CN-119798669-B - Water-soluble polysiloxane, and preparation method and application thereof

Abstract

The invention belongs to the field of polymer chemistry, and particularly relates to water-soluble polysiloxane, and a preparation method and application thereof. A water-soluble polysiloxane having a structure as shown in formula I: Wherein R1 is aminoethylaminopropyl, R2 is vinyl or phenyl, x+y=100%, x=35% -100% and excluding 100%. The water-soluble polysiloxane has hydrophilicity and adjustable solubility, and the solubility in water can be regulated and controlled by regulating the proportion of various groups in the formula, so that the water-soluble polysiloxane can be widely applied to the fields of paint, cosmetics, medicines and the like.

Inventors

• CHENG XIAO
• GUO XIAOLEI
• ZHOU CHUANJIAN
• LONG TENG
• WANG HUA

Assignees

• 山东大学

Dates

Publication Date

20260512

Application Date

20241219

Claims (2)

1. 1. A method for preparing water-soluble polysiloxane, which is characterized in that the water-soluble polysiloxane has a structure shown in a formula I: A formula I; wherein R1 is aminoethylaminopropyl, R2 is vinyl or phenyl, x+y=100%; the preparation method of the water-soluble polysiloxane is one selected from the following 1) to 9): 1) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 8.6g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 185.4g, reacting for 0.5h at 90-110 ℃ under inert atmosphere, heating to 140-160 ℃ and reacting for 0.5-1 h, and performing reduced pressure distillation after the reaction to obtain water-soluble polysiloxane with X=90.2%, wherein the solubility of the water-soluble polysiloxane in water is 92g/100mL; 2) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 17.2g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 164.8g, reacting for 1h at 90-110 ℃ under inert atmosphere, then heating to 140-160 ℃ for reacting for 0.5-1 h, and performing reduced pressure distillation after the reaction to obtain water-soluble polysiloxane with X=79.9%, wherein the solubility of the water-soluble polysiloxane in water is 78g/100mL; 3) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 25.8g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 144.2g, reacting for 1.5 hours at 90-110 ℃ under inert atmosphere, heating to 140-160 ℃ and reacting for 0.5-1 hour, and performing reduced pressure distillation after the reaction to obtain water-soluble polysiloxane with X=69.9%, wherein the solubility of the water-soluble polysiloxane in water is 54g/100mL; 4) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 34.4g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 123.6g, reacting for 2 hours at 90-110 ℃ under inert atmosphere, heating to 140-160 ℃ and reacting for 0.5-1 hour, and performing reduced pressure distillation after the reaction to obtain water-soluble polysiloxane with X=60.2%, wherein the solubility of the water-soluble polysiloxane in water is 25g/100mL; 5) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 43g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 103g, reacting for 3 hours at 90-110 ℃ under inert atmosphere, heating to 140-160 ℃ for reacting for 0.5-1 hour, and distilling under reduced pressure after the reaction to obtain water-soluble polysiloxane with the concentration of X=49.7%, wherein the solubility of the water-soluble polysiloxane in water is 11g/100mL; 6) Mixing tetramethyl tetravinyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the amount of the tetramethyl tetravinyl cyclosiloxane is 51.6g, the amount of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 82.4g, reacting for 4 hours at 90-110 ℃ under inert atmosphere, heating to 140-160 ℃ and reacting for 0.5-1 hour, and performing reduced pressure distillation after the reaction to obtain water-soluble polysiloxane with X=41.1%, wherein the solubility of the water-soluble polysiloxane in water is 2g/100mL; 7) Mixing methyl phenyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the content of the methyl phenyl cyclosiloxane is 13.6g, the content of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 185.4g, the reaction is carried out under an inert atmosphere at 90-110 ℃ for 1h, the temperature is raised to 140-160 ℃ for 0.5-1 h, and the reduced pressure distillation is carried out after the reaction, so that the water-soluble polysiloxane with X=90.2% is obtained, wherein the solubility of the water-soluble polysiloxane in water is 86g/100mL; 8) Mixing methylphenyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the concentration of the methylphenyl cyclosiloxane is 27.2g, the concentration of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 164.8g, the reaction is carried out under an inert atmosphere, the reaction is carried out for 2 hours at 90-110 ℃, the temperature is raised to 140-160 ℃ and the reaction is carried out for 0.5-1 hour, and the reduced pressure distillation is carried out after the reaction, so that the water-soluble polysiloxane with X=80.4% is obtained, wherein the solubility of the water-soluble polysiloxane in water is 36g/100mL; 9) Mixing methyl phenyl cyclosiloxane, N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane, a catalyst and deionized water, wherein the content of the methyl phenyl cyclosiloxane is 40.8g, the content of the N- (beta-aminoethyl-gamma-aminopropyl) methyldimethoxy silane is 144.2g, the methyl phenyl cyclosiloxane is reacted under an inert atmosphere for 3 hours at 90-110 ℃, then the temperature is raised to 140-160 ℃ for 0.5-1 hour, and the water-soluble polysiloxane with X=69.8% is obtained after the reaction and reduced pressure distillation, wherein the solubility of the water-soluble polysiloxane in water is 10g/100mL; the catalyst comprises at least one of tetramethylammonium hydroxide, tetramethylammonium hydroxide silicon alkoxide, sodium hydroxide, and potassium hydroxide.
2. 2. The use of the water-soluble polysiloxane obtained by the preparation method according to claim 1 in the fields of water-based paint, cosmetics, drug carriers or environmental protection.

Description

Water-soluble polysiloxane, and preparation method and application thereof Technical Field The invention belongs to the field of polymer chemistry, and particularly relates to water-soluble polysiloxane, and a preparation method and application thereof. Background The disclosure of this background section is only intended to increase the understanding of the general background of the invention and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art already known to those of ordinary skill in the art. Polysiloxanes are widely used in various fields due to their excellent chemical stability, thermal stability and biocompatibility. Traditional silicone materials are predominantly hydrophobic, which has limitations in some applications where hydrophilic properties are required. In order to prepare a polysiloxane material having hydrophilicity, on one hand, a hydrophilic monomer may be copolymerized with a siloxane monomer, but generally the siloxane monomer has poor compatibility with the hydrophilic monomer due to large hydrophobicity, and on the other hand, a polysiloxane having hydrophilic side chains may be prepared by introducing hydrophilic groups such as amino groups, hydroxyl groups, etc. into the polysiloxane structure, to prepare a polysiloxane material having good water solubility. However, existing polysiloxanes contain a large variety of hydrophilic side chains per molecule, and hydrophilicity and solubility are difficult to control. Disclosure of Invention In order to solve the defects in the prior art, the invention provides water-soluble polysiloxane, a preparation method and application thereof, wherein the water-soluble polysiloxane has hydrophilicity and adjustable solubility, and the solubility in water can be regulated and controlled by regulating the proportion of various groups in a formula, so that the water-soluble polysiloxane can be widely applied to the fields of paint, cosmetics, medicines and the like. In order to achieve the above object, the present invention is realized by the following technical scheme: in a first aspect, the present invention provides a water-soluble polysiloxane having a structure as shown in formula I: wherein R 1 is aminoethylaminopropyl, R 2 is vinyl or phenyl, x+y=100%, x=35% -100% and excluding 100%. Preferably, when R 2 is vinyl, x=50% -100% and does not include 100%. Further preferably, when R 2 is vinyl, x=70% -95%. Preferably, when R 2 is phenyl, x=70% -100% and does not include 100%. Further preferably, when R 2 is phenyl, x=80% to 95%. In a second aspect, the present invention provides a process for the preparation of a water-soluble polysiloxane as described in the first aspect, comprising the steps of: and mixing silane, aminoethylaminopropyl silane, a catalyst and deionized water, reacting in an inert atmosphere, and distilling under reduced pressure after the reaction to obtain the water-soluble polysiloxane. Preferably, the silane comprises at least one of tetramethyl tetravinyl cyclotetrasiloxane, dimethoxy methyl vinyl silane, methyl vinyl diethoxy silane, methyl bis (trimethylsiloxy) vinyl silane, methylphenyl cyclosiloxane, dimethoxy methylphenyl silane, and diethoxy methylphenyl silane. Preferably, the aminoethylaminopropyl silane comprises at least one of N- (β -aminoethyl- γ -aminopropyl) methyldimethoxy silane and N- (β -aminoethyl- γ -aminopropyl) methyldiethoxy silane. Preferably, the catalyst comprises at least one of tetramethylammonium hydroxide (TMHA), tetramethylammonium hydroxide silicon alkoxide, sodium hydroxide, and potassium hydroxide. Preferably, the reaction temperature is 40-200 ℃ and the reaction time is 0.5-10 h. Preferably, the reaction is performed in two steps, wherein the reaction is performed at 90-110 ℃ for 0.5-3 hours, and then the temperature is raised to 140-160 ℃ for 0.5-1 hour. In a third aspect, the present invention provides the use of a water-soluble polysiloxane according to the first aspect in the field of aqueous paints, cosmetics, pharmaceutical carriers or environmental protection. The beneficial effects obtained by one or more of the technical schemes of the invention are as follows: The water-soluble polysiloxane can effectively adjust the solubility of the water-soluble polysiloxane in water by adjusting the proportion of hydrophilic groups in the water-soluble polysiloxane, so as to meet the requirements of different application scenes. The synthetic method of the water-soluble polysiloxane is simple to operate, can realize high-efficiency synthesis under milder conditions, and has good operability. The water-soluble polysiloxane can be widely applied to the fields of water-based paint, cosmetics, drug carriers and the like, and has great potential in the fields of environmental protection and biological medicine. Drawings The accompanying drawings, which are included to provide a further understanding of the invention and are inc