CN105505108A - Waterborne fireproof coating and preparation method thereof - Google Patents
Waterborne fireproof coating and preparation method thereof Download PDFInfo
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- CN105505108A CN105505108A CN201510887069.5A CN201510887069A CN105505108A CN 105505108 A CN105505108 A CN 105505108A CN 201510887069 A CN201510887069 A CN 201510887069A CN 105505108 A CN105505108 A CN 105505108A
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- multipolymer
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34922—Melamine; Derivatives thereof
-
- 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
- C09D5/18—Fireproof paints including high temperature resistant paints
- C09D5/185—Intumescent paints
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Paints Or Removers (AREA)
- Fireproofing Substances (AREA)
Abstract
The invention discloses a waterborne fireproof coating and a preparation method thereof. The waterborne fireproof coating comprises raw materials as follows: water-based resin, a water-based curing agent, a nanoscale copolymer, melamine, pentaerythritol and water, wherein the nanoscale copolymer comprises bis(chloroethyl) phosphate, diethylenetriamine, potassium iodide, sodium hydroxide, zirconium oxychloride, graphene and distilled water. According to the preparation method of the waterborne fireproof coating, an intumescent flame retardant system is adopted and has the advantages of high heat stability, environment friendliness and the like; alpha-zirconium phosphate and graphene form the nanoscale copolymer having multiple lamellae and containing rich phosphorus elements through a condensation reaction, and the nanoscale copolymer as a phosphorus element provider in a flame retardant system has a multi-lamella structure and a physical blocking effect. The nanoscale copolymer has the characteristics that the specific surface area is large, the adsorbability is high and the surface contains a large quantity of negative charges, and can realize good dispersion and substrate adhesion by means of the unique surface effect in resin.
Description
Technical field
The present invention relates to technical field of coatings, particularly relate to a kind of aqueous fire-proof coating and preparation method thereof.
Background technology
So far, fire retardant coating system focuses mostly in solvent based coating system.Along with the enhancing of people's environmental consciousness, volatile organic matter (VOC) burst size is low, strong adhesion, the water-borne coatings good to material surface adaptability enter into the sight line of people gradually, and capture Coating Market rapidly.
Frie retardant coating for flame-retardant system, can reduce VOC burst size with phosphorus-carbon-nitrogen greatly, but the restriction that the shortcomings such as the more weak and poor heat stability of its sticking power are usually applied.And Graphene is as the novel material of current research field, there is the performance such as high-specific surface area, excellent chemical stability.Graphene can reduce coat-thickness in coating system, increases advantages such as the sticking power of base material, makes it be widely used in coating.Based on such advantage, propose a kind of aqueous fire-proof coating of research and development.
Summary of the invention
For the problems referred to above, the invention provides a kind of aqueous fire-proof coating and preparation method thereof, alpha zirconium phosphate and Graphene are formed a kind of multi-disc layer by condensation reaction, be rich in the nano level multipolymer of phosphoric, as the supplier of phosphoric in flame-retardant system, improve the thermostability of coating and the sticking power with base material.
For realizing above-mentioned purpose of the present invention, the invention provides a kind of aqueous fire-proof coating, being made up of following raw material: water-base resin, waterborne curing agent, nano level multipolymer, trimeric cyanamide, tetramethylolmethane, water; Described nano level multipolymer is made up of Dichloroethyl phosphoric acid ester, diethylenetriamine, potassiumiodide, sodium hydroxide, zirconium oxychloride, Graphene, distilled water.
The invention provides a kind of preparation method of aqueous fire-proof coating, comprise the following steps.
Step 1, by 3 ~ 5g Dichloroethyl phosphoric acid ester, 10 ~ 50ml diethylenetriamine, 0.1 ~ 0.5g potassiumiodide joins in 150 ~ 200ml5% sodium hydroxide solution, obtain mixture, after mixture being placed in ice-water bath mix and blend 12 ~ 24h, at room temperature crystallization 1 ~ 3 day, then vacuum-drying at 50 ~ 80 DEG C, namely obtains product A.
Step 2, by product A and 3 ~ 5g zirconium oxychloride (ZrOCl
28H
2o) join in 100ml distilled water, at the stirred in water bath 12 ~ 24h of 80 ~ 100 DEG C, being filtered to pH with distilled water wash is 5 ~ 6, and vacuum-drying at 50 ~ 80 DEG C, obtains alpha zirconium phosphate.
Step 3, alpha zirconium phosphate and 0.2 ~ 0.5g Graphene join in 100ml distilled water, and 50 ~ 80 DEG C are stirred 1 ~ 3h, afterwards vacuum-drying at 50 ~ 80 DEG C, obtain the nano level multipolymer that a kind of multi-disc layer is rich in phosphoric.
Step 4, get the mixture (in mass ratio 3:1:1 mixing) of the above-mentioned nano level multipolymer of 30 ~ 50g, trimeric cyanamide, tetramethylolmethane, join in the mixed solution of 100 ~ 200g water and 100 ~ 200g water-base resin, in ball mill, disperse 1 ~ 2h, obtain the mother liquor of frie retardant coating.
Step 5, get after 25 ~ 50g waterborne curing agent mixes with 50 ~ 100g water, then mix with the ratio of the mother liquor of frie retardant coating 1:3 ~ 4 in mass ratio, to obtain final product.
Described water-base resin is Ar555 epoxy resin, H228A epoxy resin, E44 epoxy emulsion, E51 epoxy emulsion, E20 epoxy emulsion.
Described waterborne curing agent is Aq419, H228B, W651, W650.
Compared with prior art beneficial effect of the present invention.
Aqueous fire-proof coating provided by the invention and preparation method thereof, selects expanding fire retardant system, has thermostability high, the advantages such as environmental protection.A kind of nano level multipolymer that alpha zirconium phosphate and Graphene are formed by condensation reaction, as the phosphoric supplier in flame-retardant system, has multi-disc Rotating fields, physical barrier effect.Further, this nano level multipolymer has that specific surface area is large, adsorptivity is strong, surface with the feature of a large amount of negative charges, in resin, good dispersion and the sticking power with base material can be reached by means of the surface effects of uniqueness.
Accompanying drawing explanation
Fig. 1 is nano level multipolymer synthesis mechanism figure.
Embodiment
The present invention is further described below in conjunction with specific embodiment.
The present embodiment provides a kind of aqueous fire-proof coating, is made up of following raw material: water-base resin, waterborne curing agent, nano level multipolymer, trimeric cyanamide, tetramethylolmethane, water; Described nano level multipolymer is made up of Dichloroethyl phosphoric acid ester, diethylenetriamine, potassiumiodide, sodium hydroxide, zirconium oxychloride, Graphene, distilled water.
Refer to Fig. 1, the present embodiment also provides a kind of preparation method of aqueous fire-proof coating, comprises the following steps.
Step 1, by 3g Dichloroethyl phosphoric acid ester, 15ml diethylenetriamine, 0.3g potassiumiodide joins in 150ml5% sodium hydroxide solution, obtain mixture, after mixture being placed in ice-water bath mix and blend 24h, at room temperature crystallization 2 days, vacuum-drying at 60 DEG C, namely obtains product A again.
Step 2, by product A and 3g zirconium oxychloride (ZrOCl
28H
2o) join in 100ml distilled water, at the stirred in water bath 12h of 80 DEG C, being filtered to pH with distilled water wash is 5 ~ 6, and vacuum-drying at 60 DEG C, obtains alpha zirconium phosphate.
Step 3, join in 100ml distilled water by alpha zirconium phosphate and 0.3g Graphene, 50 DEG C are stirred 3h, afterwards vacuum-dryings at 80 DEG C, obtain a kind of multi-disc layer, are rich in the nano level multipolymer of phosphoric.
Step 4, get the mixture (in mass ratio 3:1:1 mixing) of the above-mentioned nano level multipolymer of 40g, trimeric cyanamide, tetramethylolmethane, join in the mixed solution of 100g water and 100g water-base resin, in ball mill, disperse 1h, obtain the mother liquor of frie retardant coating.
Step 5, get after 50g waterborne curing agent mixes with 100g water, then mix with the ratio of the mother liquor of frie retardant coating 1:3 in mass ratio, obtain frie retardant coating.
Claims (5)
1. an aqueous fire-proof coating, is characterized in that, is made up of following raw material: water-base resin, waterborne curing agent, nano level multipolymer, trimeric cyanamide, tetramethylolmethane, water; Described nano level multipolymer is made up of Dichloroethyl phosphoric acid ester, diethylenetriamine, potassiumiodide, sodium hydroxide, zirconium oxychloride, Graphene, distilled water.
2. a preparation method for aqueous fire-proof coating, is characterized in that, comprises the following steps:
Step 1,3 ~ 5g Dichloroethyl phosphoric acid ester, 10 ~ 50ml diethylenetriamine, 0.1 ~ 0.5g potassiumiodide to be joined in 150 ~ 200ml5% sodium hydroxide solution, obtain mixture; After mixture being placed in ice-water bath mix and blend 12 ~ 24h, at room temperature crystallization 1 ~ 3 day, then vacuum-drying at 50 ~ 80 DEG C, namely obtains product A;
Step 2, by product A and 3 ~ 5g zirconium oxychloride (ZrOCl
28H
2o) join in 100ml distilled water, at the stirred in water bath 12 ~ 24h of 80 ~ 100 DEG C, being filtered to pH with distilled water wash is 5 ~ 6, and vacuum-drying at 50 ~ 80 DEG C, obtains alpha zirconium phosphate;
Step 3, join in 100ml distilled water by alpha zirconium phosphate and 0.2 ~ 0.5g Graphene, 50 ~ 80 DEG C are stirred 1 ~ 3h, afterwards vacuum-dryings at 50 ~ 80 DEG C, obtain the nano level multipolymer that a kind of multi-disc layer is rich in phosphoric;
Step 4, get the mixture of the above-mentioned nano level multipolymer of 30 ~ 50g, trimeric cyanamide, tetramethylolmethane, join in the mixed solution of 100 ~ 200g water and 100 ~ 200g water-base resin, in ball mill, disperse 1 ~ 2h, obtain the mother liquor of frie retardant coating;
Step 5, get after 25 ~ 50g waterborne curing agent mixes with 50 ~ 100g water, then mix in the ratio of 1:3 ~ 4 with the mother liquor of described frie retardant coating, to obtain final product.
3. the preparation method of aqueous fire-proof coating as claimed in claim 2, it is characterized in that, described water-base resin is Ar555 epoxy resin, H228A epoxy resin, E44 epoxy emulsion, E51 epoxy emulsion, E20 epoxy emulsion etc.
4. the preparation method of aqueous fire-proof coating as claimed in claim 2, it is characterized in that, described waterborne curing agent is Aq419, H228B, W651, W650 etc.
5. the preparation method of aqueous fire-proof coating as claimed in claim 2, it is characterized in that, in described step 4, nano level multipolymer, trimeric cyanamide, tetramethylolmethane mix in the ratio of 3:1:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510887069.5A CN105505108A (en) | 2015-11-27 | 2015-11-27 | Waterborne fireproof coating and preparation method thereof |
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| CN201510887069.5A CN105505108A (en) | 2015-11-27 | 2015-11-27 | Waterborne fireproof coating and preparation method thereof |
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| CN105505108A true CN105505108A (en) | 2016-04-20 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106987231A (en) * | 2017-05-05 | 2017-07-28 | 西南大学 | Application of the heterogeneous couplings of zirconium phosphonate graphene oxide in friction material is prepared |
| CN107033732A (en) * | 2016-12-07 | 2017-08-11 | 李光明 | A kind of graphene coating and preparation method thereof |
| WO2018095360A1 (en) * | 2016-11-23 | 2018-05-31 | 厦门大学 | Water-based intumescent fire-resistant coating based on modified graphene oxide, and method for fabrication thereof |
| CN108841229A (en) * | 2018-07-12 | 2018-11-20 | 山东佳星环保科技有限公司 | A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof |
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| CN1986423A (en) * | 2006-12-19 | 2007-06-27 | 王必庆 | Process of preparing zirconia and yttria with Y-doped cubic zirconia powder |
| CN101058411A (en) * | 2006-12-08 | 2007-10-24 | 北京化工大学 | Sphere analogous alpha-zirconium phosphate and preparing method thereof |
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| CN103861559A (en) * | 2014-03-12 | 2014-06-18 | 陕西科技大学 | Zirconia-modified graphene and method for removing fluorine ions in water |
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| CN101058411A (en) * | 2006-12-08 | 2007-10-24 | 北京化工大学 | Sphere analogous alpha-zirconium phosphate and preparing method thereof |
| CN1986423A (en) * | 2006-12-19 | 2007-06-27 | 王必庆 | Process of preparing zirconia and yttria with Y-doped cubic zirconia powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018095360A1 (en) * | 2016-11-23 | 2018-05-31 | 厦门大学 | Water-based intumescent fire-resistant coating based on modified graphene oxide, and method for fabrication thereof |
| CN107033732A (en) * | 2016-12-07 | 2017-08-11 | 李光明 | A kind of graphene coating and preparation method thereof |
| CN106987231A (en) * | 2017-05-05 | 2017-07-28 | 西南大学 | Application of the heterogeneous couplings of zirconium phosphonate graphene oxide in friction material is prepared |
| CN108841229A (en) * | 2018-07-12 | 2018-11-20 | 山东佳星环保科技有限公司 | A kind of graphene expansion type low-smoke fireproof coating and preparation method thereof |
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Address after: 110141 Yao village, Yuhong Township, Yuhong District, Liaoning, Shenyang Applicant after: Shenyang Shunfeng New Materials Co., Ltd Address before: 110141 Yao village, Yuhong Township, Yuhong District, Liaoning, Shenyang Applicant before: Shenyang Shunfeng Metro Building Materials Co., Ltd. |
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Application publication date: 20160420 |
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