CN112457809A - Heat-activated non-primary-adhesion halogen-free flame-retardant sealant and preparation method and application thereof - Google Patents
Heat-activated non-primary-adhesion halogen-free flame-retardant sealant and preparation method and application thereof Download PDFInfo
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- CN112457809A CN112457809A CN202011376017.9A CN202011376017A CN112457809A CN 112457809 A CN112457809 A CN 112457809A CN 202011376017 A CN202011376017 A CN 202011376017A CN 112457809 A CN112457809 A CN 112457809A
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The invention discloses a thermally activated non-primary-adhesion halogen-free flame-retardant sealant as well as a preparation method and application thereof, wherein the sealant comprises a component A and a component B, and the component A comprises: 5-20 parts of allyl glycidyl ether, 10-30 parts of glycidol, 1-10 parts of 5, 6-epoxyhexyltriethoxysilane, 15-45 parts of glycidyl furfuryl ether, 3-8 parts of an emulsifier and 70-100 parts of a solvent; the component B comprises: 3-6 parts of curing agent, 2-8 parts of halogen-free flame retardant, 0.5-1.5 parts of toughening agent, 5-12 parts of emulsifier and 20-30 parts of solvent. The halogen-free flame-retardant sealant (aqueous system) with excellent bonding capability is obtained through formula design, and no VOC is discharged when the sealant is used; the characteristic of no initial adhesion is beneficial to transportation and storage of the wallpaper material, and a large amount of release paper can be saved; the sealant is easy to peel at normal temperature, cannot cause damage to the wallpaper, and can be conveniently and circularly adhered.
Description
Technical Field
The invention relates to the technical field of sealants, in particular to a thermally activated halogen-free flame-retardant sealant without initial adhesion and a preparation method and application thereof.
Background
The wallpaper is an interior decoration material for pasting wall surfaces, and is widely used for interior decoration of houses, offices, hotels, and the like. The material is not limited to paper, and may include other materials. In order to be suitable for various public and famous building houses with higher fireproof requirements and decorative wall surfaces with more wood materials in various household rooms, most of wallpaper adopts fireproof materials at present. The paper is mainly divided into two types, one type is surface fireproof wallpaper, a flame retardant is added into a plastic coating, and base paper is common non-flame retardant paper; the other is overall fireproof wallpaper, which is the wallpaper with a flame-retardant formula adopted on the surface coating layer and the base paper. Both methods have higher requirements on the wallpaper material, the wallpaper material needs to be modified or coated, the process is complex and has certain pollution to the environment, and the solvent is mainly used in the preparation process.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the technical defects of the background technology and provides a thermally activated halogen-free flame retardant sealant without initial adhesion as well as a preparation method and application thereof. The halogen-free flame-retardant sealant (aqueous system) with excellent bonding capability is obtained through formula design, and the sealant system does not volatilize organic solvent and discharge VOC when in use; the sealant has excellent flame retardant property and good adhesive force to most base materials; the characteristic of no initial adhesion is very beneficial to transportation and storage of wallpaper materials, and the use of a large amount of release paper (isolation paper, release paper and silicone oil paper) can be saved; in addition, the sealant is easy to peel at normal temperature, so that the wallpaper cannot be damaged, and the circulating bonding operation can be conveniently carried out.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the heat-activated non-primary-adhesion halogen-free flame-retardant sealant comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 5-20 parts of allyl glycidyl ether, 10-30 parts of glycidol, 1-10 parts of 5, 6-epoxyhexyltriethoxysilane, 15-45 parts of glycidyl furfuryl ether, 3-8 parts of an emulsifier and 70-100 parts of a solvent; the component B comprises the following raw materials in parts by weight: 3-6 parts of curing agent, 2-8 parts of halogen-free flame retardant, 0.5-1.5 parts of toughening agent, 5-12 parts of emulsifier and 20-30 parts of solvent.
Preferably, the curing agent is at least one of hexamethylene diamine, decamethylene diamine and dodecane diamine.
Preferably, the emulsifier is at least one of polyacrylamide, polyglycerol ester and sucrose fatty acid ester.
Preferably, the halogen-free flame retardant is epoxy-containing cyclotriphosphazene derivative, and the derivative is one or more of hexa (4-hydroxymethylphenoxy) cyclotriphosphazene hexaglycidyl ether, hexa (4-carboxyphenoxy) hexaglycidyl ester and hexa (4-aminophenoxy) dodecaglycidyl amine.
Preferably, the toughening agent is at least one of carboxyl liquid nitrile rubber, carboxyl-terminated liquid nitrile rubber, polysulfide rubber and liquid silicone rubber.
Preferably, the solvent is at least one of ethanol, acetone and water.
The preparation method of the thermally activated non-initial-adhesion halogen-free flame-retardant sealant comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.2-0.9 to obtain the sealant.
The thermally activated halogen-free flame-retardant sealant without initial adhesion is applied, the sealant is coated on the lower surface of a common wallpaper base body, the wallpaper base body is heated to 50 ℃ and dried for half an hour, the wallpaper material which does not need to be protected by release paper and has a flame-retardant function is obtained, the wallpaper material is placed on a part needing to be bonded, and is subjected to infrared heating for cross-linking polymerization, so that the attaching effect is achieved.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the flame-retardant epoxy monomer containing a dopo structure is added into the formula, so that the halogen-free flame-retardant sealant (aqueous system) with excellent bonding capability is designed, and the sealant system does not volatilize organic solvent and discharge VOC when in use; the sealant has excellent flame retardant property and good adhesive force to most base materials; the characteristic of no initial adhesion is very beneficial to transportation and storage of wallpaper materials, and the use of a large amount of release paper (isolation paper, release paper and silicone oil paper) can be saved; in addition, the sealant is easy to peel at normal temperature, so that the wallpaper cannot be damaged, and the circulating bonding operation can be conveniently carried out.
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
Example 1
The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant disclosed by the embodiment comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 10 parts of allyl glycidyl ether, 20 parts of glycidol, 6 parts of 5, 6-epoxyhexyltriethoxysilane, 30 parts of glycidyl furfuryl ether, 5 parts of polyacrylamide and 85 parts of ethanol; the component B comprises the following raw materials in parts by weight: 4 parts of a curing agent, 6 parts of hexa (4-hydroxymethylphenoxy) cyclotriphosphazene hexaglycidyl ether, 1 part of carboxyl liquid nitrile rubber, 10 parts of polyglycerol ester and 25 parts of acetone.
The curing agent consists of ethylenediamine and decamethylenediamine in the mass ratio of 1: 1.
The preparation method of the thermally activated non-primary-adhesion halogen-free flame-retardant sealant correspondingly comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: mixing the component A and the component B according to the mass ratio of 1: 0.5, and uniformly mixing to obtain the halogen-free flame retardant sealant.
Example 2
The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant disclosed by the embodiment comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 5 parts of allyl glycidyl ether, 10 parts of glycidol, 1 part of 5, 6-epoxy hexyl triethoxysilane, 15 parts of glycidyl furfuryl ether, 3 parts of polyglycerol ester and 70 parts of acetone; the component B comprises the following raw materials in parts by weight: 3 parts of curing agent, 2 parts of hexa (4-carboxyphenoxy) hexaglycidyl ester, 0.5 part of carboxyl-terminated liquid nitrile rubber, 5 parts of polyacrylamide and 20 parts of water.
The curing agent is dodecanediamine.
The preparation method of the thermally activated non-primary-adhesion halogen-free flame-retardant sealant correspondingly comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.3 to obtain the halogen-free flame retardant sealant.
Example 3
The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant disclosed by the embodiment comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 20 parts of allyl glycidyl ether, 30 parts of glycidol, 10 parts of 5, 6-epoxyhexyltriethoxysilane, 45 parts of glycidyl furfuryl ether, 8 parts of sucrose fatty acid ester and 100 parts of ethanol; the component B comprises the following raw materials in parts by weight: 3 parts of a curing agent, 2 parts of hexa (4-aminophenoxy) dodecaglycidyl amine, 1.5 parts of polysulfide rubber, 12 parts of sucrose fatty acid ester and 30 parts of water.
The curing agent is dodecanediamine.
The preparation method of the thermally activated non-primary-adhesion halogen-free flame-retardant sealant correspondingly comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.6 to obtain the halogen-free flame retardant sealant.
Example 4
The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant disclosed by the embodiment comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 5 parts of allyl glycidyl ether, 25 parts of glycidol, 1 part of 5, 6-epoxyhexyltriethoxysilane, 25 parts of glycidyl furfuryl ether, 3 parts of polyglycerol ester and 80 parts of acetone; the component B comprises the following raw materials in parts by weight: 5 parts of curing agent, 2 parts of hexa (4-carboxyphenoxy) hexaglycidyl ester, 0.5 part of carboxyl-terminated liquid nitrile rubber, 5 parts of polyacrylamide and 20 parts of water.
The curing agent is decamethylene diamine.
The preparation method of the thermally activated non-primary-adhesion halogen-free flame-retardant sealant correspondingly comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.2 to obtain the halogen-free flame retardant sealant.
Example 5
The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant disclosed by the embodiment comprises a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 15 parts of allyl glycidyl ether, 12 parts of glycidol, 7 parts of 5, 6-epoxyhexyltriethoxysilane, 25 parts of glycidyl furfuryl ether, 6 parts of polyglycerol ester and 90 parts of ethanol; the component B comprises the following raw materials in parts by weight: 3 parts of a curing agent, 2 parts of hexa (4-carboxyphenoxy) hexaglycidyl ester, 0.5 part of liquid silicone rubber, 9 parts of polyglycerol ester and 30 parts of ethanol.
The curing agent is hexamethylene diamine.
The preparation method of the thermally activated non-primary-adhesion halogen-free flame-retardant sealant correspondingly comprises the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the halogen-free flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.5 to obtain the halogen-free flame retardant sealant.
The heat-activated non-initial-adhesion halogen-free flame-retardant sealant prepared in the examples 1 to 5 is subjected to related performance tests, and the test results are shown in table 1:
table 1 test results of the related performances of thermally activated non-primary-adhesion halogen-free flame-retardant sealant prepared in examples 1 to 5
The application method of the thermally activated halogen-free flame retardant sealant without initial adhesion in the embodiment 1-5 is as follows:
(1) fully and uniformly mixing the component A and the component B to obtain aqueous emulsion with moderate viscosity;
(2) uniformly coating a layer of wet film on the back surface of the wallpaper by using the emulsion through a film scraper, and then drying to obtain a layer of thin film material without viscosity on the back surface of the wallpaper;
(3) cutting the decorative wallpaper into a proper size, applying the decorative wallpaper on the surface of furniture, heating the decorative wallpaper by using a heating device (infrared heating), activating the viscosity performance of the film, and completing adhesion within ten seconds;
(4) after accidental ignition occurs, once the wallpaper is burnt through by flame, the adhesion layer can quickly form a compact carbon layer, so that the flame is prevented from further burning the base material, and the flame-retardant behavior is achieved.
The above description is not intended to limit the present invention, and the present invention is not limited to the above examples. Those skilled in the art should also realize that changes, modifications, additions and substitutions can be made without departing from the true spirit and scope of the invention.
Claims (8)
1. The thermally-activated non-primary-adhesion halogen-free flame-retardant sealant is characterized by comprising a component A and a component B, wherein the component A comprises the following raw materials in parts by weight: 5-20 parts of allyl glycidyl ether, 10-30 parts of glycidol, 1-10 parts of 5, 6-epoxyhexyltriethoxysilane, 15-45 parts of glycidyl furfuryl ether, 3-8 parts of an emulsifier and 70-100 parts of a solvent; the component B comprises the following raw materials in parts by weight: 3-6 parts of curing agent, 2-8 parts of halogen-free flame retardant, 0.5-1.5 parts of toughening agent, 5-12 parts of emulsifier and 20-30 parts of solvent.
2. The heat-activated non-tack, halogen-free, flame retardant sealant of claim 1 wherein the curing agent is at least one of hexamethylene diamine, decamethylene diamine, and dodecane diamine.
3. The heat-activated non-tack, halogen-free, flame retardant sealant of claim 1 wherein the emulsifier is at least one of polyacrylamide, polyglycerol ester, sucrose fatty acid ester.
4. The heat-activated no-tack, halogen-free, flame retardant sealant according to claim 1 wherein the halogen-free flame retardant is an epoxy group containing cyclotriphosphazene derivative selected from one or more of hexakis (4-hydroxymethylphenoxy) cyclotriphosphazene hexaglycidyl ether, hexakis (4-carboxyphenoxy) hexaglycidyl ester, and hexakis (4-aminophenoxy) dodecaglycidyl amine.
5. The heat-activated non-tack halogen-free flame retardant sealant according to claim 1 wherein the toughening agent is at least one of a carboxyl group liquid nitrile rubber, a carboxyl group terminated liquid nitrile rubber, a polysulfide rubber, and a liquid silicone rubber.
6. The heat-activated non-tack halogen-free flame retardant sealant according to claim 1 wherein the solvent is at least one of ethanol, acetone and water.
7. The preparation method of the heat-activated non-tack halogen-free flame retardant sealant according to claim 1, characterized by comprising the following steps:
s1: weighing raw materials according to parts by weight, and uniformly stirring and mixing allyl glycidyl ether, glycidol, 5, 6-epoxy hexyl triethoxysilane, glycidyl furfuryl ether, an emulsifier and a solvent to obtain a component A for later use;
s2: weighing the raw materials according to the weight part, and uniformly stirring and mixing the curing agent, the flame retardant, the toughening agent, the emulsifier and the solvent to obtain the component B for later use;
s3: and uniformly mixing the component A and the component B according to the mass ratio of 1: 0.2-0.9 to obtain the sealant.
8. The application of the heat-activated halogen-free flame-retardant sealant without initial adhesion as claimed in any one of claims 1 to 7, wherein the sealant is coated on the lower surface of a wallpaper substrate, the wallpaper substrate is heated to 50 ℃ and dried for half an hour to obtain a wallpaper material with a flame-retardant function without the protection of release paper, the wallpaper material is placed on a part needing bonding, and the wallpaper material is subjected to infrared heating for crosslinking polymerization to achieve a bonding effect.
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| CN202011376017.9A CN112457809B (en) | 2020-11-30 | 2020-11-30 | Heat-activated non-primary-adhesion halogen-free flame-retardant sealant and preparation method and application thereof |
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| CN202011376017.9A CN112457809B (en) | 2020-11-30 | 2020-11-30 | Heat-activated non-primary-adhesion halogen-free flame-retardant sealant and preparation method and application thereof |
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| CN112457809A true CN112457809A (en) | 2021-03-09 |
| CN112457809B CN112457809B (en) | 2023-04-07 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481899A (en) * | 2015-11-27 | 2016-04-13 | 长沙欧赛新材料有限公司 | Novel halogen-free cyclotriphosphazene compound and its preparation method and use |
| CN109401704A (en) * | 2018-10-30 | 2019-03-01 | 湖南柯盛新材料有限公司 | A kind of high solid content water epoxy adhesive and preparation method thereof |
| CN110396387A (en) * | 2019-09-04 | 2019-11-01 | 宁波咖飞姆新材料有限公司 | A kind of hot activation is without just viscous sealant and its preparation method and application |
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2020
- 2020-11-30 CN CN202011376017.9A patent/CN112457809B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481899A (en) * | 2015-11-27 | 2016-04-13 | 长沙欧赛新材料有限公司 | Novel halogen-free cyclotriphosphazene compound and its preparation method and use |
| CN109401704A (en) * | 2018-10-30 | 2019-03-01 | 湖南柯盛新材料有限公司 | A kind of high solid content water epoxy adhesive and preparation method thereof |
| CN110396387A (en) * | 2019-09-04 | 2019-11-01 | 宁波咖飞姆新材料有限公司 | A kind of hot activation is without just viscous sealant and its preparation method and application |
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