CN111040716A - Preparation method and application of phosphorus-containing flame-retardant polyurethane adhesive - Google Patents
Preparation method and application of phosphorus-containing flame-retardant polyurethane adhesive Download PDFInfo
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- CN111040716A CN111040716A CN201911354142.7A CN201911354142A CN111040716A CN 111040716 A CN111040716 A CN 111040716A CN 201911354142 A CN201911354142 A CN 201911354142A CN 111040716 A CN111040716 A CN 111040716A
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- melamine
- formaldehyde
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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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
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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
- 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
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
Abstract
The invention discloses a preparation method and application of a phosphorus-containing flame-retardant polyurethane adhesive, which comprises the following steps: step 1, preparing melamine-formaldehyde coated ammonium polyphosphate microcapsules; step 2, preparing polyurethane resin; step 3, adding the prepared polyurethane resin into melamine-formaldehyde coated ammonium polyphosphate microcapsules for blending and compounding; and 4, pouring the compound liquid into a polytetrafluoroethylene mold to prepare a melamine-formaldehyde coated ammonium polyphosphate type flame-retardant polyurethane adhesive sample, wherein the adhesive is applied to the polyester lining cloth finished by the flame retardant. According to the invention, the inorganic ammonium polyphosphate is coated in the melamine-formaldehyde macromolecular chain segment, is used as a physically added flame retardant, and is compounded with the polyurethane adhesive to obtain the adhesive with flame retardance, so that the comprehensive flame retardance of a polyester lining cloth product is realized, and the safety of the textile in use is improved.
Description
Technical Field
The invention relates to the field of preparation of high-molecular adhesives, in particular to a preparation method and application of a phosphorus-containing flame-retardant polyurethane adhesive.
Background
With the increase of population density, the development of flame-retardant textiles is increasingly demanded in order to reduce the probability of fire and the harm caused by the fire. The textile fabric can be realized by a flame-retardant after-finishing technology, and most of adhesives used for bonding different fabrics are combustible, and release a large amount of smoke and toxic gas in the combustion process to influence the fire rescue work. Therefore, in order to meet social needs, the development of flame retardant adhesives for textiles is urgent.
The Thermoplastic Polyurethane (TPU) is a block polymer consisting of diisocyanate, oligomer poly-polyol and chain extender, has the advantages of high bonding speed, no toxicity, simple implementation process and better bonding strength and flexibility with the terylene lining cloth. The traditional halogen flame retardant, such as decabromodiphenyl ether, does not meet the OEKO-TEX Standard 100 Standard and cannot be applied to textiles, and the novel environment-friendly phosphorus-nitrogen organic flame retardant can be used as an additive to be blended and compounded with a polyurethane adhesive due to the characteristics of low toxicity, low smoke, excellent flame retardant property and the like, so that flame retardance is realized, and a mat is laid for further realizing comprehensive flame retardance of textiles.
Disclosure of Invention
The invention aims to provide a preparation method and application of a phosphorus-containing flame-retardant polyurethane adhesive.
In order to realize the purpose of the invention, the invention adopts the following technical scheme: a preparation method of a phosphorus-containing flame-retardant polyurethane adhesive comprises the following steps: step 1, preparing melamine-formaldehyde coated ammonium polyphosphate microcapsules, wherein the preparation of the melamine-formaldehyde coated ammonium polyphosphate microcapsules comprises the following steps: step a, adding melamine and formaldehyde with a certain molar ratio into a reaction kettle, adjusting the pH value to be alkalescent by using an alkali solution, and diluting the prepared melamine-formaldehyde prepolymer solution to a certain concentration for later use; b, adding a certain amount of ammonium polyphosphate into the water/alcohol mixed solution, adding a dispersing agent, and uniformly stirring to obtain a P-N dispersed phase solution; c, dropwise adding the prepolymer solution prepared in the step a into the mixed solution in the step b, and adjusting the pH value to be weakly acidic by using acid to prepare a precipitate; d, carrying out suction filtration, washing and drying to obtain melamine-formaldehyde coated ammonium polyphosphate (MAPP) microcapsules;
step 2, preparing polyurethane resin, wherein the preparation of the polyurethane resin comprises the following steps: adding diisocyanate into the reaction kettle, heating to 60-80 ℃, slowly adding polyether polyol, and reacting for 1-3 h; under the catalysis of dibutyltin dilaurate, adding 1, 4-butanediol for chain extension, and reacting for 0.5-1h to obtain polyurethane resin;
step 3, adding the prepared polyurethane resin into melamine-formaldehyde coated ammonium polyphosphate microcapsules for blending and compounding;
and 4, pouring the compound liquid into a polytetrafluoroethylene mold to prepare a melamine-formaldehyde coated ammonium polyphosphate type flame-retardant polyurethane adhesive sample.
Preferably, in step a, the melamine and formaldehyde are used in a molar ratio of 1: 2-3, the alkali solution adopts 10 percent NaHCO3Solution or NaOH solution, namely, adjusting the pH value of the solution in the reaction kettle to be alkalescent solution with the pH value of 8-9, heating the solution to 60-80 ℃, and reacting for 0.5-2h to obtain melamine-formaldehyde prepolymer solution with the concentration of 10-30 wt%.
Preferably, in step b, 10g of ammonium polyphosphate is added to 100ml of a water/ethanol mixture, and the volume ratio of water/ethanol is 1: 1-2, adopting hexadecyl trimethyl ammonium chloride as the dispersing agent, and adding 1g of hexadecyl trimethyl ammonium chloride dispersing agent into the mixed solution.
Preferably, in step c, 10-15ml of prepolymer solution is added dropwise, the solid content of the prepolymer solution is 20%, and the acid solution is HAc solution or H3PO4And (3) solution, namely adjusting the solution in the reaction kettle to a solution with the pH value of 4.5-5.
Preferably, in step c, the melamine-formaldehyde prepolymer forms a macromolecular chain segment after undergoing a condensation reaction, and is grafted to the surfaces of polyphosphate particles under the action of a coupling agent, and the macromolecules are gradually insoluble in an alcohol-water solution with the increase of the molecular chain segment, and finally become precipitates to be separated out of the solution.
Preferably, in step 2, the following parts by weight are added: 120 parts of toluene diisocyanate, 100 parts of polyether polyol, 0.5 part of dibutyltin dilaurate and 20 parts of 1, 4-butanediol.
Preferably, in the step 3, the melamine-formaldehyde coated ammonium polyphosphate microcapsules with the addition amount of 10-30% are added into the polyurethane resin, and the mixture is mechanically blended and reacted for 0.5-2h at the temperature of 60-80 ℃.
The application of the phosphorus-containing flame-retardant polyurethane adhesive is applied to polyester lining cloth finished by a flame retardant.
Compared with the prior art, the preparation method and the application of the phosphorus-containing flame-retardant polyurethane adhesive adopting the technical scheme have the following beneficial effects: the preparation method and the application of the phosphorus-containing flame-retardant polyurethane adhesive adopt a microcapsule coating technology of inorganic phosphorus flame retardants to prepare particles which can be stably dispersed in an organic phase; then physically blending and compounding with polyurethane resin to limit the degree of toxic smoke and toxic gas generated during the combustion of polyurethane, so as to obtain the adhesive with the flame retardant function; in addition, the plasticization and the stability of the phosphorus-nitrogen flame retardant in polyurethane are also beneficial to the synthesis of the adhesive; and finally, applying the flame retardant to polyester lining cloth finished by the flame retardant to obtain the omnibearing flame-retardant fabric.
Drawings
FIG. 1 is a schematic flow diagram of an embodiment of a method of making a phosphorus-containing flame retardant polyurethane adhesive of the present invention;
FIG. 2 is a schematic flow chart of the process of coating ammonium polyphosphate with melamine in this example;
fig. 3 is a schematic structural diagram of the ammonium polyphosphate microcapsule coated with melamine in this embodiment.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Fig. 1 is a schematic flow chart of a preparation method of a phosphorus-containing flame-retardant polyurethane adhesive, fig. 2 is a schematic flow chart of melamine-coated ammonium polyphosphate, and fig. 3 is a schematic structural diagram of a melamine-coated ammonium polyphosphate microcapsule, and the preparation method comprises the following steps:
step 1, preparing melamine-formaldehyde coated ammonium polyphosphate microcapsules, comprising the following steps:
step a, adding melamine and formaldehyde with a certain molar ratio into a reaction kettle, adjusting the pH value to be alkalescent by using an alkali solution, and preparing the melamine-formaldehydeAnd diluting the prepolymer solution to a certain concentration for later use. In this example, melamine and formaldehyde were used in a molar ratio of 1: 2-3, using 10% NaHCO as alkali solution3Solution or NaOH solution, namely, adjusting the pH value of the solution in the reaction kettle to be alkalescent solution with the pH value of 8-9, heating the solution to 60-80 ℃, and reacting for 0.5-2h to obtain melamine-formaldehyde prepolymer solution with the concentration of 10-30 wt%.
And b, adding a certain amount of ammonium polyphosphate into the water/alcohol mixed solution, adding a dispersing agent, and uniformly stirring to obtain a P-N dispersed phase solution. In this example, 10g of ammonium polyphosphate was added to 100ml of a water/ethanol mixture in a volume ratio of 1: 1-2, adopting hexadecyl trimethyl ammonium chloride as a dispersing agent, and adding 1g of hexadecyl trimethyl ammonium chloride dispersing agent into the mixed solution.
And c, dropwise adding the prepolymer solution prepared in the step a into the mixed solution in the step b, and adjusting the pH value to be weakly acidic by using acid to prepare a precipitate. Dripping 10-15ml of prepolymer solution, wherein the solid content of the prepolymer solution is 20%, and the acid solution is HAc solution or H solution3PO4And (3) solution, namely adjusting the solution in the reaction kettle to a solution with the pH value of 4.5-5. The melamine-formaldehyde prepolymer forms a macromolecular chain segment after condensation reaction, is grafted to the surface of polyphosphate particles under the action of a coupling agent, and gradually dissolves macromolecules in an alcohol-water solution along with the increase of the molecular chain segment, and finally becomes a precipitate to be separated out from the solution.
And d, carrying out suction filtration, washing and drying to obtain the melamine-formaldehyde coated ammonium polyphosphate (MAPP) microcapsule.
Step 2, preparing polyurethane resin, comprising the following steps: adding diisocyanate into the reaction kettle, heating to 60-80 ℃, slowly adding polyether polyol, and reacting for 1-3 h. In the embodiment, under the catalysis of dibutyltin dilaurate, 1, 4-butanediol is added for chain extension, and after reaction for 0.5-1h, polyurethane resin is prepared; the following parts by weight are added: 120 parts of toluene diisocyanate, 100 parts of polyether polyol, 0.5 part of dibutyltin dilaurate and 20 parts of 1, 4-butanediol.
Step 3, adding the prepared polyurethane resin into melamine-formaldehyde coated ammonium polyphosphate microcapsules for blending and compounding; adding 10-30% of melamine-formaldehyde coated ammonium polyphosphate microcapsule into polyurethane resin, mechanically blending, and reacting at 60-80 ℃ for 0.5-2 h.
And 4, pouring the compound liquid into a polytetrafluoroethylene mold to prepare a melamine-formaldehyde coated ammonium polyphosphate type flame-retardant polyurethane adhesive sample, and applying the adhesive to the polyester lining cloth finished by the flame retardant to obtain the omnibearing flame-retardant fabric.
The first embodiment is as follows:
the preparation method of the short-chain melamine-formaldehyde coated ammonium polyphosphate microcapsule comprises the following steps:
melamine and formaldehyde (mol ratio 1:3) in a mol ratio of 1:3 are added into a reaction kettle, and 10 percent of NaHCO is used3The pH value of the solution is adjusted to about 8, the solution is heated to 80 ℃ to react for 1h, and the melamine-formaldehyde prepolymer solution is diluted with water for later use. Mixing 10g ammonium polyphosphate (M)n500) is added into 100ml of mixed liquid of water and ethanol, the volume ratio of the water to the ethanol is 1:1, 1g of hexadecyl trimethyl ammonium chloride dispersant is added, the mixture is stirred for 0.5h, 15ml of prepolymer solution with 20 percent of solid content is dripped, the pH value is adjusted to about 5 by HAc solution, the mixture reacts for 2h at the temperature of 80 ℃, precipitates are obtained, and the short-chain melamine-formaldehyde coated APP flame retardant is obtained after suction filtration, washing and drying.
The preparation method of the short-chain melamine coated ammonium polyphosphate polyurethane adhesive comprises the following steps:
the following parts by weight are added into a reaction kettle: 120 parts of toluene diisocyanate, heating to 70 ℃ and slowly adding 100 parts of polypropylene glycol (M)n500) reacting for 2h to synthesize a polyurethane prepolymer; under the catalytic action of 0.5 part of dibutyltin dilaurate, 20 parts of 1, 4-butanediol is added for chain extension, after the reaction is carried out for 1h, 10% of MAPP microcapsules are added for mechanical blending, and after the reaction is continued for 2h at the same temperature, the mixture is poured into a polytetrafluoroethylene mold to prepare a short-chain MAPP type flame-retardant polyurethane adhesive sample.
Example two:
the preparation method of the long-chain melamine-formaldehyde coated ammonium polyphosphate microcapsule comprises the following steps:
adding melamine and formaldehyde with a molar ratio of 1:2 into a reaction kettle, adjusting the pH to be about 9 by using 10% NaOH solution, heating to 70 ℃ for reaction for 1h, and diluting the melamine-formaldehyde prepolymer solution with water for later use. Mixing 10g ammonium polyphosphate (M)n1500) was added to 100ml of a water/ethanol mixture (volume ratio 1:2), 1g of cetyltrimethylammonium chloride dispersant was added, stirring was carried out for 0.5H, 10ml of a prepolymer solution (solid content 20%) was added dropwise, and the solution was washed with H3PO4And adjusting the pH value of the solution to about 4.5, reacting at 70 ℃ for 2h to obtain a precipitate, and filtering, washing and drying to obtain the melamine-formaldehyde coated long-chain APP flame retardant.
The preparation method of the long-chain melamine coated ammonium polyphosphate polyurethane adhesive comprises the following steps:
the following parts by weight are added into a reaction kettle: 120 parts of toluene diisocyanate, heating to 70 ℃ and slowly adding 100 parts of polypropylene glycol (M)n500) reacting for 2h to synthesize a polyurethane prepolymer; under the catalytic action of 0.5 part of dibutyltin dilaurate, 20 parts of 1, 4-butanediol is added for chain extension, MAPP microcapsules (the addition amount is 10%) are added for mechanical blending after 1h of reaction, and after 2h of continuous reaction at the same temperature, the mixture is poured into a polytetrafluoroethylene mold to prepare a long-chain MAPP flame-retardant polyurethane adhesive sample.
Example three:
the preparation method of the melamine-coated ammonium polyphosphate microcapsule comprises the following steps:
adding melamine and formaldehyde with a molar ratio of 1:3 into a reaction kettle, adjusting the pH to be about 9 by using 10% NaOH solution, heating to 80 ℃ for reaction for 1h, and diluting the melamine-formaldehyde prepolymer solution with water for later use. Mixing 10g ammonium polyphosphate (M)n1500) is added into 100ml of water/ethanol mixed solution, the volume ratio of the water/ethanol is 1:2, 1g of silica coupling agent KH-550 is added, the mixture is stirred for 0.5H, 10ml of prepolymer solution with 20 percent of solid content is dripped, and H is added3PO4Adjusting the pH value of the solution to about 4.5, reacting for 2h at 80 ℃ to obtain a precipitate, and filtering, washing and drying to obtain the melamine-formaldehyde coated APP flame retardant (MAPP).
The preparation method of the melamine-coated ammonium polyphosphate polyurethane adhesive comprises the following steps:
the following parts by weight are added into a reaction kettle: 120 parts of toluene diisocyanate, heating to 70 ℃ and slowly adding 100 parts of polypropylene glycol (M)n500) reacting for 2h to synthesize a polyurethane prepolymer; under the catalytic action of 0.5 part of dibutyltin dilaurate, 20 parts of 1, 4-butanediol is added for chain extension, MAPP microcapsules (the addition amount is 10%) are added for mechanical blending after 1h of reaction, and after 2h of continuous reaction at the same temperature, the mixture is poured into a polytetrafluoroethylene mold to prepare a MAPP type flame-retardant polyurethane adhesive sample.
And finally, testing the performance of the MAPP microcapsule compound polyurethane adhesive by an oxygen index meter and a strong tensile tester to obtain the adhesive with the limit oxygen index of more than 28 percent and still maintaining the tensile strength of more than 30MPa and the elongation at break of more than 300 percent.
The foregoing is a preferred embodiment of the present invention, and it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (8)
1. A preparation method of a phosphorus-containing flame-retardant polyurethane adhesive is characterized by comprising the following steps: the method comprises the following steps: step 1, preparing melamine-formaldehyde coated ammonium polyphosphate microcapsules, wherein the preparation of the melamine-formaldehyde coated ammonium polyphosphate microcapsules comprises the following steps: step a, adding melamine and formaldehyde with a certain molar ratio into a reaction kettle, adjusting the pH value to be alkalescent by using an alkali solution, and diluting the prepared melamine-formaldehyde prepolymer solution to a certain concentration for later use; b, adding a certain amount of ammonium polyphosphate into the water/alcohol mixed solution, adding a dispersing agent, and uniformly stirring to obtain a P-N dispersed phase solution; c, dropwise adding the prepolymer solution prepared in the step a into the mixed solution in the step b, and adjusting the pH value to be weakly acidic by using acid to prepare a precipitate; d, carrying out suction filtration, washing and drying to obtain melamine-formaldehyde coated ammonium polyphosphate (MAPP) microcapsules;
step 2, preparing polyurethane resin, wherein the preparation of the polyurethane resin comprises the following steps: adding diisocyanate into the reaction kettle, heating to 60-80 ℃, slowly adding polyether polyol, and reacting for 1-3 h; under the catalysis of dibutyltin dilaurate, adding 1, 4-butanediol for chain extension, and reacting for 0.5-1h to obtain polyurethane resin;
step 3, adding the prepared polyurethane resin into melamine-formaldehyde coated ammonium polyphosphate microcapsules for blending and compounding;
and 4, pouring the compound liquid into a polytetrafluoroethylene mold to prepare a melamine-formaldehyde coated ammonium polyphosphate type flame-retardant polyurethane adhesive sample.
2. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in step a, melamine and formaldehyde are mixed in a molar ratio of 1: 2-3, the alkali solution adopts 10 percent NaHCO3Solution or NaOH solution, namely, adjusting the pH value of the solution in the reaction kettle to be alkalescent solution with the pH value of 8-9, heating the solution to 60-80 ℃, and reacting for 0.5-2h to obtain melamine-formaldehyde prepolymer solution with the concentration of 10-30 wt%.
3. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in step b, 10g of ammonium polyphosphate is added into 100ml of a water/ethanol mixed solution, and the volume ratio of water/ethanol is 1: 1-2, adopting hexadecyl trimethyl ammonium chloride as the dispersing agent, and adding 1g of hexadecyl trimethyl ammonium chloride dispersing agent into the mixed solution.
4. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in the step c, 10-15ml of prepolymer solution is dropwise added, the solid content of the prepolymer solution is 20%, and the acid solution is HAc solution or H3PO4And (3) solution, namely adjusting the solution in the reaction kettle to a solution with the pH value of 4.5-5.
5. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in the step c, the melamine-formaldehyde prepolymer forms a macromolecular chain segment after condensation reaction, the macromolecular chain segment is grafted to the surfaces of polyphosphate particles under the action of a coupling agent, and the macromolecules are gradually insoluble in an alcohol-water solution along with the increase of the molecular chain segment, and finally become precipitates to be separated out from the solution.
6. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in step 2, the following parts by weight are added: 120 parts of toluene diisocyanate, 100 parts of polyether polyol, 0.5 part of dibutyltin dilaurate and 20 parts of 1, 4-butanediol.
7. The method of preparing the phosphorus-containing flame retardant polyurethane adhesive according to claim 1, wherein: in the step 3, melamine-formaldehyde coated ammonium polyphosphate microcapsules with the addition amount of 10-30% are added into the polyurethane resin, and are mechanically blended to react for 0.5-2h at the temperature of 60-80 ℃.
8. The application of the phosphorus-containing flame-retardant polyurethane adhesive is characterized in that: the adhesive is applied to the polyester lining cloth finished by the flame retardant.
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