Non-ionic surfactant and preparation method thereof

Abstract

The invention relates to the field of surfactant preparation, in particular to a nonionic surfactant and a preparation method thereof. The invention provides a non-ionic surface active agent. The non-ionic surface active agent is prepared from the following components in parts by weight: 25-30 parts of polyoxyethylene alkyl ether; 15 to 20 parts of polypropylene ether; 5 to 7 parts of dioctyl sodium sulfosuccinate; 5-7 parts of ethanol; and 3-5 parts of propylene glycol. The structures of polyoxyethylene alkyl ether and polypropylene ether are easy to chemically modify and compound, and a micelle fence layer with a special structure can be formed by combining a substrate formed by mixing polyoxyethylene alkyl ether and polypropylene ether with ethanol, and can be combined with dioctyl sodium sulfosuccinate and propylene glycol which are added later, so that the hydration degree of the surfactant is increased, the cloud point is increased, and the pH value of the surfactant is increased. The property stability is kept in a high-temperature environment. The invention also provides a preparation method of the nonionic surfactant, which improves the production efficiency and reduces the energy consumption and production cost on the premise of ensuring the stability and high quality of the product.

Description

Technical Field

[0001] The invention relates to the field of surfactant preparation, and in particular to a nonionic surfactant and a preparation method thereof. Background Art

[0002] Nonionic surfactants are surfactants that do not dissociate in aqueous solution. Their molecular structure is composed of hydrophilic groups and hydrophobic groups, of which the hydrophilic groups are mainly polyoxyethylene groups, polyols

[0003] (such as glycerol, polyethylene glycol, sorbitol, etc.) as well as alcohol amides, amine oxides, etc.; the hydrophobic groups are long-chain fatty acids or long-chain fatty alcohols and alkyl or aromatic groups, which are combined with the hydrophilic groups by ester bonds or ether bonds.

[0004] Surfactants are widely used in various fields such as textiles, pharmaceuticals, cosmetics, food, civil engineering, mining, and washing because they can significantly reduce the interfacial tension of substances. In these fields, non-ionic surfactants have received more and more attention due to their unique properties and broad application prospects. When non-ionic surfactants are used in fields with relatively high ambient temperatures such as high-temperature industrial cleaning and textile printing and dyeing, turbid phase separation will occur, causing them to become insoluble in water. The main reason for this phenomenon is that non-ionic surfactants have a low cloud point and are unstable under high temperature conditions. In addition to being unstable under high temperature environments, existing non-ionic surfactants also have problems such as high production costs and the possibility of environmental pollution caused by production waste.

[0005] Therefore, it is necessary to invent a nonionic surfactant that is resistant to high temperatures, has low production costs and is environmentally friendly. Summary of the invention

[0006] In view of the above existing technical problems, a nonionic surfactant and a preparation method thereof are provided. The nonionic surfactant prepared by the method has a good cloud point, aqueous solution viscosity, low water content and residual monomer content. The raw materials and additives used in the preparation method of the invention are environmentally friendly materials, which conforms to the concept of green chemistry.

[0007] The present invention discloses a nonionic surfactant, comprising the following components in parts by weight:

[0008] 25-30 parts of polyoxyethylene alkyl ether; 15-20 parts of polypropylene ether; 5-7 parts of sodium diisooctyl sulfosuccinate; 5-7 parts of ethanol; 3-5 parts of propylene glycol.

[0009] The present invention also discloses a method for preparing a nonionic surfactant, comprising the following steps:

[0010] Preparation of S1 mixed solution: Add polyoxyethylene alkyl ether to the reactor, then add ethanol and start stirring. After stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then heat up and add the catalyst. After the catalyst is added, control the pressure and temperature in the reactor and maintain stirring. After the reaction is completed, a mixed solution is obtained;

[0011] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Ammonia water is then added to the distillate and the temperature is raised and stirred for 1 to 2 hours. After the stirring is completed, the temperature is lowered and cooled. Then, acid solution is added to adjust the pH. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0012] Preferably, in the step of preparing the mixed solution S1, the stirring speed of the reactor is 500 to 1500 rpm.

[0013] Preferably, in the step of preparing the mixed solution S1, the catalyst is boron trifluoride etherate complex.

[0014] Preferably, in the step of preparing the mixed solution S1, the mass ratio of the boron trifluoride ether complex to the polyoxyethylene alkyl ether is 1:(19-20).

[0015] Preferably, in the step of preparing the S1 mixed solution, the reaction temperature of the reactor is 60-70° C.; and the reaction pressure of the reactor is 2-3 MPa.

[0016] Preferably, in the S2 nonionic surfactant preparation step, the volume ratio of the ammonia water to the distillate is 1:(1-2).

[0017] Preferably, in the step of preparing the S2 nonionic surfactant, the temperature of the heating and stirring after adding the ammonia water is 85-100°C.

[0018] Preferably, in the S2 nonionic surfactant preparation step, the cooling is lowered to 25-28° C.; the cooling time after cooling is 5-8 hours.

[0019] Preferably, in the S2 nonionic surfactant preparation step, the acid solution is carbonic acid, and the adjusted pH value is 6.5-7.

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

[0021] The present invention provides a nonionic surfactant and a preparation method thereof. Polyoxyethylene alkyl ether and polypropylene ether are selected as base materials in the raw materials, sodium diisooctyl sulfosuccinate, ethanol and propylene glycol, and boron trifluoride ether complex are used as catalysts. The structures of polyoxyethylene alkyl ether and polypropylene ether are easy to be chemically modified and compounded. The substrate composed of the two mixed together with ethanol can form a micelle fence layer with a special structure, which will be combined with sodium diisooctyl sulfosuccinate and propylene glycol added later, and will not be crowded around the polar groups of the base material, so that the steric hindrance will be reduced, thereby increasing the hydration degree of the surfactant, so that the cloud point is increased, and the properties are kept stable in a high temperature environment. Glycerol will be adsorbed and solubilized on the micelle interface to form hydrogen bonds with water, increase the water content of the micelle, destroy the iceberg structure of the micelle, cause the polarity of the medium to decrease, limit the micellization of the surfactant, further increase the cloud point, and increase the stability of the nonionic surfactant in a high temperature environment. The addition of sodium diisooctyl sulfosuccinate to the raw materials is an additive that can further increase the cloud point without damaging other properties of the nonionic surfactant.

[0022] During the preparation process, by adjusting the ratio of raw materials and optimizing parameters such as reaction temperature, pressure, stirring speed, etc., the production efficiency is improved and the energy consumption and production costs are reduced while ensuring the stability and high quality of the product.

[0023] The raw materials and additives used in the preparation method of the present invention are all environmentally friendly materials, which conforms to the concept of green chemistry. DETAILED DESCRIPTION

[0024] The following examples are provided for a better understanding of the present invention, but are not intended to limit the best mode of implementation, nor to limit the content and protection scope of the present invention. Any product identical or similar to the present invention obtained by anyone under the inspiration of the present invention or by combining the features of the present invention with other prior arts shall fall within the protection scope of the present invention.

[0025] If no specific experimental steps or conditions are specified in the examples, the conventional experimental steps or conditions described in the literature in the field can be used. If no manufacturer is specified for the reagents or instruments used, they are all conventional reagent products that can be obtained commercially.

[0026] Embodiment 1: A nonionic surfactant, composed of the following components in parts by weight:

[0027] 25 parts of polyoxyethylene alkyl ether; 15 parts of polypropylene ether; 5 parts of sodium diisooctyl sulfosuccinate; 5 parts of ethanol; 3 parts of propylene glycol.

[0028] A method for preparing a nonionic surfactant comprises the following steps:

[0029] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 500rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19; after the catalyst is added, the pressure in the reactor is controlled to 2MPa, the reaction temperature of the reactor is 60℃, and the stirring reaction is maintained for 3h, and a mixed solution is obtained after the reaction is completed.

[0030] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Ammonia water is then added to the distillate and the temperature is raised to 85°C and stirred for 1 to 2 hours, wherein the volume ratio of ammonia water to distillate is 1:1. After the stirring is completed, the temperature is lowered to 25°C and cooled for 5 hours. Carbonic acid is then added to adjust the pH to 6.5. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0031] Embodiment 2: A nonionic surfactant, composed of the following components in parts by weight:

[0032] 26 parts of polyoxyethylene alkyl ether; 16 parts of polypropylene ether; 5.5 parts of sodium diisooctyl sulfosuccinate; 5.5 parts of ethanol; 3.5 parts of propylene glycol.

[0033] A method for preparing a nonionic surfactant comprises the following steps:

[0034] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 700rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.2; after the catalyst is added, the pressure in the reactor is controlled to 2.2MPa, the reaction temperature of the reactor is 62℃, and the stirring reaction is maintained for 3.3h, and a mixed solution is obtained after the reaction is completed.

[0035] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 90°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.4. After the stirring is completed, the temperature is lowered to 25°C and cooled for 5.5 hours. Carbonic acid is then added to adjust the pH to 6.6. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0036] Embodiment 3: A nonionic surfactant, composed of the following components in parts by weight:

[0037] 27 parts of polyoxyethylene alkyl ether; 17 parts of polypropylene ether; 6 parts of sodium diisooctyl sulfosuccinate; 6 parts of ethanol; 4 parts of propylene glycol.

[0038] A method for preparing a nonionic surfactant comprises the following steps:

[0039] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 900rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.4; after the catalyst is added, the pressure in the reactor is controlled to 2.4MPa, the reaction temperature of the reactor is 64℃, and the stirring reaction is maintained for 3.6h, and a mixed solution is obtained after the reaction is completed.

[0040] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 95°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.6. After the stirring is completed, the temperature is lowered to 27°C and cooled for 6 hours. Carbonic acid is then added to adjust the pH to 6.7. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0041] Embodiment 4: A nonionic surfactant, composed of the following components in parts by weight:

[0042] 28 parts of polyoxyethylene alkyl ether; 18 parts of polypropylene ether; 6.5 parts of sodium diisooctyl sulfosuccinate; 7 parts of ethanol; 4.5 parts of propylene glycol.

[0043] A method for preparing a nonionic surfactant comprises the following steps:

[0044] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 1100rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.6; after the catalyst is added, the pressure in the reactor is controlled to 2.6MPa, the reaction temperature of the reactor is 66℃, and the stirring reaction is maintained for 3.6h. After the reaction is completed, a mixed solution is obtained.

[0045] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 95°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.8. After the stirring is completed, the temperature is lowered to 28°C and cooled for 6.5 hours. Carbonic acid is then added to adjust the pH to 6.8. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0046] Embodiment 5: A nonionic surfactant, composed of the following components in parts by weight:

[0047] 29 parts of polyoxyethylene alkyl ether; 30 parts of polypropylene ether; 7 parts of sodium diisooctyl sulfosuccinate; 6.5 parts of ethanol; 5 parts of propylene glycol.

[0048] A method for preparing a nonionic surfactant comprises the following steps:

[0049] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 1300rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.8; after the catalyst is added, the pressure in the reactor is controlled to 2.8MPa, the reaction temperature of the reactor is 68℃, and the stirring reaction is maintained for 3.8h. After the reaction is completed, a mixed solution is obtained.

[0050] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 100°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.8. After the stirring is completed, the temperature is lowered to 28°C and cooled for 7 hours. Carbonic acid is then added to adjust the pH to 6.9. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0051] Embodiment 6: A nonionic surfactant, composed of the following components in parts by weight:

[0052] 30 parts of polyoxyethylene alkyl ether; 29 parts of polypropylene ether; 7 parts of sodium diisooctyl sulfosuccinate; 7 parts of ethanol; 5 parts of propylene glycol.

[0053] A method for preparing a nonionic surfactant comprises the following steps:

[0054] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 1500rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:20; after the catalyst is added, control the pressure in the reactor to 3MPa, the reaction temperature of the reactor to 70℃, and maintain stirring reaction for 4h, and obtain a mixed solution after the reaction is completed.

[0055] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Ammonia water is then added to the distillate and the temperature is raised to 100°C and stirred for 1 to 2 hours, wherein the volume ratio of ammonia water to distillate is 1:2. After the stirring is completed, the temperature is lowered to 28°C and cooled for 7 hours. Carbonic acid is then added to adjust the pH to 7. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0056] Comparative Example 1: A nonionic surfactant, composed of the following components in parts by weight:

[0057] 29 parts of polyoxyethylene alkyl ether; 30 parts of polypropylene ether; 6.5 parts of ethanol; 5 parts of propylene glycol.

[0058] A method for preparing a nonionic surfactant comprises the following steps:

[0059] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 1300rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.8; after the catalyst is added, the pressure in the reactor is controlled to 2.8MPa, the reaction temperature of the reactor is 68℃, and the stirring reaction is maintained for 3.8h. After the reaction is completed, a mixed solution is obtained.

[0060] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 100°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.8. After the stirring is completed, the temperature is lowered to 28°C and cooled for 7 hours. Carbonic acid is then added to adjust the pH to 6.9. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0061] Comparative Example 2: A nonionic surfactant, composed of the following components in parts by weight:

[0062] 29 parts of polyoxyethylene alkyl ether; 30 parts of polypropylene ether; 7 parts of sodium diisooctyl sulfosuccinate; 6.5 parts of ethanol.

[0063] A method for preparing a nonionic surfactant comprises the following steps:

[0064] Preparation of S1 mixed solution: add polyoxyethylene alkyl ether into the reactor, then add ethanol and start stirring, the stirring speed of the reactor is 1300rpm, after stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then increase the temperature and add boron trifluoride ether complex, wherein the mass ratio of boron trifluoride ether complex to polyoxyethylene alkyl ether is 1:19.8; after the catalyst is added, the pressure in the reactor is controlled to 2.8MPa, the reaction temperature of the reactor is 68℃, and the stirring reaction is maintained for 3.8h. After the reaction is completed, a mixed solution is obtained.

[0065] Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Then, aqueous ammonia is added to the distillate and the temperature is raised to 100°C and stirred for 1 to 2 hours, wherein the volume ratio of aqueous ammonia to distillate is 1:1.8. After the stirring is completed, the temperature is lowered to 28°C and cooled for 7 hours. Carbonic acid is then added to adjust the pH to 6.9. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

[0066] The performance of the nonionic surfactants prepared in Examples 1 to 6 and Comparative Examples 1 to 2 was tested, and the test data are shown in the following table:

[0067]

[0068] It can be seen from the test data in the above table that the performance of the nonionic surfactants prepared in Examples 1 to 6 is better than that of Comparative Examples 1 to 2. Comparative Example 1 is a nonionic surfactant prepared according to the experimental conditions of Example 5 by removing sodium diisooctyl sulfosuccinate from the raw material; Comparative Example 2 is a nonionic surfactant prepared according to the experimental conditions of Example 5 by removing propylene glycol from the raw material. The aqueous solution of the nonionic surfactant prepared in Comparative Examples 1 to 2 has a low viscosity, a high water content, a high residual monomer content, and a low turbidity point. Compared with the nonionic surfactants shown in Examples 1 to 6, the properties are more unstable and not suitable for use in high temperature environments. This is because sodium diisooctyl sulfosuccinate or propylene glycol is not added in Comparative Examples 1 to 2, so the micelle fence layer with a special structure formed by polyoxyethylene alkyl ether, polypropylene ether, and ethanol cannot form a good connection with water, and will not reduce the spatial hindrance of the nonionic surfactant, so the prepared nonionic surfactant will have poor performance. Among Examples 1 to 6, Examples 5 and 6 have the best properties.

[0069] Obviously, the above embodiments are merely examples for the purpose of clear explanation, and are not intended to limit the implementation methods. For those skilled in the art, other different forms of changes or modifications can be made based on the above description. It is not necessary and impossible to list all the implementation methods here. The obvious changes or modifications derived from these are still within the scope of protection of the invention.

Claims

1. A nonionic surfactant, characterized in that It is composed of the following ingredients in parts by weight: 25-30 parts of polyoxyethylene alkyl ether; 15-20 parts of polypropylene ether; 5-7 parts of sodium diisooctyl sulfosuccinate; 5-7 parts of ethanol; 3-5 parts of propylene glycol.

2. A method for preparing a nonionic surfactant, characterized in that: The following steps are involved: Preparation of S1 mixed solution: Add polyoxyethylene alkyl ether to the reactor, then add ethanol and start stirring. After stirring evenly, add polypropylene ether, propylene glycol and sodium diisooctyl sulfosuccinate in sequence and stir evenly, then heat up and add the catalyst. After the catalyst is added, control the pressure and temperature in the reactor and maintain stirring. After the reaction is completed, a mixed solution is obtained; Preparation of S2 non-ionic surfactant: The mixed solution obtained in step S1 is subjected to reduced pressure distillation and the distillate is collected. Ammonia water is then added to the distillate and the temperature is raised and stirred for 1 to 2 hours. After the stirring is completed, the temperature is lowered and cooled. Then, acid solution is added to adjust the pH. After the adjustment is completed, the non-ionic surfactant is obtained by rotary evaporation under reduced pressure.

3. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the S1 mixed solution preparation step, the stirring speed of the reactor is 500-1500 rpm.

4. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the step of preparing the mixed solution S1, the catalyst is boron trifluoride etherate complex.

5. The method for preparing a nonionic surfactant according to claim 4, characterized in that: In the step of preparing the mixed solution S1, the mass ratio of the boron trifluoride ether complex to the polyoxyethylene alkyl ether is 1:(19-20).

6. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the S1 mixed solution preparation step, the reaction temperature of the reactor is 60-70° C.; the reaction pressure of the reactor is 2-3 MPa.

7. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the S2 nonionic surfactant preparation step, the volume ratio of the ammonia water to the distillate is 1:(1-2).

8. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the step of preparing the S2 nonionic surfactant, the temperature of the heating and stirring after adding the ammonia water is 85-100°C.

9. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the S2 nonionic surfactant preparation step, the temperature is cooled to 25-28° C. and the cooling time after cooling is 5-8 hours.

10. The method for preparing a nonionic surfactant according to claim 2, characterized in that: In the S2 nonionic surfactant preparation step, the acid solution is carbonic acid, and the adjusted pH value is 6.5-7.

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