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

Abstract

The invention belongs to the technical field of fine chemical engineering preparation, and particularly relates to a mineral oil defoaming agent synthesized by a one-step one-bath method and a preparation method thereof. The mineral oil defoaming agent is prepared from the following components in parts by mass: 40 to 50 parts of mineral oil, 34 to 45 parts of fatty acid, 10 to 20 parts of polyethylene glycol, 5 to 10 parts of defoaming aid and 0.1 to 0.3 part of catalyst A. According to the invention, fatty acid and polyethylene glycol are directly subjected to esterification reaction in mineral oil, so that the esterification reaction is more thorough, generated water is more quickly and thoroughly removed, the compatibility and stability of a system are stronger, the self-emulsifying ability of the generated defoaming agent is stronger, and defoaming substances are easier to uniformly disperse; the prepared mineral oil defoaming agent is low in surface tension, good in chemical stability, small in dosage and high in defoaming speed.

Description

Technical Field

[0001] The invention belongs to the technical field of fine chemical preparation, and specifically relates to a mineral oil defoamer synthesized by a one-step one-bath method and a preparation method thereof. Background Art

[0002] Defoamers, also known as defoamers, are additives that reduce surface tension, inhibit the generation of foam or eliminate existing foam. Defoamers are mainly divided into three categories: mineral oils, silicones and polyethers, and are used in various fields such as washing, textile printing and dyeing, coatings and building materials, food processing, papermaking, and pharmaceuticals. For example, low-foam laundry detergents, sewage treatment, coatings manufacturing, industrial fermentation and other industries on the market currently have varying degrees of demand for defoamers.

[0003] At present, mineral oil defoamers are mainly used in coatings and other fields, and are mainly composed of mineral oil, fatty acid metal soap, fatty acid amide, fatty alcohol and polyether. Mineral oil itself has a certain defoaming effect, but it is difficult to disperse quickly and effectively in the water phase, and the defoaming performance is not good. It mainly acts as a carrier; therefore, emulsifiers and water-insoluble defoaming material particles (here refers to fatty acids and metal soaps) must be added to mineral oil defoamers. Mineral oil accounts for 70% to 85% of the total amount of traditional mineral oil defoamers. Since mineral oil is a non-renewable resource, the use of renewable resource carriers has become a development trend, but it is currently impossible to completely replace mineral oil. Some small-scale replacement products cannot meet performance requirements, which has become an urgent problem to be solved. At the same time, due to the different raw materials used by each company, differences in production processes, and the lack of universality in the emulsification of mineral oil, the current mineral oil emulsifiers are prone to cause unstable defoamer products, large batch differences, and oil stratification after long storage time, which affects the use effect and storage shelf life.

[0004] Therefore, it is now necessary to develop a defoamer that reduces the proportion of non-renewable resources (mineral oil), has high dispersibility in the water phase, and has high defoaming performance. Summary of the invention

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

[0006] To achieve the above purpose, the present invention provides the following technical solutions.

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

[0008] Furthermore, the mineral oil is one of a group I base oil, a 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, and the molar ratio of PEG200 to PEG400 is 3 to 10:1.

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

[0012] Furthermore, the fatty acid metal soap is at least one of difatty acid aluminum and trifatty acid aluminum; the difatty acid aluminum is at least one of 2 (tetradecanoic acid) aluminum, 2 (pentadecanoic acid) aluminum, 2 (hexadecanoic acid) aluminum, and 2 (octadecanoic acid) aluminum; the trifatty acid aluminum is at least one of tridodecanoic acid aluminum, tritetradecanoic acid aluminum, tripentadecanoic acid aluminum, trihexadecanoic acid aluminum, and trioctadecanoic acid aluminum.

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

[0014] A method for preparing a mineral oil defoamer by a one-step one-bath method comprises the following steps: Step 1: Mixing the raw materials to form a uniform slurry; Step 2, slurry low vacuum esterification reaction; Step 3: After esterification, the slurry is cooled, filtered and impurities are removed to finally obtain a mineral oil defoamer.

[0015] Furthermore, step 1 specifically includes: adding mineral oil, fatty acid, polyethylene glycol and catalyst A (HY type molecular sieve) in sequence into a homogenizing container with stirring, heating and low vacuum, mixing them, and obtaining a slurry.

[0016] Furthermore, step 2 is specifically as follows: stirring the slurry of step 1 at 110°C to 150°C for 3 to 6 hours, then adding a defoaming aid fatty acid metal soap and stirring the reaction at 90°C to 120°C for 1 to 2 hours, and the reactor pressure is -0.3 Mpa to -0.6 Mpa.

[0017] Furthermore, the filtering and impurity removal in step 3 is carried out by a vacuum 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 molecular sieve) required for adding 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] The present invention uses fatty acid and polyethylene glycol to directly carry out esterification reaction in mineral oil, so that the esterification reaction is more thorough, the generated water is removed faster and more thoroughly, the system compatibility and stability are stronger, the generated defoamer has stronger self-emulsification ability, the defoaming substance is easier to be evenly dispersed, and the prepared mineral oil defoamer has low surface tension, good chemical stability, small dosage and fast defoaming speed.

[0022] The invention has simpler process and uses less non-renewable resources to prepare a mineral oil defoamer with excellent comprehensive performance. DETAILED DESCRIPTION

[0023] In order to make those skilled in the art better understand the technical solution of the present invention, the present invention is further described below in conjunction with specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. These embodiments should be understood to be only used to illustrate the present invention and not to limit the protection scope of the present invention. After reading the contents recorded in the present invention, all other embodiments obtained after various changes or modifications made to the present invention based on the technical solution and embodiments of the present invention also fall within the scope of protection of the claims of the present invention.

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

[0025] Furthermore, the mineral oil is one of a group I base oil, a 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, and the molar ratio of PEG200 to PEG400 is 3 to 10:1.

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

[0029] A method for preparing a mineral oil defoamer by a one-step one-bath method comprises the following steps: Step 1, adding mineral oil, fatty acid, polyethylene glycol and catalyst A (HY type molecular sieve) in sequence into a homogenizing container with stirring, heating and low vacuum to mix and obtain slurry; Step 2, stirring the slurry of step 1 at 110°C to 150°C for 3 to 6 hours, then adding a defoaming aid fatty acid metal soap and stirring the reaction at 90°C to 120°C for 1 to 2 hours, and the pressure of the reactor is -0.3 Mpa to -0.6 Mpa; Step 3: After esterification, the slurry is cooled and filtered to remove impurities. The filtering and impurity removal is carried out by a vacuum filter to finally obtain a mineral oil defoamer.

[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 molecular sieve) required for adding 1 mol of fatty acid is 1-2 g.

[0032] Example 1.

[0033] The preparation method of the one-step one-bath method for synthesizing a mineral oil defoamer is as follows: 40 parts of a type of base oil are weighed and added into a homogenizing container, the stirrer is turned on, the speed is adjusted to 250 r / min, 42.1 parts of octadecanoic acid, 10.56 parts of polyethylene glycol 200, 7.04 parts of polyethylene glycol 400, and 0.3 parts of catalyst A (HY type molecular sieve) are added into a homogenizing container (wherein 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), stirring and mixing are continued to be uniform to obtain a mixed material, the temperature is raised to 130°C, maintained for 5 hours, and after the reaction is completed, the mixture is cooled to 100°C; 8 parts of a defoaming aid aluminum di(octadecanoate) are added to the reacted material, the mixture is stirred at 100°C for 1 hour, and cooled to room temperature; the slurry is filtered through 300 mesh to remove the catalyst and impurities, and the mineral oil defoamer is obtained.

[0034] Example 2.

[0035] The preparation method of the one-step one-bath method for synthesizing a mineral oil defoamer is as follows: 45 parts of Class II base oil are weighed and added into a homogenizing container, the stirrer is turned on, the speed is adjusted to 250 r / min, 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) are added into a homogenizing container (wherein 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), stirring and mixing are continued to be uniform to obtain a mixed material, the temperature is raised to 130°C, maintained for 5 hours, and after the reaction is completed, the mixture is cooled to 100°C; 8 parts of a defoaming aid aluminum tris(hexadecanoate) are added to the reacted material, the mixture is stirred at 100°C for 1 hour, and cooled to room temperature; the slurry is filtered through 300 mesh to remove the catalyst and impurities, and the mineral oil defoamer is obtained.

[0036] Example 3.

[0037] The preparation method of the one-step one-bath method for synthesizing a mineral oil defoamer is as follows: weigh 50 parts of liquid paraffin, add it into a homogenizing container, turn on the stirrer, 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) into the homogenizing container (wherein 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 to stir and mix evenly to obtain a mixed material, heat it to 130°C, keep it for 5 hours, and after the reaction is completed, cool it to 100°C; add 7 parts of defoaming aid tri(tetradecanoic acid) aluminum to the reacted material, keep stirring at 100°C for 1 hour, and cool it to room temperature; filter the slurry through 300 mesh to remove the catalyst and impurities, and obtain the mineral oil defoamer.

[0038] Example 4.

[0039] The preparation method of the one-step one-bath method for synthesizing a mineral oil defoamer is as follows: weigh 50 parts of white oil, add it into a homogenizing container, turn on the stirrer, 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) into a homogenizing container (wherein 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 to stir and mix evenly to obtain a mixed material, heat it to 130°C, keep it for 5 hours, and after the reaction is completed, cool it to 100°C; add 9 parts of defoaming aid tri(dodecanoic acid) aluminum to the reacted material, keep stirring at 100°C for 1 hour, and cool it to room temperature; filter the slurry through 300 mesh to remove the catalyst and impurities, and obtain the mineral oil defoamer.

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

[0041] Dispersion density of emulsion r (g / ml), calculated according to formula (1): (1) Where: m 1 —The mass of the 500ml measuring cylinder, in grams (g); m 2—Total mass of the measuring cylinder and the emulsion, in grams (g); V —The volume of the emulsion in the measuring cylinder after dispersion, in milliliters (ml); The greater the dispersion density, the better the defoaming effect of the defoamer. The test results are shown in Table 1.

[0042] Table 1 Dispersion density of Examples 1 to 4 and a commercially available mineral oil defoamer (NXZ1390).

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

[0044] It can be seen from the test results in Table 1 that the defoaming performance of the mineral oil defoamer prepared in Examples 1 to 4 of the present invention is better than that of the mineral oil defoamer (NXZ-1390), which shows 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; and the mineral oil occupancy rate in the present invention is lower than that of the traditional mineral oil occupancy rate.

[0045] This specific embodiment is merely an explanation of the present invention and is not a limitation of the present invention. After reading this specification, those skilled in the art may make non-creative modifications to the present embodiment as needed. However, as long as they are within the scope of the claims of the present invention, they are protected by the patent law.

Claims

1. A mineral oil defoamer synthesized by a one-step one-bath method, characterized in that: The invention comprises the following components in parts by weight: 40 to 50 parts of mineral oil, 34 to 45 parts of fatty acid, 10 to 20 parts of polyethylene glycol, 5 to 10 parts of defoaming aid, and 0.1 to 0.3 parts of catalyst A.

2. The mineral oil defoamer synthesized by the one-step one-bath method according to claim 1, characterized in that: The mineral oil is one of a type I base oil, a type II base oil, liquid paraffin or white oil.

3. The mineral oil defoamer synthesized by the one-step one-bath method according to claim 1, characterized in that: The fatty acid is one of dodecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid or octadecanoic acid.

4. The mineral oil defoamer synthesized by the one-step one-bath method according to claim 1, characterized in that: The polyethylene glycol is a combination of PEG200 and PEG400, and the molar ratio of PEG200 to PEG400 is 3-10:

1.

5. The mineral oil defoamer synthesized by the one-step one-bath method according to claim 1, characterized in that: The defoaming aid is fatty acid metal soap; the fatty acid metal soap is at least one of difatty acid aluminum and trifatty acid aluminum.

6. The mineral oil defoamer synthesized by the one-step one-bath method according to claim 1, characterized in that: The catalyst A is HY type molecular sieve.

7. A method for preparing a synthetic mineral oil defoamer by a one-step one-bath method, characterized in that: The following steps are involved: Step 1: Mix the raw materials to form a uniform slurry; Step 2, slurry low vacuum esterification reaction; Step 3: After esterification, the slurry is cooled, filtered and impurities are removed to finally obtain a mineral oil defoamer.

8. The method for preparing a one-step one-bath synthetic mineral oil defoamer according to claim 7, characterized in that: The step 1 specifically comprises: adding mineral oil, fatty acid, polyethylene glycol and catalyst A in sequence into a homogenizing container with stirring, heating and low vacuum, and mixing them to obtain a slurry.

9. The method for preparing a one-step one-bath synthetic mineral oil defoamer according to claim 8, characterized in that: The molar ratio of fatty acid to polyethylene glycol is 2-2.5:

1.

10. The method for preparing a one-step one-bath synthetic mineral oil defoamer according to claim 7, characterized in that: The step 2 is specifically as follows: stirring the slurry of step 1 at 110°C to 150°C for 3 to 6 hours, then adding a defoaming agent and stirring the reaction at 90°C to 120°C for 1 to 2 hours, and the pressure of the reactor is -0.3 Mpa to -0.6 Mpa.

Images