CN112973198A - Powder defoaming agent and preparation method and application thereof - Google Patents

Powder defoaming agent and preparation method and application thereof Download PDF

Info

Publication number
CN112973198A
CN112973198A CN202110242374.4A CN202110242374A CN112973198A CN 112973198 A CN112973198 A CN 112973198A CN 202110242374 A CN202110242374 A CN 202110242374A CN 112973198 A CN112973198 A CN 112973198A
Authority
CN
China
Prior art keywords
defoaming agent
powder
parts
reaction kettle
sodium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110242374.4A
Other languages
Chinese (zh)
Other versions
CN112973198B (en
Inventor
王梅玲
周青烽
冯猛
王斌
蒋建生
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guangdong Zhongke Hongtai New Materials Co ltd
Original Assignee
Guangdong Zhonglianbang Fine Chemical Co ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guangdong Zhonglianbang Fine Chemical Co ltd filed Critical Guangdong Zhonglianbang Fine Chemical Co ltd
Priority to CN202110242374.4A priority Critical patent/CN112973198B/en
Publication of CN112973198A publication Critical patent/CN112973198A/en
Application granted granted Critical
Publication of CN112973198B publication Critical patent/CN112973198B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/02Foam dispersion or prevention
    • B01D19/04Foam dispersion or prevention by addition of chemical substances
    • B01D19/0404Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
    • B01D19/0409Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G65/00Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
    • C08G65/02Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
    • C08G65/26Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
    • C08G65/2603Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
    • C08G65/2606Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
    • C08G65/2609Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Dispersion Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Degasification And Air Bubble Elimination (AREA)

Abstract

The invention discloses a powder defoaming agent and a preparation method and application thereof, wherein the powder defoaming agent for a polycarboxylate water reducer cement mortar system comprises the following components in parts by weight: 5-25 parts of an organic silicon defoaming agent, 5-20 parts of a polyether foam inhibitor and 60-90 parts of a solid carrier, wherein the polyether foam inhibitor has a structure shown in a formula 1: CH (CH)2=CH‑CH2‑(PO)m‑(EO)n‑O‑R1Formula 1 wherein R1Is C1~C20M is 0 to 20, and n is 0 to 20. The powder defoaming agent is used for a polycarboxylate water reducer cement mortar system and has a good defoaming and foam inhibiting effect.

Description

Powder defoaming agent and preparation method and application thereof
Technical Field
The invention relates to the technical field of defoaming agents for a polycarboxylate water reducer cement mortar system, and particularly relates to a powder defoaming agent and a preparation method and application thereof.
Background
With the development of cement mortar technology, a high-performance water reducing agent has become one of indispensable components in the use process of cement mortar. The polycarboxylic acid water reducing agent is a concrete admixture which can reduce the water consumption for mixing under the condition of keeping the slump constant of concrete basically. The polycarboxylic acid water reducing agent mostly belongs to an anionic surfactant, has a dispersing effect on cement particles after being added into a cement mortar mixture, can improve the workability, reduce the unit water consumption and improve the fluidity of the cement mortar mixture; or the unit cement consumption is reduced, the cement is saved, and the development hotspot and direction of the water reducing agent technology in recent years are formed.
In the using process of the common polycarboxylic acid water reducing agent cement mortar, bubbles can be caused by physical stirring of production equipment, chemical reaction among various auxiliary agents and uneven proportion of reagents and water, and meanwhile, some surface active ingredients for reducing the surface tension are always reserved in the production process of the polycarboxylic acid water reducing agent, so that a large amount of micro bubbles can be introduced in the process of mixing the cement mortar, the introduced bubbles are aggregated into large bubbles through vibration, and the quality and the density of the cement mortar can be greatly influenced by the bubbles, so that the durability and the strength of the cement mortar can be reduced. Because the defoaming agent has certain pertinence to a mixed system, and different defoaming agents and different mixing amounts have different defoaming effects on the system, the prior defoaming agent specially used for cement mortar is few, and particularly the defoaming agent used for a polycarboxylic acid water reducing agent cement mortar system is less.
Therefore, a powder defoaming agent is needed to solve the problems of the prior art.
Disclosure of Invention
The invention aims to provide a powder defoaming agent which has a good defoaming and foam inhibiting effect when being used for a polycarboxylate water reducer cement mortar system.
The invention also aims to provide a preparation method of the powder defoaming agent, and the powder defoaming agent with better defoaming and foam inhibiting effects is prepared by the preparation method.
The invention also aims to provide an application of the powder defoaming agent in a polycarboxylate water reducer cement mortar system.
In order to achieve the purpose, the invention provides a powder defoaming agent for a polycarboxylate water reducer cement mortar system, which comprises the following components in parts by weight:
5-25 parts of an organic silicon defoaming agent;
5-20 parts of a polyether foam inhibitor;
60-90 parts of a solid carrier;
the polyether suds suppressor has the structure of formula 1:
CH2=CHCH2-(PO)m-(EO)n-O-R1
formula 1
In the formula 1R1The alkyl group is C1-C20, m is 0-20, and n is 0-20.
Compared with the prior art, the powder defoaming agent comprises an organic silicon defoaming agent, a polyether foam inhibitor and a solid carrier, wherein the organic silicon defoaming agent has better defoaming capability but poor foam inhibition capability. In the preparation of the polyether foam inhibitor, a series of polyether foam inhibitors with different performances can be obtained by changing the ratio of an initiator, ethylene oxide and propylene oxide and the polymerization mode (block or random), so that although the polyether foam inhibitor is commonly used for foam inhibition, the polyether foam inhibitor has different foam inhibition capabilities due to different alkyl positions, different relative molecular masses, the presence or absence of side bonds and the number of ether bonds, and further the performances of dispersion, emulsification, lubrication and the like are influenced. Through long-term scientific experiments, the inventor of the invention finds that the polyether foam inhibitor with the structure shown in the formula 1 has excellent foam inhibition capability from accumulated mass data, has higher chemical stability because the tail end of a molecular chain is substituted by alkyl, and is suitable for being used under acid-base and high-temperature conditions. Therefore, the powder defoaming agent prepared by compounding the organic silicon defoaming agent, the solid carrier and the polyether defoaming agent with the structure shown in the formula 1 has better defoaming capability and foam inhibiting capability, and can overcome the defects of poor stability of an emulsion type defoaming agent, poor safety of a solution type defoaming agent and the like. The powder defoamer is directly mixed with the polycarboxylate water reducer cement mortar when in use, and can inhibit the regeneration of foam in the cement mortar for a long time, so the powder defoamer also has the characteristics of convenient use, safety and high stability.
Preferably, the viscosity of the polyether foam inhibitor is 100-1000 mPa.s.
Preferably, the preparation raw materials of the silicone defoaming agent comprise the following components in percentage by mass:
Figure BDA0002962266820000031
preferably, the preparation method of the silicon paste comprises the following steps: :
(1) uniformly mixing dimethyl silicone oil and gas-phase hydrophobic white carbon black, and heating and reacting for a period of time to obtain a raw material A;
(2) and cooling the raw material A to room temperature to obtain the silicon paste.
Preferably, the viscosity of the dimethyl silicone oil is 500-3000 mPa.s, and the viscosity of the dimethyl silicone oil is preferably 1000-3000 mPa.s; the specific surface area of the white carbon black is 100-500 m2The specific surface area of the white carbon black is preferably 200-250 m2The particle size of the white carbon black is 1-10 mu m; the mass ratio of the dimethyl silicone oil to the gas-phase hydrophobic white carbon black is (20-30) to (1-10).
Preferably, in the step (1) of the preparation method of the silicon paste, the dimethyl silicone oil and the gas-phase hydrophobic white carbon black are uniformly mixed and then react for 4-6 hours at 150-200 ℃.
Preferably, the thickener of the present invention is selected from at least one of carboxymethyl cellulose, propylene glycol alginate, methyl cellulose, sodium starch phosphate, sodium carboxymethyl cellulose, sodium alginate, casein, sodium polyacrylate, polyoxyethylene, and polyvinylpyrrolidone.
Preferably, the preparation method of the silicone defoaming agent comprises the following steps:
(1) adding the silicon paste and the emulsifier into a reaction kettle, and heating and stirring for a period of time;
(2) slowly dripping water at a certain temperature into the reaction kettle in the step (1), quickly dripping the rest water after phase inversion of the system, and continuously reacting for a period of time after dripping is finished;
(3) and (3) adding the thickening agent into the reaction kettle in the step (2), stirring for a period of time, stopping heating, and continuing stirring for a period of time to obtain the organic silicon defoaming agent.
Preferably, the heating temperature in the step (1) of the preparation method of the organic silicon defoaming agent is 75-80 ℃, the stirring speed is 2500-3000 rpm, and the stirring time is 1-2 hours; the temperature of the water in the step (2) is 70-75 ℃, and the continuous reaction time is 60-90 min; and (4) stirring for 30min in the step (3), stopping heating, and continuing stirring for 30-60 min.
Preferably, the emulsifier of the present invention comprises at least one of Span20, Span40, Span60, Span80, Tween20, Tween40, Tween60 and Tween 80.
Preferably, the preparation method of the polyether foam inhibitor with the structure of formula 1 comprises the following steps:
(1) putting an initiator fatty alcohol and a catalyst into a high-pressure reaction kettle, and sequentially sealing, vacuumizing and replacing with nitrogen;
(2) heating the high-pressure reaction kettle in the step (1) to a certain temperature, introducing a mixture of ethylene oxide and propylene oxide, controlling a certain pressure, absorbing until the kettle pressure is zero, and removing small molecules while the kettle is hot;
(3) adding the sodium alkoxide solution into the high-pressure reaction kettle in the step (2), and vacuumizing for a period of time at a certain temperature;
(4) and (4) cooling the high-pressure reaction kettle in the step (3) to below a certain temperature, adding halogenated alkane, reacting for a period of time at a certain temperature and pressure, and reducing the pressure and the temperature to obtain the halogen-free halogen.
Preferably, in the step (1) of the preparation method of formula 1 of the present invention, nitrogen is substituted for 3 times, and nitrogen is substituted for the nitrogen until the oxygen content is less than 0.01%; raising the temperature of the high-pressure reaction kettle to 85-100 ℃, and controlling the pressure to be 0.35-0.45 MPa; in the step (3), the temperature is 95 ℃, the vacuum pressure is 0.08-0.09 MPa, and the time is 1 h; and (4) cooling the high-pressure reaction kettle in the step (4) to below 40 ℃, adding halogenated alkane, and heating to 100-110 ℃, wherein the pressure is 0.35-0.45 MPa, and the time is 3-4 hours.
PreferablyThe initiator fatty alcohol of the present invention includes at least one of allyl alcohol, butanol, propylene glycol, glycerin and pentaerythritol; the catalyst is at least one of potassium hydroxide and sodium hydroxide; the sodium alkoxide is at least one of sodium methoxide, potassium methoxide and sodium ethoxide; the halogenated alkane being CpH2p+1Cl or CpH2p+1Br, wherein p is 1-10. The catalyst comprises, by mass, 5-10 parts of initiator fatty alcohol, 0.1-1 part of catalyst, 1-5 parts of sodium alkoxide, 1-5 parts of halogenated alkane, 10-30 parts of ethylene oxide and 40-60 parts of propylene oxide.
Preferably, the solid carrier of the present invention is selected from at least one of anhydrous sodium sulphate, sodium carbonate, sodium metasilicate, talcum powder, diatomaceous earth, phosphate, starch, bentonite, attapulgite, 4A zeolite, calcium carbonate, industrial salts and sodium tripolyphosphate.
In order to achieve the above object, the present invention further provides a preparation method of the above powder defoaming agent, comprising the steps of:
(1) uniformly mixing the organic silicon defoaming agent, the polyether foam inhibitor and the solid carrier according to the formula ratio to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
Compared with the prior art, the organic silicon defoaming agent with strong defoaming capability and the polyether defoaming agent with excellent foam inhibiting capability and the structure shown in the formula 1 are compounded to prepare the powder defoaming agent, and the powder defoaming agent has better defoaming capability and foam inhibiting capability.
In order to realize the purpose, the invention also provides an application of the powder defoaming agent in a polycarboxylate water reducer cement mortar system.
Compared with the prior art, the powder defoamer can be directly mixed with the polycarboxylic acid water reducing agent cement mortar when in use, and can inhibit the regeneration of foam in the cement mortar for a long time.
Detailed Description
The purpose, technical solution and advantages of the present invention will be further described by the following embodiments, but the present invention is not limited thereto. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The powder defoaming agent of the embodiment is used for a polycarboxylate water reducing agent cement mortar system, and comprises the following components in parts by weight:
5 parts of an organic silicon defoaming agent;
5 parts of a polyether foam inhibitor;
90 parts of calcium carbonate;
the preparation method of the organic silicon defoaming agent comprises the following steps:
(1) adding 25 mass percent of silicon paste and 5 mass percent of Span20 into a reaction kettle, and stirring at 75 ℃ at a stirring speed of 2500rpm for 2 hours;
(2) slowly dripping 69.4 percent hot water into the reaction kettle in the step (1), quickly dripping the rest water after the system is subjected to phase inversion, and continuously reacting for 70min after the dripping is finished, wherein the temperature of the hot water is 70 ℃;
(3) adding 0.6% by mass of carboxymethyl cellulose into the reaction kettle in the step (2), stirring for 30min, stopping heating, and continuing stirring for 40min to obtain an organic silicon defoaming agent;
the preparation method of the silicon paste comprises the following steps:
(1) dimethyl silicone oil with the viscosity of 1000mPa.s and the specific surface area of 200m2Uniformly mixing/g of gas-phase hydrophobic white carbon black, and reacting at 150 ℃ for 6 hours to obtain a raw material A, wherein the mass ratio of the dimethyl silicone oil to the gas-phase hydrophobic white carbon black is 4: 1, the particle size of the white carbon black is 10 mu m;
(2) cooling the raw material A to room temperature to prepare silicon paste;
the preparation method of the polyether foam inhibitor comprises the following steps:
(1) putting allyl alcohol and potassium hydroxide into a high-pressure reaction kettle, sequentially sealing, vacuumizing and replacing with nitrogen for 3 times, and replacing with nitrogen until the oxygen content is less than 0.01%;
(2) raising the temperature of the high-pressure reaction kettle in the step (1) to 85 ℃, introducing a mixture of ethylene oxide and propylene oxide, controlling the pressure to be 0.35MPa, absorbing until the kettle pressure is zero, and removing small molecules while the kettle is hot;
(3) adding a sodium methoxide solution into the high-pressure reaction kettle in the step (2), and vacuumizing for 1h at 95 ℃ under the vacuum pressure of 0.08 MPa;
(4) reducing the temperature of the high-pressure reaction kettle in the step (3) to 35 ℃, and adding C2H5Cl reacts for 4 hours at 100 ℃ and 0.35MPa, and the polyether foam inhibitor shown as the following compound 1 is prepared by decompression and cooling;
wherein allyl alcohol 5 parts, potassium hydroxide 0.2 parts, sodium methoxide solution 1 part, C2H5Cl 2 parts, ethylene oxide 15 parts and propylene oxide 50 parts;
CH2=CH-CH2-(PO)12-(EO)6-O-C2H5
compound 1
The preparation method of the powder defoaming agent comprises the following steps:
(1) uniformly mixing 5 parts of an organic silicon defoaming agent, 5 parts of a polyether foam inhibitor and 90 parts of calcium carbonate to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
Example 2
The powder defoaming agent of the embodiment is used for a polycarboxylate water reducing agent cement mortar system, and comprises the following components in parts by weight:
10 parts of an organic silicon defoaming agent;
5 parts of a polyether foam inhibitor;
85 parts of sodium carbonate;
the preparation method of the organic silicon defoaming agent comprises the following steps:
(1) adding 22 mass percent of silicon paste and 8 mass percent of Tween80 into a reaction kettle, and stirring at the stirring speed of 2800rpm at 80 ℃ for 1 h;
(2) slowly dripping 69.7% hot water into the reaction kettle in the step (1), quickly dripping the rest water after the system is subjected to phase inversion, and continuously reacting for 65min after the dripping is finished, wherein the temperature of the hot water is 73 ℃;
(3) adding sodium carboxymethylcellulose with the mass fraction of 0.3% into the reaction kettle in the step (2), stirring for 30min, stopping heating, and continuing stirring for 50min to obtain an organic silicon defoaming agent;
the preparation method of the organic silicon defoaming agent comprises the following steps:
(1) dimethyl silicone oil with the viscosity of 2000mPa.s and the specific surface area of 250m2Uniformly mixing/g of gas-phase hydrophobic white carbon black, and reacting at 180 ℃ for 5 hours to obtain a raw material A, wherein the mass ratio of the dimethyl silicone oil to the gas-phase hydrophobic white carbon black is 4: 1, the particle size of the white carbon black is 10 mu m;
(2) cooling the raw material A to room temperature to prepare silicon paste;
the preparation method of the polyether foam inhibitor comprises the following steps:
(1) putting allyl alcohol and sodium hydroxide into a high-pressure reaction kettle, sequentially sealing, vacuumizing and replacing with nitrogen for 3 times, and replacing with nitrogen until the oxygen content is less than 0.01%;
(2) raising the temperature of the high-pressure reaction kettle in the step (1) to 95 ℃, introducing a mixture of ethylene oxide and propylene oxide, controlling the pressure to be 0.40MPa, absorbing until the kettle pressure is zero, and removing small molecules while the kettle is hot;
(3) adding the sodium ethoxide solution into the high-pressure reaction kettle in the step (2), and vacuumizing for 1h at 95 ℃ under the vacuum pressure of 0.08 MPa;
(4) cooling the high-pressure reaction kettle in the step (3) to 35 ℃, and adding C3H7Br is reacted for 3.5 hours at 105 ℃ and 0.40MPa, and the polyether foam inhibitor shown as the following compound 2 is prepared after decompression and cooling;
wherein, calculated by weight portion, 8 portions of allyl alcohol, 0.5 portion of sodium hydroxide, 3 portions of sodium ethoxide solution and C3H7Br3 parts, ethylene oxide 20 parts and propylene oxide 55 parts;
CH2=CH-CH2-(PO)13-(EO)7-O-C3H7
compound 2
The preparation method of the powder defoaming agent comprises the following steps:
(1) uniformly mixing 10 parts of an organic silicon defoaming agent, 5 parts of a polyether foam inhibitor and 85 parts of sodium carbonate to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
Example 3
The powder defoaming agent of the embodiment is used for a polycarboxylate water reducing agent cement mortar system, and comprises the following components in parts by weight:
10 parts of an organic silicon defoaming agent;
10 parts of a polyether foam inhibitor;
80 parts of sodium tripolyphosphate;
the preparation method of the organic silicon defoaming agent comprises the following steps:
(1) adding 28 mass percent of silicon paste and 7 mass percent of Span80 into a reaction kettle, and stirring at the stirring speed of 3000rpm for 2 hours at 75 ℃;
(2) slowly dripping 64.2 percent hot water into the reaction kettle in the step (1), quickly dripping the rest water after the system is subjected to phase inversion, and continuously reacting for 85min after the dripping is finished, wherein the temperature of the hot water is 70 ℃;
(3) adding the complexing protein with the mass fraction of 0.8% into the reaction kettle in the step (2), stirring for 30min, stopping heating, and continuing stirring for 60min to obtain the organic silicon defoaming agent;
the preparation method of the silicon paste comprises the following steps:
(1) dimethyl silicone oil with the viscosity of 2500mPa.s and the specific surface area of 220m2Uniformly mixing/g of gas-phase hydrophobic white carbon black, and reacting at 200 ℃ for 6 hours to obtain a raw material A, wherein the mass ratio of the dimethyl silicone oil to the gas-phase hydrophobic white carbon black is 22: 7, the particle size of the white carbon black is 5 mu m;
(2) cooling the raw material A to room temperature to prepare silicon paste;
the preparation method of the polyether foam inhibitor comprises the following steps:
(1) putting allyl alcohol and potassium hydroxide into a high-pressure reaction kettle, sequentially sealing, vacuumizing and replacing with nitrogen for 3 times, and replacing with nitrogen until the oxygen content is less than 0.01%;
(2) raising the temperature of the high-pressure reaction kettle in the step (1) to 85 ℃, introducing a mixture of ethylene oxide and propylene oxide, controlling the pressure to be 0.35MPa, absorbing until the kettle pressure is zero, and removing small molecules while the kettle is hot;
(3) adding a sodium methoxide solution into the high-pressure reaction kettle in the step (2), and vacuumizing for 1h at 95 ℃ under the vacuum pressure of 0.09 MPa;
(4) cooling the high-pressure reaction kettle in the step (3) to 30 ℃, and adding CH3Cl reacts for 4 hours at 110 ℃ and 0.4MPa, and the polyether foam inhibitor shown as the following compound 3 is prepared by decompression and cooling;
wherein allyl alcohol 10 parts, potassium hydroxide 0.9 part, sodium methoxide solution 5 parts, CH35 parts of Cl, 30 parts of ethylene oxide and 60 parts of propylene oxide;
CH2=CH-CH2-(PO)16-(EO)6-O-CH3
compound 3
The preparation method of the powder defoaming agent comprises the following steps:
(1) uniformly mixing 10 parts of an organic silicon defoaming agent, 10 parts of a polyether foam inhibitor and 80 parts of sodium tripolyphosphate to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
Comparative example 1
The powder defoaming agent of the comparative example is used for a polycarboxylate water reducer cement mortar system and comprises the following components in parts by weight:
5 parts of an organic silicon defoaming agent;
5 parts of a high-viscosity organic silicon defoaming agent;
90 parts of calcium carbonate;
the preparation method of the silicone defoaming agent and the preparation method of the silicon paste of this comparative example are all the same as those of example 1, and the preparation method of the high-viscosity silicone defoaming agent includes:
(1) adding high-viscosity silicon paste with the mass fraction of 25% and Span20 with the mass fraction of 5% into a reaction kettle, and stirring at the stirring speed of 2500rpm at 75 ℃ for 2 h;
(2) slowly dripping 69.4 percent hot water into the reaction kettle in the step (1), quickly dripping the rest water after the system is subjected to phase inversion, and continuously reacting for 70min after the dripping is finished, wherein the temperature of the hot water is 70 ℃;
(3) adding 0.6 mass percent of carboxymethyl cellulose into the reaction kettle in the step (2), stirring for 30min, stopping heating, and continuing stirring for 40min to prepare the high-viscosity organic silicon defoaming agent;
the high-viscosity silicon paste can be prepared by the following method:
(1) dimethyl silicone oil with viscosity of 40000mPa.s and specific surface area of 200m2Uniformly mixing/g of gas-phase hydrophobic white carbon black, and reacting at 150 ℃ for 6 hours to obtain a raw material A, wherein the mass ratio of the dimethyl silicone oil to the gas-phase hydrophobic white carbon black is 4: 1, the particle size of the white carbon black is 10 mu m;
(2) and cooling the raw material A to room temperature to obtain the high-viscosity silicon paste.
Comparative example 2
The powder defoaming agent of the comparative example is used for a polycarboxylate water reducer cement mortar system and comprises the following components in parts by weight:
10 parts of defoaming and foam inhibiting agent;
90 parts of calcium carbonate;
the preparation method of the defoaming and foam inhibiting agent of the comparative example comprises the following steps:
(1) adding 20 mass percent of silicon paste, 14 mass percent of polyether foam inhibitor and 5 mass percent of Span20 into a reaction kettle, and stirring at 75 ℃ at a stirring speed of 2500rpm for 2 hours;
(2) slowly dripping 60.4 percent hot water into the reaction kettle in the step (1), quickly dripping the rest water after the system is subjected to phase inversion, and continuously reacting for 70min after the dripping is finished, wherein the temperature of the hot water is 70 ℃;
(3) adding 0.6 mass percent of carboxymethyl cellulose into the reaction kettle in the step (2), stirring for 30min, stopping heating, and continuing stirring for 40min to prepare the defoaming and foam inhibiting agent;
the preparation methods of the polyether suds suppressor and the silicon paste were the same as those of example 1.
The preparation method of the powder defoaming agent of the comparative example comprises the following steps:
(1) uniformly mixing 10 parts of defoaming and foam inhibiting agent and 90 parts of calcium carbonate to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
At present, the defoaming performance evaluation method of the defoaming agent is most commonly used for testing the static defoaming time and the foam inhibition time of the defoaming agent on foam in an aqueous solution. Due to the fact that the polycarboxylic acid water reducer cement mortar is high in solid content, contains various additives, is subjected to high-speed shearing and mixing, has air bubble distribution and has the diffusion rate of the defoaming agent, the defoaming performance of the defoaming agent in an aqueous solution is obviously different from that of the defoaming agent in the polycarboxylic acid water reducer cement mortar, and therefore the influence of evaluation media and conditions on the defoaming effect is ignored in many polycarboxylic acid water reducer cement mortar defoaming agent testing methods. In order to more truly and effectively evaluate the defoaming performance of the prepared powder defoaming agent in the polycarboxylate water reducer cement mortar, the defoaming effect of the powder defoaming agent is evaluated by adopting the density recovery rate of the cement mortar. The slurry preparation is simulated by referring to the national standard GB/T19139-2003 oil well cement test method, the performance of the powder defoamer in the polycarboxylate superplasticizer cement mortar system can be intuitively reflected, and the experimental data is closer to the true value.
Preparation method of polycarboxylic acid water reducing agent cement mortar
(1) Accurately weighing cement and other solid materials, and then fully and uniformly mixing;
(2) accurately weighing mixing water and a liquid additive, mixing the mixing water and the liquid additive, filling the mixture into a stirring cup, starting a motor and keeping the rotation speed of 4000rpm +/-200 rpm so as to completely disperse the additive in the mixing water;
(3) uniformly adding the solid mixed material into a stirring cup, wherein the process is guaranteed to be completed within 15 s;
(4) after all the solid mixed materials are added into the mixing water, covering a stirring cup cover, and then continuously stirring for 35s +/-1 s at the rotating speed of 12000rpm +/-500 rpm to prepare cement mortar;
(5) and adding a fluid loss agent PVA2488 and a drag reducer SXY into the cement mortar to prepare the polycarboxylic acid water reducer cement mortar, wherein the addition amounts of the fluid loss agent PVA2488 and the drag reducer SXY are respectively 0.5 percent and 0.3 percent of the mass of the cement mortar.
Application of powder defoaming agent to polycarboxylate superplasticizer cement mortar
Taking 1 part of cement mortar and six parts of polycarboxylic acid water reducing agent cement mortar, selecting five parts of polycarboxylic acid water reducing agent cement mortar as an experimental group, and the other part of polycarboxylic acid water reducing agent cement mortar as a blank control group, respectively adding 0.1 mass percent of the powder defoaming agent in the examples 1-3 and the comparative examples 1-2 into the experimental group to prepare polycarboxylic acid water reducing agent cement mortar containing the powder defoaming agent, respectively testing the density of the polycarboxylic acid water reducing agent cement mortar containing the powder defoaming agent, the density of the cement mortar and the density of the polycarboxylic acid water reducing agent cement mortar in the blank control group by referring to the regulation of the 6 th part of GB/T19139 Suan-2003 oil well cement test method, and calculating the density recovery rate (R) of the polycarboxylic acid water reducing agent cement mortar according to the following formula. The greater the density recovery value, the better the defoaming effect of the defoaming agent, and the test results are shown in table 1:
Figure BDA0002962266820000121
in the formula: p1-cement mortar Density (g/cm)3) (ii) a Density (g/cm) of P2-polycarboxylic acid water reducer cement mortar3) (ii) a Pp 3-polycarboxylic acid water reducing agent cement mortar density (g/cm3) containing powder defoamer, wherein P1 is 1.850g/cm3,P2=1.781g/cm3
TABLE 1 results of Density recovery of polycarboxylic acid water reducing agent cement mortars of examples 1 to 3 and comparative examples 1 to 2
Figure BDA0002962266820000122
Comparing example 1 with comparative example 1, the density recovery ratio of the polycarboxylic acid water reducing agent cement mortar of example 1 is greater than that of comparative example 1, which shows that the defoaming performance of the powder defoaming agent of example 1 is better than that of comparative example 1, because the silicone defoaming agent and the high viscosity silicone defoaming agent used in comparative example 1 both belong to silicone defoaming agents, and the silicone defoaming agent has better defoaming capability but poorer foam inhibition capability, while the polyether defoaming agent having better foam inhibition capability and the silicone defoaming agent having better defoaming capability are used in example 1, so that the defoaming performance of the powder defoaming agent of comparative example 1 is not as good as that of example 1.
Comparing example 1 with comparative example 2, the density recovery of the polycarboxylic acid water reducing agent cement mortar of example 1 is greater than that of comparative example 2, which indicates that the defoaming performance of the powder defoaming agent of example 1 is better than that of comparative example 2, which indicates that the defoaming performance of the powder defoaming agent cannot be improved by the emulsification reaction of the silicon paste with the polyether defoaming agent.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A powder defoaming agent for a polycarboxylate water reducer cement mortar system is characterized by comprising the following components in parts by weight:
5-25 parts of an organic silicon defoaming agent;
5-20 parts of a polyether foam inhibitor;
60-90 parts of a solid carrier;
the polyether suds suppressor has the structure of formula 1:
CH2=CH-CH2-(PO)m-(EO)n-O-R1
formula 1
R in the formula 11Is C1~C20M is 0 to 20, and n is 0 to 20.
2. The powder antifoaming agent of claim 1, wherein the viscosity of the polyether suds suppressor is 100 to 1000 mPa.s.
3. The powder defoaming agent of claim 1, wherein the silicone defoaming agent is prepared from the following raw materials in percentage by mass:
Figure FDA0002962266810000011
4. the powder antifoaming agent of claim 3, wherein the preparation method of the silicon paste comprises:
(1) uniformly mixing dimethyl silicone oil and gas-phase hydrophobic white carbon black, and heating and reacting for a period of time to obtain a raw material A;
(2) and cooling the raw material A to room temperature to obtain the silicon paste.
5. The powder antifoaming agent of claim 3, wherein the thickener is at least one selected from the group consisting of carboxymethylcellulose, propylene glycol alginate, methylcellulose, sodium starch phosphate, sodium carboxymethylcellulose, sodium alginate, casein, sodium polyacrylate, polyoxyethylene, and polyvinylpyrrolidone.
6. The powder defoaming agent of any one of claims 3 to 5, wherein the preparation method of the silicone defoaming agent comprises the following steps:
(1) adding the silicon paste and the emulsifier into a reaction kettle, and heating and stirring for a period of time;
(2) slowly dripping the water with a certain temperature into the reaction kettle in the step (1), quickly dripping the residual water after the phase inversion of the system, and continuously reacting for a period of time after the dripping is finished;
(3) and (3) adding the thickening agent into the reaction kettle in the step (2), stirring for a period of time, stopping heating, and continuing stirring for a period of time to obtain the organic silicon defoaming agent.
7. The powder defoamer of claim 1, wherein the polyether defoamer of formula 1 is prepared by a process comprising:
(1) putting an initiator fatty alcohol and a catalyst into a high-pressure reaction kettle, and sequentially sealing, vacuumizing and replacing with nitrogen;
(2) heating the high-pressure reaction kettle in the step (1) to a certain temperature, introducing a mixture of ethylene oxide and propylene oxide, controlling a certain pressure, absorbing until the kettle pressure is zero, and removing small molecules while the kettle is hot;
(3) adding a sodium alkoxide solution into the high-pressure reaction kettle in the step (2), and vacuumizing for a period of time at a certain temperature;
(4) and (3) cooling the high-pressure reaction kettle in the step (3) to below a certain temperature, adding halogenated alkane, reacting for a period of time at a certain temperature and pressure, and reducing the pressure and the temperature to obtain the halogen-free halogen-.
8. The powder defoamer of claim 1, wherein said solid carrier is selected from at least one of anhydrous sodium sulphate, sodium carbonate, sodium metasilicate, talc, diatomaceous earth, phosphates, starch, bentonite, attapulgite, zeolite 4A, calcium carbonate, industrial salts and sodium tripolyphosphate.
9. The preparation method of the powder defoaming agent according to any one of claims 1 to 8, comprising the steps of:
(1) uniformly mixing the organic silicon defoaming agent, the polyether foam inhibitor and the solid carrier according to the formula ratio to obtain a raw material B;
(2) and granulating the raw material B through a granulator and drying to obtain the powder defoaming agent.
10. The application of the powder defoaming agent as claimed in any one of claims 1 to 8 in a polycarboxylate water reducer cement mortar system.
CN202110242374.4A 2021-03-04 2021-03-04 Powder defoaming agent and preparation method and application thereof Active CN112973198B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110242374.4A CN112973198B (en) 2021-03-04 2021-03-04 Powder defoaming agent and preparation method and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110242374.4A CN112973198B (en) 2021-03-04 2021-03-04 Powder defoaming agent and preparation method and application thereof

Publications (2)

Publication Number Publication Date
CN112973198A true CN112973198A (en) 2021-06-18
CN112973198B CN112973198B (en) 2022-11-11

Family

ID=76352742

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110242374.4A Active CN112973198B (en) 2021-03-04 2021-03-04 Powder defoaming agent and preparation method and application thereof

Country Status (1)

Country Link
CN (1) CN112973198B (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114534320A (en) * 2021-12-31 2022-05-27 南通市晗泰化工有限公司 Micro-explosion slow-release type defoaming agent and preparation process thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3912652A (en) * 1973-12-17 1975-10-14 Dow Corning Defoaming composition useful in jet dyeing
US20120053277A1 (en) * 2010-08-31 2012-03-01 E. I. Du Pont De Nemours And Company Matting agent composition containing low molecular weight polytrimethylene ether glycol
CN106345148A (en) * 2016-10-21 2017-01-25 中国石油集团川庆钻探工程有限公司长庆固井公司 Siloxane foam inhibitor as well as preparation method and application thereof
CN107428883A (en) * 2015-02-05 2017-12-01 阿朗新科德国有限责任公司 Include the composition of the microgel based on NBR

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3912652A (en) * 1973-12-17 1975-10-14 Dow Corning Defoaming composition useful in jet dyeing
US20120053277A1 (en) * 2010-08-31 2012-03-01 E. I. Du Pont De Nemours And Company Matting agent composition containing low molecular weight polytrimethylene ether glycol
CN107428883A (en) * 2015-02-05 2017-12-01 阿朗新科德国有限责任公司 Include the composition of the microgel based on NBR
CN106345148A (en) * 2016-10-21 2017-01-25 中国石油集团川庆钻探工程有限公司长庆固井公司 Siloxane foam inhibitor as well as preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114534320A (en) * 2021-12-31 2022-05-27 南通市晗泰化工有限公司 Micro-explosion slow-release type defoaming agent and preparation process thereof

Also Published As

Publication number Publication date
CN112973198B (en) 2022-11-11

Similar Documents

Publication Publication Date Title
CN112973198B (en) Powder defoaming agent and preparation method and application thereof
CN106633559B (en) A kind of high-performance polyethylene polyvinyl butyral resin and preparation method thereof
CN109608632B (en) Concrete anti-mud sacrificial agent and preparation method thereof
CN111646725A (en) Wet-mixed mortar plasticity stabilizer and preparation method thereof
CN110681186A (en) Powder defoaming agent with lasting foam inhibition performance and preparation method thereof
CN113372570B (en) Lignin glyceryl ether phosphate and preparation method and application thereof
CN107935826A (en) Good fatty alcohol block polyether of a kind of low-temperature stability and its preparation method and application
CN112159151B (en) Pumping agent and preparation method thereof
CN111389057A (en) Preparation method of organic silicon defoaming agent
CN110776603A (en) Preparation method of polycarboxylic acid mud-resistant water reducer synthesized by sodium lignosulfonate
CN113929389B (en) High-strength lightweight concrete and preparation method thereof
CN111825372B (en) Polycarboxylic acid high-performance water reducing agent and preparation method thereof
CN113480229A (en) Composite liquid chromium removal agent and preparation method and application thereof
CN113577841A (en) Preparation method of foam-inhibiting defoaming agent for production of gray paperboard
CN109354917B (en) Water-based calcium stearate emulsion and preparation method thereof
CN113797598A (en) Preparation method of organosilicon defoaming composition
CN115322360B (en) Preparation method and application of unit alcohol polymer block polyether
CN116639905B (en) Additive for mortar and preparation method thereof
CN114835433B (en) Stone powder concrete regulator based on modified particles
CN117342820B (en) Composite polycarboxylate superplasticizer and preparation method thereof
CN110922546B (en) Phenyl hydroxyl compound ATRP method modified polycarboxylic acid slump retaining agent and preparation method thereof
CN112724050B (en) Phosphorus-free alkali-resistant solubilizer and preparation and application thereof
CN118001788A (en) Organic silicon defoamer and preparation method thereof
CN111203150B (en) Nonionic surfactant and preparation method thereof
CN109970894B (en) Polymer type concrete defoaming agent, preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CP03 Change of name, title or address

Address after: Room 1908, building B1, Everbright we Valley, No.4, headquarters 2nd Road, Songshanhu hi tech Industrial Development Zone, Dongguan City, Guangdong Province, 523000

Patentee after: Guangdong Zhongke Hongtai New Materials Co.,Ltd.

Country or region after: China

Address before: Room 1908, building B1, Everbright we Valley, No.4, headquarters 2nd Road, Songshanhu hi tech Industrial Development Zone, Dongguan City, Guangdong Province, 523000

Patentee before: GUANGDONG ZHONGLIANBANG FINE CHEMICAL CO.,LTD.

Country or region before: China