Dimethicone emulsion and preparation method thereof

Abstract

The invention discloses a simethicone emulsion and a preparation method thereof. The simethicone emulsion comprises the following raw materials: 60-65 parts of simethicone, 22-29 parts of deionized water, 6-8 parts of an emulsifier and 0.1-0.2 part of a temperature resistance improver. The emulsifier is a composition of iso-tridecanol polyoxyethylene polyoxypropylene ether and branched-chain secondary alcohol polyoxyethylene ether, and the temperature-resistant improver is a composition of one or two of iso-tridecanol polyoxyethylene ether (5) sodium sulfate or secondary alcohol polyoxyethylene ether sodium sulfate in any proportion. Compared with the prior art, the method provided by the invention has the advantages of simple equipment, simple process and low energy consumption, and the prepared dimethyl silicone oil emulsion has good storage stability, good temperature-resistant stability and small particle size, and is especially suitable for being used as a sewing thread smoothing agent or a fabric smoothing agent.

Description

Technical Field

[0001] The invention relates to a dimethyl silicone oil emulsion and a preparation method thereof, belonging to the technical field of organic silicon. Background Art

[0002] Dimethyl silicone oil emulsion has the advantages of good stability, non-flammability, non-volatility, non-toxicity, no odor, high temperature resistance, corrosion resistance, oxidation resistance, and can be diluted with water in any proportion. It can be widely used in rubber, cosmetics, textile, demoulding, leather and other industries, playing the role of waterproofing, lubrication, demoulding and so on.

[0003] Dimethyl silicone oil emulsion is widely used in textiles. It can be used as the main component of linting oil to reduce the friction coefficient between the needle and the fabric and prevent the linting steel needle from overheating; it can be used as a sewing thread smoothener to provide excellent lubricity and thermal stability, which can greatly improve the quality of the sewing thread. The friction coefficient of the finished sewing thread is low and it is not easy to break during high-speed sewing; it can be used as a leather brightener to provide good brightness and smoothness, and has good environmental performance; it can also be used as a wig softener to give all kinds of wigs excellent smoothness and elasticity, etc. However, dimethyl silicone oil is difficult to emulsify due to its hydrophobicity, and the emulsion is not easy to store for a long time, and the stability is poor. The storage time of dimethyl silicone oil emulsion currently available on the market is generally 12 months, and the emulsion is easy to float and break at high temperature, resulting in adhesion to the fabric, which brings inconvenience to production.

[0004] At present, there are few domestic manufacturers that can produce stable dimethyl silicone oil emulsions, and the market for high-stability methyl silicone oil emulsions is almost monopolized by multinational companies. Some smaller manufacturers are even unable to produce dimethyl silicone oil emulsions, or they are unable to produce stable dimethyl silicone oil emulsions. The dimethyl silicone oil emulsions produced usually float and stratify after being placed for a few months, causing huge losses to downstream production. The emulsification process is the core of preparing dimethyl silicone oil emulsions. At present, the emulsification process of dimethyl silicone oil is mainly based on mechanical phase inversion coarse emulsification plus homogenizer method. This method is a step-by-step method with high energy consumption and complex process. Summary of the invention

[0005] The purpose of the present invention is to solve the problem that dimethyl silicone oil emulsion in the prior art cannot be stably stored for a long time, and to provide a dimethyl silicone oil emulsion that can be stably stored for a long time.

[0006] Another object of the present invention is to provide a method for preparing the above-mentioned dimethyl silicone oil emulsion, which can significantly reduce the emulsification phase transition viscosity, quickly and easily emulsify the dimethyl silicone oil, is simple to operate, and has low energy consumption.

[0007] In order to achieve the above object, the present invention adopts the following technical solutions:

[0008] A dimethyl silicone oil emulsion, comprising the following raw materials in parts by weight: 60-65 parts of dimethyl silicone oil, 22-29 parts of deionized water, 6-8 parts of emulsifier, and 0.1-0.2 parts of temperature resistance enhancer;

[0009] The emulsifier is a composition of isomeric tridecanol polyoxyethylene polyoxypropylene ether and branched secondary alcohol polyoxyethylene ether; the emulsifier used in the present invention can significantly reduce the emulsification phase transition viscosity, has extremely low requirements for emulsification equipment, and can quickly and simply prepare a dimethyl silicone oil emulsion with high solid content and low viscosity, and has a small particle size, good centrifugal stability, and good freeze-thaw stability.

[0010] In the molecular structure of the isomeric tridecanol polyoxyethylene polyoxypropylene ether, the number of oxyethylene groups is 7 to 9, and the number of oxypropylene groups is 2 to 4.

[0011] The temperature resistance enhancing agent is one of isomeric tridecanol polyoxyethylene ether (5) sodium sulfate or secondary alcohol polyoxyethylene ether (15-S-5) sodium sulfate or a combination of the two in any proportion.

[0012] Furthermore, the emulsifier is a composition of isomeric tridecanol polyoxyethylene polyoxypropylene ether and branched secondary alcohol polyoxyethylene ether in a mass ratio of (1-5):1.

[0013] Furthermore, the viscosity of the dimethyl silicone oil at 25° C. is 1000 cst to 5000 cst.

[0014] Furthermore, the temperature resistance enhancing agent is a composition of isomeric tridecanol polyoxyethylene ether (5) sodium sulfate and secondary alcohol polyoxyethylene ether (15-S-5) sodium sulfate in a mass ratio of 0.75:1, which can significantly improve heat storage stability and boiling stability.

[0015] The preparation method of the above-mentioned dimethyl silicone oil emulsion comprises the following steps:

[0016] (1) Add dimethyl silicone oil, emulsifier, and temperature-resistant enhancer into a high-speed disperser in sequence according to the metering ratio, and mix them evenly at a speed of 400 to 600 rpm;

[0017] (2) Add deionized water in batches, increase the speed of the high-speed disperser to 1400-1500 rpm, and disperse at high speed for 30-40 minutes. After the emulsion is evenly dispersed, continue to add deionized water;

[0018] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300-500 rpm, and the dispersion is continued for 10-15 minutes to obtain a dimethyl silicone oil emulsion.

[0019] The dimethyl silicone oil emulsion is used as a sewing thread smoothing agent or a fabric smoothing agent.

[0020] Compared with the prior art, the present invention has the following beneficial effects:

[0021] 1) The emulsion prepared by traditional emulsifiers such as linear fatty alcohol polyoxyethylene ethers has the problems of poor stability, high phase transition viscosity, large emulsion particle size, etc. The emulsifiers used in the present invention are all isomeric alcohol polyoxyethylene ethers, which can significantly reduce the phase transition viscosity, improve the emulsification efficiency, have low requirements for emulsification equipment, reduce production costs, and the prepared emulsion has good storage stability, good temperature stability, and small particle size;

[0022] 2) At present, the main method for emulsifying dimethyl silicone oil is a mechanical phase transfer rough emulsification method plus a high-pressure homogenizer post-processing method, which has the problems of high energy consumption and complex production process. The present invention adopts a one-step emulsification method, which simplifies the process, has simple equipment and low energy consumption;

[0023] 3) The dimethyl silicone oil emulsion prepared by the present invention has a small particle size, a freeze-thaw stability of more than 20 times, and a room temperature storage time of up to 36 months;

[0024] 4) The content of commercially available dimethyl silicone oil emulsion is basically ≤60%, while the content of the dimethyl silicone oil emulsion prepared by the present invention is 65-70%, which can effectively reduce transportation costs, reduce energy consumption, and meet environmental protection requirements;

[0025] 5) The present invention adopts a common high-speed disperser as the emulsification equipment of the emulsion. Compared with the high-pressure homogenizer, the equipment is simple, the production cost is low and the particle size of the emulsion produced is smaller. DETAILED DESCRIPTION

[0026] The technical solution of the present invention is described clearly and completely below in conjunction with specific embodiments.

[0027] In the following embodiments and comparative examples, the temperature resistance enhancers used are compositions of sodium sulfate of isotridecyl alcohol polyoxyethylene ether (5) and sodium sulfate of secondary alcohol polyoxyethylene ether (15-S-5) at a mass ratio of 0.75:1; the branched secondary alcohol polyoxyethylene ether TMN-10 and branched secondary alcohol polyoxyethylene ether TMN-6 used are purchased from Dow Chemical; the linear fatty alcohol polyoxyethylene ether AEO-4, AEO-5, AEO-9, and AEO-15 used are purchased from Petronas, and the isotridecyl alcohol polyoxyethylene ether 1305, 1307, and 1310 are purchased from Tongkun Company, but are not limited thereto.

[0028] Example 1

[0029] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 6.7 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 1.3 grams of branched secondary alcohol polyoxyethylene ether TMN-10, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 7 oxyethylene groups and 2 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0030] Preparation method of dimethyl silicone oil emulsion:

[0031] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0032] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0033] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0034] Example 2

[0035] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 4 grams of branched secondary alcohol polyoxyethylene ether TMN-6, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 9 oxyethylene groups and 3 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0036] Preparation method of dimethyl silicone oil emulsion:

[0037] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0038] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0039] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0040] Example 3

[0041] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 22 grams of deionized water, 6.2 grams of an emulsifier (composed of 3.1 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 3.1 grams of branched secondary alcohol polyoxyethylene ether TMN-6, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 9 oxyethylene groups and 3 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0042] Preparation method of dimethyl silicone oil emulsion:

[0043] (1) 62 g of dimethyl silicone oil, 6.2 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0044] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0045] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0046] Example 4

[0047] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 2000 cst at 25°C, 29 grams of deionized water, 7.8 grams of an emulsifier (composed of 3.9 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 3.9 grams of branched secondary alcohol polyoxyethylene ether TMN-6, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 9 oxyethylene groups and 3 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0048] Preparation method of dimethyl silicone oil emulsion:

[0049] (1) 62 g of dimethyl silicone oil, 7.8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0050] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0051] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0052] Example 5

[0053] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 5000 cst at 25°C, 29 grams of deionized water, 7.8 grams of an emulsifier (composed of 3.9 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 3.9 grams of branched secondary alcohol polyoxyethylene ether TMN-6, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 9 oxyethylene groups and 3 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0054] Preparation method of dimethyl silicone oil emulsion:

[0055] (1) 62 g of dimethyl silicone oil, 7.8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0056] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0057] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300 rpm, and the dispersion is carried out for 20 minutes to obtain a dimethyl silicone oil emulsion.

[0058] Example 6

[0059] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 6.4 grams of an emulsifier (composed of 5.3 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether 1307P and 1.1 grams of branched secondary alcohol polyoxyethylene ether TMN-10, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 7 oxyethylene groups and 2 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0060] Preparation method of dimethyl silicone oil emulsion:

[0061] (1) 62 g of dimethyl silicone oil, 6.4 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0062] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0063] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0064] Example 7

[0065] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 6.4 grams of an emulsifier (composed of 3.2 grams of isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether and 3.2 grams of branched secondary alcohol polyoxyethylene ether TMN-6, wherein the molecular structure of the isomeric tridecyl alcohol polyoxyethylene polyoxypropylene ether comprises 9 oxyethylene groups and 3 oxypropylene groups), and 0.1 grams of a temperature resistance enhancer.

[0066] Preparation method of dimethyl silicone oil emulsion:

[0067] (1) 62 g of dimethyl silicone oil, 6.4 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0068] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0069] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0070] Comparative Example 1

[0071] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of isomeric tridecanol polyoxyethylene ether 1305 and 4 grams of isomeric tridecanol polyoxyethylene ether 1307), and 0.1 grams of a temperature resistance enhancer.

[0072] Preparation method of dimethyl silicone oil emulsion:

[0073] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0074] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0075] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0076] Comparative Example 2

[0077] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of isomeric tridecanol polyoxyethylene ether 1305 and 4 grams of isomeric tridecanol polyoxyethylene ether 1310), and 0.1 grams of a temperature resistance enhancer.

[0078] Preparation method of dimethyl silicone oil emulsion:

[0079] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0080] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0081] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0082] Comparative Example 3

[0083] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of isomeric tridecanol polyoxyethylene ether 1305 and 4 grams of branched secondary alcohol polyoxyethylene ether TMN-10), and 0.1 grams of a temperature resistance enhancer.

[0084] Preparation method of dimethyl silicone oil emulsion:

[0085] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0086] (2) Add deionized water in batches of 3 g / time, increase the speed of the high-speed disperser to 1440 rpm, and disperse at high speed for 40 minutes. Continue to add deionized water after the emulsion is evenly dispersed;

[0087] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 500 rpm, and the dispersion is carried out for 15 minutes to obtain a dimethyl silicone oil emulsion.

[0088] Comparative Example 4

[0089] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of linear fatty alcohol polyoxyethylene ether AEO-4 and 4 grams of linear fatty alcohol polyoxyethylene ether AEO-15), and 0.1 grams of a temperature resistance enhancer.

[0090] Preparation method of dimethyl silicone oil emulsion:

[0091] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0092] (2) Deionized water was added in batches of 3 g / time, and the speed of the high-speed disperser was increased to 1440 rpm. The phase inversion viscosity was relatively large, and the dispersion time was 90 min. After the emulsion was evenly dispersed, deionized water was continued to be added;

[0093] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300 rpm, and the dispersion is carried out for 20 minutes to obtain a dimethyl silicone oil emulsion.

[0094] Comparative Example 5

[0095] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of linear fatty alcohol polyoxyethylene ether AEO-5 and 4 grams of linear fatty alcohol polyoxyethylene ether AEO-15), and 0.1 grams of a temperature resistance enhancer.

[0096] Preparation method of dimethyl silicone oil emulsion:

[0097] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0098] (2) Deionized water was added in batches of 3 g / time, and the speed of the high-speed disperser was increased to 1440 rpm. The phase inversion viscosity was relatively large, and the dispersion time was 90 min. After the emulsion was evenly dispersed, deionized water was continued to be added;

[0099] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300 rpm, and the dispersion is carried out for 20 minutes to obtain a dimethyl silicone oil emulsion.

[0100] Comparative Example 6

[0101] A dimethyl silicone oil emulsion comprises the following raw materials: 62 grams of dimethyl silicone oil with a viscosity of 1000 cst at 25°C, 29 grams of deionized water, 8 grams of an emulsifier (composed of 4 grams of linear fatty alcohol polyoxyethylene ether AEO-7 and 4 grams of linear fatty alcohol polyoxyethylene ether AEO-9), and 0.1 grams of a temperature resistance enhancer.

[0102] Preparation method of dimethyl silicone oil emulsion:

[0103] (1) 62 g of dimethyl silicone oil, 8 g of emulsifier, and 0.1 g of temperature-resistant enhancer were sequentially added into a high-speed disperser and mixed at a speed of 500 rpm for 10 minutes;

[0104] (2) Deionized water was added in batches of 3 g / time, and the speed of the high-speed disperser was increased to 1440 rpm. The phase inversion viscosity was relatively large, and the dispersion time was 1 h. After the emulsion was evenly dispersed, deionized water was continued to be added;

[0105] (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300 rpm, and the dispersion is carried out for 20 minutes to obtain a dimethyl silicone oil emulsion.

[0106] 1. The particle size, centrifugal stability, heat storage stability and freeze-thaw stability of the dimethyl silicone oil emulsions prepared in Examples 1-7 and Comparative Examples 1-6 were tested. The particle size test was performed using Dandong Bettersize 2600 to test the particle sizes D50 and D90. The centrifugal stability test method was as follows: 6-7 ml of the emulsion was placed in a centrifuge tube, placed in a Xiangyi L55 centrifuge, and run at 3000r for 30min to observe whether it was stratified. The heat storage stability test method was as follows: 60 g of the emulsion was placed in a 100 ml plastic transparent bottle, placed in a 45°C incubator, and the emulsion was observed until unstable states such as stratification and oil floating appeared, and the number of days was recorded. The freeze-thaw stability test method was as follows: 60 g of the emulsion was placed in a 100 ml plastic transparent bottle, placed in a refrigerator at minus 10°C to completely freeze it, taken out, and placed at room temperature until the frozen emulsion melted into a flowing liquid, and the emulsion was observed to be unstable such as stratification and oil floating. If the emulsion was stable, it was continued to be placed in a refrigerator for freezing and solidification, and the operation was repeated, and the number of times was recorded. The test results are shown in Table 1:

[0107] Table 1

[0108]

[0109] It can be seen from the test results in Table 1 that, compared with the dimethyl silicone oil emulsions prepared in Comparative Examples 1-6, the dimethyl silicone oil emulsions prepared by the methods of Examples 1-7 of the present invention have smaller particle sizes and better stability.

[0110] 2. Test the high temperature stability of the dimethyl silicone oil emulsions prepared in Examples 1, 2, 3, and 6.

[0111] Test method: Take 10 grams of dimethyl silicone oil emulsion, add water to 1000 grams, put it on the electric stove and boil it at 100℃ for 20 minutes, turn off the electric stove, and observe the wall of the beaker and the floating situation on the surface of the solution. The test results are shown in Table 2:

[0112] Table 2 High temperature stability test results

[0113] Dimethicone emulsion High temperature stability Example 1 There is no floating on the surface of the emulsion, and no oily substance appears on the wall of the cup Example 2 There is no floating on the surface of the emulsion, and no oily substance appears on the wall of the cup Example 3 There is no floating on the surface of the emulsion, and no oily substance appears on the wall of the cup Example 6 There is no floating on the surface of the emulsion, and no oily substance appears on the wall of the cup

[0114] According to the test results in Table 2, the dimethyl silicone oil emulsion prepared in the embodiment of the present invention has good high temperature stability.

[0115] 3. Application testing

[0116] (1) The dimethyl silicone oil emulsion prepared in Examples 1-2 of the present invention was used as a sewing thread smoothing agent to test its smoothness, and compared with the dimethyl silicone oil emulsions prepared in Comparative Examples 2, 3, and 5, and commercially available domestic sewing thread smoothing agent product A (dimethyl silicone oil emulsion, solid content 61.2%, heat storage stability 2 days) and foreign sewing thread smoothing agent product A (dimethyl silicone oil emulsion, solid content 60.5%, heat storage stability 4 days).

[0117] Test method: The amount of sewing thread smoothing agent is 2% (owf), the bath ratio is 1:10, and the concentration of sewing thread smoothing agent is calculated according to (owf) and bath ratio. The sewing thread smoothing agent is diluted to the corresponding concentration with deionized water, and the pH is adjusted to 5.0 with acetic acid to obtain the smoothing agent working solution. The cotton cheese yarn (single yarn weight 1kg) is immersed in the smoothing agent working solution, immersed at 40℃ for 30min, dehydrated and dried, and balanced tested at constant temperature and humidity (20±1℃, 65±2%RH) for 24h. The dynamic friction coefficient of the finished yarn with stainless steel at a pre-tension of 30cN is tested using a yarn dynamic friction coefficient tester (drawing rate 60m / min, test 1min). The lower the dynamic friction coefficient, the better the yarn smoothness.

[0118] According to the GB / T 3916-2013 method, the breaking strength of the yarn was tested using a Changyi Fangyi YG020A electronic single yarn strength tester, and the average value was taken after 50 tests.

[0119] The test results are shown in Table 3:

[0120] Table 3 Dynamic friction coefficient and breaking strength test results

[0121] Dimethicone emulsion Dynamic friction coefficient Breaking strength(cN) Blank Yarn breakage 257.3 Example 1 0.238 249.5 Example 2 0.227 251.3 Comparative Example 2 0.416 254.1 Comparative Example 3 0.399 252.7 Comparative Example 5 0.401 250.6 Domestic sewing thread smoothing agent product A 0.319 242.9 Foreign sewing thread smoothing agent product A 0.323 250.6

[0122] According to the test results in Table 3, it can be seen that compared with comparative examples 2, 3, 5 and the domestic sewing thread smoother product A and foreign sewing thread smoother product A commonly used in this field, the cotton bobbin yarn treated with embodiments 1-2 of the present invention as a sewing thread smoother can significantly reduce the dynamic friction coefficient and ensure that the breaking strength decreases less.

[0123] (2) The dimethyl silicone oil emulsions prepared in Examples 1-2 of the present invention were used as fabric smoothing agents to test their smoothness, and were compared with the dimethyl silicone oil emulsions prepared in Comparative Examples 2, 3, and 5, as well as commercially available domestic fabric smoothing agent product B (dimethyl silicone oil emulsion, solid content 60.3%, heat storage stability 1 day) and foreign fabric smoothing agent product B (dimethyl silicone oil emulsion, solid content 63.2%, heat storage stability 3 days).

[0124] Test method: Dilute the fabric smoothing agent with deionized water to a concentration of 30g / L solution, and use acetic acid to adjust the pH to 5.0 to obtain the working solution. Immerse the cotton knitted fabric and the polyester knitted fabric in the working solution respectively, and after being padded twice by a small padder (with a liquid rate of 90%), dry (105℃, 10min), and then balance the test at a constant temperature and humidity (20±1℃, 65±2%RH) for 24h. The hand touch method is used to evaluate the smoothness of the finished fabric. No less than 5 professionals are selected to participate in the evaluation. The unfinished fabric is used as a blank sample, and the smoothness is set as 1 point. The highest score is 5 points, and the lowest score is 1 point. The average value is taken. The larger the value, the better the smoothness.

[0125] The test results are shown in Table 4:

[0126] Table 4 Hand feel test results

[0127]

[0128]

[0129] According to the experimental results in Table 4, compared with Comparative Examples 2, 3, 5 and the domestic fabric smoothing agent product B and foreign fabric smoothing agent product B commonly used in the art, the all-cotton knitted fabrics and all-polyester knitted fabrics treated with the dimethyl silicone oil emulsion prepared in Examples 1-2 of the present invention as a fabric smoothing agent have excellent smoothing properties, which are more outstanding than the smoothness of commercial products.

Claims

1. A dimethyl silicone oil emulsion, characterized in that: The dimethyl silicone oil emulsion comprises the following raw materials in parts by weight: 60-65 parts of dimethyl silicone oil, 22-29 parts of deionized water, 6-8 parts of emulsifier, and 0.1-0.2 parts of temperature resistance enhancer; The emulsifier is a composition of isomeric tridecanol polyoxyethylene polyoxypropylene ether and branched secondary alcohol polyoxyethylene ether; The temperature resistance enhancing agent is one of isomeric tridecanol polyoxyethylene ether (5) sodium sulfate or secondary alcohol polyoxyethylene ether (15-S-5) sodium sulfate or a combination of the two in any proportion.

2. The dimethyl silicone oil emulsion according to claim 1, characterized in that The emulsifier is a composition of isomeric tridecanol polyoxyethylene polyoxypropylene ether and branched secondary alcohol polyoxyethylene ether in a mass ratio of (1-5):

1.

3. The dimethyl silicone oil emulsion according to claim 1, characterized in that In the molecular structure of the isomeric tridecanol polyoxyethylene polyoxypropylene ether, the number of oxyethylene groups is 7 to 9, and the number of oxypropylene groups is 2 to 4.

4. The dimethyl silicone oil emulsion according to claim 1, characterized in that The viscosity of the dimethyl silicone oil at 25° C. is 1000 cst to 5000 cst.

5. The dimethyl silicone oil emulsion according to claim 1, 2, 3 or 4, characterized in that: The temperature resistance enhancing agent is a composition of isomeric tridecanol polyoxyethylene ether (5) sodium sulfate and secondary alcohol polyoxyethylene ether (15-S-5) sodium sulfate in a mass ratio of 0.75:

1.

6. The method for preparing the dimethyl silicone oil emulsion according to any one of claims 1 to 5, characterized in that: The following steps are involved: (1) Add dimethyl silicone oil, emulsifier, and temperature-resistant enhancer into a high-speed disperser in sequence according to the metering ratio, and mix them evenly at a speed of 400 to 600 rpm; (2) Add deionized water in batches, increase the speed of the high-speed disperser to 1400-1500 rpm, and disperse at high speed for 30-40 minutes. After the emulsion is evenly dispersed, continue to add deionized water; (3) After the phase inversion is completed, the remaining deionized water is quickly added, the speed of the high-speed disperser is reduced to 300-500 rpm, and the dispersion is continued for 10-15 minutes to obtain a dimethyl silicone oil emulsion.

7. Use of the dimethyl silicone oil emulsion according to any one of claims 1 to 5 as a sewing thread smoothing agent or a fabric smoothing agent.

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