CN111040677B - Flame retardant, flame-retardant adhesive composition, flame-retardant adhesive tape and preparation method thereof - Google Patents
Flame retardant, flame-retardant adhesive composition, flame-retardant adhesive tape and preparation method thereof Download PDFInfo
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- CN111040677B CN111040677B CN201911405455.0A CN201911405455A CN111040677B CN 111040677 B CN111040677 B CN 111040677B CN 201911405455 A CN201911405455 A CN 201911405455A CN 111040677 B CN111040677 B CN 111040677B
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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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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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
- C09J11/04—Non-macromolecular additives inorganic
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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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/10—Adhesives in the form of films or foils without carriers
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2289—Oxides; Hydroxides of metals of cobalt
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Adhesive Tapes (AREA)
Abstract
The invention relates to a flame retardant which is characterized by comprising the following components in parts by weight: 1-4 parts of nitroso compound, 3-7 parts of phosphate and 10-20 parts of first solvent; and a flame-retardant adhesive composition and an adhesive tape with the flame retardant and a preparation method thereof. Compared with the prior art, the formation of drops can be effectively avoided through the nitroso compound, and the polarity of the phosphate molecules can be further reduced through the nitroso compound, so that the compatibility of the phosphate molecules and the acrylic polymer is improved, and the performance of the acrylic adhesive is not influenced by the addition of the flame retardant. The flame-retardant adhesive composition is added with the flame-retardant synergist with the oxygen-containing group, so that the flame-retardant synergist can provide the oxygen-containing group for phosphate, and the phosphate can well exert a flame-retardant effect. Therefore, the flame-retardant adhesive tape has good flame-retardant effect, can avoid the generation of dripping objects, and simultaneously keeps good adhesive force.
Description
Technical Field
The invention relates to the field of flame-retardant adhesive tapes, and in particular relates to a flame retardant, a flame-retardant adhesive composition, a flame-retardant adhesive tape and a preparation method thereof.
Background
The flame-retardant adhesive tape is an adhesive tape with flame retardance, and is widely applied to fixing and wrapping various electronic components such as plasma and liquid crystal televisions, displays, automobile wire harnesses and the like. Currently, most widely used flame retardant tapes employ one or more halogen-containing flame retardants, which have environmental and safety problems, and the european union has mandated the prohibition of using halogen-containing flame retardant tapes. However, the halogen-free flame retardant on the market does not show excellent flame retardant performance, has small addition amount and poor flame retardant effect, has the problems of poor compatibility of the flame retardant and a high-molecular adhesive, influence on product quality and the like due to the large addition amount, and cannot ensure the performance. Among the commonly used halogen-free flame retardants, phosphates are widely used, but phosphates have problems of high volatility, poor heat resistance, and unsatisfactory compatibility, and have disadvantages such as generation of dripping during combustion.
Disclosure of Invention
The first technical problem to be solved by the present invention is to provide a flame retardant capable of avoiding the generation of dripping objects in view of the prior art.
The second technical problem to be solved by the invention is to provide a flame-retardant adhesive composition which has good flame-retardant effect and good adhesive force and can effectively avoid the generation of dripping matters aiming at the prior art.
The third technical problem to be solved by the present invention is to provide a flame retardant adhesive tape with good flame retardant effect, good adhesive force and capable of effectively avoiding the generation of dripping objects.
The fourth technical problem to be solved by the invention is to provide a preparation method of the flame retardant adhesive tape in view of the prior art.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the flame retardant is characterized by comprising the following components in parts by weight:
1-4 parts of nitroso compound,
3-7 parts of phosphate,
10-20 parts of a first solvent.
Further, the nitroso compound is dinitrosopentamethylenetetramine. The nitroso compound can wrap at the phosphate surface, decomposes earlier and produces gaseous inflation when being heated to reduce heat around, when the temperature continues to rise, nitroso compound decomposes completely, and the phosphate just begins to decompose this moment, and at high temperature, the water of decomposition sublimates into water vapour in the twinkling of an eye, effectively avoids the formation of drippage. In addition, the nitroso compound can further reduce the polarity of the phosphate molecules, so that the compatibility of the phosphate molecules and the acrylic polymer is improved, and the performance of the acrylic adhesive is not influenced by the addition of the flame retardant.
Further, the phosphate is at least one of ammonium polyphosphate, triphenyl phosphate, sodium hexametaphosphate or sodium tripolyphosphate.
Further, the solvent is at least one of acetone, ammonia water or ethanol.
The technical scheme adopted by the invention for further solving the second technical problem is as follows: the flame-retardant adhesive composition with the flame retardant is characterized by comprising the following components in parts by weight:
wherein, the main monomer is butyl acrylate, and the functional monomer comprises one or a combination of a plurality of methyl methacrylate, n-butyl methacrylate and 2-hydroxyethyl acrylate.
Further, the flame-retardant synergist is nano cobalt oxide. The mechanism of the phosphorus-based flame retardant for its flame-retardant action is to promote dehydration and carbonization at the initial decomposition of the high polymer. The dehydration carbonization step is necessarily dependent on the oxygen-containing group of the high polymer, the molecular structure of the acrylic polymer is less in oxygen-containing group, the nano cobalt oxide serving as a flame-retardant synergist is added to cover the surface of the acrylic polymer, and the phosphate is enabled to better exert the flame-retardant effect by providing the oxygen-containing group for the phosphate.
Further, the second solvent is at least one of ethyl acetate, toluene, formamide or butanone.
Further, the copolymer is SK-1502D, the second solvent is a mixture of ethyl acetate and formamide, and the crosslinking agent is Y-75.
The technical scheme adopted by the invention for further solving the third technical problem is as follows: a flame-retardant adhesive tape with the flame-retardant adhesive composition.
The technical scheme adopted by the invention for further solving the fourth technical problem is as follows: the preparation method of the flame-retardant adhesive tape with the flame-retardant adhesive composition is characterized by comprising the following steps of:
(1) preparation of the flame retardant: adding a nitroso compound, phosphate and ethanol into a reaction vessel according to the mass parts, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding the flame-retardant synergist and the prepared flame retardant into a second solvent according to the mass parts, stirring at 40-60 ℃ until the flame-retardant synergist and the prepared flame retardant are completely dissolved, then adding the solution into the copolymer, stirring for 0.5h, finally adding the cross-linking agent, and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the prepared flame-retardant adhesive composition is uniformly coated on release paper, the coating thickness is 80-140 mu m, the release paper is dried for 3 min-5 min at 85-90 ℃, and then the release paper is attached to another release paper and rolled to prepare the required flame-retardant adhesive tape.
Compared with the prior art, the invention has the advantages that: the flame retardant comprises a nitroso compound, wherein the nitroso compound can be coated on the surface of phosphate and is firstly decomposed to generate gas expansion when being heated, so that the surrounding heat is reduced, when the temperature is continuously increased, the nitroso compound is completely decomposed, the phosphate is decomposed, and at high temperature, the decomposed water is instantly sublimated into water vapor, so that the formation of drops is effectively avoided. In addition, the nitroso compound can further reduce the polarity of the phosphate molecules, so that the compatibility of the phosphate molecules and the acrylic polymer is improved, and the performance of the acrylic adhesive is not influenced by the addition of the flame retardant. Meanwhile, the flame-retardant synergistic agent with the oxygen-containing group is added into the flame-retardant adhesive composition, so that the flame-retardant synergistic agent can provide the oxygen-containing group for phosphate, and the phosphate can better exert the flame-retardant effect. In conclusion, the flame-retardant adhesive tape has good flame-retardant effect, can avoid the generation of dripping objects, and simultaneously keeps good adhesive force.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1:
(1) preparation of the flame retardant: adding 1 part of dinitrosopentamethylenetetramine, 3 parts of triphenyl phosphate and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 5 parts of nano cobalt oxide and 8 parts of the flame retardant prepared in the embodiment into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 1 part of cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the embodiment is uniformly coated on release paper, the coating thickness is 130 μm, the release paper is dried at 90 ℃ for 3min, and then the release paper is attached to another release paper and rolled to prepare the required flame-retardant adhesive tape.
Example 2:
(1) preparation of the flame retardant: adding 4 parts of dinitrosopentamethylenetetramine, 7 parts of triphenyl phosphate and 15 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 2 parts of nano cobalt oxide and 15 parts of the flame retardant prepared in the embodiment into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.5 part of cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the embodiment is uniformly coated on release paper, the coating thickness is 130 μm, the release paper is dried at 90 ℃ for 3min, and then the release paper is attached to another release paper and rolled to prepare the required flame-retardant adhesive tape.
Example 3:
(1) preparation of the flame retardant: adding 2 parts of dinitrosopentamethylenetetramine, 5 parts of triphenyl phosphate and 20 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 3 parts of nano cobalt oxide and 10 parts of the flame retardant prepared in the embodiment into 20 parts of formamide, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the embodiment is uniformly coated on release paper, the coating thickness is 130 μm, the release paper is dried at 90 ℃ for 3min, and then the release paper is attached to another release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 1:
(1) preparation of the flame retardant: adding 7 parts of triphenyl phosphate and 15 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 5 parts of nano cobalt oxide and 10 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 2:
(1) preparation of the flame retardant: adding 6 parts of dinitrosopentamethylenetetramine, 5 parts of triphenyl phosphate and 15 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 4 parts of nano cobalt oxide and 10 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 3:
(1) preparation of the flame retardant: adding 4 parts of dinitrosopentamethylenetetramine and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 5 parts of nano cobalt oxide and 8 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 4:
(1) preparation of the flame retardant: adding 3 parts of dinitrosopentamethylenetetramine, 10 parts of triphenyl phosphate and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 5 parts of nano cobalt oxide and 8 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 5:
(1) preparation of the flame retardant: adding 3 parts of dinitrosopentamethylenetetramine, 3 parts of triphenyl phosphate and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 8 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the flame retardant is completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.7 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.), and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 6:
(1) preparation of the flame retardant: adding 3 parts of dinitrosopentamethylenetetramine, 3 parts of triphenyl phosphate and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 8 parts of nano cobalt oxide and 8 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.7 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 7:
(1) preparation of the flame-retardant adhesive composition: adding 3 parts of nano cobalt oxide into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide is completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.), and stirring for 20min to obtain the required flame-retardant adhesive composition;
(2) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
Comparative example 8:
(1) preparation of the flame retardant: adding 2 parts of dinitrosopentamethylenetetramine, 5 parts of triphenyl phosphate and 10 parts of ethanol into a three-neck flask, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding 3 parts of nano cobalt oxide and 20 parts of the flame retardant prepared in the comparative example into 20 parts of ethyl acetate, stirring at 40-60 ℃ until the nano cobalt oxide and the flame retardant are completely dissolved, then adding the solution into 100 parts of SK-1502D (produced by Sundao chemical Co., Ltd.), stirring for 0.5h, finally adding 0.8 part of a cross-linking agent (Y-75 produced by Sundao chemical Co., Ltd.) and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: the flame-retardant adhesive composition prepared in the comparative example is uniformly coated on a piece of release paper, the coating thickness is 130 μm, the release paper is dried for 3min at 90 ℃, and then the release paper is attached to another piece of release paper and rolled to prepare the required flame-retardant adhesive tape.
The performance test of the flame retardant tapes obtained in examples 1 to 3 and comparative examples 1 to 8 was performed, and the test results are shown in table 1. The adhesive force test adopts the following method: cutting a sample into a size of 20mm × 180mm, placing the sample in a constant temperature environment for 2hr, attaching the sample to a SUS304 plate polished in advance, repeatedly rolling the sample with a 2kg weight for 3 times, testing the sample after 20min by using a double-arm type tensile machine, peeling the sample at an angle of 180 degrees, measuring the sample at a speed of 300mm/min and a distance of more than 150mm, and recording test data.
The flame retardant test method comprises the following steps: the tape was prepared as a sample having a length of 200. + -.5 mm and a width of 50. + -.1 mm, rolled up along the longitudinal axis into a cylinder having a diameter of 13mm, marked 125mm from one end of the cylinder, and stuck with a pressure sensitive adhesive over the mark (the 75mm length overlap) and then tested using the AUTO-SPA horizontal vertical tester according to UL94 standard.
As can be seen from the test results, the products in the embodiments 1 to 3 have good flame retardant effect, and simultaneously, good adhesive force is ensured, and the generation of burning drips can be effectively avoided.
As can be seen from the above examples 1 to 3 and comparative examples 1 to 2, a proper amount of the nitroso compound can improve the flame retardancy of the product and ensure the adhesive force of the product, while an excessive amount reduces the adhesive force of the product. As can be seen from examples 1 to 3 and comparative examples 1, 2 and 4, the appropriate amount of the nitroso compound prevents the generation of combustion drips and ensures the adhesion of the product, while an excessive amount reduces the adhesion of the product. As can be seen from the above examples 1-3 and comparative examples 3-4, a proper amount of phosphate can improve the flame retardant property and ensure the adhesive force of the product, and an excessive amount of phosphate can reduce the adhesive force of the product. As can be seen from examples 1 to 3 and comparative examples 5 to 6, a proper amount of the flame retardant synergist can improve the flame retardant property of the product and ensure the adhesive force of the product, and excessive amount of the flame retardant synergist can reduce the adhesive force. As can be seen from examples 1 to 3 and comparative examples 7 to 8, a proper amount of flame retardant can improve the flame retardant property of the product and ensure the adhesive force of the product, and an excessive amount of flame retardant can reduce the adhesive force.
Table 1: formulations and test results of examples of the present invention and comparative examples
Note: the flame retardant grade VTM-0 is excellent, VTM-1 is qualified, and above VTM-2 is unqualified.
Claims (6)
1. The flame-retardant adhesive composition is characterized by comprising the following components in parts by weight:
100 parts of copolymer formed by copolymerizing main monomers and functional monomers,
8-15 parts of a flame retardant agent,
2-5 parts of flame-retardant synergist containing oxygen-containing groups,
20-30 parts of a second solvent,
0.5 to 1.0 part of a crosslinking agent,
the flame retardant comprises the following components in parts by weight:
1-4 parts of nitroso compound,
3-7 parts of triphenyl phosphate,
10-20 parts of a first solvent,
the nitroso compound is dinitrosopentamethylenetetramine, the first solvent is ethanol, wherein the main monomer is butyl acrylate, and the functional monomer comprises one or a combination of methyl methacrylate, n-butyl methacrylate and 2-hydroxyethyl acrylate.
2. The flame retardant adhesive composition of claim 1 wherein the flame retardant synergist is nano cobalt oxide.
3. The flame retardant adhesive composition of claim 1 wherein the second solvent is at least one of ethyl acetate, toluene, formamide, or butanone.
4. The flame retardant adhesive composition of any one of claims 1 to 3 wherein the copolymer is SK-1502D, the second solvent is a mixture of ethyl acetate and formamide, and the crosslinking agent is Y-75.
5. A flame retardant adhesive tape having the flame retardant adhesive composition of any one of claims 1 to 4.
6. A method of preparing the flame retardant adhesive tape of claim 5, comprising the steps of:
(1) preparation of the flame retardant: adding a nitroso compound, triphenyl phosphate and ethanol into a reaction vessel according to the mass parts, uniformly mixing, performing ultrasonic treatment at 45 ℃ for 30min, adding ammonia water to adjust the pH value to 9.0, performing magnetic stirring reaction for 1h, filtering and drying to obtain the required flame retardant;
(2) preparation of the flame-retardant adhesive composition: adding the flame-retardant synergist and the prepared flame retardant into a second solvent according to the mass parts, stirring at 40-60 ℃ until the flame-retardant synergist and the prepared flame retardant are completely dissolved, then adding the solution into the copolymer, stirring for 0.5h, finally adding the cross-linking agent, and stirring for 20min to obtain the required flame-retardant adhesive composition;
(3) preparing a flame-retardant adhesive tape: and uniformly coating the prepared flame-retardant adhesive composition on release paper, wherein the coating thickness is 80-140 mu m, drying at 85-90 ℃ for 3-5 min, attaching the release paper to another piece of release paper, and rolling to obtain the required flame-retardant adhesive tape.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911405455.0A CN111040677B (en) | 2019-12-31 | 2019-12-31 | Flame retardant, flame-retardant adhesive composition, flame-retardant adhesive tape and preparation method thereof |
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| CN201911405455.0A CN111040677B (en) | 2019-12-31 | 2019-12-31 | Flame retardant, flame-retardant adhesive composition, flame-retardant adhesive tape and preparation method thereof |
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| CN111040677B true CN111040677B (en) | 2021-11-12 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101208469A (en) * | 2005-04-19 | 2008-06-25 | 精炼株式会社 | Flame-retardant metal-coated fabric and gasket comprising the same for electromagnetic-wave shielding |
| CN107684682A (en) * | 2016-08-04 | 2018-02-13 | 天津盛安消科科技有限公司 | A kind of extinguishing chemical for fire extinguisher |
| CN108264858A (en) * | 2018-02-11 | 2018-07-10 | 浙江天和树脂有限公司 | A kind of new A B glue being bonded for acryl plates and preparation method thereof |
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| US9975841B2 (en) * | 2014-05-19 | 2018-05-22 | Megamatter, Inc. | Large molecule and polymer flame retardants |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101208469A (en) * | 2005-04-19 | 2008-06-25 | 精炼株式会社 | Flame-retardant metal-coated fabric and gasket comprising the same for electromagnetic-wave shielding |
| CN107684682A (en) * | 2016-08-04 | 2018-02-13 | 天津盛安消科科技有限公司 | A kind of extinguishing chemical for fire extinguisher |
| CN108264858A (en) * | 2018-02-11 | 2018-07-10 | 浙江天和树脂有限公司 | A kind of new A B glue being bonded for acryl plates and preparation method thereof |
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