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CN116640313A - Hydrophilic modified organic silicon composition and preparation method thereof - Google Patents

Hydrophilic modified organic silicon composition and preparation method thereof Download PDF

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Publication number
CN116640313A
CN116640313A CN202310433590.6A CN202310433590A CN116640313A CN 116640313 A CN116640313 A CN 116640313A CN 202310433590 A CN202310433590 A CN 202310433590A CN 116640313 A CN116640313 A CN 116640313A
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hydrophilic
organic silicon
silicone composition
modified silicone
preparing
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陈捷
饶树良
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Guangzhou Dx Chemical Co ltd
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Guangzhou Dx Chemical Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42Block-or graft-polymers containing polysiloxane sequences
    • C08G77/46Block-or graft-polymers containing polysiloxane sequences containing polyether sequences
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/10Block- or graft-copolymers containing polysiloxane sequences
    • C08L83/12Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Silicon Polymers (AREA)

Abstract

A hydrophilic modified organic silicon composition and a preparation method thereof relate to the technical field of organic synthesis; the preparation method comprises the following steps: 1) Taking hydrophilic raw materials and excessive organic silicon monomers to react to obtain crude reaction material crude material preparation materials; 2) Heating the crude reaction material and adding a low-boiling point organic solvent, removing part of unreacted organosilicon monomers under negative pressure, heating and removing the rest of unreacted organosilicon monomers under negative pressure to obtain the hydrophilic modified organosilicon composition. The water solubility and transparency of the product are improved by controlling the proportion of reactants to enable the hydrophilic modification reaction to be thorough, and meanwhile, excessive organic silicon monomers are removed under the conditions of heating and negative pressure, so that the content of free organic silicon monomers in the product is reduced, and the odor of the product is reduced. The organic silicon monomer in the reaction substrate is excessive, so that the reaction of the hydrophilic modified raw material is ensured to be complete as much as possible, and the existence of the hydrophilic modified raw material with poor structural stability in the product is reduced, thereby improving the transparency and the pH stability of the aqueous solution.

Description

Hydrophilic modified organic silicon composition and preparation method thereof
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a hydrophilic modified organic silicon composition and a preparation method thereof.
Background
Hydrophilic modified organosilicon products are prepared by introducing hydrophilic groups onto siloxane and polysiloxane groups, so that the hydrophilia of the siloxane and polysiloxane is improved, and the use of the siloxane or polysiloxane in water-soluble products is increased. The hydrophilically modified organosilicon product has excellent water solubility, conditioning and moistening characteristics and strong affinity with hair and skin; can reduce the greasy feeling and sticky feeling of the organosilicon product. The compound has good compounding performance, can be compatible with various organic cosmetic components, has foam increasing and stabilizing functions in a foam formula system, and can keep the foam fullness and durability of the formula. When the mask is used as a mask humectant, the air permeability and the moisture retention of the mask essence can be improved, and the absorption of the non-woven fabric to the essence can be increased. Meanwhile, because of the unique air permeability and moisturizing and lubricating properties, the skin care product can also endow skin with glossiness when applied to the skin care product. The wide range of applications in personal care products are: cream, facial mask, water for moisturizing, shaving cream, hand cleanser, etc.
Currently, products on the market suffer from more or less the following drawbacks: 1. the smell is large; some silicone materials have a relatively high odor and if the material remains too much in the product, it can directly affect the product odor and thus the formulator's use in the final formulation. 2. The transparency of the aqueous solution is poor; mainly because the degree of hydrophilic modification reaction is insufficient, some siloxane monomers are not connected with hydrophilic groups, so that the transparency of aqueous solution is poor, and the aqueous solution cannot be used in transparent products. 3. The pH value of the aqueous solution is unstable; when the hydrophilically modified silicone product is formulated as an aqueous solution, the pH of the aqueous solution decreases after a period of time. It is well known that most of the personal care products are water, which directly results in unstable pH in the formulation when applied to the personal care product. 4. The organosilicon content in the product is low; some products can make the transparency and smell of the aqueous solution good by reducing the content of organic silicon. However, the characteristics of the organosilicon such as lubricity and softness are obviously reduced, and even when part of the products are subjected to infrared and nuclear magnetism identification, the characteristic peaks of siloxane cannot be detected.
Disclosure of Invention
In order to overcome the defects of the prior art, one of the purposes of the invention is to provide a preparation method of a hydrophilic modified organic silicon composition, and the prepared product has the characteristics of small smell, high transparency and good pH stability.
It is a second object of the present invention to provide a hydrophilically modified silicone composition.
One of the purposes of the invention is realized by adopting the following technical scheme:
a method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and excessive organic silicon monomers to react to obtain crude materials;
2) Heating the crude material and adding a low-boiling point organic solvent, removing part of unreacted organic silicon monomers under negative pressure, heating and removing the rest of unreacted organic silicon monomers under negative pressure to obtain the hydrophilic modified organic silicon composition.
Further, in step 1), the molar ratio of the hydrophilic raw material to the organic silicon monomer is 1: (1.01-1.5).
Further, the organic silicon monomer is any one or more than two of polydimethylsiloxane, dimethyldiethoxysilane, diethoxysilane, tetraethoxysilane, trimethylethoxysilane, dimethylethoxysilane, vinyltriethoxysilane and dimethylvinylethoxysilane.
Further, the hydrophilic raw material is any one or more than two of polyethylene glycol, polypropylene glycol and methoxy polyethylene glycol, and the polymerization degree of the hydrophilic raw material is 10-40.
Further, in the step 1), an acid/base catalyst with the mass fraction of 0.1-1% is added in the reaction, the reaction temperature is 70-130 ℃, and the reaction time is 20-40h.
Further, the acid/base catalyst is any one or more than two of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate, potassium carbonate, triethanolamine and aminomethylpropanol, or any one or more than two of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid and nitric acid.
Further, in step 1), the method further comprises a pretreatment step of raw materials, and the operation of the pretreatment step comprises the following steps: removing low molecular weight components from the hydrophilic feedstock.
Further, in the step 2), the specific operation is as follows: heating the crude material to 50-80 ℃ and adding a low-boiling point organic solvent, removing part of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree, then heating to 80-140 ℃ and removing the rest of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree to obtain the hydrophilic modified organosilicon composition.
Further, in step 2), the hydrophilically modified silicone composition is further added with a stabilizing aid in an amount of 50 to 5000 ppm; the stabilizing auxiliary agent is one or more than two of vitamin E, tocopheryl acetate, pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), tea polyphenol, butyl hydroxy anisole, dibutyl hydroxy toluene, propylene glycol and tert-butyl hydroquinone.
The second purpose of the invention is realized by adopting the following technical scheme:
a hydrophilically modified silicone composition is prepared by the method for preparing a hydrophilically modified silicone composition.
Compared with the prior art, the invention has the beneficial effects that:
according to the preparation method of the hydrophilically modified organic silicon composition, disclosed by the invention, the hydrophilization modification reaction is thoroughly carried out by controlling the proportion of reactants, so that the water solubility and transparency of a product are improved, and meanwhile, excessive organic silicon monomers are removed under the conditions of heating and negative pressure by a two-step method, so that the content of free organic silicon monomers in the product is reduced, and the odor of the product is reduced. Meanwhile, the organic silicon monomer in the reaction substrate is excessive, so that the reaction of the hydrophilic modified raw material is ensured to be complete as much as possible, and the existence of the hydrophilic modified raw material with poor structural stability in the product is reduced, thereby improving the pH stability.
The hydrophilic modified organic silicon composition has the advantages of small smell, high transparency, good pH stability and remarkable structural characteristics.
Drawings
FIG. 1 is an infrared spectrum of a silicone composition of example 1 of the present invention.
FIG. 2 is an infrared spectrum of the product of comparative example 1 of the present invention.
FIG. 3 is an infrared spectrum of the product of comparative example 2 of the present invention.
FIG. 4 is a graph of the transparency of the silicone composition of example 1 of the present invention versus the products of comparative examples 1-2.
Detailed Description
The present invention will be further described with reference to the following specific embodiments, and it should be noted that, on the premise of no conflict, new embodiments may be formed by any combination of the embodiments or technical features described below.
In order to solve the problems of large smell, low transparency, poor pH stability and the like of the organic silicon solution in the prior art, the invention provides the following technical scheme:
a method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and excessive organic silicon monomers to react to obtain crude materials;
2) Heating the crude material and adding a low-boiling point organic solvent, removing part of unreacted organic silicon monomers under negative pressure, heating and removing the rest of unreacted organic silicon monomers under negative pressure to obtain the hydrophilic modified organic silicon composition.
Further, in step 1), the molar ratio of the hydrophilic raw material to the organic silicon monomer is 1: (1.01-1.5). The organic silicon monomer in the reaction substrate is excessive, so that the reaction of the hydrophilic modified raw material is ensured to be complete as much as possible, and the existence of the hydrophilic modified raw material with poor structural stability in the product is reduced, thereby improving the pH stability.
Further, the organic silicon monomer is one or more than two of polydimethylsiloxane, dimethyldiethoxysilane, diethoxysilane, tetraethoxysilane, trimethylethoxysilane, dimethylethoxysilane, vinyltriethoxysilane and dimethylvinylethoxysilane.
Further, the hydrophilic raw material is a hydrophilic organic matter with a molecular weight ranging from 400 to 2000, preferably, the hydrophilic raw material is any one or more of polyethylene glycol (PEG), polypropylene glycol (PPG) and methoxypolyethylene glycol (MPEG), and the polymerization degree of the hydrophilic raw material is 10 to 40.
Further, in the step 1), an acid/base catalyst with the mass fraction of 0.1-1% is added in the reaction, the reaction temperature is 70-130 ℃, and the reaction time is 20-40h. The transparency of the hydrophilically modified organosilicon composition is high and is related to the degree of hydrophilization modification, and the more thorough the hydrophilization modification is, the better the water solubility is, and the higher the transparency is.
Further, in step 1), the acid/base catalyst is any one or more than two of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate, potassium carbonate, triethanolamine and aminomethylpropanol, or any one or more than two of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid and nitric acid. The acid/base catalyst adopted by the invention has poor compatibility with products, so that the acid/base catalyst is easy to separate from the products in the later period.
Further, in step 1), the method further comprises a pretreatment step of raw materials, and the operation of the pretreatment step comprises the following steps: removing low molecular weight components from the hydrophilic feedstock. The removal means in the following examples is a system for removing substances having a polymerization degree of less than 10 from a hydrophilic material by selecting a system for extraction under a normal negative pressure or a system for azeotropic separation with a low boiling point solvent.
Further, in the step 2), the specific operation is as follows: heating the crude material to 50-80 ℃ and adding a low-boiling point organic solvent, removing part of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree, then heating to 80-140 ℃ and removing the rest of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree to obtain the hydrophilic modified organosilicon composition. Preferably, the organic solvent is an alcohol solvent, and further, the alcohol solvent is any one or more of methanol, ethanol and isopropanol.
Further, in step 2), the hydrophilically modified silicone composition is further added with a stabilizing aid in an amount of 50 to 5000 ppm; the stabilizing auxiliary agent is any one or more than two of vitamin E, tocopheryl acetate, pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), tea polyphenol, butyl Hydroxy Anisole (BHA), dibutyl hydroxy toluene (BHT), propylene Glycol (PG) and tert-butyl hydroquinone (TBHQ). The invention can improve the stability of the product by adding the stabilizing auxiliary agent.
Example 1
A method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers; in this example and the following examples, the low molecular weight substance in the hydrophilic raw material is water or a substance having a polymerization degree of less than 10, and the low molecular weight substance in the organosilicon monomer is mainly water;
2) Mixing hydrophilic raw materials with excessive organic silicon monomers, and adding 0.5% of alkali catalyst by mass fraction for reaction at 105 ℃ for 30 hours to obtain crude materials;
wherein the organosilicon monomer is polydimethylsiloxane, the hydrophilic raw material is polyethylene glycol (PEG 10-40), and the molar ratio of the hydrophilic modified raw material to the organosilicon monomer is 1:1.3, wherein the alkali catalyst is sodium hydroxide;
3) Heating the crude material to 65 ℃ and adding a low-boiling point organic solvent, removing part of unreacted organosilicon monomers under the negative pressure of not less than 0.08MPa in vacuum degree, then heating to 110 ℃ and removing the rest of unreacted organosilicon monomers under the negative pressure of not less than 0.08MPa in vacuum degree to obtain a first material; wherein the organic solvent is ethanol; the means for removing unreacted silicone monomer in this example and the following examples are: and (3) reducing the boiling point of the material under the condition of negative pressure not less than 0.08MPa, so that the low-boiling point material is separated from the system.
4) Removing catalyst precipitate from said first material at a temperature (-10-50 ℃), by a means including but not limited to: standing for layering, filtering with filter cloth or filter element, and centrifuging; filtering through a filter element with the diameter of 1-5 mu m so as to remove the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition; wherein the stabilizing aid is tocopheryl acetate.
Example 2
A method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers;
2) Mixing hydrophilic raw materials with excessive organic silicon monomers, and adding 0.1% of alkali catalyst by mass fraction for reaction at 70 ℃ for 40 hours to obtain crude materials;
wherein the organosilicon monomer is tetraethoxysilane, the hydrophilic raw material is polypropylene glycol (PPG 10-40), and the mol ratio of the hydrophilic modified raw material to the organosilicon monomer is 1:1.01, wherein the base catalyst is sodium carbonate;
3) Heating the crude material to 50 ℃ and adding a low-boiling point organic solvent, removing part of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa, then heating to 80 ℃ and removing the rest of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa to obtain a first material; wherein the organic solvent is methanol;
4) Removing catalyst sediment in the first material at a certain temperature, filtering through a filter element with the diameter of 1-5 mu m, thereby removing the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition; wherein the stabilizing auxiliary agent is vitamin E.
Example 3
A method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers;
2) Mixing hydrophilic raw materials with excessive organic silicon monomers, and adding an acid catalyst with the mass fraction of 0.7% for reaction, wherein the reaction temperature is 120 ℃ and the reaction time is 25 hours, so as to obtain a crude material;
wherein the organosilicon monomer is vinyl triethoxysilane, the hydrophilic raw material is methoxy polyethylene glycol (MPEG 10-40), and the mole ratio of the hydrophilic modified raw material to the organosilicon monomer is 1:1.3, wherein the acid catalyst is sulfuric acid;
3) Heating the crude material to 70 ℃ and adding a low-boiling point organic solvent, removing part of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa, then heating to 120 ℃ and removing the rest of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.8MPa to obtain a first material; wherein the organic solvent is isopropanol;
4) Removing catalyst sediment in the first material at a certain temperature, filtering through a filter element with the diameter of 1-5 mu m, thereby removing the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition; wherein the stabilizing auxiliary is pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate).
Example 4
A method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers;
2) Mixing hydrophilic raw materials with excessive organic silicon monomers, and adding an acid catalyst with the mass fraction of 1% to react at 130 ℃ for 20 hours to obtain a crude material;
wherein the organosilicon monomer is dimethylvinylethoxysilane, the hydrophilic raw material is polyethylene glycol (PEG 10-40), and the molar ratio of the hydrophilic modified raw material to the organosilicon monomer is 1:1.5, the acid catalyst is hydrochloric acid;
3) Heating the crude material to 80 ℃ and adding a low-boiling point organic solvent, removing part of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa, then heating to 140 ℃ and removing the rest of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa to obtain a first material; wherein the organic solvent is isopropanol;
4) Removing catalyst sediment in the first material at a certain temperature, filtering through a filter element with the diameter of 1-5 mu m, thereby removing the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition; wherein the stabilizing auxiliary is tert-butylhydroquinone.
Comparative example 1
This comparative example is a hydrophilically modified silicone product purchased from a company in China.
Comparative example 2
This comparative example is a hydrophilically modified silicone product from International company.
Comparative example 3
A method for producing a silicone composition, the comparative example differs from example 1 only in that: the preparation method comprises the following steps:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers;
2) Mixing hydrophilic raw materials with an equal amount of organic silicon monomers, and adding 0.5% of alkali catalyst by mass fraction for reaction at 105 ℃ for 30 hours to obtain a crude material;
3) And removing catalyst sediment in the crude material at a certain temperature, filtering through a filter element with the diameter of 1-5 mu m, thereby removing the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition.
Comparative example 4
A method for producing a silicone composition, the comparative example differs from example 1 only in that: the preparation method comprises the following steps:
1) Taking hydrophilic raw materials and organic silicon monomers and removing low molecular weight components in the hydrophilic raw materials and the organic silicon monomers;
2) Mixing excessive hydrophilic raw materials with an organosilicon monomer, and adding 0.5% by mass of alkali catalyst for reaction at 105 ℃ for 30 hours to obtain a crude material;
4) Removing unreacted hydrophilic raw materials in the crude material in an azeotropic separation system with a low-boiling solvent, removing catalyst sediment in the crude material, filtering through a filter element with the diameter of 1-5 mu m to remove the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition; wherein the stabilizing auxiliary agent is vitamin E.
Comparative example 5
A method for producing a silicone composition, the comparative example differs from example 1 only in that: the preparation method comprises the following steps:
1) Mixing hydrophilic raw materials with excessive organic silicon monomers, and adding 0.5% of alkali catalyst by mass fraction for reaction at 105 ℃ for 30 hours to obtain crude materials;
2) Heating the crude material to 50 ℃ and adding a low-boiling point organic solvent, removing part of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa, then heating to 80 ℃ and removing the rest of the organic silicon monomers under the negative pressure with the vacuum degree not less than 0.08MPa to obtain a first material;
3) And removing catalyst sediment in the first material at a certain temperature, filtering through a filter element with the diameter of 1-5 mu m, thereby removing the catalyst and other impurities, and adding a stabilizing auxiliary agent to obtain the hydrophilic modified organosilicon composition.
Performance testing
1. Quality index test
The hydrophilically modified silicone compositions of examples 1 to 4 and comparative examples 3 to 4 were subjected to quality index test, and the results are shown in table 1.
TABLE 1
Referring to table 1, the silicone composition of the present invention has the characteristics of small odor, high transparency, and good pH stability. The organosilicon composition of comparative examples 3-4 has higher content of hydrophilic raw materials, and unreacted organosilicon monomers and impurities are not sufficiently removed, and the appearance is qualified, but the content of D4 and D5 is too high, the characteristic peak is small, the odor of 10% aqueous solution is large, the transparency is too low at 48 ℃, and the pH value stability is poor; the method shows that the content of the organic silicon monomer is low, the organic silicon content is low, and the characteristic peak is small; and the remaining silicone monomer is not sufficiently removed, resulting in a large odor and poor water solubility, affecting transparency. In comparative example 5, the hydrophilic raw material has a certain low molecular weight substance, and the pH value stability is poor, which indicates that the introduction of the low molecular weight substance can easily hydrolyze the product structure, reduce the pH stability and influence the transparency.
2. pH stability test of Silicone compositions
The silicone composition of example 1 and the products of comparative examples 1-2 were prepared as 10% aqueous solutions, and then left at 48℃and room temperature, respectively, for 30 days, and the changes in pH were recorded, and the results are shown in Table 2.
TABLE 2
Referring to table 2, the silicone composition of the present invention, which was left at different temperatures for 30 days, had no significant change in pH and was high in stability; the product of comparative example 1 was left at 48℃for 30 days, and its pH was lowered below the standard. The product of comparative example 2 was left at 48℃for 30 days, and its pH was significantly lowered, indicating poor pH stability.
3. Infrared spectroscopic detection
Referring to FIGS. 1-3, 799.65cm in the IR spectrum of the silicone composition of example 1 of the present invention -1 The position has obvious Si-C characteristic peak; the product of comparative example 1 has no visible Si-C characteristic peak at the corresponding position, which indicates that the organosilicon content in the structure is very low; the product of comparative example 2 had Si-C characteristic peaks at the corresponding positions.
4. Transparency contrast test
Referring to fig. 4, the silicone composition of example 1 of the present invention was formulated as a 10% aqueous solution, and had an immediate light transmittance of 98.5% and a light transmittance of 98.1% after being left at 48 ℃ for 30 days; the instant light transmittance of the 10% aqueous solution prepared by the product of the comparative example 1 is 97.1%, the light transmittance is 96.9% after the product is placed for 30 days at 48 ℃, and the light transmittance is relatively stable, and the organic silicon monomer is little or no, so that the hydrolysis does not exist, and the light transmittance does not change; the product of comparative example 2 was formulated as a 10% aqueous solution having an immediate light transmittance of 0% and a light transmittance of 0% after 30 days at 48 ℃. The stability of the product is poor, and the material is obviously hydrolyzed before the water solution is prepared.
Overall, the overall performance of example 1 was significantly better than that of comparative examples 1 and 2.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.

Claims (10)

1. A method of preparing a hydrophilically modified silicone composition comprising the steps of:
1) Taking hydrophilic raw materials and excessive organic silicon monomers to react to obtain crude materials;
2) Heating the crude material and adding a low-boiling point organic solvent, removing part of unreacted organic silicon monomers under negative pressure, heating and removing the rest of unreacted organic silicon monomers under negative pressure to obtain the hydrophilic modified organic silicon composition.
2. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: in the step 1), the molar ratio of the hydrophilic raw material to the organic silicon monomer is 1: (1.01-1.5).
3. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: the organic silicon monomer is any one or more than two of polydimethylsiloxane, dimethyldiethoxysilane, diethoxysilane, tetraethoxysilane, trimethylethoxysilane, dimethylethoxysilane, vinyltriethoxysilane and dimethylvinylethoxysilane.
4. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: the hydrophilic raw material is any one or more than two of polyethylene glycol, polypropylene glycol and methoxy polyethylene glycol, and the polymerization degree of the hydrophilic raw material is 10-40.
5. A method of preparing a hydrophilically modified silicone composition as set forth in any one of claims 1 to 4, characterized in that: in the step 1), an acid/alkali catalyst with the mass fraction of 0.1-1% is also added in the reaction, the reaction temperature is 70-130 ℃, and the reaction time is 20-40h.
6. A method of preparing a hydrophilically modified silicone composition as set forth in claim 5, characterized in that: the acid/base catalyst is any one or more than two of sodium hydroxide, potassium hydroxide, ammonia water, sodium carbonate, potassium carbonate, triethanolamine and aminomethylpropanol, or any one or more than two of sulfuric acid, hydrochloric acid, acetic acid, phosphoric acid and nitric acid.
7. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: in the step 1), the method further comprises a pretreatment step of raw materials, wherein the operation of the pretreatment step comprises the following steps: removing low molecular weight components from the hydrophilic feedstock.
8. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: in the step 2), the specific operation is as follows: heating the crude material to 50-80 ℃ and adding a low-boiling point organic solvent, removing part of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree, then heating to 80-140 ℃ and removing the rest of unreacted organosilicon monomers under the negative pressure of 0.07-0.1MPa in vacuum degree to obtain the hydrophilic modified organosilicon composition.
9. A method of preparing a hydrophilically modified silicone composition as set forth in claim 1, characterized in that: in the step 2), the hydrophilic modified organosilicon composition is further added with a stabilizing auxiliary agent with the content of 50-5000 ppm; the stabilizing auxiliary agent is one or more than two of vitamin E, tocopheryl acetate, pentaerythritol tetra (di-tert-butyl hydroxy hydrocinnamate), tea polyphenol, butyl hydroxy anisole, dibutyl hydroxy toluene, propylene glycol and tert-butyl hydroquinone.
10. A hydrophilically modified silicone composition characterized by: made by a method of preparing a hydrophilically modified silicone composition as set forth in any one of claims 1-9.
CN202310433590.6A 2023-04-20 2023-04-20 Hydrophilic modified organic silicon composition and preparation method thereof Pending CN116640313A (en)

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