Mineral oil defoaming agent synthesized by one-step one-bath method and preparation method thereof

Abstract

The present application belongs to the technical field of fine chemical preparation, and particularly relates to a mineral oil defoaming agent synthesized by one-bath one-step method and a preparation method thereof. The mineral oil defoaming agent comprises the following components in parts by mass: 40-50 parts of mineral oil, 34-45 parts of fatty acid, 10-20 parts of polyethylene glycol, 5-10 parts of defoaming auxiliary, and 0.1-0.3 parts of catalyst A. The present application directly performs esterification reaction on the fatty acid and the polyethylene glycol in the mineral oil, so that the esterification reaction is more complete, the generated water is more quickly and completely removed, the system compatibility and stability are stronger, the generated defoaming agent has stronger self-emulsifying capacity, defoaming substances are more easily uniformly dispersed, the prepared mineral oil defoaming agent has low surface tension, good chemical stability, small dosage, and fast defoaming speed.

Description

Technical Field

[0001] This invention belongs to the field of fine chemical preparation technology, specifically a mineral oil defoamer synthesized by a one-step one-bath method and its preparation method. Background Technology

[0002] Defoamers, also known as foam reducers, are additives that inhibit foam formation or eliminate existing foam by reducing surface tension. Defoamers are mainly divided into three categories: mineral oil-based, silicone-based, and polyether-based, and are used in various fields such as detergents, textile printing and dyeing, coatings and building materials, food processing, papermaking, and pharmaceuticals. For example, industries such as low-foaming laundry detergents, wastewater treatment, paint manufacturing, and industrial fermentation all have varying degrees of demand for defoamers.

[0003] Currently, mineral oil defoamers are mainly used in coatings and other fields, and are primarily composed of mineral oil, fatty acid metal soaps, fatty acid amides, fatty alcohols, and polyethers. While mineral oil itself has some defoaming properties, it is difficult to disperse quickly and effectively in an aqueous phase, resulting in poor defoaming performance; its main function is as a carrier. Therefore, emulsifiers and water-insoluble defoaming particles (referring to fatty acids and metal soaps) must be added to mineral oil defoamers. Traditionally, mineral oil accounts for 70%–85% of the total composition in mineral oil defoamers. Since mineral oil is a non-renewable resource, utilizing renewable resource carriers has become a development trend. However, it is currently impossible to completely replace mineral oil, and some products with only small-scale replacements cannot meet performance requirements, becoming a problem that urgently needs to be solved. Furthermore, current mineral oil emulsifiers, due to differences in raw materials and production processes used by various manufacturers, lack universality in emulsifying mineral oil, easily lead to product instability, large batch variations, and oil separation phenomena after prolonged storage, affecting performance and shelf life.

[0004] Therefore, there is a need to develop a defoamer that reduces the proportion of non-renewable resources (mineral oil), has high dispersibility in the aqueous phase, and has high defoaming performance. Summary of the Invention

[0005] In view of the shortcomings of the prior art described above, the purpose of this invention is to provide a method for preparing a mineral oil defoamer synthesized in a one-step, one-bath process. This method can solve the problems of high proportion of non-renewable resources (mineral oil), poor dispersion performance in aqueous phase (poor emulsification), and poor defoaming performance in the prior art.

[0006] To achieve the above objectives, the present invention provides the following technical solution.

[0007] A mineral oil defoamer synthesized by a one-step, one-bath method comprises the following components in parts by weight: 40-50 parts mineral oil, 34-45 parts fatty acid, 10-20 parts polyethylene glycol, 5-10 parts defoaming aid, and 0.1-0.3 parts catalyst A.

[0008] Furthermore, mineral oil is one of Group I base oil, Group II base oil, liquid paraffin, or white oil.

[0009] Furthermore, the fatty acid is one of dodecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, or octadecanoic acid.

[0010] Furthermore, the polyethylene glycol is a combination of PEG200 and PEG400, with a molar ratio of PEG200 to PEG400 of 3 to 10:1.

[0011] Furthermore, the defoaming agent is a fatty acid metal soap.

[0012] Furthermore, the fatty acid metal soap is at least one of aluminum difatty acid and aluminum trifatty acid; the aluminum difatty acid is at least one of aluminum di(tetradecanoic acid), aluminum di(pentadecanoic acid), aluminum di(hexadecanoic acid), and aluminum di(octadecanoic acid); the aluminum trifatty acid is at least one of aluminum tri(dodecanoic acid), aluminum tri(tetradecanoic acid), aluminum tri(pentadecanoic acid), aluminum tri(hexadecanoic acid), and aluminum tri(octadecanoic acid).

[0013] Furthermore, catalyst A is a HY-type molecular sieve.

[0014] A one-step, one-bath method for preparing a mineral oil defoamer includes the following steps: Step 1: Mixing the raw materials to form a uniform slurry; Step 2: Low-vacuum esterification reaction of slurry; Step 3: After esterification, the slurry is cooled and filtered to remove impurities, finally yielding the mineral oil defoamer.

[0015] Further, step 1 specifically involves adding mineral oil, fatty acids, polyethylene glycol, and catalyst A (HY type molecular sieve) in sequence to a homogenization container equipped with stirring, heating, and low vacuum for mixing to obtain a slurry.

[0016] Further, step 2 specifically involves: stirring the slurry from step 1 at 110℃~150℃ for 3 to 6 hours, then adding the defoaming agent, fatty acid metal soap, and stirring at 90℃~120℃ for 1 to 2 hours, with the reactor pressure at -0.3 MPa~-0.6 MPa.

[0017] Furthermore, the filtration and impurity removal in step 3 is carried out using a pressure-reducing filter.

[0018] Preferably, the molar ratio of fatty acid to polyethylene glycol is 2 to 2.5:1.

[0019] Preferably, the amount of catalyst A (HY type molecular sieve) required to add 1 mol of fatty acid is 1-2 g.

[0020] Compared with the prior art, the beneficial effects of the present invention are as follows.

[0021] This invention uses fatty acids and polyethylene glycol to directly esterify in mineral oil, making the esterification reaction more thorough and the generated water removed more quickly and completely, resulting in stronger system compatibility and stability. The defoamer produced has stronger self-emulsifying ability, and the defoaming substance is easier to disperse evenly. The resulting mineral oil defoamer has low surface tension, good chemical stability, low dosage, and fast defoaming speed.

[0022] This invention provides a simpler process and a method for preparing a mineral oil defoamer with superior overall performance using fewer non-renewable resources. Detailed Implementation

[0023] To enable those skilled in the art to better understand the technical solutions of this invention, the invention will be further described below with reference to specific embodiments. Obviously, the described embodiments are merely a part of the embodiments of this invention, and not all of them. These embodiments should be understood as being used only to illustrate the invention and not to limit the scope of protection of the invention. After reading the contents of this invention, all other embodiments obtained by making various modifications or alterations to the invention based on the technical solutions and embodiments of this invention also fall within the scope of protection of the claims of this invention.

[0024] A mineral oil defoamer synthesized by a one-step, one-bath method comprises the following components in parts by weight: 40-50 parts mineral oil, 34-45 parts fatty acid, 10-20 parts polyethylene glycol, 5-10 parts defoaming aid, and 0.1-0.3 parts catalyst A (HY type molecular sieve).

[0025] Furthermore, mineral oil is one of Group I base oil, Group II base oil, liquid paraffin, or white oil.

[0026] Furthermore, the fatty acid is one of dodecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, or octadecanoic acid.

[0027] Furthermore, the polyethylene glycol is a combination of PEG200 and PEG400, with a molar ratio of PEG200 to PEG400 of 3 to 10:1.

[0028] Furthermore, the defoaming agent is a fatty acid metal soap; the fatty acid metal soap is at least one of aluminum difatty acid and aluminum trifatty acid; the aluminum difatty acid is at least one of aluminum di(tetradecanoic acid), aluminum di(pentadecanoic acid), aluminum di(hexadecanoic acid), and aluminum di(octadecanoic acid); the aluminum trifatty acid is at least one of aluminum tri(dodecanoic acid), aluminum tri(tetradecanoic acid), aluminum tri(pentadecanoic acid), aluminum tri(hexadecanoic acid), and aluminum tri(octadecanoic acid).

[0029] A one-step, one-bath method for preparing a mineral oil defoamer includes the following steps: Step 1: Add mineral oil, fatty acids, polyethylene glycol and catalyst A (HY type molecular sieve) in sequence to a homogenization container equipped with stirring, heating and low vacuum for mixing to obtain a slurry; Step 2: Stir the slurry from Step 1 at 110℃~150℃ for 3 to 6 hours, then add the defoaming agent fatty acid metal soap and stir at 90℃~120℃ for 1 to 2 hours. The pressure of the reactor is -0.3 MPa~-0.6 MPa. Step 3: After esterification, the slurry is cooled and filtered to remove impurities. The filtration and impurity removal are carried out by a vacuum filter, and finally, mineral oil defoamer is obtained.

[0030] Preferably, the molar ratio of fatty acid to polyethylene glycol is 2 to 2.5:1.

[0031] Preferably, the amount of catalyst A (HY type molecular sieve) required to add 1 mol of fatty acid is 1-2 g.

[0032] Example 1.

[0033] The preparation method of mineral oil defoamer by one-step one-bath synthesis is as follows: Weigh 40 parts of a type I base oil and add it to a homogenization container. Turn on the stirrer and adjust the speed to 250 r / min. Add 42.1 parts of octadecanoic acid, 0.56 parts of polyethylene glycol 200, 7.04 parts of polyethylene glycol 400, and 0.3 parts of catalyst A (HY type molecular sieve) to the homogenization container (where the molar ratio of octadecanoic acid to polyethylene glycol is 2.1:1, and the molar ratio of polyethylene glycol 200 to polyethylene glycol 400 is 3:1). Continue stirring and mixing evenly to obtain a mixture. Heat to 130℃ and maintain for 5 hours. After the reaction is completed, cool to 100℃. Add 8 parts of defoaming agent dicoctadecanoic acid aluminum to the reacted material, maintain at 100℃ and stir for 1 hour, and cool to room temperature. Filter the slurry through a 300-mesh filter to remove the catalyst and impurities to obtain the mineral oil defoamer.

[0034] Example 2.

[0035] The preparation method of mineral oil defoamer by one-step one-bath synthesis is as follows: Weigh 45 parts of Group II base oil and add it to a homogenization container. Turn on the stirrer and adjust the speed to 250 r / min. Add 37.3 parts of palmitic acid, 10.5 parts of polyethylene glycol 200, 7 parts of polyethylene glycol 400, and 0.2 parts of catalyst A (HY type molecular sieve) to the homogenization container (where the molar ratio of palmitic acid to polyethylene glycol is 2.2:1, and the molar ratio of polyethylene glycol 200 to polyethylene glycol 400 is 4:1). Continue stirring and mixing evenly to obtain a mixture. Heat to 130℃ and maintain for 5 hours. After the reaction is completed, cool to 100℃. Add 8 parts of defoaming agent tris(hexadecanoic acid) aluminum to the reacted material, maintain at 100℃ and stir for 1 hour, and cool to room temperature. Filter the slurry through a 300-mesh filter to remove catalyst and impurities to obtain the mineral oil defoamer.

[0036] Example 3.

[0037] The preparation method of mineral oil defoamer by one-step one-bath synthesis is as follows: Weigh 50 parts of liquid paraffin and add it to a homogenization container. Turn on the stirrer and adjust the speed to 250 r / min. Add 35.72 parts of palmitic acid, 10.36 parts of polyethylene glycol 200, 3.67 parts of polyethylene glycol 400, and 0.25 parts of catalyst A (HY type molecular sieve) to the homogenization container (where the molar ratio of palmitic acid to polyethylene glycol is 2.3:1, and the molar ratio of polyethylene glycol 200 to polyethylene glycol 400 is 5.7:1). Continue stirring and mixing evenly to obtain a mixture. Heat to 130℃ and maintain for 5 hours. After the reaction is completed, cool to 100℃. Add 7 parts of defoaming agent tris(tetradecanoic acid) aluminum to the reacted material, maintain at 100℃ and stir for 1 hour, and cool to room temperature. Filter the slurry through a 300-mesh filter to remove the catalyst and impurities to obtain the mineral oil defoamer.

[0038] Example 4.

[0039] The preparation method of mineral oil defoamer by one-step one-bath synthesis is as follows: Weigh 50 parts of white oil and add it to a homogenization container. Turn on the stirrer and adjust the speed to 250 r / min. Add 34.30 parts of tetradecanoic acid, 12.68 parts of polyethylene glycol 200, 2.82 parts of polyethylene glycol 400, and 0.2 parts of catalyst A (HY type molecular sieve) to the homogenization container (where the molar ratio of tetradecanoic acid to polyethylene glycol is 2.4:1, and the molar ratio of polyethylene glycol 200 to polyethylene glycol 400 is 9:1). Continue stirring and mixing evenly to obtain a mixture. Heat to 130℃ and maintain for 5 hours. After the reaction is completed, cool to 100℃. Add 9 parts of aluminum tris(dodecanoic acid) defoamer to the reacted material, maintain at 100℃ and stir for 1 hour, and cool to room temperature. Filter the slurry through a 300-mesh filter to remove the catalyst and impurities to obtain the mineral oil defoamer.

[0040] The defoaming performance of the mineral oil defoamers in Examples 1-4 was tested and compared with that of a commercially available defoamer (NXZ-1390). The specific test methods are as follows: Weigh 50g of styrene-acrylic emulsion and 50ml of water into a beaker, add the defoamer to be tested with a mass fraction of 1.0‰, stir at 1500 r / min for 15 min, and immediately after stopping stirring, transfer the emulsion from the beaker into a container with a mass fraction of 1.0‰. m 1 The volume of the emulsion was read from a 500ml graduated cylinder and recorded as follows: V The total mass of the measuring cylinder and the emulsion is weighed and denoted as . m 2 .

[0041] Emulsion dispersion density r (g / ml), calculated according to formula (1): (1) In the formula: m 1 —The mass of a 500ml graduated cylinder, in grams (g); m 2—Total mass of graduated cylinder and emulsion, in grams (g); V —The volume of the dispersed emulsion in the graduated cylinder, in milliliters (ml). A higher dispersion density indicates a better defoaming effect of the defoamer. The test results are shown in Table 1.

[0042] Table 1 shows the dispersion density of the mineral oil defoamers in Examples 1-4 and commercially available (NXZ1390).

[0043] Note: Add 50g of water to 50g of emulsion; add 0.1g of defoamer; stir at 1500r / min for 15min.

[0044] As can be seen from the test results in Table 1, the defoaming performance of the mineral oil defoamers prepared in Examples 1 to 4 of the present invention is better than that of the mineral oil defoamer (NXZ-1390). This indicates that the mineral oil defoamer of the present invention has excellent defoaming performance, and the defoaming ability of the mineral oil defoamer is effectively improved by the one-step one-bath process. Furthermore, the mineral oil content in the present invention is lower than that in the traditional mineral oil content.

[0045] This specific embodiment is merely an explanation of the present invention and is not intended to limit the invention. After reading this specification, those skilled in the art can make modifications to this embodiment without contributing any inventive step, but such modifications are protected by patent law as long as they are within the scope of the claims of the present invention.

Claims

1. A method for preparing a one-step, one-bath synthetic mineral oil defoamer, characterized in that, The raw materials include the following components in parts by weight: 40-50 parts mineral oil, 34-45 parts fatty acid, 10-20 parts polyethylene glycol, 5-10 parts defoaming agent, and 0.1-0.3 parts catalyst A, which is HY type molecular sieve. The preparation method includes the following steps: Step 1: Add mineral oil, fatty acids, polyethylene glycol and catalyst A to a homogenization container equipped with stirring, heating and low vacuum and mix to obtain a slurry; Step 2: Stir the slurry from Step 1 at 110℃~150℃ for 3 to 6 hours, then add the defoaming agent and stir at 90℃~120℃ for 1 to 2 hours. The pressure of the reactor is -0.3 MPa~-0.6 MPa. Step 3: After esterification, the slurry is cooled and filtered to remove impurities, finally yielding the mineral oil defoamer.

2. The method for preparing a one-step, one-bath synthetic mineral oil defoamer according to claim 1, characterized in that, The molar ratio of fatty acids to polyethylene glycol is (2-2.5):

1.

3. The method for preparing a one-step, one-bath synthetic mineral oil defoamer according to claim 1, characterized in that, The mineral oil is one of Group I base oil, Group II base oil, liquid paraffin, or white oil.

4. The method for preparing a one-step, one-bath synthetic mineral oil defoamer according to claim 1, characterized in that, The fatty acid is one of dodecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, or octadecanoic acid.

5. The method for preparing a one-step, one-bath synthetic mineral oil defoamer according to claim 1, characterized in that, The polyethylene glycol is a combination of PEG200 and PEG400, with a molar ratio of PEG200 to PEG400 of (3-10):

1.

6. The method for preparing a one-step, one-bath synthetic mineral oil defoamer according to claim 1, characterized in that, The defoaming agent is a fatty acid metal soap; the fatty acid metal soap is at least one of aluminum difatty acid and aluminum trifatty acid.

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