A silicone elastomer prepolymer emulsion softener and its preparation method and application

Abstract

The invention discloses a silicone elastomer prepolymer emulsion softener and its preparation method and application, wherein the preparation method comprises the steps of: adding polyetheramine and terminal epoxy silicone oil to a flask in a molar ratio of 0-1:2, then adding a solvent accounting for 0-30% of the total amount of the terminal epoxy silicone oil, stirring evenly, heating to 70-110°C and reacting for 0-6 hours to obtain a mixed solution; adding an aminosilane coupling agent to the mixed solution for pre-reaction, the reaction time is 0-1 hour, then adding an emulsifier and an emulsifier, stirring evenly, slowly adding a mixture of acid and water for emulsification, and finally filtering the material for standby use. The silicone elastomer prepolymer emulsion softener prepared by the method of the present invention has good stability and wide applicability. The textile fabric treated by the method has adjustable hydrophilicity, soft hand feel and good smoothness. The key is that its meat elasticity is significantly better than that of general silicone softeners.

Description

Technical Field

[0001] The invention relates to the technical field of polymer materials, and in particular to an organosilicon elastomer prepolymer emulsion softener and a preparation method and application thereof. Background Art

[0002] Silicone elastomers have been widely used in textiles, personal care, construction and other fields due to their excellent softness, delicate skin feel, lasting stiffness, physiological inertness, breathability, gloss and other properties. In addition to the above advantages, silicone elastomers with multi-functional reactivity can also form a network cross-linked structure to further improve the elasticity of silicone elastomers. When external force is applied, the microstructure of the elastomer will change, and when the external force is removed, the elastomer will return to its original state. Compared with traditional linear structure silicone, its resilience is significantly better. Using this function on textiles can give textiles excellent meat elasticity and wrinkle resistance, which is deeply favored by customers.

[0003] Generally, silicone elastomers are made of a two-component composite emulsion of vinyl silicone oil and hydrogen silicone oil, which is reacted under a Pt series catalyst, as shown in the application document with patent publication number CN106832300A. In the textile industry, the amino structure in amino silicone products can give textiles a noticeable soft and smooth feel, and its feel style is favored by customers. However, the presence of amino groups will greatly affect the activity of Pt series catalysts, making the two components incompatible.

[0004] Therefore, the prior art still needs to be improved and developed. Summary of the invention

[0005] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a silicone elastomer prepolymer emulsion softener and a preparation method and application thereof, aiming to solve the problems of poor stability of the silicone softener prepared by the prior art and poor softness and elasticity when used to treat textile fabrics.

[0006] The technical solution of the present invention is as follows:

[0007] A method for preparing a silicone elastomer prepolymer emulsion softener, comprising the steps of:

[0008] Add polyetheramine and terminal epoxy silicone oil into a flask at a molar ratio of 0-1:2, then add a solvent accounting for 0-30% of the total amount of the terminal epoxy silicone oil, stir evenly, heat to 70-110°C and react for 0-6 hours to obtain a mixed solution;

[0009] Add aminosilane coupling agent to the mixed solution for pre-reaction, the reaction time is 0-1 hour, then add auxiliary emulsifier and emulsifier, stir evenly, slowly add a mixture of acid and water for emulsification, and finally filter out the material for standby use.

[0010] The preparation method of the organic silicone elastomer prepolymer emulsion softener, wherein the terminal epoxy silicone oil is a polyether-modified polysiloxane terminated with epoxy groups at both ends, and its structural formula is: Wherein p is between 40-350, q is between 1-15, r is between 0-8, and its molecular weight is between 4000-30000.

[0011] The method for preparing the silicone elastomer prepolymer emulsion softener, wherein the solvent is one of isopropyl alcohol, ethylene glycol monobutyl ether, diethylene glycol butyl ether and dimethyl-2,4-pentanediol.

[0012] The method for preparing the silicone elastomer prepolymer emulsion softener, wherein the aminosilane coupling agent is one of KH-550, KH-602, KH-603, HD-121 and GP-108.

[0013] In the method for preparing the silicone elastomer prepolymer emulsion softener, the auxiliary emulsifier is one or both of glycerol and sorbitol solution.

[0014] The method for preparing the silicone elastomer prepolymer emulsion softener, wherein the emulsifier is a fatty alcohol polyoxyethylene ether surfactant.

[0015] The method for preparing the silicone elastomer prepolymer emulsion softener, wherein the acid is one of glacial acetic acid and citric acid.

[0016] A silicone elastomer prepolymer emulsion softener is prepared by the preparation method of the silicone elastomer prepolymer emulsion softener of the present invention.

[0017] An application of an organosilicon elastomer prepolymer emulsion softener, wherein the organosilicon elastomer prepolymer emulsion softener of the invention is used to treat textile fabrics.

[0018] Beneficial effects: The present invention provides a method for preparing a silicone elastomer prepolymer emulsion softener. The silicone elastomer prepolymer emulsion softener prepared by the method of the present invention has good stability and wide applicability. The hydrophilicity of the textile fabric treated by the method can be adjusted, and the textile fabric has a soft hand feel and good smoothness. The key is that the elasticity is significantly better than that of the general silicone softener. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1The present invention is a flow chart of a method for preparing a silicone elastomer prepolymer emulsion softener. DETAILED DESCRIPTION

[0020] The present invention provides a silicone elastomer prepolymer emulsion softener and a preparation method and application thereof. To make the purpose, technical scheme and effect of the present invention clearer and more specific, the present invention is further described in detail below. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0021] See also Figure 1 , Figure 1 The present invention provides a method for preparing a silicone elastomer prepolymer emulsion softener, as shown in the figure, which comprises the steps of:

[0022] S10, adding polyetheramine and terminal epoxy silicone oil into a flask at a molar ratio of 0-1:2, and then adding a solvent accounting for 0-30% of the total amount of the terminal epoxy silicone oil, stirring evenly, heating to 70-110° C. and reacting for 0-6 hours to obtain a mixed solution;

[0023] S20, adding an aminosilane coupling agent to the mixed solution for pre-reaction, the reaction time is 0-1 hour, then adding an emulsifier and an emulsifier, stirring evenly, slowly adding a mixture of acid and water for emulsification, and finally filtering the material for standby use.

[0024] The organic silicon elastomer prepolymer emulsion softener in the present invention is prepared by uniformly mixing a reactive organic silicon polymer with an emulsifier, an auxiliary emulsifier and an acid in a certain proportion and emulsifying with water. The organic silicon elastomer prepolymer emulsion softener prepared by the method of the present invention has good stability and wide applicability. The hydrophilicity of the textile fabric treated by the organic silicon elastomer prepolymer emulsion softener can be adjusted, and the textile fabric has a soft hand feel and good smoothness. The key is that the elasticity is significantly better than that of the general organic silicon softener.

[0025] In some embodiments, the structural formula of the polyetheramine is H2N(C2H4O) m (C(CH3)CH2O) n NH2 corresponds to one of the commercially available products such as Huntsman's D230, D400, ED-600, ED-900 and other series products, but is not limited thereto.

[0026] In some embodiments, the epoxy-terminated silicone oil is a polyether-modified polysiloxane terminated with epoxy groups at both ends, and its structural formula is: Wherein p is between 40-350, q is between 1-15, r is between 0-8, and its molecular weight is between 4000-30000. In order to achieve better synthesis effect, it is preferred that the molecular weight of the epoxy-terminated silicone oil is controlled within the range of 6000-25000.

[0027] In some embodiments, the solvent is one of isopropyl alcohol, ethylene glycol monobutyl ether, diethylene glycol butyl ether and dimethyl-2,4-pentanediol.

[0028] In some embodiments, the aminosilane coupling agent is one of KH-550, KH-602, KH-603, HD-121 and GP-108. In order to obtain better crosslinking performance and emulsion stability, the amount of the aminosilane coupling agent is preferably controlled between 1-8% (the ratio of the mass of the aminosilane coupling agent to the total mass of the epoxy-terminated silicone oil and the polyetheramine).

[0029] In some embodiments, the co-emulsifier is one or both of glycerol and sorbitol solution. In order to obtain a better hand feel effect, the amount of the co-emulsifier is preferably controlled at 30-100% (the ratio of the mass of the co-emulsifier to the total mass of the terminal epoxy silicone oil, polyetheramine and aminosilane coupling agent).

[0030] In some embodiments, the emulsifier is a fatty alcohol polyoxyethylene ether surfactant, preferably an isomeric tridecanol polyoxyethylene ether surfactant, corresponding to one or a mixture of BASF products TO-5 and TO-7. In order to obtain a better hand feel effect, the amount of the emulsifier is preferably controlled within 10% (the ratio of the mass of the emulsifier to the total mass of the terminal epoxy silicone oil, the polyether amine and the amino silane coupling agent).

[0031] In some embodiments, the acid is one of glacial acetic acid and citric acid.

[0032] In some embodiments, a silicone elastomer prepolymer emulsion softener is also provided, wherein the softener is prepared by the preparation method of the silicone elastomer prepolymer emulsion softener of the present invention.

[0033] In some embodiments, an application of an organosilicon elastomer prepolymer emulsion softener is also provided, wherein the organosilicon elastomer prepolymer emulsion softener of the present invention is used to treat textile fabrics. The organosilicon elastomer prepolymer emulsion softener prepared by the method of the present invention has good stability and wide applicability. The hydrophilicity of the textile fabric treated with the organosilicon elastomer prepolymer emulsion softener can be adjusted, and the textile fabric has a soft feel and good smoothness. The key is that the elasticity is significantly better than that of general organosilicon softeners.

[0034] The present invention will be further explained below by means of specific embodiments:

[0035] Example 1

[0036] Based on a concentration of 30% organic silicon polymer content, 2g of polyetheramine D-400 and 80g of terminal epoxy silicone oil with a molecular weight of about 8000 are added to a four-necked flask, and then 8g of isopropanol is added. Stirring is started. After mixing evenly, the temperature is raised to 80°C and the reaction is carried out at a constant temperature for 6h. Then 0.82g of silane coupling agent KH-602 is added and the reaction is continued for 1 hour. Then 40g of auxiliary emulsifier sorbitol (70%) is added, and 4.0g and 4.2g of emulsifiers TO-5 and TO-7 are added respectively. After stirring evenly, 2.4g / 127.98g of glacial acetic acid / water is slowly added for emulsification. Finally, an organic silicon elastomer prepolymer emulsion softener with a silicon content of 30% is obtained, which is marked as organic silicon elastomer prepolymer emulsion softener 1.

[0037] Example 2

[0038] Based on a concentration of 30% organic silicon polymer content, 80 g of terminal epoxy silicone oil with a molecular weight of about 25,000 was added to a four-necked flask, and then 6.4 g of silane coupling agent KH-603 was added, and then the temperature was raised to 70°C, and the reaction was continued for 0.5 hours, and then 80 g of co-emulsifier glycerol was added, and emulsifiers TO-5 and TO-7 were added in an amount of 6.0 g and 2.2 g respectively. After stirring evenly, citric acid / water was slowly added in an amount of 2.4 g / 111 g for emulsification, and finally an organic silicon elastomer prepolymer emulsion softener with a silicon content of 30% was obtained, which was marked as organic silicon elastomer prepolymer emulsion softener 2.

[0039] Example 3

[0040] Based on a concentration of 30% silicone polymer content, 4g of polyetheramine ED-900 and 80g of terminal epoxy silicone oil with a molecular weight of about 6000 are added to a four-necked flask, and then 25.2g of dimethyl-2,4-pentanediol is added. Stirring is started. After mixing evenly, the temperature is raised to 90°C and the reaction is carried out at a constant temperature for 4h. Then 3.2g of silane coupling agent GP-108 is added and the reaction is continued for 1 hour. Then, 20g / 6.16g of co-emulsifier glycerol / sorbitol (70%) is added, and 2.0g and 5.2g of emulsifiers TO-5 and TO-7 are added respectively. After stirring evenly, 1.2g / 151.91g of glacial acetic acid / water is slowly added for emulsification. Finally, a silicone elastomer prepolymer emulsion softener with a silicon content of 30% is obtained, which is marked as silicone elastomer prepolymer emulsion softener 3.

[0041] Example 4

[0042] Based on a concentration of 30% silicone polymer content, 1.54g of polyetheramine D-230 and 80g of terminal epoxy silicone oil with a molecular weight of about 6000 are added to a four-necked flask, and stirring is started. After mixing evenly, the temperature is raised to 90°C and the reaction is carried out at a constant temperature for 2h. Then, 0.82g of silane coupling agent KH-603 is added, and then 80g of auxiliary emulsifier glycerol is added, and emulsifiers TO-5 and TO-7 are added in an amount of 4.0g and 2.7g respectively. After stirring evenly, glacial acetic acid / water is slowly added in a ratio of 1.2g / 104.28 for emulsification, and finally a silicone elastomer prepolymer emulsion softener with a silicon content of 30% is obtained, which is marked as silicone elastomer prepolymer emulsion softener 4.

[0043] Example 5

[0044] With a silicone polymer content of 30%, 1.14g of polyetheramine D-400 and 80g of terminal epoxy silicone oil with a molecular weight of about 14000 are added to a four-necked flask, and then 24g of diethylene glycol butyl ether is added, stirring is started, and after mixing evenly, the temperature is raised to 100°C, and the reaction is carried out at a constant temperature for 4h, and then 3.24g of silane coupling agent HD-121 is added, and the reaction is continued for 1 hour, and then 60g of co-emulsifier glycerol is added, and 3.0g and 3.2g of emulsifiers TO-5 and TO-7 are added respectively. After stirring evenly, 3g / 103.69g of glacial acetic acid / water is slowly added for emulsification, and finally a silicone elastomer prepolymer emulsion softener with a silicon content of 30% is obtained, which is marked as silicone elastomer prepolymer emulsion softener 5.

[0045] Example 6

[0046] With a silicone polymer content of 30%, 1g of polyetheramine ED-600 and 80g of terminal epoxy silicone oil with a molecular weight of about 20,000 are added to a four-necked flask, and then 16g of ethylene glycol monobutyl ether is added. Stirring is started. After mixing evenly, the temperature is raised to 110°C and the reaction is carried out at a constant temperature for 3h. Then 1.6g of silane coupling agent KH-550 is added and the reaction is continued for 0.5 hour. Then 50g of co-emulsifier glycerol is added, and 3.0g and 4.2g of emulsifiers TO-5 and TO-7 are added respectively. After stirring evenly, citric acid / water is slowly added in an amount of 2.3g / 117.23g for emulsification. Finally, a silicone elastomer prepolymer emulsion softener with a silicon content of 30% is obtained, which is marked as silicone elastomer prepolymer emulsion softener 6.

[0047] Stability evaluation:

[0048] The stability of various silicone elastomer prepolymer emulsion softeners obtained in Examples 1-6 above was tested, as shown in Table 1.

[0049] Table 1 Stability test results

[0050]

[0051] Performance evaluation:

[0052] The emulsions prepared in the above-mentioned implementation cases 1-6 were configured into 80 g / L working solutions, and pure white pure cotton stretch fabrics were finished and fixed at 150-160° C. for 120 seconds. The emulsions were numbered 1-6 in sequence. The results are shown in Table 2.

[0053] Evaluation method: The feel is mainly evaluated in terms of smoothness and fineness, and is blindly touched by multiple experts, with 5 being the best and 1 being the worst.

[0054] Hydrophilicity evaluation: Add water drops on the surface of the finished fabric and calculate the time it takes for the water drop to completely spread and absorb on the fabric, in seconds.

[0055] Table 2 Performance test results

[0056]

[0057] It can be seen from the results in Table 1 and Table 2 that the silicone elastomer prepolymer emulsion softener prepared by the present invention has good stability and wide applicability. The hydrophilicity of the textile fabric treated therewith can be adjusted, and the fabric has a soft hand feel and good smoothness. The key is that the elasticity is significantly better than that of the general silicone softener.

[0058] It should be understood that the application of the present invention is not limited to the above examples. For ordinary technicians in this field, improvements or changes can be made based on the above description. All these improvements and changes should fall within the scope of protection of the claims attached to the present invention.

Claims

1. A method for preparing a silicone elastomer prepolymer emulsion softener, characterized in that: Includes steps: 1.14g of polyetheramine D-400 and 80g of terminal epoxy silicone oil with a molecular weight of 14000 are added to a four-necked flask, and then 24g of diethylene glycol butyl ether is added, and stirring is started. After mixing evenly, the temperature is raised to 100°C, and the reaction is carried out at a constant temperature for 4h, and then 3.24g of silane coupling agent HD-121 is added, and the reaction is continued for 1 hour, and then 60g of auxiliary emulsifier glycerol is added, and 3.0g and 3.2g of emulsifiers TO-5 and TO-7 are added respectively. After stirring evenly, 3g / 103.69g of glacial acetic acid / water is slowly added for emulsification, and finally a silicone elastomer prepolymer emulsion softener with a silicon content of 30% is obtained; The epoxy-terminated silicone oil is a polyether-modified polysiloxane terminated with epoxy groups at both ends, and the structural formula is: Where p is between 40-350, q is between 1-15, and r is between 0-8.

2. A silicone elastomer prepolymer emulsion softener, characterized in that: The softener is prepared by the method for preparing the silicone elastomer prepolymer emulsion softener according to claim 1.

3. An application of a silicone elastomer prepolymer emulsion softener, characterized in that: The silicone elastomer prepolymer emulsion softener according to claim 2 is used for treating textile fabrics.

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