CN-121988077-A - High-temperature-resistant environment-friendly defoamer and preparation method thereof

CN121988077ACN 121988077 ACN121988077 ACN 121988077ACN-121988077-A

Abstract

The invention relates to the field of high-temperature-resistant environment-friendly defoamers, in particular to a high-temperature-resistant environment-friendly defoamer and a preparation method thereof, which are used for solving the technical problems of poor high-temperature resistance, easiness in demulsification and layering at high temperature, weak defoaming and foam inhibition effects and insufficient environment friendliness of the traditional organic silicon defoamer; the high-temperature silicone grease is prepared by mixing phenyl-polyether-epoxy tri-modified polysiloxane and modified hydrophobic fumed silica to prepare high-temperature silicone grease, then preparing a water phase from a composite emulsifier, glycerol and deionized water, dropwise adding the high-temperature silicone grease into the water phase to prepare a pre-emulsion, adding xanthan gum into the pre-emulsion after high-shear homogenization to thicken and stabilize the pre-emulsion, and filtering to obtain the high-temperature-resistant environment-friendly defoaming agent.

Inventors

WANG XUE
HU ZHIREN
ZHANG YU
SUN HUI
LI HONG
WANG KUNPENG
SUN LU
CHEN QI
CAI YIMING
YANG ZHIMING

Assignees

鞍钢栗田(鞍山)水处理有限公司

Dates

Publication Date: 20260508
Application Date: 20260409

Claims (9)

1. The high-temperature-resistant environment-friendly defoamer is characterized by comprising the following components in parts by weight: 30-40 parts of phenyl-polyether-epoxy tri-modified polysiloxane, 1.5-3.0 parts of modified hydrophobic fumed silica, 4-7 parts of composite emulsifier, 1-2 parts of glycerol, 0.1-0.4 part of xanthan gum and 40-60 parts of deionized water; wherein the phenyl-polyether-epoxy tri-modified polysiloxane is prepared by the following steps: Step a1, octamethyl cyclotetrasiloxane, D4H cyclotetrasiloxane, 1, 3-tetramethyl disiloxane, octaphenyl cyclotetrasiloxane and trifluoromethane sulfonic acid are added into a three-neck flask for stirring reaction, then anhydrous sodium bicarbonate is added for stirring, filtering and rotary evaporation are carried out, and drying is carried out, thus obtaining phenyl modified hydrogen-containing polysiloxane intermediate; Step a2, adding ethylene glycol monoallyl ether, polyethylene glycol monoallyl ether, karstedt catalyst and toluene into a three-neck flask, stirring, dropwise adding phenyl modified hydrogen-containing polysiloxane intermediate-toluene solution, heating for continuous reaction, cooling, performing rotary evaporation, extracting with n-hexane, performing rotary evaporation on an organic phase again, and drying to obtain phenyl-polyether double-modified polysiloxane; And a3, adding the phenyl-polyether double-modified polysiloxane, epichlorohydrin and tetrabutylammonium bromide into a three-neck flask, stirring, cooling, dropwise adding a sodium hydroxide solution, continuously stirring, adding dichloromethane, extracting, washing, drying, rotary evaporation concentrating, and drying to obtain the phenyl-polyether-epoxy three-modified polysiloxane.
2. The high temperature resistant environment friendly defoamer according to claim 1, wherein the dosage ratio of octamethyl cyclotetrasiloxane, D4H cyclotetrasiloxane, 1, 3-tetramethyl disiloxane, octaphenyl cyclotetrasiloxane, trifluoromethanesulfonic acid and anhydrous sodium bicarbonate in step a1 is 25-31g, 15.0-18.8g, 1.4-1.8g, 1.95-2.43g, 0.08-0.10g, 2.2-2.8g, the dosage ratio of ethylene glycol monoallyl ether, polyethylene glycol monoallyl ether, toluene and phenyl modified hydrogen polysiloxane intermediate-toluene solution in step a2 is 22-24g, 27-29g, 14.4-15.7mL, the dosage ratio of phenyl-polyether bismodified polysiloxane, epichlorohydrin, tetrabutylammonium bromide and sodium hydroxide solution in step a3 is 21-23g, 26-29g, 2.4-15.7 mL.
3. The high temperature resistant environment friendly defoamer of claim 1, wherein the Karstedt catalyst in step a2 is used in an amount of 9-11ppm based on the total system mass.
4. The high-temperature-resistant environment-friendly defoamer according to claim 1, wherein the phenyl-modified hydrogen-containing polysiloxane intermediate-toluene solution in the step a2 is a solution prepared by mixing the phenyl-modified hydrogen-containing polysiloxane intermediate and toluene according to a dosage ratio of 13g to 14.4 mL.
5. The high temperature resistant environment-friendly defoamer of claim 1, wherein the mass fraction of sodium hydroxide solution in step a3 is 40%.
6. The high-temperature-resistant environment-friendly defoamer of claim 1, wherein the modified hydrophobic fumed silica is prepared by the following steps: Adding hydrophobic fumed silica into toluene, performing ultrasonic dispersion, transferring into a three-neck flask, and dripping The glycidol ether oxypropyl trimethoxy silane is heated, stirred continuously, cooled, filtered, washed, dried in vacuum, crushed and sieved to obtain the modified hydrophobic fumed silica.
7. The high temperature resistant environment friendly defoamer of claim 6, wherein said hydrophobic fumed silica, toluene and The dosage ratio of the glycidol ether oxypropyl trimethoxy silane is 10-12g to 80-96mL to 1.2-1.4g.
8. A method for preparing the high temperature resistant environment-friendly defoamer, which is characterized by comprising the following steps: Weighing 30-40 parts of phenyl-polyether-epoxy tri-modified polysiloxane, 1.5-3.0 parts of modified hydrophobic fumed silica, 4-7 parts of composite emulsifier, 1-2 parts of glycerol, 0.1-0.4 part of xanthan gum and 40-60 parts of deionized water according to parts by weight for standby; Adding phenyl-polyether-epoxy tri-modified polysiloxane and modified hydrophobic fumed silica into a reaction kettle, stirring, cooling to obtain a high Wen Guigao, adding deionized water into another reaction kettle, sequentially adding a composite emulsifier and glycerol, heating and stirring to obtain a water phase, dripping high-temperature silicone paste into the water phase, and stirring after dripping to obtain a pre-emulsion; step three, transferring the pre-emulsion into a high-shear homogenizer for homogenization, and controlling the average particle size of the emulsion And then cooling, adding xanthan gum, stirring at a low speed, filtering and discharging to obtain the high-temperature-resistant environment-friendly defoamer.
9. The preparation method of the high-temperature-resistant environment-friendly defoamer according to claim 8, wherein the composite emulsifier is compounded by alkyl glycoside, fatty alcohol polyoxyethylene ether and span-80 according to a mass ratio of 2:2:1.

Description

High-temperature-resistant environment-friendly defoamer and preparation method thereof Technical Field The invention relates to the field of high-temperature-resistant environment-friendly defoamers, in particular to a high-temperature-resistant environment-friendly defoamer and a preparation method thereof. Background The defoamer is a key functional auxiliary agent in industrial production and is widely applied to the fields of chemical industry, printing and dyeing, wastewater treatment and the like. The traditional organosilicon defoamer mostly takes polydimethylsiloxane as a main component, has poor high temperature resistance, and is easy to cause problems of demulsification layering, suddenly reduced defoaming efficiency and the like in a high-temperature and high-shear system. It is difficult to combine compatibility, foam inhibition and high temperature stability with simple polyether or phenyl modified silicone oil. The common hydrophobic fumed silica is easy to agglomerate and has poor compatibility with a matrix, so that the long-acting use performance of the product is further limited. With the increasingly strict environmental protection requirements, the traditional defoamer containing volatile organic compounds and nondegradable components can not meet the environmental protection production requirements. The current market lacks a water-based organic silicon defoamer which has the advantages of quick defoaming, long-acting foam inhibition, high-temperature stability and environmental friendliness, and is difficult to adapt to industrial application under the working condition of high Wen Yanke. Therefore, developing a high-efficiency defoamer with stable structure, high temperature resistance and environmental protection has important practical value and market prospect. Disclosure of Invention In order to overcome the technical problems, the invention aims to provide a high-temperature-resistant environment-friendly defoaming agent and a preparation method thereof. The aim of the invention can be achieved by the following technical scheme: in a first aspect, the application provides a high-temperature-resistant environment-friendly defoamer, which comprises the following components in parts by weight: 30-40 parts of phenyl-polyether-epoxy tri-modified polysiloxane, 1.5-3.0 parts of modified hydrophobic fumed silica, 4-7 parts of composite emulsifier, 1-2 parts of glycerol, 0.1-0.4 part of xanthan gum and 40-60 parts of deionized water; wherein the phenyl-polyether-epoxy tri-modified polysiloxane is prepared by the following steps: Step a1, octamethyl cyclotetrasiloxane, D4H cyclotetrasiloxane, 1, 3-tetramethyl disiloxane, octaphenyl cyclotetrasiloxane and trifluoromethanesulfonic acid are added into a three-neck flask provided with a stirrer, a thermometer and an air duct, nitrogen is introduced for protection, stirring reaction is carried out for 24-26H under the condition that the temperature is 25-30 ℃ and the stirring rate is 300-400r/min, anhydrous sodium bicarbonate is added after the reaction is completed, stirring is carried out for 60-65min, filtering is carried out, rotary evaporation is carried out on filtrate, and then the filtrate is placed into a vacuum drying box, and drying is carried out for 6-7H under the condition that the temperature is 80-85 ℃ to obtain a phenyl modified hydrogen-containing polysiloxane intermediate; step a2, adding ethylene glycol monoallyl ether, polyethylene glycol monoallyl ether, karstedt catalyst and toluene into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant pressure dropping funnel, introducing nitrogen for protection, stirring for 15-20min under the conditions of 80-85 ℃ and stirring speed of 300-400r/min, dropping phenyl modified hydrogen-containing polysiloxane intermediate-toluene solution into the three-neck flask by using the constant pressure dropping funnel, controlling the dropping to be completed within 90-100min, heating to 100 ℃ for continuous reaction for 5-7h, cooling to room temperature after the reaction is completed, performing rotary evaporation, extracting for 3-4 times by using n-hexane, performing rotary evaporation again on an organic phase, then placing the organic phase in a vacuum drying box, and drying for 4-5h under the conditions of 80-85 ℃ to obtain phenyl-polyether double-modified polysiloxane; Adding phenyl-polyether double-modified polysiloxane, epichlorohydrin and tetrabutylammonium bromide into a three-neck flask provided with a stirrer, a thermometer, an air duct and a constant pressure dropping funnel, introducing nitrogen for protection, stirring for 6-7h at the temperature of 80-85 ℃ and the stirring rate of 300-400r/min, cooling to room temperature, dropwise adding sodium hydroxide solution, continuously stirring for 4-5h at the temperature of 50-55 ℃, adding dichloromethane for extraction after the reaction is completed, washing an organic phase with deionized water