add 1 g of potassium methoxide, and react at 120 °C for 2 h to obtain mixture N5;

[0056] Step 3: Finally, add 5 g of MQ silicone resin (molar ratio of M to Q is 1.0:1.0) and 10 g of polyether-modified polysiloxane (R2 is CH3; x is 300, y is 10, z is 3, g is 30, h is 40), and keep the temperature at 120 °C for 2 h to obtain the silicone composition.

[0057] Example 6

[0058] Step 1: Add 30 g of HMe2SiO(HSiMeO) 30 (SiMe2O) 80 SiMe2H, 24 g of octafluoropentyl methacrylate, and 25 g of hydroxybutyl acrylate into the reaction vessel, dropwise add 0.2 g of isopropyl alcohol solution of chloroplatinic acid, and react at 130 °C for 1 h to obtain mixture M6;

[0059] Step 2: After the reaction is completed, continue to add 3 g of methyltriacetoxysilane and 3.8 g of hydrophobic silica to the reaction vessel for mixing, dropwise add 2 g of tetramethylammonium hydroxide, and react at 130 °C for 1 h to obtain mixture N6;

[0060] Step 3: Finally, add 7 g of MQ silicone resin (molar ratio of M to Q is 1.2:1.0) and 5 g of polyether-modified polysiloxane (R2 is CH3; x is 400, y is 5, z is 4, g is 40, h is 60), and keep the temperature at 130 °C for 1 h to obtain the silicone composition.

[0061] Example 7

[0062] Step 1: Add 22 g of H2MeSiO(SiMeHO) 25 (SiMe2O) 120 SiMeH2, 25 g of hexafluorobutyl acrylate, and 25 g of hydroxyethyl acrylate into the reaction vessel, dropwise add 0.05 g of isopropyl alcohol solution of chloroplatinic acid, and react at 105 °C for 2 h to obtain mixture M7;

[0063] Step 2: After the reaction is completed, continue to add 3.2 g of ethyltriethoxysilane and 6.5 g of hydrophobic silica to the reaction vessel for mixing, dropwise add 1.5 g of β-hydroxyethyltrimethylamine, and react at 150 °C for 1 h to obtain mixture N7;

[0064] Step 3: Finally, add 8.75 g of MQ silicone resin (molar ratio of M to Q is 1.1:1.0) and 8 g of polyether-modified polysiloxane (R2 is H; x is 500, y is 1, z is 5, g is 15, h is 30), and keep the temperature at 150 °C for 1 h to obtain the silicone composition.

[0065] Comparative Example 1

[0066] Step 1: Add 20 g of HMe2SiO(HSiMeO)(SiMe2O)SiMe2H and 50 g of trifluoroethyl acrylate into a reaction vessel, dropwise add 0.2 g of isopropyl alcohol solution of chloroplatinic acid, and react at 80 °C for 4 h to obtain mixture M8; 200

[0067] Step 2: After the reaction is completed, continue to add 4 g of 3-methacryloxypropyltrimethoxysilane and 10 g of hydrophobic silica into the reaction vessel for mixing, dropwise add 1 g of NaOH, and react at 80 °C for 4 h to obtain mixture N8;

[0068] Step 3: Finally, add 10 g of MQ silicone resin (molar ratio of M to Q is 0.4:1.0) and 4.8 g of polyether-modified polysiloxane (R2 is H; x is 10, y is 50, z is 3, g is 1, h is 0), and keep warm at 80 °C for 4 h to obtain the organosilicon composition.Comparative Example 2

[0069] Step 1: Add 35 g of H2MeSiO(HSiMeO)(SiMe2O)SiMeH2 and 40 g of hydroxypropyl acrylate into a reaction vessel, dropwise add 0.01 g of isopropyl alcohol solution of chloroplatinic acid, and react at 90 °C for 3 h to obtain mixture M9; 40 (SiMe2O) 20

[0070] Step 2: After the reaction is completed, continue to add 2 g of vinyltriethoxysilane and 8 g of hydrophobic silica into the reaction vessel for mixing, dropwise add 2 g of KOH, and react at 90 °C for 3 h to obtain mixture N9;

[0071] Step 3: Finally, add 8 g of MQ silicone resin (molar ratio of M to Q is 0.5:1.0) and 4.99 g of polyether-modified polysiloxane (R2 is CH3; x is 50, y is 40, z is 4, g is 5, h is 6), and keep warm at 90 °C for 3 h to obtain the organosilicon composition.Comparative Example 3

[0072] Step 1: Add 45 g of H2MeSiO(HSiMeO)5(SiMe2O)SiMeH2, 15 g of hexafluorobutyl acrylate and 15 g of hydroxybutyl acrylate into a reaction vessel, dropwise add 0.1 g of isopropyl alcohol solution of chloroplatinic acid, and react at 100 °C for 2 h to obtain mixture M3; 50

[0073] Step 2: After the reaction is completed, continue to add 3 g of hydrophobic silica into the reaction vessel for mixing, dropwise add 2 g of potassium silanolate, and react at 100 °C for 2 h to obtain mixture N10;

[0074] Step 3: Finally, add 10 g of MQ silicone resin (the molar ratio of M to Q is 0.6:1.0) and 9.9 g of polyether-modified polysiloxane (R2 is COCH3; x is 100, y is 30, z is 5, g is 10, h is 12), and keep it at 100 °C for 2 h to obtain the silicone composition. Comparative Example 4

[0075] Step 1: Add 50 g of HMe2SiO(HSiMeO) 10 (SiMe2O) 100 SiMeH2, 17.4 g of hexafluorobutyl methacrylate, and 19 g of hydroxyisopropyl acrylate into the reaction vessel, dropwise add 0.1 g of isopropyl alcohol solution of chloroplatinic acid, and react at 110 °C for 1 h to obtain mixture M4;

[0076] Step 2: After the reaction is completed, continue to add 8 g of dimethyldiethoxysilane to the reaction vessel for mixing, dropwise add 0.5 g of sodium ethoxide, and react at 110 °C for 2 h to obtain mixture N11;

[0077] Step 3: Finally, add 3 g of MQ silicone resin (the molar ratio of M to Q is 0.8:1.0) and 2 g of polyether-modified polysiloxane (R2 is H; x is 200, y is 20, z is 6, g is 20, h is 20), and keep it at 110 °C for 2 h to obtain the silicone composition. Comparative Example 5

[0078] Step 1: Add 25 g of H2MeSiO(HSiMeO) 20 (SiMe2O) 150 SiMe2H, 23.35 g of octafluoropentyl acrylate, and 24 g of hydroxypropyl acrylate into the reaction vessel, dropwise add 0.15 g of isopropyl alcohol solution of chloroplatinic acid, and react at 120 °C for 1 h to obtain mixture M5;

[0079] Step 2: After the reaction is completed, continue to add 3.5 g of tetraethyl orthosilicate and 8 g of hydrophobic silica to the reaction vessel for mixing, dropwise add 1 g of potassium methoxide, and react at 120 °C for 2 h to obtain mixture N5;

[0080] Step 3: Finally, add 15 g of MQ silicone resin (the molar ratio of M to Q is 1.0:1.0), and keep it at 120 °C for 2 h to obtain the silicone composition. Comparative Example 6

[0081] Step 1: Add 30 g of HMe2SiO(HSiMeO) 30 (SiMe2O) 80SiMe2H, 24 g of octafluoropentyl methacrylate and 25 g of hydroxybutyl acrylate were added to a reaction vessel, and 0.2 g of an isopropanol solution of chloroplatinic acid was added dropwise. The reaction was carried out at 130 °C for 1 h to obtain a mixture M6;

[0082] Step 2: After the reaction was completed, 3 g of methyltriacetoxysilane and 3.8 g of hydrophobic silica were further added to the reaction vessel and mixed. 2 g of tetramethylammonium hydroxide was added dropwise. The reaction was carried out at 130 °C for 1 h to obtain a mixture N6;

[0083] Step 3: Finally, 12 g of polyether-modified polysiloxane (R2 is CH3; x is 400, y is 5, z is 4, g is 40, h is 60) was added, and the temperature was kept at 130 °C for 1 h to obtain the organosilicon composition.

[0084] Examples 8-14 and Comparative Examples 7-12 prepared organosilicon emulsions according to the existing well-known technology, and prepared organosilicon emulsions S1-S7 and organosilicon emulsions SE1-SE6 respectively

[0085] The specific preparation method was as follows: 40 g of the organosilicon composition, 8 g of Span 80 and 12 g of fatty alcohol polyoxyethylene ether were fully mixed by stirring for 20 min. After completion, the temperature of the above system was raised to 80 °C, and then the system temperature was maintained. 40 g of water was slowly added, and the stirring speed was increased until the system became an oil-in-water emulsion. Another 20 g of water was added until the mass concentration of the emulsion was 50%. The crude emulsion was further emulsified by a colloid mill, and finally the emulsion with a solid content of 25% was diluted with an aqueous solution of a polyacrylic acid thickener.

[0086] Performance testing of organosilicon emulsions

[0087] (1) Defoaming and antifoaming performance testing method: An aqueous solution of sodium dodecylbenzenesulfonate with a mass fraction of 0.5% was used as the foaming medium. 50 ml of the above foaming medium was added to a 100 ml stoppered graduated cylinder, and then 0.01 of the organosilicon emulsion was added. It was shaken 50 times in the vertical direction, and the time for the foam to disappear to the liquid level was recorded, which was the defoaming time T

[0088] 50 , shaken 100 times again and the defoamer time T was recorded 100 , shaken 200 times again and the defoaming time T was recorded 200 , the shorter the defoaming time, the better the defoaming and antifoaming performance of the organosilicon emulsion. At the same time, the more times of shaking, the shorter the defoaming time, and the better the anti-decay performance of the defoaming and antifoaming performance of the organosilicon emulsion.

[0089]

[0090] (2) Compatibility performance testing:

[0091] After allowing the mixture of the foam-suppressing and anti-foaming performance-tested foaming medium and the silicone emulsion to stand for 24 h, observe the compatibility of the silicone emulsion in the foaming medium. The more precipitation occurs, the worse the compatibility. Here, "0" indicates no precipitation, "+" indicates precipitation, and the more "+" there are, the more severe the precipitation is.

[0092]

Claims

1. A silicone composition, characterized in that, It consists of the following components: A. Hydrogen-containing polyorganosiloxane: the dosage is 20 - 50% of the total mass of the organosilicon composition; B. Hydroxyalkyl acrylate, the dosage is 15 - 25% of the total mass of the organosilicon composition; C. Fluoroacrylate, the dosage is 15 - 25% of the total mass of the organosilicon composition D. Catalyst I is isopropyl alcohol solution of chloroplatinic acid, and the dosage is 0.01% - 0.2% of the total mass of the organosilicon composition E. Coupling agent, the dosage is 1 - 4% of the total mass of the organosilicon composition; F. Silicon dioxide, the dosage is 2 - 10% of the total mass of the organosilicon composition; H. MQ silicone resin, the dosage is 3 - 10% of the total mass of the organosilicon composition; I. Catalyst II is a basic catalyst, and the dosage is 0.5 - 2% of the total mass of the organosilicon composition; J. Polyether-modified polysiloxane, the dosage is 2 - 10% of the total mass of the organosilicon composition; The preparation method of the organosilicon composition is as follows: Step 1: Add the hydrogen-containing polyorganosiloxane, fluoroacrylate and hydroxyalkyl acrylate into a reaction vessel, dropwise add Catalyst I, and react at 80 - 130 °C for 1 - 4 h to obtain a mixture M; Step 2: After the reaction is completed, continue to add the coupling agent and silicon dioxide to mix in the reaction vessel, dropwise add the basic catalyst, and react at 80 - 150 °C for 1 - 4 h to obtain a mixture N; Step 3: Finally, add MQ resin and polyether-modified polysiloxane, and keep warm at 80 - 150 °C for 1 - 4 h to obtain the organosilicon composition.

2. The organosilicon composition according to claim 1, characterized in that, The structural general formula of the hydrogen-containing polyorganosiloxane is as follows: H a Me 3-a SiO(SiMeHO) b (SiMe2O) c SiMe 3-a H a Where Me is methyl, subscript a is 1 or 2, subscript b is an integer from 1 to 40, and subscript c is an integer from 20 to 200.

3. The organosilicon composition according to claim 1, characterized in that, The structural general formula of the hydroxyalkyl acrylate is as follows: In the molecular structure, R is hydrogen; R 0 is selected from 1-hydroxyethyl, 2-hydroxyethyl, 1-hydroxypropyl, 2-hydroxypropyl, 3-hydroxypropyl, 1-hydroxyisopropyl, 2-hydroxyisopropyl, 3-hydroxyisopropyl, 1-hydroxybutyl, 2-hydroxybutyl, 3-hydroxybutyl or 4-hydroxybutyl.

4. The silicone composition according to claim 1, wherein The fluoroacrylate is selected from trifluoroethyl acrylate, trifluoroethyl methacrylate, hexafluorobutyl acrylate, hexafluorobutyl methacrylate, octafluoropentyl acrylate, octafluoropentyl methacrylate.

5. An organosilicon composition according to claim 1, characterized in that, The structural formula of the coupling agent is: (Y(CH2) n ) P Si(OR 1 ) q Among them, R 1 is selected from methyl, ethyl, propyl, butyl; p is 0 or 1, q is an integer from 1 to 4, p + q = 4, n is an integer from 0 to 16; Y is selected from methyl, amino, methacryloyloxy, epoxy, vinyl, mercapto, cyano; specifically selected from: 3-methacryloxypropyltrimethoxysilane, vinyltriethoxysilane, 3-aminopropyltrimethoxysilane, 12-aminododecyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, dimethyldiethoxysilane, methyltriethoxysilane, methyltriacetoxysilane, tetraethyl orthosilicate, dimethyldiethoxysiloxane, ethyltriethoxysilane, propyltrimethoxysilane.

6. An organosilicon composition according to claim 1, characterized in that, The silicon dioxide is hydrophobic silicon dioxide.

7. An organosilicon composition according to claim 1, characterized in that The MQ silicone resin described above is composed of the chain unit (CH3)3SiO l / 2 (M unit) and the chain unit SiO 4 / 2 (Q unit) to form an MQ resin, and the molar ratio between the two is (0.4 to 1.2):1.

0.

8. An organosilicon composition according to claim 1, characterized in that, The Catalyst II is selected from NaOH, KOH, potassium silanolate, sodium silanolate, sodium methoxide, sodium ethoxide, potassium methoxide, potassium ethoxide, b-hydroxyethyl trimethylamine, tetramethylammonium hydroxide.

9. An organosilicon composition according to claim 1, characterized in that, The structural formula of the polyether-modified polysiloxane is as follows: MD x (CH3GSiO) y M Among them, M is the chain segment (CH3)3SiO l / 2 , D is the chain segment (CH3)2SiO 2 / 2 ; G is a polyether group, represented by the following structural general formula: –(CH2) z (EO) g (PO) h R 2 , where R 2 is -H or -CH3 or -COCH3; the subscripts x , y , z , g , h are the degrees of polymerization, x is an integer from 10 to 500; y is an integer from 1 to 50; z is an integer from 3 to 6; g is an integer from 1 to 40; h is an integer from 0 to 60, and the dosage is 2 - 10% of the total mass of the silicone composition.

Images