CN108905304B - Preparation method of organic silicon defoaming agent - Google Patents
Preparation method of organic silicon defoaming agent Download PDFInfo
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- CN108905304B CN108905304B CN201811088538.7A CN201811088538A CN108905304B CN 108905304 B CN108905304 B CN 108905304B CN 201811088538 A CN201811088538 A CN 201811088538A CN 108905304 B CN108905304 B CN 108905304B
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- 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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Abstract
The invention discloses a preparation method of an organic silicon defoaming agent, which takes vacuum pump condensed waste liquid in the production process of silicon rubber as an initial raw material, obtains a mixture through the steps of adsorption, synthesis and the like, and mixes and emulsifies the mixture, fumed silica, an emulsifying agent, water and the like to obtain the organic silicon defoaming agent. The invention effectively utilizes the condensed and collected liquid of the vacuum pump and converts the organic silicon waste liquid into the organic silicon defoaming agent with high added value. Meanwhile, the waste liquid synthetic product is used for replacing dimethyl silicone oil, so that the preparation cost of the organic silicon defoamer is reduced.
Description
Technical Field
The invention relates to a preparation method of a chemical auxiliary agent, and particularly relates to a preparation method of an organic silicon defoaming agent.
Background
At present, silicone rubber and other downstream products are produced by organic silicon enterprises, some siloxane low-molecular waste liquid is produced, the main sources of the siloxane low-molecular waste liquid are raw material dehydration and product low-vacuum pump condensate removal in the silicone rubber production process, and the main component of the siloxane low-molecular waste liquid is dimethyl siloxane mixed ring bodies and contains impurities such as rust, lubricating oil and the like. The rust and the lubricating oil in the waste liquid can not be removed by simple treatment, and the obtained waste liquid can not be directly used for producing high-quality and high-value downstream products. The waste liquid is generally sold for synthesizing a plurality of colored and odorous organosilicon low-end products, and the resource utilization efficiency is low.
The organic silicon waste liquid is usually filtered, washed, rectified and the like to remove impurities, but the filtering can only remove incompatible impurities in the system, the washing can generate a large amount of industrial waste water, the environmental protection pressure is increased, the energy consumption of rectification and impurity removal is high, and the cost is higher.
In many industrial production processes, such as printing and dyeing, fermentation, papermaking, coating, medicine, oil field exploitation, water treatment and the like, a large amount of foam is generated due to operations of stirring, vibration, boiling or addition of an easy-foaming auxiliary agent and the like, and if the foam is not properly treated, the foam brings troubles to the production, such as influence on normal operation of the production, reduction of effective loading capacity of equipment, reduction of product quality and production capacity and the like. The most effective and economically convenient method for eliminating and suppressing foam is to add an antifoaming agent. The organic silicon defoamer is widely applied due to the characteristics of strong defoaming capability, good thermal stability, strong physiological and chemical inertness, no toxicity, no harm, no secondary pollution and the like. Patent CN103830938A describes a preparation method of an organosilicon defoamer, which is prepared by emulsifying dimethyl silicone oil, a nonionic surfactant and other components under specific conditions. Patent CN103877755A discloses an organosilicon antifoaming agent and a preparation method thereof, which is prepared from dimethyl silicone oil, hydroxy silicone oil, silicon dioxide, fatty amine polyoxyethylene ether, hydrocarbonated oil, emulsifier, thickener, water and the like through the steps of heating, stirring, heat preservation and the like. Patent CN104225965A discloses an organosilicon defoamer and a preparation method thereof, which is prepared by mixing and emulsifying dimethicone, high boiling silicone oil, a thickener, water, an emulsifier, fumed silica and the like. However, the preparation of the silicone defoaming agent reported in the above patents all uses silicone oil as a main raw material, and the silicone defoaming agent is prepared by methods such as stirring and emulsification, and patent CN104225965A utilizes high-boiling silicone oil, but only uses the silicone oil in combination with methyl silicone oil, so that the dosage is small, the silicone waste liquid and waste gas cannot be fully utilized, and the cost is high.
Disclosure of Invention
In order to solve the problems of low utilization rate of organic silicon waste liquid and high cost of an organic silicon defoaming agent, the condensed liquid of a vacuum pump is adsorbed by activated carbon to remove rust and peculiar smell, the adsorbed waste liquid is mixed with hexamethyldisiloxane, a synthetic reaction is carried out under the catalysis of cation exchange resin to obtain a mixture of polysiloxane and lubricating oil, and the mixture is used for replacing methyl silicone oil to prepare the defoaming agent.
The preparation method of the organic silicon defoaming agent provided by the invention comprises the following steps:
(1) adsorbing and decolorizing waste liquid collected by a vacuum pump in the production process of silicon rubber by adopting activated carbon to obtain a product a, mixing the product a with hexamethyldisiloxane, reacting under the action of a ring-opening polymerization catalyst to obtain a product b, and removing low molecules from the product b at 180 ℃ of 150 and preferably at 160 ℃ to obtain a product c;
(2) adding the product c into the reaction vessel, heating to 130-160 ℃, adding the fumed silica while stirring, and continuing stirring for 3-6h after the mixture is uniformly stirred to obtain silicon paste;
(3) adding the silicon paste into a container, heating to 50-70 ℃, adding an emulsifier and water while stirring, uniformly mixing, and emulsifying for 20-30min by using the emulsifier to obtain the organic silicon defoaming agent.
The components of the waste liquid condensed and collected by the vacuum pump are 95-98% of dimethyl siloxane mixed ring bodies, 1-2% of mechanical impurities and 1-3% of lubricating oil.
The adsorption condition of the active carbon is that the temperature is 15-35 ℃ and the adsorption time is 10-30 min.
The mass of the hexamethyldisiloxane accounts for 0.8-1.2% of the mass of the product a, the dosage of the ring-opening polymerization catalyst accounts for 4-8% of the mass of the product a, the reaction temperature is 60-90 ℃, and the reaction time is 2.5-4.5 h.
The ring-opening polymerization catalyst is any one of cation exchange resin, tetramethyl ammonium hydroxide, potassium hydroxide and concentrated sulfuric acid.
The gas-phase white carbon black in the step (2) accounts for 4-6% of the mass of the product c; in the step (3), the mass ratio of the silicon paste to the emulsifier to the water is 1: 0.05-0.08: 8-10.
The emulsifier is a mixture of Span-80 and Tween-80, and the mass ratio of the emulsifier to the emulsifier is 1: 1-1.4.
The stirring speed of the emulsifying machine is 2500-. Compared with the prior art, the invention has the advantages that:
1. the invention effectively utilizes the condensed and collected liquid of the vacuum pump and converts the organic silicon waste liquid into the organic silicon defoaming agent with high added value.
2. The waste liquid synthesized product is used for replacing dimethyl silicone oil, so that the synthesis cost of the organic silicon defoamer is reduced.
3. The waste liquid contains partial lubricating oil components, which can play a certain defoaming role and make full use of all the components in the waste liquid.
Detailed Description
Example 1:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 30min at 15 ℃ by using activated carbon, mixing the adsorbed waste liquid, hexamethyldisiloxane and cation exchange resin according to the mass ratio of 100:0.8:6, reacting for 4h at 80 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100g of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 4g of fumed silica while stirring, and stirring for 3 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1:1. Adding 100g of silicon paste into a container, heating to 60 ℃, adding 800g of water while stirring, then adding 5g of emulsifier, and emulsifying at 3500r/min for 20min after uniformly mixing to obtain the organic silicon defoamer.
Example 2:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 25min by adopting activated carbon at 25 ℃, mixing the adsorbed waste liquid, hexamethyldisiloxane and cation exchange resin according to the mass ratio of 100:0.8:4, reacting for 4.5h at 90 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100g of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 5g of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.1. Adding 100g of silicon paste into a container, heating to 60 ℃, adding 850g of water while stirring, then adding 6g of emulsifier, uniformly mixing, and emulsifying for 25min at 3000r/min to obtain the organic silicon defoamer.
Example 3:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 15min at 35 ℃ by using activated carbon, mixing the adsorbed waste liquid, hexamethyldisiloxane and potassium hydroxide according to the mass ratio of 100:1:6, reacting for 3h at 80 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100g of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 6g of fumed silica while stirring, and stirring for 6 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.2. Adding 100g of silicon paste into a container, heating to 60 ℃, adding 950g of water while stirring, then adding 7g of emulsifier, and emulsifying for 30min at 2500r/min after uniform mixing to obtain the organic silicon defoamer.
Example 4:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 25min by adopting activated carbon at 25 ℃, mixing the adsorbed waste liquid, hexamethyldisiloxane and tetramethylammonium hydroxide according to the mass ratio of 100:1.2:8, reacting for 3.5h at 60 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100kg of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 5kg of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.3. Adding 100kg of silicon paste into a container, heating to 60 ℃, adding 1000kg of water while stirring, then adding 8kg of emulsifier, uniformly mixing, and emulsifying for 30min at 3000r/min to obtain the organic silicon defoamer.
Example 5:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 25min by adopting activated carbon at 25 ℃, mixing the adsorbed waste liquid, hexamethyldisiloxane and concentrated sulfuric acid according to the mass ratio of 100:1.0:8, reacting for 2.5h at 80 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100kg of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 5kg of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.4. Adding 100kg of silicon paste into a container, heating to 60 ℃, adding 950kg of water while stirring, then adding 7kg of emulsifier, uniformly mixing, and emulsifying for 30min at 3000r/min to obtain the organic silicon defoamer.
Example 6:
adsorbing waste liquid collected by a vacuum pump in the production process of silicon rubber for 25min by adopting activated carbon at 25 ℃, mixing the adsorbed waste liquid, hexamethyldisiloxane and cation exchange resin according to the mass ratio of 100:0.9:6, reacting for 4h at 80 ℃ to obtain a mixture, and removing low molecules from the mixture at 160 ℃ for 2h to obtain a synthetic product. And adding 100kg of the synthetic product into a reaction container, heating to 150 ℃, slowly adding 5kg of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.2. Adding 100kg of silicon paste into a container, heating to 60 ℃, adding 950kg of water while stirring, then adding 7kg of emulsifier, uniformly mixing, and emulsifying for 30min at 3000r/min to obtain the organic silicon defoamer.
Comparative example 1
Adding 100 parts of 500mpa.s methyl silicone oil into a reaction vessel, heating to 150 ℃, slowly adding 5 parts of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.2. Adding 100 parts of silicon paste into a container, heating to 60 ℃, adding 950 parts of water while stirring, then adding 7 parts of emulsifier, uniformly mixing, and emulsifying for 30min at 3000r/min to obtain the organic silicon defoamer.
Comparative example 2
Adding 100 parts of 1000mpa.s methyl silicone oil into a reaction vessel, heating to 150 ℃, slowly adding 5 parts of fumed silica while stirring, and stirring for 4.5 hours after all the fumed silica is added until the product is in a uniform paste shape to obtain the silicon paste. Mixing Span-80 and Tween-80 as an emulsifier according to the mass ratio of 1: 1.4. Adding 100 parts of silicon paste into a container, heating to 60 ℃, adding 950 parts of water while stirring, then adding 7 parts of emulsifier, uniformly mixing, and emulsifying for 30min at 3000r/min to obtain the organic silicon defoamer.
And (3) defoaming performance detection:
the defoaming agents of the above examples and comparative examples were tested according to GB/T26527-2011 and the results are shown in Table 1:
TABLE 1 comparison of defoaming Properties of defoaming agent
Claims (6)
1. A preparation method of an organic silicon defoaming agent is characterized by comprising the following steps:
(1) the method comprises the steps of adsorbing and decoloring waste liquid collected by a vacuum pump in the production process of silicon rubber by using activated carbon to obtain a product a, mixing the product a with hexamethyldisiloxane, reacting under the action of a ring-opening polymerization catalyst to obtain a product b, removing low molecules from the product b at the temperature of 150-;
(2) adding the product c into the reaction vessel, heating to 130-160 ℃, adding the fumed silica while stirring, and continuing stirring for 3-6h after the mixture is uniformly stirred to obtain silicon paste;
(3) adding the silicon paste obtained in the step (2) into a container, heating to 50-70 ℃, adding an emulsifier and water while stirring, uniformly mixing, and emulsifying for 20-30min by using the emulsifier to obtain the organic silicon defoaming agent.
2. The method for preparing the silicone antifoaming agent of claim 1, wherein the activated carbon adsorption conditions are a temperature of 15 ℃ to 35 ℃ and an adsorption time of 10 to 30 min.
3. The method for preparing the silicone defoaming agent according to claim 1, wherein the mass of hexamethyldisiloxane is 0.8-1.2% of the mass of the product a, the amount of the ring-opening polymerization catalyst is 4-8% of the mass of the product a, the reaction temperature is 60-90 ℃, the reaction time is 2.5-4.5h to obtain a product b, and the low molecular weight of the product b is removed at 160 ℃ to obtain a product c.
4. The method for preparing the silicone defoaming agent according to claim 1, wherein the fumed silica in step (2) accounts for 4-6% of the mass of the product c; in the step (3), the mass ratio of the silicon paste to the emulsifier to the water is 1: 0.05-0.08: 8-10.
5. The method for preparing the silicone antifoaming agent of claim 1, wherein the emulsifier is a mixture of Span-80 and Tween-80, and the mass ratio is 1: 1-1.4.
6. The method for preparing the silicone antifoaming agent of claim 1, wherein the stirring speed of the emulsifying machine is 2500-.
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| CN100427671C (en) * | 2004-12-10 | 2008-10-22 | 曹治平 | Moderate temperature prnited and dyed organosilicon anti-bubbling and its preparing method |
| CN102343165A (en) * | 2011-10-20 | 2012-02-08 | 山东大易化工有限公司 | Efficient silicone defoaming agent |
| CN104225965B (en) * | 2014-09-24 | 2015-11-18 | 湖北兴瑞化工有限公司 | A kind of silicone defoaming agent and preparation method thereof |
| CN105504290A (en) * | 2015-12-24 | 2016-04-20 | 开封中节能再生能源有限公司 | Antifoaming agent for household garbage leachate treatment system and desulfurization slurry foam |
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