CN110564196A - preparation and use method of high-hardness antibacterial floor hardening agent - Google Patents
preparation and use method of high-hardness antibacterial floor hardening agent Download PDFInfo
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- CN110564196A CN110564196A CN201910804198.1A CN201910804198A CN110564196A CN 110564196 A CN110564196 A CN 110564196A CN 201910804198 A CN201910804198 A CN 201910804198A CN 110564196 A CN110564196 A CN 110564196A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
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- E—FIXED CONSTRUCTIONS
- E04—BUILDING
- E04F—FINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
- E04F15/00—Flooring
- E04F15/12—Flooring or floor layers made of masses in situ, e.g. seamless magnesite floors, terrazzo gypsum floors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Architecture (AREA)
- Structural Engineering (AREA)
- Plant Pathology (AREA)
- Civil Engineering (AREA)
- Inorganic Chemistry (AREA)
- Floor Finish (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of terraces, and aims to provide a preparation method and a use method of a high-hardness antibacterial terrace hardening agent. The preparation method comprises the following steps: adding methyl orthosilicate into ethanol at the temperature of 0-10 ℃ under the stirring condition, and continuously stirring; adding hydrochloric acid water solution 20 times at intervals of 20min, and stirring continuously after adding; adding zinc oxide sol while stirring; continuing stirring, and aging at 20 deg.C for 2 days; and adding the aged composite sol and isopropanol into the nano floor hardening agent, stirring, adding a hardening accelerator into the mixture, and stirring to finally obtain the high-hardness antibacterial floor hardening agent. According to the invention, the nano zinc oxide sol is used as an inorganic antibacterial material and added into the floor hardener, and the zinc oxide as an antibacterial material has excellent stability compared with silver ions, so that the phenomena of activity disappearance and seepage in the floor hardener are avoided, and the antibacterial performance of the floor is ensured.
Description
Technical Field
The invention relates to the technical field of terraces, in particular to a preparation method and a use method of a high-hardness antibacterial terrace hardening agent.
Background
With the development of economy and the improvement of the living standard of people, the public places have more and more requirements on high-quality large-scale terraces, and various functional terraces are produced at the same time, especially in places with higher requirements on environmental sanitation and safety, such as medical institutions like sterile workshops and sterile rooms. At present, the most kinds of floor coatings are common epoxy floor coatings, polyurethane floor coatings and the like, and the antibacterial effect is achieved in the floor coatings by adding silver ion type antibacterial agents and quaternary ammonium salt antibacterial agents. Such as chinese invention patent CN201810833643.2 and chinese invention patent CN 201710204776.9. However, the two antibacterial agents have poor use effect in the permeation type floor hardening agent, and the quaternary ammonium salt antibacterial agent can be dissolved out in the floor use process because the active silver ion antibacterial agent is easy to lose efficacy in a strong acid or strong alkali solution.
Disclosure of Invention
the invention aims to solve the technical problem of overcoming the defects in the prior art and provides a preparation and use method of a high-hardness antibacterial floor hardening agent.
The preparation method of the high-hardness antibacterial floor hardening agent comprises the following steps:
(1) adding 40-50 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at the temperature of 0-10 ℃ under the stirring condition, and continuously stirring for 10 min; adding 5-10 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M for 20 times, wherein the interval is 20min each time, and continuously stirring for 10h after the addition is finished;
(2) Adding 20-40 parts by mass of zinc oxide sol into the mixture obtained in the step (1) under the condition of stirring; stirring for 30min, and aging at 20 deg.C for 2 days;
(3) Adding the aged composite sol and 10 parts by mass of isopropanol into 70-50 parts by mass of nano floor hardener, stirring for 30min, adding a hardening accelerator accounting for 3-5 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness antibacterial floor hardener.
in the present invention, the stirring rate in the step (1) is 100 r/min.
in the invention, the stirring speed in the step (2) is 100-200 r/min.
In the invention, the solid content of the zinc oxide sol is 30%, the particle size of sol particles is 10-20 nm, and the solvent used by the sol is ethanol.
In the invention, the nano floor hardener is a solvent-based inorganic nano hardener based on silicon alkoxide hydrolysis prepolymerization, the solid content is more than 60%, and the pH value is 6-8.
In the present invention, the hardening accelerator is a crosslinking agent containing tin.
In the present invention, the hardening accelerator is dibutyltin dilaurate, and the purity thereof is 95%.
The invention further provides a use method of the high-hardness antibacterial floor hardening agent, which specifically comprises the following steps:
(1) Polishing a self-leveling cement floor with the concrete strength grade of C20 or C30 by using a 200-mesh polishing sheet, pouring a high-hardness antibacterial floor hardening agent on the surface of the floor according to the using amount of 1 kilogram per square meter, and uniformly coating the high-hardness antibacterial floor hardening agent;
(2) Covering the terrace with a plastic film, standing for 2 hours, and then uncovering the plastic film; and naturally drying for 8 hours, and polishing the floor by using a polishing sheet of 200-300 meshes.
Description of the inventive principles:
The nano floor hardening agent based on silicon alkoxide hydrolysis prepolymerization has the advantages of high hardness, chemical pollution resistance, good durability and the like, can be applied to floor surfaces of various types such as concrete, cement and the like, and forms a hardened layer on the surface of the concrete or the cement in a penetration mode, thereby achieving the hardening and dust removal effects of the cement. However, the hardener solution has poor compatibility with ionic antibacterial agents, and the phenomenon of seepage easily occurs in the use process of the floor regardless of silver ions or quaternary ammonium salt antibacterial agents, so that the performance of the floor is affected.
The nano zinc oxide introduced by the invention is an antibacterial inorganic oxide with stable property, can be stably suspended in the floor hardening agent permeable layer, can effectively prevent the phenomenon of seepage of the antibacterial agent by adding the nano zinc oxide, and simultaneously achieves the antibacterial effect of the floor. By adding the nano zinc oxide antibacterial material, inorganic components of the nano zinc oxide antibacterial material penetrate into a pore structure of a cement base body to form a whole with the cement base body, so that an interface between different layers is eliminated, the problem that the terrace is easy to peel off due to weak binding force between layers is solved, and the skeleton structure of the cement base body forms powerful support for the wear resistance and strength of the terrace, so that the terrace with the structure has good durability and strength, and meanwhile, the terrace has good bactericidal performance. The hardening accelerator is added to make the hardening agent to be cured more quickly and to be integrated with the concrete.
Compared with the prior art, the invention has the technical effects that:
According to the invention, the nano zinc oxide sol is used as an inorganic antibacterial material and added into the floor hardener, and the zinc oxide as an antibacterial material has excellent stability compared with silver ions, so that the phenomena of activity disappearance and seepage in the floor hardener are avoided, and the antibacterial performance of the floor is ensured.
Detailed Description
In the invention, the nano zinc oxide sol, the nano floor hardening agent and the hardening accelerator are all commercially available products. For example, the nano zinc oxide sol in the following examples is selected from XT-0806-54-1 product of Shanghai lane field nano materials Co., Ltd; the solid content of the zinc oxide sol product is 30%, the particle size of sol particles is 10-20 nm, and the solvent used by the sol is ethanol. The nano floor hardener is a nano hardener X760 of Hangzhou Nagu new material company Limited; the product is a solvent-based inorganic nano hardener based on silicon alkoxide hydrolysis prepolymerization, the solid content is more than 60%, and the pH value is 6-8. The hardening accelerator is selected from the group consisting of alatin reagent, cat # D100274; the active ingredient is dibutyltin dilaurate, and the purity is 95%.
The invention is further described below by way of examples.
Example 1
Adding 40 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at 0 ℃ under the stirring condition of 100r/min, stirring for 10min, adding 5 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M in 20 times at intervals of 20min, and stirring for 10 hr; adding 40 parts by mass of nano zinc oxide sol under the stirring condition of 100r/min, stirring for 30min, and aging for 2days at 20 ℃; adding the aged composite sol into 70 parts by mass of nano terrace hardening agent, and continuously adding 10 parts by mass of isopropanol; and after stirring for 30min, adding a hardening accelerator accounting for 3 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness antibacterial terrace hardening agent.
The use method of the high-hardness antibacterial floor hardener is as follows (the following examples and comparative examples are the same):
After a self-leveling cement floor with the concrete strength grade of C20 or C30 is polished and leveled by a 200-mesh polishing sheet, pouring a high-hardness antibacterial floor hardening agent on the surface of the floor according to the amount of 1 kilogram per square meter, and then uniformly coating the high-hardness antibacterial floor hardening agent; covering the terrace with a plastic film, standing for 2 hours, and then uncovering the plastic film; after naturally drying for 8 hours, polishing the terrace by using a 200-300-mesh polishing sheet.
Example 2
Adding 45 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at the temperature of 5 ℃ and under the stirring condition of 100r/min, stirring for 10min, adding 7 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M in 20 times, and stirring for 10hr at intervals of 20 min; adding 30 parts by mass of nano zinc oxide sol under the stirring condition of 200r/min, stirring for 30min, and aging for 2days at 20 ℃; adding the aged composite sol into 60 parts by mass of nano terrace hardening agent, and continuously adding 10 parts by mass of isopropanol; and after stirring for 30min, adding a hardening accelerator accounting for 4 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness antibacterial terrace hardening agent.
Example 3
Adding 50 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at 10 ℃ under the stirring condition of 100r/min, stirring for 10min, adding 10 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M in 20 times, each time for 20min, and then stirring for 10 hr; adding 20 parts by mass of nano zinc oxide sol under the stirring condition of 150r/min, stirring for 30min, and aging for 2days at 20 ℃; adding the aged composite sol into 50 parts by mass of nano terrace hardening agent, and continuously adding 10 parts by mass of isopropanol; and after stirring for 30min, adding a hardening accelerator accounting for 5 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness antibacterial terrace hardening agent.
Comparative example 1
Adding 50 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at 10 ℃ under the stirring condition of 100r/min, stirring for 10min, adding 10 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M in 20 times, each time for 20min, and then stirring for 10 hr; aging at 20 deg.C for 2 days; adding the aged composite sol into 70 parts by mass of nano terrace hardening agent, and continuously adding 10 parts by mass of isopropanol; and after stirring for 30min, adding a hardening accelerator accounting for 5 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness floor hardening agent.
Staphylococcus aureus is used as a strain, and the test is carried out according to an industrial standard JC/T897-2002 (antibacterial ceramic product detection standard). Meanwhile, the hardening agents in the embodiments and the comparative examples are applied to floor manufacturing, and then the Mohs hardness and the wear resistance of each sample are tested according to a conventional testing method.
Table 1 shows the results of tests on the antibacterial, mohs hardness and abrasion resistance of different floor samples (4 square centimeter area).
TABLE 1
sample (I) | Example 1 | example 2 | Example 3 | Comparative example 1 |
bacteriostatic ratio (%) | 92% | 90% | 95% | 0% |
Mohs hardness | 7 | 7 | 7 | 7 |
Abrasion resistance ratio | 352 | 330 | 361 | 380 |
as can be seen from the data in the table, in the range of the test requirements, compared with the sample (comparative example 1) without the antibacterial agent nano zinc oxide, the antibacterial performance of the terrace sample prepared by the invention is obviously better. Meanwhile, the Mohs hardness and the wear resistance of the concrete terrace sample block are not obviously changed.
Claims (8)
1. A preparation method of a high-hardness antibacterial floor hardening agent is characterized by comprising the following steps:
(1) Adding 40-50 parts by mass of methyl orthosilicate into 40 parts by mass of ethanol at the temperature of 0-10 ℃ under the stirring condition, and continuously stirring for 10 min; adding 5-10 parts by mass of hydrochloric acid aqueous solution with the molar concentration of 2M for 20 times, wherein the interval is 20min each time, and continuously stirring for 10h after the addition is finished;
(2) adding 20-40 parts by mass of zinc oxide sol into the mixture obtained in the step (1) under the condition of stirring; stirring for 30min, and aging at 20 deg.C for 2 days;
(3) Adding the aged composite sol and 10 parts by mass of isopropanol into 70-50 parts by mass of nano floor hardener, stirring for 30min, adding a hardening accelerator accounting for 3-5 per mill of the mass ratio of the mixture into the mixture, and stirring for 30min to finally obtain the high-hardness antibacterial floor hardener.
2. The method according to claim 1, wherein the stirring rate in the step (1) is 100 r/min.
3. The method according to claim 1, wherein the stirring rate in the step (2) is 100 to 200 r/min.
4. the method according to claim 1, wherein the zinc oxide sol has a solid content of 30%, the particle size of sol particles is 10-20 nm, and the solvent used in the sol is ethanol.
5. The method as claimed in claim 1, wherein the nano floor hardener is a solvent-based inorganic nano hardener based on a silicon alkoxide hydrolysis pre-polymerization, the solid content is above 60%, and the pH value is between 6 and 8.
6. The method according to claim 1, wherein the hardening accelerator is a tin-containing crosslinking agent.
7. The method of claim 1, wherein the hardening accelerator is dibutyltin dilaurate having a purity of 95%.
8. the use method of the high-hardness antibacterial floor hardening agent prepared by the method of claim 1 is characterized by comprising the following steps:
(1) Polishing a self-leveling cement floor with the concrete strength grade of C20 or C30 by using a 200-mesh polishing sheet, pouring a high-hardness antibacterial floor hardening agent on the surface of the floor according to the using amount of 1 kilogram per square meter, and uniformly coating the high-hardness antibacterial floor hardening agent;
(2) Covering the terrace with a plastic film, standing for 2 hours, and then uncovering the plastic film; and naturally drying for 8 hours, and polishing the floor by using a polishing sheet of 200-300 meshes.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN114575555A (en) * | 2022-03-30 | 2022-06-03 | 杭州格灵新材料科技有限公司 | Preparation method of high-hardness cement-based self-leveling nano-hardening decorative terrace |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102190448A (en) * | 2010-12-03 | 2011-09-21 | 中国科学院上海硅酸盐研究所 | Composite broadband antireflecting film and preparation method thereof |
CN103013189A (en) * | 2012-10-12 | 2013-04-03 | 舟山市普陀夏和材料技术有限公司 | Glass anti-reflection coating liquid and application method of glass anti-reflection coating liquid in anti-reflection glass preparation |
CN106479240A (en) * | 2016-09-17 | 2017-03-08 | 浙江大学自贡创新中心 | The preparation method of osmosis type self-leveling cement anti-static and abrasion-resistant floor coatings |
CN106565278A (en) * | 2016-11-04 | 2017-04-19 | 浙江省建筑科学设计研究院有限公司 | High-permeability concrete sealed waterproofing agent and preparation method thereof |
CN109266058A (en) * | 2018-09-18 | 2019-01-25 | 湖南凯斯利新材料有限公司 | A kind of catalysis process and application method of aqueous inorganic nano paint |
CN110156366A (en) * | 2018-02-01 | 2019-08-23 | 成都今天化工有限公司 | A method of preparing nano antifouling type cement hardener |
-
2019
- 2019-08-28 CN CN201910804198.1A patent/CN110564196A/en active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102190448A (en) * | 2010-12-03 | 2011-09-21 | 中国科学院上海硅酸盐研究所 | Composite broadband antireflecting film and preparation method thereof |
CN103013189A (en) * | 2012-10-12 | 2013-04-03 | 舟山市普陀夏和材料技术有限公司 | Glass anti-reflection coating liquid and application method of glass anti-reflection coating liquid in anti-reflection glass preparation |
CN106479240A (en) * | 2016-09-17 | 2017-03-08 | 浙江大学自贡创新中心 | The preparation method of osmosis type self-leveling cement anti-static and abrasion-resistant floor coatings |
CN106565278A (en) * | 2016-11-04 | 2017-04-19 | 浙江省建筑科学设计研究院有限公司 | High-permeability concrete sealed waterproofing agent and preparation method thereof |
CN110156366A (en) * | 2018-02-01 | 2019-08-23 | 成都今天化工有限公司 | A method of preparing nano antifouling type cement hardener |
CN109266058A (en) * | 2018-09-18 | 2019-01-25 | 湖南凯斯利新材料有限公司 | A kind of catalysis process and application method of aqueous inorganic nano paint |
Non-Patent Citations (2)
Title |
---|
丁浩等: "《纳米抗菌技术》", 31 January 2008, 化学工业出版社 * |
曹茂盛等: "《材料合成与制备方法》", 31 July 2018, 哈尔滨工业大学出版社 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114575555A (en) * | 2022-03-30 | 2022-06-03 | 杭州格灵新材料科技有限公司 | Preparation method of high-hardness cement-based self-leveling nano-hardening decorative terrace |
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Application publication date: 20191213 |