Compound emulsifier as well as preparation method and application thereof

Abstract

The invention provides a compound emulsifier as well as a preparation method and application thereof. The compound emulsifier comprises isomeric alcohol polyoxyethylene ether and polyether modified silicone oil as shown in a formula I, n is selected from an integer from 13 to 40, and m is an integer from 20 to 70. The compound emulsifier disclosed by the invention comprises the isomeric alcohol polyoxyethylene ether and the polyether modified silicone oil, and through synergistic cooperation of the isomeric alcohol polyoxyethylene ether and the polyether modified silicone oil, the influence of an amino silicone oil emulsion system on the hand feeling and fastness of a finished fabric can be effectively reduced, and meanwhile, the stability of the amino silicone oil emulsion system can also be improved. # imgabs0 #

Description

Technical Field

[0001] The invention relates to the technical field of textile finishing auxiliaries, and in particular to a composite emulsifier and a preparation method and application thereof. Background Art

[0002] Amino silicone oil is a product in which some methyl groups (including side chains and terminal positions) in dimethyl silicone oil are replaced by amino hydrocarbon groups. The presence of amino hydrocarbon groups gives silicone oil reactivity, adsorption and lubrication properties, so it has been widely used in textile softening finishing agents. Amino silicone oil with a high amino content has better emulsification and emulsion stability, and has more anchoring points on textile fabrics, which makes it more adsorbable on fabrics, but at the same time, the treated fabrics are more prone to yellowing, which also limits the application scenarios of such silicone oils. In addition, compared with block silicone oils with self-emulsification functions, amino silicone oils need to be emulsified with the help of emulsifiers before they can be prepared into emulsions for textile finishing. When using the emulsion for finishing, the emulsifier molecules hinder the reaction of amino silicone oil with textiles and hinder the free movement of the siloxane segments of amino silicone oil. Therefore, excessive use of emulsifiers will lead to a decrease in the feel and finishing fastness of the fabric after finishing with amino silicone oil emulsions.

[0003] At present, the emulsifiers commonly used in amino silicone oil systems are alkylphenol polyoxyethylene ether (APEO) and isomeric alcohol polyoxyethylene ether (AEO). Among them, although alkylphenol polyoxyethylene ether has excellent emulsification effect, it has the disadvantages of being toxic to the environment, difficult to biodegrade, and its biodegradable metabolites are potentially harmful to the environment. Isomeric alcohol polyoxyethylene ether is an important polyoxyethylene type nonionic surfactant. It has the advantages of strong emulsification ability, high surface activity, resistance to hard water, good chemical stability and environmental compatibility in a wide pH range, and is therefore widely used in the fields of textiles, leather, daily chemical cleaning, etc. Since isomeric alcohol polyoxyethylene ether is a water-soluble emulsifier, it has a great influence on the hydrophilicity, feel and washing fastness of the fabric, and the pour point and glass transition temperature of isomeric alcohol polyoxyethylene ether are relatively high. A higher pour point and a higher glass transition temperature are not conducive to emulsification and will reduce the low-temperature storage stability of the prepared emulsion. At the same time, the surface adsorbed film formed by a single, pure isomeric alcohol polyoxyethylene ether as an emulsifier is not arranged tightly, and the formed film strength is low, which will also lead to poor stability of the emulsion.

[0004] Therefore, there is an urgent need for a composite emulsifier and a preparation method and application thereof to solve the deficiencies of the prior art. Summary of the invention

[0005] The object of the present invention is to provide a composite emulsifier and a preparation method and application thereof, wherein the composite emulsifier can reduce the influence of an amino silicone oil emulsion system on the hydrophilicity, hand feel and washing fastness of fabrics after finishing, and can also improve the stability of the amino silicone oil emulsion system.

[0006] To achieve the above object, the present invention provides a composite emulsifier, comprising isomeric alcohol polyoxyethylene ether and a polyether-modified silicone oil as shown in Formula 1:

[0007]

[0008] Wherein, n is selected from an integer of 13 to 40, and m is selected from an integer of 20 to 70.

[0009] Compared with the prior art, the composite emulsifier of the present invention comprises polyether-modified silicone oil and isomeric alcohol polyoxyethylene ether, wherein the polyethylene glycol segment in the polyether-modified silicone oil is a hydrophilic segment, has excellent hygroscopicity, and can improve hydrophilicity; the organic silicon oxygen segment has significant hydrophobicity, and due to the flexibility of the main chain and the lower intermolecular force, it shows lower viscosity and surface tension than hydrocarbons, and has a stronger film-forming ability. By adjusting the length of the polyethylene glycol segment and the organic silicon oxygen segment in the polyether-modified silicone oil, the HLB value of the composite emulsifier can be regulated to match the amino silicone oil with different HLB values, thereby obtaining a better emulsification effect. In addition, the long-chain unbranched structure of the polyether-modified silicone oil of the present invention and the distribution of its hydrophilic groups are conducive to reducing interfacial tension in water, and can form a charged hydrophilic protective layer on the surface of the emulsion particles. At the same time, due to the large relative molecular mass, it can form a larger steric hindrance on the surface of the emulsion particles, thereby reducing the mutual aggregation of oil droplets and making the emulsion more stable. And because the polyether-modified silicone oil itself has a certain hand feel, based on the principle of similar compatibility, the polyether-modified silicone oil of the present invention has good compatibility with the amino silicone oil, and the presence of the O element on the polyether-modified silicone oil can reduce the influence on the stability of the amino silicone oil emulsion and the influence on the hand feel and fastness of the finished product. The present invention can overcome the disadvantages of the high pour point and glass transition temperature of the isomeric alcohol polyoxyethylene ether emulsifier affecting the low-temperature stability of the amino silicone oil emulsion by compounding the water-soluble isomeric alcohol polyoxyethylene ether with the oil-soluble polyether-modified silicone oil, and can make the polar OH on the long chain of the polyether-modified silicone oil cooperate with the isomeric alcohol polyoxyethylene ether at the oil-water interface to form an interface film with a relatively tight directional arrangement and high strength, so that the interface film can exert resistance to better prevent the polymerization between the emulsion particles, thereby achieving the purpose of improving the stability of the amino silicone oil emulsion system.

[0010] As a preferred technical solution, the mass ratio of the isomeric alcohol polyoxyethylene ether of the present invention to the polyether-modified silicone oil is 1 to 5: 1. Specifically, the mass ratio of the isomeric alcohol polyoxyethylene ether of the present invention to the polyether-modified silicone oil can be, but is not limited to, 1: 1, 2: 1, 2.4: 1, 3.6: 1, 4: 1, 4.6: 1, 5: 1.

[0011] As a preferred technical solution, the isomeric alcohol polyoxyethylene ether of the present invention is selected from at least one of isomeric decanol polyoxyethylene ether, isomeric undecanol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether.

[0012] The second aspect of the present invention provides a method for preparing the aforementioned composite emulsifier, comprising:

[0013] (1) Preparation of polyether-modified silicone oil: hydrogen-terminated silicone oil and allyl polyethylene glycol are mixed in a solvent at elevated temperature, a platinum catalyst is added to react, and the polyether-modified silicone oil is obtained by post-treatment;

[0014] (2) Preparation of composite emulsifier: The polyether-modified silicone oil and the isomeric alcohol polyoxyethylene ether are stirred and mixed uniformly.

[0015] Specifically, the preparation route of the polyether-modified silicone oil of the present invention is as follows:

[0016]

[0017] wherein n is selected from an integer of 13 to 40, and m is selected from an integer of 20 to 70. The present invention reacts the terminal hydrogen silicone oil having the above molecular weight range with allyl polyethylene glycol, and can adjust the siloxy segment and the ether segment in the polyether-modified silicone oil by selecting terminal hydrogen silicone oil and allyl polyethylene glycol of different molecular weights, thereby obtaining a polyether-modified silicone oil with an HLB value of 8 to 14 to match the amino silicone oil with an HBL value of 8 to 14, thereby obtaining a better emulsification effect, and can adjust the structure of the polyether-modified silicone oil according to actual needs to meet the needs of different hand feel and hydrophilic properties of the product after finishing with the amino silicone oil emulsion system.

[0018] As a preferred technical solution, the molar ratio of active hydrogen in the hydrogen-terminated silicone oil of the present invention to vinyl in the allyl polyethylene glycol is 1:1 to 1.5. Specifically, the molar ratio of active hydrogen in the hydrogen-terminated silicone oil of the present invention to vinyl in the allyl polyethylene glycol can be, but is not limited to, 1:1, 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5.

[0019] As a preferred technical solution, based on the sum of the masses of the terminal hydrogen silicone oil and the allyl polyethylene glycol, the amount of the platinum catalyst added in the present invention is 1ppm to 30ppm. Specifically, the amount of the platinum catalyst added can be, but is not limited to, 1ppm, 2ppm, 4ppm, 6ppm, 8ppm, 10ppm, 12ppm, 14ppm, 16ppm, 18ppm, 20ppm, 25ppm, 30ppm.

[0020] As a preferred technical solution, the platinum catalyst of the present invention is selected from at least one of chloroplatinic acid, Custer's catalyst and Speier's catalyst, and the solvent is selected from at least one of isopropanol and ethylene glycol monobutyl ether.

[0021] As a preferred technical solution, the post-treatment of the present invention is specifically to distill the reaction liquid after the mixed reaction until the solvent is removed.

[0022] As a preferred technical solution, in (1), the present invention mixes and heats to 70°C to 80°C, the reaction temperature is 70°C to 85°C, and the reaction time is 3h to 12h. Specifically, the present invention mixes and heats to a temperature of but not limited to 70°C, 72°C, 74°C, 76°C, 78°C, 80°C; the reaction temperature can be but not limited to 70°C, 72°C, 74°C, 76°C, 78°C, 80°C, 83°C, 85°C; the reaction time can be but not limited to 3h, 4h, 6h, 8h, 10h, 12h.

[0023] As a preferred technical solution, in (2), the temperature of the stirring and mixing of the present invention is 25°C to 30°C, the time is 30min to 60min, and the speed is 50r / min to 100r / min. Specifically, the temperature of the stirring and mixing of the present invention may be, but not limited to, 25°C, 26°C, 27°C, 28°C, 29°C, 30°C; the time of the stirring and mixing may be, but not limited to, 30min, 35min, 40min, 45min, 50min, 55min, 60min; the speed of the stirring and mixing is 50r / min, 60r / min, 70r / min, 80r / min, 90r / min, 100r / min.

[0024] The third aspect of the present invention provides an application of the aforementioned composite emulsifier in amino silicone oil. The mass ratio of amino silicone oil to composite emulsifier may be 1:0.1 to 0.6. Specifically, the mass ratio of amino silicone oil to composite emulsifier may be, but is not limited to, 1:0.1, 1:0.2, 1:0.3, 1:0.4, 1:0.5, 1:0.6. Applying the composite emulsifier of the present invention to the amino silicone oil emulsion system can reduce the impact on the feel and fastness of the fabric after finishing, and at the same time improve the stability of the amino silicone oil emulsion system. DETAILED DESCRIPTION

[0025] In order to better illustrate the purpose, technical scheme and beneficial effects of the present invention, the present invention will be further described below in conjunction with specific embodiments. It should be noted that the following implementation method is a further explanation of the present invention and should not be used as a limitation of the present invention.

[0026] Example 1

[0027] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0028]

[0029] Wherein, n is 13, m is 25, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether to polyether modified silicone oil is 2:1.

[0030] The preparation method of the composite emulsifier comprises:

[0031] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72°C. Then 20 ppm of chloroplatinic acid was added and reacted at 75°C for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil.

[0032] (2) 200 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0033] Example 2

[0034] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0035]

[0036] Wherein, n is 20, m is 45, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 2:1.

[0037] The preparation method of the composite emulsifier comprises:

[0038] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1540 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 2038 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0039] (2) 200 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0040] Example 3

[0041] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0042]

[0043] Among them, n is 35, m is 62, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 2:1.

[0044] The preparation method of the composite emulsifier comprises:

[0045] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 2650 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 2786 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0046] (2) 200 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0047] Example 4

[0048] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0049]

[0050] Wherein, n is 13, m is 25, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether to polyether modified silicone oil is 3:1.

[0051] The preparation method of the composite emulsifier comprises:

[0052] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.2 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0053] (2) 300 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0054] Example 5

[0055] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0056]

[0057] Among them, n is 13, m is 25, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 4:1.

[0058] The preparation method of the composite emulsifier comprises:

[0059] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.2 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0060] (2) 400 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0061] Example 6

[0062] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0063]

[0064] Among them, n is 13, m is 25, and the mass ratio of isomeric tridecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 2:1.

[0065] The preparation method of the composite emulsifier comprises:

[0066] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.2 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in ethylene glycol monobutyl ether and heated to 75° C., and then 25 ppm of chloroplatinic acid was added, and the mixture was reacted at 78° C. for 9 h. The solvent was evaporated under vacuum until the ethylene glycol monobutyl ether was removed to obtain polyether-modified silicone oil;

[0067] (2) 200 g of isomeric tridecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 28° C. for 45 min at a stirring speed of 70 r / min to obtain a composite emulsifier.

[0068] Example 7

[0069] This embodiment provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0070]

[0071] Among them, n is 13, m is 25, and the mass ratio of isomeric decanol polyoxyethylene ether and polyether modified silicone oil is 2:1.

[0072] The preparation method of the composite emulsifier comprises:

[0073] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.0 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 78° C., and then 18 ppm of chloroplatinic acid was added, and the mixture was reacted at 83° C. for 8 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0074] (2) 200 g of isomeric decanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 30° C. for 50 min at a stirring speed of 90 r / min to obtain a composite emulsifier.

[0075] Comparative Example 1

[0076] This comparative example provides a composite emulsifier, including the polyether-modified silicone oil shown below.

[0077]

[0078] Among them, n is 13 and m is 25.

[0079] The preparation method of the composite emulsifier comprises:

[0080] 1 mol of terminal hydrogen silicone oil with a molecular weight of 1022 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72°C. Then 20 ppm of chloroplatinic acid was added and reacted at 75°C for 10 hours. The solvent was evaporated in vacuo until the isopropanol was removed to obtain polyether modified silicone oil.

[0081] Comparative Example 2

[0082] This comparative example provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether, and the isomeric undecanol polyoxyethylene ether is commonly available on the market.

[0083] Comparative Example 3

[0084] This comparative example provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0085]

[0086] Wherein, n is 13, m is 25, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether to polyether modified silicone oil is 1:2.

[0087] The preparation method of the composite emulsifier comprises:

[0088] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0089] (2) 100 g of isomeric undecanol polyoxyethylene ether and 200 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0090] Comparative Example 4

[0091] This comparative example provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0092]

[0093] Among them, n is 13, m is 25, and the mass ratio of isomeric undecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 6:1.

[0094] The preparation method of the composite emulsifier comprises:

[0095] (1) 1 mol of hydrogen-terminated silicone oil with a molecular weight of 1022 and 1.5 mol of allyl polyethylene glycol with a molecular weight of 1158 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h. The solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0096] (2) 600 g of isomeric undecanol polyoxyethylene ether and 100 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0097] Comparative Example 5

[0098] This comparative example provides a composite emulsifier, including isomeric undecanol polyoxyethylene ether and the polyether-modified silicone oil shown below.

[0099]

[0100] Among them, the mass ratio of isomeric undecyl alcohol polyoxyethylene ether and polyether modified silicone oil is 2:1.

[0101] The preparation method of the composite emulsifier comprises:

[0102] (1) 1 mol of a side chain hydrogen-containing silicone oil with a molecular weight of 1500 and 1.5 mol of allyl polyoxyethylene polyoxypropylene methyl ether (TPEG) with a molecular weight of 2400 were mixed in isopropanol and heated to 72° C., and then 20 ppm of chloroplatinic acid was added, and the mixture was reacted at 75° C. for 10 h, and the solvent was evaporated under vacuum until the isopropanol was removed to obtain a polyether-modified silicone oil;

[0103] (2) 100 g of isomeric undecanol polyoxyethylene ether and 50 g of polyether-modified silicone oil were stirred and mixed at 25° C. for 35 min at a stirring speed of 80 r / min to obtain a composite emulsifier.

[0104] The composite emulsifiers prepared in Examples 1 to 7 and Comparative Examples 1 to 5 were added to the amino silicone oil system to obtain amino silicone oil emulsions, wherein the mass ratio of the composite emulsifier, amino silicone oil and water was 0.3:1:5. The prepared amino silicone oil emulsion was applied to polyester fiber in an amount of 25 g / L. After the polyester fiber was treated with the amino silicone oil emulsions of Examples 1 to 7 and Comparative Examples 1 to 5 and regained moisture, the hydrophilicity, hand feel, water washing fastness and stability were tested. The test method is as follows, and the results are shown in Table 1.

[0105] 1. Hydrophilicity: Use the static water dripping method, use a standard tube (25 drops / mL) to drop a drop of water from 1 cm away from the fabric, and determine the hydrophilicity based on the time it takes for the water drop to be completely absorbed. The shorter the time, the better the hydrophilicity.

[0106] 2. Hand feel: The actual hand feel evaluation method is adopted. The finished fabric samples are cooled and moistened. Five senior hand feel evaluation professionals comprehensively evaluate the lubricity, softness, fluffiness, etc. The hand feel of the original polyester fabric is rated as 1 point, and the best hand feel evaluation is 5 points. The average value is taken.

[0107] 3. Washing fastness: Take a cloth with an area of ​​50x 50cm and use the WASHTEC-P washing fastness tester to test it. The water temperature is 40℃. Put the samples into the test cups, tighten the cup lids, install them on the rotating rack, and cover the door. The machine speed is 40±2rpm, simulating the process of washing clothes in a washing machine. The washing time is 30min. After washing, place it in a room temperature of 30℃ and 50% humidity environment to dry naturally for 12h. Then, 5 senior feel evaluation professionals will evaluate the feel. The feel of the original polyester fabric is rated as 1 point, and the best feel evaluation is 5 points. The average value is taken.

[0108] 4. Stability

[0109] (1) High temperature stability: Place 80 g / L of the sample at 50 °C for 12 h and observe whether phase separation such as stratification occurs to determine its high temperature stability;

[0110] (2) Low temperature stability: Place 80 g / L of the sample at 5 °C for 12 h and observe whether phase separation such as stratification occurs to determine its low temperature stability;

[0111] (3) Acid stability: Place 80 g / L of the sample at pH = 2 for 12 h and observe whether phase separation such as stratification occurs to determine its acid stability;

[0112] (4) Alkali stability: 80 g / L of the sample was placed under pH = 10 for 12 h, and the alkali stability was determined by observing whether phase separation such as stratification occurred;

[0113] Table 1 Performance test results of Examples 1 to 7 and Comparative Examples 1 to 5

[0114]

[0115] It can be seen from the test results in Table 1 that, compared with Comparative Examples 1 to 5, the amino silicone oil emulsion system comprising the composite emulsifier of Examples 1 to 7 of the present invention has better hydrophilicity, water washing fastness, hand feel and stability.

[0116] Specifically, by comparing the performance data of Example 1 and Comparative Examples 1 to 2, it can be seen that when the composite emulsifier contains only the polyether-modified silicone oil of the present invention, the stability, low-temperature resistance, acid and alkali resistance of the amino silicone oil emulsion system are poor, probably because the polyether-modified silicone oil has a large molecular weight, low permeability, and is difficult to form micelles; when the composite emulsifier contains only isomeric alcohol polyoxyethylene ether, since the emulsifier does not contain Si-O segments with a softening function, the hand feel is poor, and since the pour point and glass transition temperature of the isomeric alcohol polyoxyethylene ether are high, its low-temperature stability is poor.

[0117] By comparing the performance data of Example 1 and Comparative Examples 3 to 4, it can be seen that when the mass of the polyether-modified aminosilicone oil in the composite emulsifier is lower than the range of the present invention, its feel will be affected; when the mass of the polyether-modified aminosilicone oil exceeds the range of the present invention, its stability will be affected.

[0118] By comparing the performance data of Example 1 and Comparative Example 5, it can be seen that when a polyether-modified silicone oil containing branches is used, the stability of the emulsion will be reduced. This may be because when the branched structure in the silicone oil is compounded with isomeric alcohol polyoxyethylene ether, the steric hindrance of the branches is large, which reduces the compatibility of the silicone oil with the emulsifier and amino silicone oil in the system, resulting in the formed interfacial film being not dense enough, thereby affecting the stability of the emulsion.

[0119] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention is described in detail with reference to the preferred embodiments, it is not limited to those listed in the embodiments. Those skilled in the art should understand that the technical solution of the present invention can be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A composite emulsifier, characterized in that: Including isomeric alcohol polyoxyethylene ether and polyether modified silicone oil shown in formula 1: Wherein, n is selected from an integer of 13 to 40, and m is an integer of 20 to 70.

2. The composite emulsifier according to claim 1, characterized in that The mass ratio of the isomeric alcohol polyoxyethylene ether to the polyether-modified silicone oil is 1 to 5:

1.

3. The composite emulsifier according to claim 1, characterized in that The isomeric alcohol polyoxyethylene ether is selected from at least one of isomeric decanol polyoxyethylene ether, isomeric undecanol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether.

4. The method for preparing the composite emulsifier according to any one of claims 1 to 3, characterized in that: include: (1) Preparation of polyether-modified silicone oil: mixing hydrogen-terminated silicone oil and allyl polyethylene glycol in a solvent, heating the mixture, adding a platinum catalyst to react, and performing post-treatment to obtain the polyether-modified silicone oil; (2) Preparation of composite emulsifier: The polyether-modified silicone oil and the isomeric alcohol polyoxyethylene ether are stirred and mixed uniformly.

5. The method for preparing the composite emulsifier according to claim 4, characterized in that: The molar ratio of active hydrogen in the hydrogen-terminated silicone oil to vinyl in the allyl polyethylene glycol is 1:1 to 1.

5. The amount of platinum catalyst added is 1 to 30 ppm.

6. The method for preparing the composite emulsifier according to claim 4, characterized in that: Based on the sum of the masses of the hydrogen-terminated silicone oil and the allyl polyethylene glycol, the added amount of the platinum catalyst is 1 ppm to 30 ppm.

7. The method for preparing the composite emulsifier according to claim 4, characterized in that: The platinum catalyst is selected from at least one of chloroplatinic acid, Custer's catalyst and Speier's catalyst, and the solvent is selected from at least one of isopropanol and ethylene glycol monobutyl ether.

8. The method for preparing the composite emulsifier according to claim 4, characterized in that: In (1), the mixing is carried out and the temperature is raised to 70°C to 80°C, the reaction temperature is 70°C to 85°C, and the reaction time is 3h to 12h.

9. The method for preparing the composite emulsifier according to claim 4, characterized in that: In (2), the stirring and mixing is performed at a temperature of 25° C. to 30° C., for a time of 30 min to 60 min, and at a rotation speed of 50 r / min to 100 r / min.

10. Use of the composite emulsifier according to any one of claims 1 to 3 in amino silicone oil.

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