Hand feeling agent for high polymer material and preparation method of hand feeling agent

By preparing the intermediate reactor containing silicone and fluoro-containing silicone monomers to react with fatty acids, the problems of poor compatibility, dispersion and heat resistance of existing hand feel agents with polymer materials are solved, and good performance of hand feel agents for polymer materials are achieved.

CN119613727APending Publication Date: 2025-03-14FENGHUA RES INST OF NINGBO INST OF ENG
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Patent Information

Application Number
CN202411888545.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-20
Publication Date
2025-03-14

AI Technical Summary

Technical Problem

The existing hand feel agents have poor compatibility, dispersion and heat resistance with polymer materials such as plastics, rubbers and chemical fibers.

Method used

The handle agent for polymer materials is prepared by acidic aqueous solution of the siloxane-containing monomer and the fluoro-containing silicone monomer, and reacting the intermediate reactor with the molten fatty acid.

Benefits of technology

It has achieved monodispersed, good compatibility and excellent heat resistance of the handle agent for polymer materials, and is suitable for plastics, rubbers and chemical fibers.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a feeling agent for a high polymer material and a preparation method of the feeling agent, and relates to the technical field of organic materials. The invention discloses a preparation method of a feeling agent for a high polymer material. The preparation method comprises the following steps: blending an acidic aqueous solution containing a siloxane monomer and an alkaline pH value regulator to obtain an intermediate reactant system; blending the intermediate reactant system with an acidic aqueous solution containing a fluorine-containing siloxane monomer, and adding an alkaline pH value regulator to regulate the pH value so as to obtain an intermediate reactant; and adding the intermediate reactant and molten fatty acid into the reaction kettle, and stirring for reaction to obtain the hand feeling agent for the high polymer material. The fluorine-containing and silicon-containing auxiliary agent with monodispersity, good compatibility and excellent heat resistance is synthesized through simple and efficient chemical reaction, and the fluorine-containing and silicon-containing auxiliary agent is mainly used in the polymer fields of plastics, rubber, chemical fibers and the like.
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Description

Technical Field

[0001] The invention relates to the technical field of organic materials, and in particular to a polymer material feeling agent and a preparation method thereof. Background Art

[0002] Polymer materials are increasingly becoming one of the indispensable materials in daily life. Polymer products that come into contact with human skin feel uncomfortable due to the high hardness of polymer materials. In order to improve the comfort of plastic, a feel agent is generally added to polymer products. The feel agent is a chemical agent with a soft texture, good toughness and scratch resistance, which can make the surface of the product have an excellent touch. When combined with resin or leveling agent, it will have an extremely smooth and silky feel, improve the stickiness and excessive softness of the paint surface, and can also create a sand texture or frosted feel. The feel agent generally refers to lubricating substances such as silicones with low surface energy, such as polysiloxanes, and fluorines such as polytetrafluoroethylene.

[0003] The patent (patent number CN116376295A) discloses a reactive feel agent, which includes bihydroxyl silicone oil, oleic acid amide and erucic acid amide. By using bihydroxyl silicone oil to introduce polysiloxane segments into the polyurethane molecular structure through chemical bonds, and compounding a small amount of oleic acid amide and erucic acid amide, it can provide an ideal comprehensive feel without affecting the reactivity of bihydroxyl silicone oil, that is, elastic, plump, soft and baby-like touch effects. The patent (patent number CN116715855B) discloses an oleophobic skin feel agent and a preparation method thereof. The feel agent is obtained by three-dimensional cross-linking of perfluoro units, silicone units and polyether units. The end of the skin feel feel agent has a hydrophilic polyether unit, which can increase the solubility of the feel agent. At the same time, it also has a perfluoro unit, which further reduces the surface tension, and can make the feel agent more oleophobic, so that it can completely not absorb oil, so that the surface will not become sticky due to oil absorption under long-term use, and the durability of the smooth feel of the fabric is improved. The patent (patent number CN104927057B) discloses a new aminophenyl modified silicone oil, which can be used as a hand feeling agent. It has the characteristics of anti-fouling, quick drying, fluffy hand feeling, good stability, etc., which is more suitable for market needs. These hand feeling agents have great problems in compatibility, dispersibility, heat resistance, etc. with polymer materials such as plastics, rubber and chemical fibers. Summary of the invention

[0004] The purpose of the present invention is to provide a polymer material feel agent and a preparation method thereof, so as to solve the following technical problems: Existing hand feeling agents have poor compatibility, dispersibility and heat resistance with polymer materials such as plastics, rubber and chemical fibers.

[0005] The purpose of the present invention can be achieved through the following technical solutions: A method for preparing a polymer material feel agent, comprising the following steps: S1: Mixing an acidic aqueous solution containing a siloxane monomer and an alkaline pH adjuster to adjust the pH to 10-11, and controlling the temperature to 25-27° C. to obtain an intermediate reactant system; S2: Stir the intermediate reactant system prepared in S1 to produce a white precipitate, add an acidic aqueous solution containing a fluorine-containing siloxane monomer, add an alkaline pH adjuster to adjust the pH value to 8-10, control the temperature to 25-27° C., let it stand, centrifuge, filter, wash and dry the precipitate to obtain an intermediate reactant; S3: Add the intermediate reactant and molten fatty acid into the reactor, stir and react for 4-5 hours, vacuum extract and crush to obtain a polymer material feel agent.

[0006] As a further solution of the present invention: the mass ratio of siloxane monomer to fluorine-containing siloxane monomer in the intermediate reactant system in S2 is 20-50:0.9-3; the mass ratio of intermediate reactant to fatty acid in S3 is 80-90:10-20.

[0007] As a further embodiment of the present invention: the method for preparing the acidic aqueous solution containing siloxane monomers comprises the following steps: Add siloxane monomer and deionized water into a reaction bottle, add an acidic pH adjuster to adjust the pH value to 3-5, control the temperature to 20-25° C., stir and dissolve for 2-4 hours to obtain an acidic aqueous solution containing siloxane monomer.

[0008] As a further embodiment of the present invention: the method for preparing the acidic aqueous solution of fluorinated siloxane monomer comprises the following steps: Add fluorinated siloxane monomer and deionized water into a reaction bottle, add an acidic pH regulator to adjust the pH value to 3-5, control the temperature to 20-25° C., stir and dissolve for 4-6 hours to obtain an acidic aqueous solution of fluorinated siloxane monomer.

[0009] As a further embodiment of the present invention: the molecular structure of the siloxane monomer is:

[0010] In the formula, R is -CH 2 =CH 2 、-CH 2 -CH 3 、-CH 2 -CH 2 -CH 3、 Any of glycidyloxypropyl or phenyl; R 1 -CH 3 or -CH 2 -CH 3Any one of R 2 -CH 3 or -CH 2 -CH 3 Any one of R 3 -CH 3 or -CH 2 -CH 3 Any one of .

[0011] As a further embodiment of the present invention: the molecular structure of the fluorinated siloxane monomer is:

[0012] In the formula, R is -(F m C) n CH 3 , n≥2, m≥2; R 1 -CH 3 or -CH 2 -CH 3 Any one of R 2 -CH 3 or -CH 2 -CH 3 Any one of R 3 -CH 3 or -CH 2 -CH 3 Any one of .

[0013] As a further embodiment of the present invention: the acidic pH value regulator is dilute hydrochloric acid.

[0014] As a further embodiment of the present invention: the alkaline pH value regulator is an inorganic base or a fatty amine.

[0015] As a further embodiment of the present invention: the inorganic base is any one of sodium hydroxide, potassium hydroxide and lithium hydroxide.

[0016] As a further embodiment of the present invention: the fatty amine is any one of ethylenediamine, triethylamine, diethylenetriamine and ammonia water.

[0017] As a further embodiment of the present invention, the fatty acid is a fatty monoacid or a fatty diacid; the molecular formula of the fatty diacid is HOOC(CH 2 ) n COOH, wherein n≥7; the molecular formula of the fatty acid is CH 3 (CH 2 ) n (OH) m COOH, where n≥10, m=0 or 1.

[0018] As a further solution of the present invention: the specific steps of vacuum extraction in S3 are: vacuum extraction degree is -0.05 to -0.1 MPa, and extraction is performed for 2-3 hours.

[0019] A polymer material feeling agent is prepared by any one of the above preparation methods.

[0020] Beneficial effects of the present invention: The present invention uses a siloxane-containing monomer and a fluorine-containing siloxane monomer to react to obtain an intermediate reactant; and uses the intermediate reactant and a molten fatty acid reactor to obtain a polymer material feel agent. The present invention synthesizes a class of fluorine-containing and silicon-containing additives with monodispersity, good compatibility, and excellent heat resistance through a simple and efficient chemical reaction, which is mainly used in polymer fields such as plastics, rubbers, and chemical fibers. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] The present invention will be further described below in conjunction with the accompanying drawings.

[0022] Figure 1 This is a SEM photo of the feel agent prepared in Example 4 of the present application; Figure 2 This is a particle size distribution data diagram of the product of the hand feeling agent prepared in Example 4 of the present application tested using a laser force distribution instrument. DETAILED DESCRIPTION

[0023] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] Example 1 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of phenyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 500 rpm and dissolve for 2 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25° C. until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70° C. for 5 h to obtain an intermediate reactant. S5: 800g of the intermediate reaction product and 200g of 180°C molten 12-hydroxystearic acid were added into the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0025] The preparation method of the polypropylene plastic sample includes the following steps: 3g of the polymer material prepared in Example 1 is blended with a hand feeling agent and 97g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0026] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 3 g of the polymer material prepared in Example 1 with a feeling agent and 97 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0027] Example 2 The preparation method of a polypropylene plastic sample comprises the following steps: 5 g of the polymer material prepared in Example 1 is blended with a feeling agent and 95 g of polypropylene plastic (brand EPS30R) at 230° C., extruded into granules, and injection molded into a 2 mm sample at 230° C. to obtain a polypropylene plastic sample.

[0028] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 1 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0029] Example 3 The preparation method of a polypropylene plastic sample comprises the following steps: 8 g of the polymer material prepared in Example 1 is blended with a feeling agent and 92 g of polypropylene plastic (brand EPS30R) at 230°C, extruded into granules, and injection molded into a 2 mm sample at 230°C to obtain a polypropylene plastic sample.

[0030] The preparation method of a thermoplastic elastomer TPE plastic sample comprises the following steps: 8 g of the polymer material prepared in Example 1 is blended with a feeling agent and 92 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180° C., extruded into granules, and injection molded into a 2 mm sample at 180° C. to obtain a thermoplastic elastomer TPE plastic sample.

[0031] Example 4 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of vinyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 500 rpm and dissolve for 2 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25° C. until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70° C. for 5 h to obtain an intermediate reactant. S5: 800g of the intermediate reaction product and 200g of 180°C molten 12-hydroxystearic acid were added into the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0032] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 4 is blended with a hand feeling agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0033] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 4 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0034] Example 5 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of vinyl trimethylethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 500 rpm and dissolve for 2 hours to obtain an acidic aqueous solution containing siloxane monomers; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25° C. until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70° C. for 5 h to obtain an intermediate reactant. S5: 800g of the intermediate reaction product and 200g of 180°C molten 12-hydroxystearic acid were added into the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0035] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 5 is blended with a feel agent and 95g of polypropylene plastic (brand EPS30R) at 230°C, extruded and granulated, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0036] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 5 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0037] Example 6 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of phenyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 500 rpm and dissolve for 2 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25° C. until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70° C. for 5 h to obtain an intermediate reactant. S5: 800g of the intermediate reaction product and 200g of 180°C molten stearic acid were added to the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0038] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 6 is blended with a feel agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded and granulated, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0039] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 6 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0040] Example 7 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of phenyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 500 rpm and dissolve for 2 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25° C. until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70° C. for 5 h to obtain an intermediate reactant. S5: 800g of the intermediate reaction product and 200g of 180°C molten adipic acid were added to the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0041] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 7 is blended with a feel agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0042] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 7 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0043] Example 8 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of phenyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 4, control the temperature to 25°C, stir at a speed of 1000 rpm and stir to dissolve for 3 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: Add 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20°C, stir at 1000 rpm and dissolve for 5 hours to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 11, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 200 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added, and ethylenediamine is added to adjust the pH value to 8. The temperature is controlled at 25°C until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70°C for 5 hours to obtain an intermediate reactant. S5: Add 900g of the intermediate reaction product and 100g of 180°C molten 12-hydroxystearic acid into the reactor, stir and react for 4h, evacuate to -0.05MPa, extract for 2h, cool and air flow pulverize to obtain a polymer material feel agent.

[0044] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 8 is blended with a feel agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0045] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 8 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0046] Example 9 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of phenyltrimethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 4, control the temperature to 20°C, stir at a speed of 1000 rpm and stir to dissolve for 3 hours to obtain an acidic aqueous solution containing siloxane monomer; S2: Add 300 g of tridecafluorooctyltrimethoxysilane and 3000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 25° C., stir at 1000 rpm and dissolve for 5 hours to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 11, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 200 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added with ethylenediamine to adjust the pH value to 8, and the temperature is controlled at 25°C until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70°C for 5 hours to obtain an intermediate reactant; S5: Add 900g of the intermediate reaction product and 100g of 180°C molten 12-hydroxystearic acid into the reactor, stir and react for 4h, evacuate to -0.05MPa, extract for 2h, cool and air flow pulverize to obtain a polymer material feel agent.

[0047] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 9 is blended with a feel agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0048] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 9 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0049] Example 10 A method for preparing a polymer material using a hand feeling agent comprises the following steps: S1: Add 200 g of 3-glycidyloxypropylmethyltriethoxysilane and 2000 mL of deionized water into a reaction bottle, add dilute hydrochloric acid to adjust the pH value to 3, control the temperature to 20° C., stir at 500 rpm and dissolve for 2 h to obtain an acidic aqueous solution containing siloxane monomer; S2: 300 g of perfluorodecyltriethoxysilane and 3000 mL of deionized water were added to a reaction bottle, dilute hydrochloric acid was added to adjust the pH value to 4, the temperature was controlled at 20° C., the stirring speed was 500 rpm, and the mixture was stirred and dissolved for 4 h to obtain an acidic aqueous solution of fluorinated siloxane monomer; S3: Mixing an acidic aqueous solution containing a siloxane monomer and ethylenediamine, adjusting the pH value to 10, and controlling the temperature to 25° C., to obtain an intermediate reactant system; S4: The intermediate reactant system prepared in S3 is stirred at a speed of 500 rpm, and a white precipitate is produced by stirring. 100 g of an acidic aqueous solution containing a fluorinated siloxane monomer is added with ethylenediamine to adjust the pH value to 8, and the temperature is controlled at 25°C until the precipitate is completely precipitated. The precipitate is centrifuged, filtered, washed, and dried at 70°C for 5 hours to obtain an intermediate reactant; S5: 800g of the intermediate reaction product and 200g of 180°C molten stearic acid were added to the reactor, stirred for reaction for 4h, evacuated to -0.05MPa, extracted for 2h, cooled and air flow crushed to obtain a polymer material feel agent.

[0050] The preparation method of the polypropylene plastic sample includes the following steps: 5g of the polymer material prepared in Example 10 is blended with a feel agent and 95g of polypropylene plastic (grade EPS30R) at 230°C, extruded into granules, and injection molded into a 2mm sample at 230°C to obtain a polypropylene plastic sample.

[0051] The preparation method of a thermoplastic elastomer TPE plastic sample includes the following steps: blending 5 g of the polymer material prepared in Example 10 with a feeling agent and 95 g of a thermoplastic elastomer TPE (commercially available industrial product) at 180°C, extruding and granulating, and injection molding into a 2 mm sample at 180°C to obtain a thermoplastic elastomer TPE plastic sample.

[0052] Comparative Example 1 The preparation method of a polypropylene plastic sample comprises the following steps: polypropylene plastic (brand name EPS30R) is injection molded into a 2 mm sample at 230° C. to obtain a polypropylene plastic sample.

[0053] Comparative Example 2 The preparation method of a thermoplastic elastomer TPE plastic sample comprises the following steps: injection molding a thermoplastic elastomer TPE (commercially available industrial product) into a 2 mm sample at 180° C. to obtain a thermoplastic elastomer TPE plastic sample.

[0054] Performance Testing (1) Sensory performance test The sensory properties of the polypropylene plastic samples and thermoplastic elastomer TPE plastic samples prepared in Examples 1-10 and Comparative Examples 1-2, such as slippery feel, oily feel, and moist feel, were comprehensively evaluated, and the evaluation was divided into excellent, good, average, poor, and very poor; the test results are shown in Table 1; Table 1: Statistical table of sensory performance test results of Examples 1-10 and Comparative Examples 1-2

[0055] It can be seen from Table 1 that the hand feeling agent prepared in the present application can impart good sensory properties to polypropylene and thermoplastic elastomer.

[0056] See also Figure 1 , the hand feeling agent prepared in Example 4 is placed on the conductive adhesive, and is placed in a scanning electron microscope for observation to obtain a SEM photo. Figure 2 The particle size distribution data of the hand feeling agent prepared in Example 4 was tested by a laser force distribution instrument; Figure 1-2 It can be seen that the hand feeling agent prepared in the present application is a monodisperse microspherical substance with a particle size between 2.5-5um. This structure is not easy to agglomerate and has high heat resistance.

[0057] The above is a detailed description of an embodiment of the present invention, but the content is only a preferred embodiment of the present invention and cannot be considered to limit the scope of implementation of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A polymer material feel agent and a preparation method thereof, characterized in that: The steps include: S1: Mixing an acidic aqueous solution containing a siloxane monomer and an alkaline pH adjuster to adjust the pH to 10-11, and controlling the temperature to 25-27° C. to obtain an intermediate reactant system; S2: Stir the intermediate reactant system prepared in S1 to produce a white precipitate, add an acidic aqueous solution containing a fluorine-containing siloxane monomer, add an alkaline pH adjuster to adjust the pH value to 8-10, control the temperature to 25-27° C., let it stand, centrifuge, filter, wash and dry the precipitate to obtain an intermediate reactant; S3: Add the intermediate reactant and molten fatty acid into the reactor, stir and react for 4-5 hours, vacuum extract and crush to obtain a polymer material feel agent.

2. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The mass ratio of the siloxane monomer to the fluorine-containing siloxane monomer in the intermediate reactant system in S2 is 20-50:0.9-3; the mass ratio of the intermediate reactant to the fatty acid in S3 is 80-90:10-20.

3. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The method for preparing the acidic aqueous solution containing siloxane monomers comprises the following steps: Add siloxane monomer and deionized water into a reaction bottle, add an acidic pH adjuster to adjust the pH value to 3-5, control the temperature to 20-25° C., stir and dissolve for 2-4 hours to obtain an acidic aqueous solution containing siloxane monomer.

4. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The method for preparing the acidic aqueous solution of the fluorinated siloxane monomer comprises the following steps: Add fluorinated siloxane monomer and deionized water into a reaction bottle, add an acidic pH regulator to adjust the pH value to 3-5, control the temperature to 20-25° C., stir and dissolve for 4-6 hours to obtain an acidic aqueous solution of fluorinated siloxane monomer.

5. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The molecular structural formula of the siloxane monomer is: In the formula, R is any one of -CH2=CH2, -CH2-CH3, glycidyloxypropyl or phenyl; R1 is any one of -CH3 or -CH2-CH3; R2 is any one of -CH3 or -CH2-CH3; R3 is any one of -CH3 or -CH2-CH3.

6. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The molecular structural formula of the fluorinated siloxane monomer is: In the formula, R is -(F m C) n CH3, n≥2, m≥2; R1 is any one of -CH3 or -CH2-CH3; R2 is any one of -CH3 or -CH2-CH3; R3 is any one of -CH3 or -CH2-CH3.

7. The method for preparing a polymer material using a hand feeling agent according to claim 1, characterized in that: The alkaline pH value regulator is an inorganic base or a fatty amine.

8. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The fatty acid is a fatty acid or a fatty diacid; the molecular formula of the fatty diacid is HOOC(CH2) n COOH, wherein n≥7; the molecular formula of the fatty acid is CH3(CH2) n (OH) m COOH, where n≥10, m=0 or 1.

9. The method for preparing a polymer material feeling agent according to claim 1, characterized in that: The specific steps of vacuum extraction in S3 are: vacuum extraction degree is -0.05 to -0.1MPa, and extraction is performed for 2-3h.

10. A polymer material feel agent, characterized in that: Prepared by the preparation method described in any one of claims 1 to 9.

Citation Information

Patent Citations

  • An organosilicon feel agent and its preparation method

    CN104927057B

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