CN109248473B - Defoaming composition - Google Patents
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- CN109248473B CN109248473B CN201811309104.5A CN201811309104A CN109248473B CN 109248473 B CN109248473 B CN 109248473B CN 201811309104 A CN201811309104 A CN 201811309104A CN 109248473 B CN109248473 B CN 109248473B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
Abstract
The invention relates to a preparation method of a defoaming composition, which consists of carrier oil, hydrophobic particles, a wetting agent, an organic silicon synergist and an emulsifier. The defoaming composition prepared by the invention has better defoaming capability in a high-viscosity system.
Description
Technical Field
The invention relates to a defoaming composition, in particular to a composition capable of removing bubbles in a viscous system and a preparation method thereof, belonging to the technical field of fine chemical engineering.
Background
Air bubbles or foam are a common phenomenon in industrial processes, and defoaming agents are often used to eliminate air bubbles or foam. At present, the defoaming agent is an indispensable fine chemical auxiliary agent in the industrial production process.
Defoamers are classified according to the active substance, and are mainly classified into silicone defoamers and non-silicone defoamers. The organic silicon defoamer mainly comprises polysiloxane, white carbon black, an emulsifier and water, and is characterized by high defoaming speed and poor compatibility with a foaming system, and easily forms silicon spots, shrinkage cavities and other defects when used for coating; the non-silicone defoaming agent generally comprises mineral oil, fatty alcohol, fatty acid ester, metal soap, fatty acid amide, polyether and the like, and has the defoaming function which is not as fast as that of silicone, but has good compatibility and high safety. In general, different application fields have different emphasis on defoaming agents, in particular, the defoaming agent for sewage treatment focuses on defoaming and foam inhibiting functions, and the coating defoaming agent requires the defoaming agent to have excellent defoaming and foam inhibiting performance, stability and compatibility, and each system has own characteristics.
In daily production and life, a viscous system is also a common system, such as ink, paint, acrylic resin, adhesive, pressure-sensitive adhesive, white latex and the like, which can not be stirred and mixed in the production process, air can be easily introduced into the system by stirring and mixing, and the air is difficult to remove, so that the appearance of the final product can be seriously affected. In fact, in high viscosity systems, it is more accurate to "degas" than "defoam" for bubble removal. According to the usual experience of use, the degassing of high-viscosity systems is still carried out by selecting products of the mineral oil type or modified silicones, essentially without using silicone products consisting of polysiloxanes and hydrophobic particles.
There are also many patents describing mineral oil type defoamers: for example, US3076768 describes defoamers comprising hydrophobic white carbon black, hydrocarbon oil and a dispersant; US4094812 describes a composition comprisingα-a method for preparing a mineral oil type antifoaming agent of a hydroxylamine derivative; US3652452 describes an antifoaming agent consisting of a rapidly cooled amine, an organic hydrocarbon; CN101903074B introduces mineral oil defoamer with mineral oil, dispersant and white carbon black dispersed; CN101445760 describes a defoaming agent comprising ethylene bisstearamide, an organic hydrocarbon and hydrophilic white carbon black as components; CN101003644 describes a defoaming agent for peritoneal adhesive which takes organic hydrocarbon and fatty acid amide as components; CN2007100251825.1 discloses a defoaming agent which takes organic hydrocarbon and aluminum stearate as components; CN201010550336.7 introduces a method for grinding by using mineral oil, wax, white carbon black, an emulsifier, oleic acid and the like, and a colloid mill circulation grinding process is adopted; CN102120107B and CN201010550282.4 describe the preparation of mineral oil type antifoaming agents by high speed milling.
However, these products are focused on eliminating bubbles formed on the liquid surface, but not on removing bubbles inside a viscous system, so that the capability of removing bubbles inside the viscous system is far from meeting the production requirement under the conditions of strong shearing force and high system viscosity.
The product obtained by combining the carrier oil, the hydrophobic particles, the wetting agent, the organic silicon synergist and the emulsifier has a good degassing effect, and can remove bubbles in ink, paint, adhesive, acrylic resin and other viscous systems.
Disclosure of Invention
The invention provides a defoaming composition which has a good effect on removing bubbles in a viscous system. The defoaming composition consists of carrier oil, hydrophobic particles, a wetting agent, an organosilicon synergist and an emulsifier:
A. carrier oil
The carrier oil is a tool carrying hydrophobic particles to permeate into the surface of bubbles in water, and refers to mineral oil with a cyclic, straight-chain and branched-chain structure consisting of two elements of hydrocarbon, and comprises base oil, white oil, alkylbenzene, naphthenic oil, liquid wax, diesel oil, engine oil and kerosene. These carrier oils are liquid at room temperature and are used alone or in combination.
The using amount of the carrier oil is 75-90% of the total mass of the defoaming composition.
B. Hydrophobic particles
The hydrophobic particles are key defoaming particles in the defoaming composition, and the hydrophobic particles refer to metal oxides and comprise one or more of silicon dioxide (commonly called white carbon black), aluminum oxide, zinc oxide or magnesium oxide. Hydrophobic white carbon black is preferably selected, and the specific surface area of the hydrophobic white carbon black is 200-500 m2/g。
Generally, the hydrophobic silica is obtained by heating and stirring hydrophilic silica and a hydrophobic agent in a reaction kettle. The materials for rendering the surface of the white carbon black hydrophobic include low-viscosity trimethylsiloxy-terminated polydimethylsiloxane, low-viscosity hydroxyl-terminated polydimethylsiloxane, hexamethyldisilazane, hexamethyldisiloxane, dimethyldiethoxysilane, methyltrimethoxysilane, methyltriethoxysilane, stearic acid, stearyl alcohol, octamethylcyclotetrasiloxane, tetramethylcyclotetrasiloxane, hexamethylcyclotrisiloxane.
The process for hydrophobizing silica is generally carried out by adding a suitable catalyst at a temperature above 80 ℃ and maintaining it for a period of time, the type and amount of hydrophobizing agent directly determining the degree of hydrophobicity of the resulting hydrophobic particles.
When preparing the defoaming composition, the hydrophobic particles with different specific surface areas and hydrophobicity are mixed in any proportion.
The hydrophobic particles account for 1-10% of the total mass of the defoaming composition.
C. Wetting agent
The wetting agent refers to water-soluble anionic and nonionic surfactants.
Anionic surfactants include alkyl sulfates, sulfonates, fatty acid or fatty acid ester sulfates, carboxylic acid soaps, phosphate esters.
The nonionic surfactant comprises alkylphenol ethoxylates, fatty alcohol-polyoxyethylene ether, polyoxyethylene-polyoxypropylene block copolymer and polyether modified polysiloxane.
The structural general formula of the polyether modified polysiloxane is as follows:
（Ⅰ）
in the formula (I), the compound is shown in the specification,mandnis the degree of polymerization of the silicon units,mis an integer of 1 to 20, and,nis an integer of 0 to 10; g is a polyether group of the formula-CH2CH2CH2O(EO) a (PO) b R1Wherein the subscriptaAndbis the degree of polymerization of EO and PO,ais in the range of 5 to 20,bis 3 to 10; r1Is a blocking group selected from a hydrogen atom, or a methyl group, or an acetyl group, or a butyl group.
The dosage of the wetting agent is 5-10% of the total mass of the defoaming composition.
D. Organosilicon synergist
The organosilicon synergist is mainly used for further improving the defoaming effect of the defoaming composition. The organosilicon synergist is a product formed by polysiloxane or lipophilic polyether modified polysiloxane and white carbon black under the action of an alkaline catalyst, and is finally diluted by a solvent or not.
The synthesis process of the organic silicon synergist can be inquired on the general technical data.
The dosage of the organosilicon synergist is 0.1-5%, preferably 0.5-3% of the total mass of the defoaming composition.
E. Emulsifier
The emulsifier is mainly used for emulsifying and dispersing carrier oil in an application system, and mainly refers to a nonionic surfactant, and comprises straight-chain fatty alcohol polyoxyethylene polyoxypropylene ether, heterogeneous fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, oleic acid polyoxyethylene ether, oleic acid polyoxyethylene polyoxypropylene ether, castor oil polyoxyethylene polyoxypropylene ether and polyether modified polysiloxane.
The dosage of the emulsifier is 1-10%, preferably 3-7% of the total mass of the defoaming composition.
According to the practical use situation, the defoaming composition disclosed by the invention is prepared into a solid product or an emulsion product.
The defoaming composition of the present invention is prepared as follows:
adding carrier oil, hydrophobic particles and a wetting agent into a container provided with an emulsification circulating pump, keeping the temperature at room temperature-150 ℃, stirring at the rotating speed of 300-3000 rpm for 0.5-4 h, and opening the emulsification circulating pump for circulation while stirring to enable the particle size distribution of the hydrophobic particles in the carrier oil to be below 1000 nm; then adding an organic silicon synergist, keeping the rotating speed, and further stirring and circulating for 0.5-2 h; and (3) cooling the temperature to be below 60 ℃, closing the circulating pump, reducing the rotating speed to be 200-800 rpm, adding the emulsifier, and stirring for 10-30 min to obtain the patent defoaming composition.
Drawings
FIG. 1 is a comparison of the transparency of the patent sample and the comparative sample after degassing in the application system.
Detailed Description
Selection of silicone wetting agent: the structural general formula of the organosilicon wetting agent is as follows:
respective subscripts in the examplesm、n、a、bAnd R1The values of (A) are as follows:
selection of organosilicon synergist: organosilicon synergist SS-1: the paint consists of a solvent, polydimethylsiloxane and hydrophobic white carbon black;
organosilicon synergist SS-2: consists of polyether, lipophilic polyether modified polysiloxane and hydrophobic white carbon black;
organosilicon synergist SS-3: the paint is prepared from polydimethylsiloxane, white carbon black, hydrophilic polyether modified polysiloxane and lipophilic polyether modified polysiloxane.
Example 1
84 parts of No. 26 white oil and 5 parts of hydrophobic white carbon black (the specific surface area is 200 m) are added into a container provided with an emulsification circulating pump2Performing chlorosilane hydrophobic treatment, wherein the hydrophobic value M = 70%) and 5 parts of lauryl polyoxyethylene (10) ether, keeping the temperature at 80 ℃, stirring at 1000rpm for 4h, and opening an emulsification circulating pump for circulation while stirring so that the particle size distribution of hydrophobic particles in carrier oil reaches 900 nm; then 1 part of SS-2 is added, and the mixture is kept onStirring and circulating for 1h at the rotating speed; and (3) reducing the temperature to 50 ℃, closing the circulating pump, reducing the rotating speed to 300rpm, adding 5 parts of isooctanol polyoxyethylene (8) ether, and stirring for 10min to obtain the de-foaming composition DA 1.
Example 2
75.5 parts of alkylbenzene and 9 parts of hydrophobic white carbon black (the specific surface area is 100 m) are added into a container provided with an emulsification circulating pump2Performing hydrophobic treatment on the simethicone, wherein the hydrophobic value M = 60%) and 9 parts of NP-10, keeping the temperature at 140 ℃, stirring at 2800rpm for 0.5h, and opening an emulsification circulating pump for circulation while stirring so that the particle size distribution of hydrophobic particles in carrier oil reaches 600 nm; then adding 4.5 parts of SS-1, keeping the rotating speed, further stirring and circulating for 0.6 h; cooling to 60 deg.C, turning off the circulating pump, reducing the rotation speed by 500rpm, adding 2 parts of octylphenol polyoxyethylene (10) ether, and stirring for 30min to obtain the debubbling composition DA 2.
Example 3
89.8 parts of naphthenic oil and 1.5 parts of hydrophobic white carbon black (the specific surface area is 380 m) are added into a container provided with an emulsification circulating pump2Silazane hydrophobization, hydrophobicity M = 65%) and 2.5 parts of D4425 (supplied by aksunobel) and 3 parts of wetting agent Silwet-4, maintaining the temperature at 100 ℃, stirring for 2.5h at 2500rpm, while turning on the circulation pump to allow the particle size distribution of the hydrophobic particles in the carrier oil to reach 800 nm; then adding 0.2 part of SS-3, keeping the rotating speed, further stirring and circulating for 2 hours; cooling to 40 deg.C, turning off the circulating pump, reducing the rotation speed to 800rpm, adding 3 parts of oleic acid polyoxyethylene (10) polyoxypropylene (2) ether, and stirring for 20min to obtain the debubbling composition DA 3.
Comparative example 1:
95.3 parts of naphthenic oil and 1.5 parts of hydrophobic white carbon black (the specific surface area is 380 m) are added into a container provided with an emulsification circulating pump2Silazane hydrophobization, hydrophobization M = 65%) and D4425 (supplied by aksounbell), maintaining the temperature at 100 ℃, stirring for 2.5h at 2500rpm, and opening the circulation pump while stirring, so that the particle size distribution of the hydrophobic particles in the carrier oil reaches 800 nm; then 0.2 part of SS is added-3, maintaining the above rotation speed, further stirring and circulating for 2 h; cooling to 40 ℃, turning off the circulating pump, reducing the rotating speed to 800rpm, adding 3 parts of oleic acid polyoxyethylene (10) polyoxypropylene (2) ether, and stirring for 20min to obtain the defoaming composition CDA 3-1.
Comparative example 2:
adding 90 parts of naphthenic oil and 1.5 parts of hydrophobic white carbon black (the specific surface area is 380 m) into a container provided with an emulsification circulating pump2Silazane hydrophobization, hydrophobization M = 65%) and 5.5 parts of D4425 (supplied by aksunobel) and the wetting agent Silwet-4, maintaining the temperature at 100 ℃, stirring for 2.5h at 2500rpm, and opening the circulation pump while stirring to achieve a particle size distribution of the hydrophobic particles in the carrier oil of 800 nm; then the temperature is reduced to 40 ℃, the circulating pump is closed, the rotating speed is reduced to 800rpm, 3 parts of oleic acid polyoxyethylene (10) polyoxypropylene (2) ether are added, and stirring is carried out for 20min, thus obtaining the defoaming composition CDA 3-2.
Comparative example 3:
adding 91.3 parts of naphthenic oil, 2.5 parts of D4425 (provided by Acksonobel) and 3 parts of wetting agent Silwet-4 into a container provided with an emulsification circulating pump, keeping the temperature at 100 ℃, stirring for 2.5 hours at the rotating speed of 2500rpm, and opening the circulation of the emulsification circulating pump while stirring to ensure that the particle size distribution of hydrophobic particles in carrier oil reaches 800 nm; then adding 0.2 part of SS-3, keeping the rotating speed, further stirring and circulating for 2 hours; and (3) cooling the temperature to 40 ℃, closing the circulating pump, reducing the rotating speed to 800rpm, adding 3 parts of oleic acid polyoxyethylene (10) polyoxypropylene (2) ether, and stirring for 20min to obtain the defoaming composition CDA 3-3.
Example 4
20 parts of liquid paraffin, 56 parts of white oil and 2 parts of hydrophobic white carbon black (the specific surface area is 80 m) are added into a container which is provided with an emulsification circulating pump at room temperature2/g, hydrophobic treatment of dimethyl silicone oil, hydrophobic value M = 60 percent) and 3 parts of hydrophobic white carbon black (specific surface area 380M)2Performing chlorosilane hydrophobic treatment, wherein the hydrophobic value M = 60%) and 7 parts of wetting agent Silwet-3, stirring for 3.5 hours at the rotating speed of 300rpm, and opening and circulating an emulsification circulating pump while stirring to ensure that the particle size distribution of hydrophobic particles in carrier oil reaches 900 nm; then 3 parts of SS-2 are added,keeping the rotating speed, further stirring and circulating for 0.6 h; and then closing the circulating pump, keeping the rotating speed at 200rpm, adding 9 parts of nonylphenol polyoxyethylene (8) ether, and stirring for 30min to obtain the de-foaming composition DA 4.
Example 5
5 parts of kerosene, 78.5 parts of alkylbenzene and 3 parts of hydrophobic white carbon black (the specific surface area is 380 m) are added into a container provided with an emulsification circulating pump2The preparation method comprises the following steps of (1)/g, performing hydrophobic treatment on the dimethyl silicone oil, wherein the hydrophobic value M = 60%) and 6 parts of wetting agent Silwet-1, raising the temperature to 100 ℃, stirring at the rotating speed of 3000rpm for 3.5h, and opening an emulsification circulating pump for circulation while stirring to enable the particle size distribution of hydrophobic particles in carrier oil to reach 900 nm; then adding 1.5 parts of SS-1, keeping the rotating speed, further stirring and circulating for 1 hour; then cooling to 50 ℃, closing a circulating pump, keeping the rotating speed at 350rpm, adding 3 parts of octylphenol polyoxyethylene (8) ether and 3 parts of C12-14 alcohol polyoxyethylene (10) ether, and stirring for 20min to obtain the de-foaming composition DA 5.
Example 6
30 parts of white oil, 25 parts of alkylbenzene, 30 parts of naphthenic oil and 1 part of hydrophobic white carbon black (the specific surface area is 200 m) are added into a container provided with an emulsification circulating pump2Perg, hydrophobic treatment of dimethyl silicone oil, hydrophobic value M = 60 percent) and 4 parts of hydrophobic white carbon black (specific surface area 380M)2Performing chlorosilane hydrophobic treatment, wherein the hydrophobic value M = 60%) and 3 parts of wetting agent Silwet-2, raising the temperature to 120 ℃, stirring at 2000rpm for 2.5h, and opening an emulsification circulating pump for circulation while stirring to ensure that the particle size distribution of hydrophobic particles in carrier oil reaches 800 nm; then adding 2 parts of SS-3, keeping the rotating speed, further stirring and circulating for 1.5 h; then cooling to 60 ℃, closing the circulating pump, keeping the rotating speed at 500rpm, adding 2 parts of castor oil polyoxyethylene (8) ether and 3 parts of oleic acid polyoxyethylene (10) ether, and stirring for 15min to obtain the de-foaming composition DA 6.
And (3) defoaming performance test:
(1) acrylic resin was used as the test medium:
the test method comprises the following steps: using an acrylic resin as a test medium, 250ml of the resin and 0.5g of a test sample were weighed into a 500ml beaker, and dispersed with a dispersion plate at 3000rpm for 10min, and the volume V of the dispersed acrylic resin was compared. The larger the value of V, the lower the density of the resin, and the worse the performance of the defoaming agent; the better the reverse.
The test results were as follows:
(2) gelatin solution was used as test medium:
heating 60 parts of tap water to 70-80 ℃, adding 40 parts of gelatin, stirring until gelatin particles are completely dissolved after the gelatin is added, adding 0.2 part of sample to be tested, stirring for 5min, standing, stirring, cooling and cooling. After 2h the transparency of the obtained solids was compared. The more transparent the solid, the better the defoaming effect of the tested sample.
The test results are shown in table and figure 1:
as demonstrated by tests in high viscosity systems of acrylic resin and gelatin solutions: the defoaming composition has good bubble removing capability and has advantages over the commercial XNZ; experiments of four samples DA3 and CDA 3-1-3 show that the organic silicon synergist and the wetting agent are good in assistance in removing bubbles.
Claims (3)
1. A defoaming composition is characterized by being prepared from carrier oil, hydrophobic particles, a wetting agent, an organosilicon synergist and an emulsifier:
A. the carrier oil is mineral oil with a cyclic, straight-chain and branched-chain structure and composed of hydrocarbon, and the using amount of the carrier oil is 75-90% of the total mass of the defoaming composition;
B. the hydrophobic particles are hydrophobic silicon dioxide, and the specific surface area of the hydrophobic particles is 200-500 m2(ii)/g; the hydrophobic particles account for 1-10% of the total mass of the defoaming composition;
C. the wetting agent is polyether modified polysiloxane and has the following structural general formula:
（Ⅰ）
in the formula (I), the compound is shown in the specification,mandnis the degree of polymerization of the silicon units,mis an integer of 1 to 20, and,nis an integer of 1 to 10; g is a polyether group of the formula-CH2CH2CH2O(EO) a (PO) b R1Wherein the subscriptaAndbis the degree of polymerization of EO and PO,ais in the range of 5 to 20,bis 3 to 10; r1Is a blocking group selected from a hydrogen atom, or a methyl group, or an acetyl group, or a butyl group;
the using amount of the wetting agent is 5-10% of the total mass of the defoaming composition;
D. the organic silicon synergist is a product formed by polysiloxane or lipophilic polyether modified polysiloxane and white carbon black under the action of an alkaline catalyst, and is finally diluted by a solvent or not; the using amount of the defoaming composition is 0.1-5% of the total mass of the defoaming composition;
E. the defoaming composition comprises an emulsifier, a defoaming agent and a defoaming agent, wherein the emulsifier is selected from straight-chain fatty alcohol polyoxyethylene polyoxypropylene ether, heterogeneous fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene, oleic acid polyoxyethylene ether, oleic acid polyoxyethylene polyoxypropylene ether, castor oil polyoxyethylene polyoxypropylene ether and polyether modified polysiloxane, and the using amount of the emulsifier is 1-10% of the total mass of the defoaming composition;
the preparation method of the defoaming composition comprises the following steps:
adding carrier oil, hydrophobic particles and a wetting agent into a container provided with an emulsification circulating pump, keeping the temperature to be between room temperature and 150 ℃, stirring at the rotating speed of 300-3000 rpm for 0.5-4 h, and opening the emulsification circulating pump for circulation while stirring to enable the particle size distribution of the hydrophobic particles in the carrier oil to be below 1000 nm; then adding an organic silicon synergist, keeping the rotating speed, and further stirring and circulating for 0.5-2 h; and (3) cooling the temperature to be below 60 ℃, closing the circulating pump, reducing the rotating speed to be 200-800 rpm, adding the emulsifier, and stirring for 10-30 min to obtain the defoaming composition.
2. The defoaming composition as claimed in claim 1, wherein the amount of the silicone synergist is 0.5-3% of the total mass of the defoaming composition.
3. The defoaming composition of claim 1, wherein the amount of the emulsifier is 3-7% of the total mass of the defoaming composition.
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| CN110433534B (en) * | 2019-08-28 | 2021-09-24 | 南京瑞思化学技术有限公司 | Preparation method of organic silicon defoaming emulsion |
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| CN110964369B (en) * | 2019-12-09 | 2022-04-12 | 天津中石化悦泰科技有限公司 | Hydrophobing agent composition and hydrophobing agent |
| CN114307260B (en) * | 2021-11-06 | 2023-10-27 | 南京瑞思化学技术有限公司 | Preparation method of polyether composition |
| CN114602214B (en) * | 2022-04-01 | 2023-04-07 | 南京瑞思化学技术有限公司 | Bio-based defoaming agent |
| CN115054953B (en) * | 2022-08-05 | 2024-04-02 | 山东圣佑高科新材料有限公司 | Efficient energy-saving organic silicon defoamer |
| CN115282644A (en) * | 2022-08-22 | 2022-11-04 | 山东师范大学实验厂有限公司 | High-efficiency modified silicon ether defoaming agent and preparation method thereof |
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| CN109248473A (en) | 2019-01-22 |
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