CN109608645B - Preparation method of self-dispersed micron-sized hydrophobic powder - Google Patents
Preparation method of self-dispersed micron-sized hydrophobic powder Download PDFInfo
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- CN109608645B CN109608645B CN201811312227.4A CN201811312227A CN109608645B CN 109608645 B CN109608645 B CN 109608645B CN 201811312227 A CN201811312227 A CN 201811312227A CN 109608645 B CN109608645 B CN 109608645B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/442—Block-or graft-polymers containing polysiloxane sequences containing vinyl polymer sequences
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/28—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/65—Water proofers or repellants
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
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- Polymers & Plastics (AREA)
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Abstract
A preparation method of self-dispersion micron-sized hydrophobic powder comprises the following steps of adding a low-molecular-weight water-soluble polymer and a hydroxy acrylic acid emulsion into water, adding organosiloxane according to a proportion, reacting to obtain a viscous white emulsion, adding an end-capping agent, adjusting pH to form gel, and drying to obtain micron-sized powdery hydrophobic powder. The wet gel is obtained by siloxane polycondensation and dispersion polymerization, and the micron-sized spherical hydrophobic powder can be obtained without mechanical crushing after drying, and has the characteristics of low cost, simple and convenient production operation, controllable hydrophobic effect of the powder, wide application scene adaptability and the like.
Description
Technical Field
The invention relates to a preparation method of self-dispersed micron-sized hydrophobic powder for the field of buildings.
Background
The water-proofing and water-proofing properties of building engineering have been a problem of concern, and various water-proofing agents and water-proofing emulsion additives have been developed in the fields of water-proofing and water-proofing of houses, bridges and other concrete buildings. The liquid waterproof agent is inconvenient to transport, is usually applied to the surface of a substrate, has poor durability and is limited in application range. The hydrophobic powder is used as one kind of waterproof agent, may be used in cement and dry mortar powder material, and may be added in small amount to reach waterproof and impervious effect and certain alkali returning resisting effect.
At present, the preparation method of hydrophobic powder mainly comprises the following steps: the preparation method comprises two modes of adding a substance with hydrophobic groups into a powder material for carrying out loading or modification and carrying out mechanical crushing after synthesizing the hydrophobic material. However, the above method has the following problems: most of the hydrophobic groups carried by the powder are physically adsorbed on the powder, the hydrophobic groups are not firmly combined with the powder, the loading rate is low, and the powder is not easy to disperse; the hydrophobic powder prepared by the latter has larger particle size, is not easy to disperse in materials, and influences the hydrophobic effect of the materials and products.
Aiming at the defects in the prior art, the invention provides a preparation method of self-dispersed micron-sized hydrophobic powder, wet gel is obtained by siloxane polycondensation and dispersion polymerization, and micron-sized spherical hydrophobic powder can be obtained without mechanical crushing after drying.
Disclosure of Invention
The invention provides a preparation method of self-dispersed micron-sized hydrophobic powder, which is based on the basic principle of a gel synthesis method, different types of organic siloxane are added into a water-soluble polymer solution containing low molecular weight, the organic siloxane is subjected to condensation reaction in an aqueous solution, and a molecular chain is adsorbed on a polymer chain and gradually grows up in the process of growing to form white emulsion and finally gel. And drying the gel to obtain micron-sized powdery hydrophobic powder.
The method comprises the following steps:
(A) adding a low-molecular-weight water-soluble polymer into the measured water, stirring and dissolving, adding a small amount of hydroxyl acrylic emulsion, and adjusting the pH of the system to 8-9 to prepare a precursor solution;
(B) slowly adding organic siloxane into the precursor solution according to the proportion, and reacting to obtain viscous white emulsion;
(C) adding a capping agent into the emulsion, wherein the amount of the capping agent is 0.1-1 wt%, adjusting the pH of the system to 9-10, standing until gel is formed, and drying to obtain the micron-sized powdery hydrophobic powder.
The low molecular weight water-soluble polymer in the step (A) of the invention comprises one or a combination of two or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, acrylic acid polymer and derivatives thereof, 2-acrylamido-2-methylpropanesulfonic acid polymer and derivatives thereof, acrylamide polymer and derivatives thereof, and natural polysaccharide and derivatives thereof.
In the step (A) of the invention, the mass concentration of the water-soluble polymer is 0.5-15%, preferably 1.5-4.5%;
in the step (A), the mass concentration of the hydroxyl acrylic emulsion is 0.1-2%, preferably 0.4-1.2%;
in step (B), the organosiloxane is one or a combination of two or more of methyltrimethoxysilane, phenyltrimethoxysilane, isooctyltriethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethoxysilane, octadecyltrimethoxysilane and gamma-glycidoxypropyltrimethoxysilane.
In step (C) of the present invention, the end-capping agent is one or a combination of two or more of trimethylmethoxysilane, methoxy (dimethyl) octylsilanalkoxysilyl compound, and silazane compound.
The mass ratio of substances in the steps (A) and (B) is 1:3-3:1, preferably 1.5:1-1: 1.5.
According to the invention, through hydroxyl condensation and dispersion polymerization reaction, hydroxyl acrylic emulsion is taken as a seed, siloxane is adsorbed on a water-soluble polymer molecular chain to complete the molecular chain growth, and white emulsion and final gel are formed. And drying the gel to obtain micron-sized powdery hydrophobic powder. The particle size and surface functional groups of the reacted particles are adjusted by adjusting the proportion of the components, so that hydrophobic powder with different particle sizes and different hydrophobic effects is obtained. The method has the characteristics of low cost, simple and convenient production operation, controllable hydrophobic effect of the powder and wide application scene adaptability, and is very suitable for large-scale industrial production.
Drawings
FIG. 1 is an SEM image at 750 times magnification of micron-sized powdery hydrophobic powder prepared in example 1.
FIG. 2 is an SEM image at 1100 times magnification of the micron-sized powdered hydrophobic powder prepared in example 1.
Detailed Description
Example 1
A preparation method of self-dispersing micron-sized hydrophobic powder comprises the following preparation steps:
weighing 96g of water, adding 3g of polyvinylpyrrolidone while stirring, fully mixing and dissolving, then adding 1g of hydroxyacrylic acid emulsion, and adjusting the pH of the system to 8-9 by using AMP-95 to obtain a precursor solution.
30g of methyltrimethoxysilane is weighed and added into the precursor solution of the (1), a mixture of 20g of methyltrimethoxysilane and 20g of dodecyl trimethoxysilane is added dropwise within 1 hour under stirring, and the reaction is continued for 20min to obtain viscous white emulsion.
Adding 2g of methoxy (dimethyl) octyl silane into the emulsion, adjusting the pH value of the system to 9-10, standing until gel is formed, and drying in an oven to obtain the micron-sized powdery hydrophobic powder.
The micron-sized powdered hydrophobic powder prepared as described above is shown in fig. 1 and 2, and the hydrophobic powder particles are uniformly dispersed and have a particle size distribution of 2-5 microns.
Example 2
A preparation method of self-dispersing micron-sized hydrophobic powder comprises the following preparation steps:
weighing 84g of water, adding 15g of 2-acrylamide-2-methylpropanesulfonic acid polymer solution (20 wt%) while stirring, fully mixing and dissolving, then adding 1g of hydroxy acrylic emulsion, and adjusting the pH of the system to 8-9 by using 10% NaOH solution to obtain a precursor solution.
30g of methyltrimethoxysilane is weighed and added into the precursor solution of the (1), a mixture of 20g of methyltrimethoxysilane and 20g of octadecyltrimethoxysilane is added dropwise within 1h while stirring, and the reaction is continued for 20min to obtain viscous white emulsion.
And adding 1g of trimethyl methoxy silane into the emulsion, adjusting the pH value of the system to 9-10, standing until gel is formed, and drying in an oven to obtain the micron-sized powdery hydrophobic powder.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (3)
1. A preparation method of self-dispersing micron-sized hydrophobic powder is characterized by comprising the following steps:
(A) adding a low-molecular-weight water-soluble polymer with the mass concentration of 1.5-4.5% into the measured water, stirring and dissolving, adding a small amount of hydroxyl acrylic emulsion with the mass concentration of 0.4-1.2%, adjusting the pH value of the system to 8-9, and preparing a precursor solution;
(B) slowly adding organic siloxane into the precursor solution according to the mass ratio of 1:1.5-1.5:1, and reacting to obtain viscous white emulsion;
(C) adding a blocking agent into the emulsion, wherein the amount of the blocking agent is 0.1-1 wt%, adjusting the pH value of the system to 9-10, standing until gel is formed, drying in an oven, and obtaining micron-sized powdery hydrophobic powder without mechanical crushing after drying;
in the step (C), the end-capping agent is one or a combination of two or more of trimethylmethoxysilane, methoxy (dimethyl) octylsilane, an alkoxysilyl compound or a silazane compound.
2. The method of preparing self-dispersed micron-sized hydrophobic powder according to claim 1, wherein the low molecular weight water-soluble polymer in the step (a) is selected from one or a combination of two or more of polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, acrylic acid polymer and derivatives thereof, 2-acrylamido-2-methylpropanesulfonic acid polymer and derivatives thereof, acrylamide polymer and derivatives thereof, and natural polysaccharide and derivatives thereof.
3. The method of preparing self-dispersed micron-sized hydrophobic powder according to claim 1, wherein in the step (B), the organosiloxane is one or more of methyltrimethoxysilane, phenyltrimethoxysilane, isooctyltriethoxysilane, dodecyltrimethoxysilane, hexadecyltrimethoxysilane, octadecyltrimethoxysilane and gamma-glycidoxypropyltrimethoxysilane.
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Family Cites Families (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3704400A1 (en) * | 1987-02-12 | 1988-08-25 | Wacker Chemie Gmbh | POWDER CONTAINING IN WATER REDISPERGABLE, ORGANO (POLY) SILOXANE AND METHOD FOR THE PRODUCTION THEREOF |
| DE102004057996A1 (en) * | 2004-12-01 | 2006-06-08 | Wacker Polymer Systems Gmbh & Co. Kg | Hydrophobic additive |
| DE102004059377A1 (en) * | 2004-12-09 | 2006-06-22 | Wacker Polymer Systems Gmbh & Co. Kg | Hydrophobic, water-redispersible polymer powder |
| CN100460427C (en) * | 2006-07-21 | 2009-02-11 | 华南理工大学 | Siloxane containing water soluble polymer emulsion and redispersible emulsion powder and its preparation method |
| CN101168584B (en) * | 2007-09-28 | 2010-10-06 | 上海东升新材料有限公司 | Redispersable latex powder emulsion, redispersable latex powder and preparation method thereof |
| US20120020106A1 (en) * | 2009-03-23 | 2012-01-26 | Cabot Corporation | particle containing a hydrophobic region and a hydrophilic region and methods to make same |
| KR101155431B1 (en) * | 2011-03-03 | 2012-06-15 | 주식회사 지오스 | Manufacturing method for silica aerogel powder |
| JP6087929B2 (en) * | 2011-09-19 | 2017-03-01 | ダウ コーニング コーポレーションＤｏｗ Ｃｏｒｎｉｎｇ Ｃｏｒｐｏｒａｔｉｏｎ | Water repellent for concrete |
| KR101518465B1 (en) * | 2014-10-17 | 2015-05-11 | 신진호 | Composition for floor material and construction method using thereof |
| CN107266938B (en) * | 2016-04-08 | 2019-12-03 | 南京唯才新能源科技有限公司 | A kind of enhanced aerogel powder and preparation method thereof |
| CN106116244A (en) * | 2016-06-28 | 2016-11-16 | 安徽真信涂料有限公司 | A kind of preparation method of alkoxy silane hydrophobic powder |
| CN108384284B (en) * | 2018-02-09 | 2020-12-29 | 航天特种材料及工艺技术研究所 | Super-hydrophobic inorganic material powder and preparation method thereof |
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