CN109096537B - Flame retardant for preparing polyurethane foam plastic - Google Patents
Flame retardant for preparing polyurethane foam plastic Download PDFInfo
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- CN109096537B CN109096537B CN201811046972.9A CN201811046972A CN109096537B CN 109096537 B CN109096537 B CN 109096537B CN 201811046972 A CN201811046972 A CN 201811046972A CN 109096537 B CN109096537 B CN 109096537B
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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
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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
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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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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- 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
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
Abstract
The invention relates to the technical field of novel functional materials, and discloses a flame retardant for preparing polyurethane foam plastic, which is prepared by utilizing the specific chemical structure of the flame retardant prepared by utilizing zinc nitrate and europium oxide, has excellent flame retardant property, heat resistance and mechanical property, and is introduced into the foamable foam precursor copolymer according to the addition amount of 0.21-0.23 percent of the mass of the polyurethane foam plastic, thereby overcoming the defects that the polyurethane has low polymerization degree, the halogen flame retardant and the phosphorus flame retardant have the problem of poor solubility in a polymer system, have the double functions of flame retardance and reinforcement, obviously prolong the service life of polyurethane foam plastic, improve the mechanical properties and heat resistance of the plastic such as tensile strength, impact strength, bending strength and the like, reduce the addition amount, obviously reduce the cost, and reduce a series of problems of environmental pollution and the like.
Description
Technical Field
The invention belongs to the technical field of novel functional materials, and particularly relates to a flame retardant for preparing polyurethane foam plastic.
Background
The foamed plastic is a high polymer material formed by dispersing a large number of gas micropores in solid plastic, has the characteristics of light weight, heat insulation, sound absorption, shock absorption and the like, has dielectric properties superior to matrix resin, and has wide application range. Almost all kinds of plastics can be made into foamed plastics, and foam molding has become an important field in plastic processing. Also called porous plastic, is plastic which is made of resin as a main raw material and has countless micropores inside. It is classified into soft and hard. It is widely used as heat-insulating, sound-insulating, packing material, shell of vehicle and ship, etc. Foam plastics, cellular plastics, plastics that contain countless cells throughout. Plastic with many tiny air holes inside. By mechanical means (foaming by introducing air or carbon dioxide while mechanically stirring) or chemical means (addition of a foaming agent). The closed hole type and the open hole type are adopted. The air holes in the closed holes are mutually isolated and have floatability; the air holes in the open pore type are communicated with each other and have no floatability. Can be made of polystyrene, polyvinyl chloride, polyurethane and other resins. Can be used as heat-insulating and sound-insulating material.
Polyurethane foam is prepared by polymerizing and foaming isocyanate and hydroxyl compound, and can be divided into soft and hard according to the hardness, wherein the soft is the main variety. In general, it has excellent elasticity, softness, elongation and compressive strength; good chemical stability, resistance to many solvents and oils; the wear resistance is excellent and is 20 times larger than that of natural sponge; it is a cushioning material excellent in processability, heat insulation properties, adhesiveness and the like, but is expensive. Polyurethane foams are typically flame retarded by the addition of flame retardants to enhance the flame retardancy of the foam to retard burning, block smoke, and even self-extinguish the fire. The existing phosphorus flame retardant and halogen flame retardant have the defect of poor solubility in a polymer system, so that the flame retardant effect is not uniform, the addition amount is large, the mechanical property and the heat resistance of polyurethane foam are reduced, and a series of problems of environmental pollution and the like are caused.
Disclosure of Invention
The invention aims to solve the existing problems, provides a flame retardant for preparing polyurethane foam plastics, overcomes the problem that halogen flame retardants and phosphorus flame retardants have poor solubility in a polymer system due to low polyurethane polymerization degree, plays a role in flame retardance and reinforcement, and obviously prolongs the service life of the polyurethane foam plastics.
The invention is realized by the following technical scheme:
a flame retardant for preparing polyurethane foam plastics is prepared by the following steps:
(1) weighing 11.0-11.2 g of zinc nitrate powder, adding the zinc nitrate powder into a flask, mixing deionized water and absolute ethyl alcohol according to the mass ratio of 1:4.0-4.5 to serve as a solvent, wherein the using amount of the solvent is 110-120 ml, magnetically stirring the mixture at 300-350 r/min until the solvent is completely dissolved, dropwise adding an ammonia water solution into the dissolved solution under stirring until no precipitate is generated, and then ultrasonically dispersing the precipitated mixture for 30-40 min to obtain a suspension mixture;
(2) preparing 95-100 ml of dilute nitric acid solution with the mass concentration of 7.0-8.0%, weighing 8.5-8.8 g of europium oxide powder, adding the europium oxide powder into a beaker, adding the prepared dilute nitric acid solution into the beaker, heating the beaker to 40-45 ℃ in a water bath, stirring the solution clockwise by using a glass rod until the solid is completely dissolved, placing the beaker into a magnetic stirring device, stirring the beaker at the speed of 300 revolutions per minute, dropwise adding urea aqueous solution into the beaker until a large amount of precipitate is generated, finally changing the solution into milky precipitate mixed solution, measuring the pH value of the precipitate mixed solution to be 8.8-9.0, stopping dropwise adding the urea solution, adding the suspended mixture prepared in the step (1), and stirring and mixing uniformly;
(3) covering a double-layer preservative film on the beaker filled with the mixture, standing and refrigerating for 6-8 hours at 0-5 ℃, filtering the precipitate obtained by standing and refrigerating, repeatedly washing the precipitate to be neutral by deionized water, collecting the precipitate, putting the precipitate into a vacuum drying box, drying the precipitate for 4-5 hours at 90-95 ℃, putting the precipitate into a crucible, and putting the crucible into a preheated muffle furnace for calcining for 6-7 hours at the calcining temperature of 580-600 ℃ to obtain the nanoscale flame retardant.
As a further description of the above aspect, the flame retardant is added in an amount of 0.21 to 0.23% by mass based on the polyurethane foam.
As a further description of the above scheme, the pH value of the aqueous ammonia solution in the step (1) is between 10.2 and 10.4.
As a further description of the above scheme, the mass concentration of the urea aqueous solution in the step (2) is 35-40%.
As a further description of the above scheme, the muffle furnace preheating temperature in the step (3) is 260-280 ℃.
As a further description of the scheme, the particle size of the nanoscale flame retardant prepared in the step (3) is 10-30 nanometers.
Compared with the prior art, the invention has the following advantages: in order to solve the problem of poor flame retardant effect in the preparation of the existing polyurethane foam plastic, the invention provides a flame retardant for preparing the polyurethane foam plastic, the prepared flame retardant has a specific chemical structure and is excellent in flame retardant property, heat resistance and mechanical property, the flame retardant is introduced into a foamable foam precursor copolymer, the problem that halogen flame retardants and phosphorus flame retardants have poor solubility in a polymer system due to low polyurethane polymerization degree is solved, the flame retardant and the reinforcing double effects are achieved, the service life of the polyurethane foam plastic is obviously prolonged, the mechanical properties and the heat resistance of the plastic such as tensile strength, impact strength, bending strength and the like are improved, the addition amount is small, the cost is obviously reduced, a series of environmental pollution and the like are reduced, and the problem that the flame retardant has poor flame retardant effect in the preparation of the existing polyurethane foam plastic is solved by the flame retardant prepared by the invention, the polyurethane foam plastic has the advantages that high mechanical stability is kept, the flame-retardant effect and the strength performance of the polyurethane foam plastic are improved, the development and the utilization of the polyurethane foam plastic are improved, the practical significance of prolonging the service life of the polyurethane foam plastic and expanding the application field of the polyurethane foam plastic can be realized, and the polyurethane foam plastic is a technical scheme which is very worthy of popularization and use.
Detailed Description
In order to make the objects, technical solutions and effects of the present invention clearer and clearer, the present invention is further described with reference to specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the present invention and are not used for limiting the technical solutions provided by the present invention.
Example 1
A flame retardant for preparing polyurethane foam plastics is prepared by the following steps:
(1) weighing 11.0 g of zinc nitrate powder, adding the zinc nitrate powder into a flask, mixing deionized water and absolute ethyl alcohol according to a mass ratio of 1:4.05 to serve as a solvent, wherein the usage amount of the solvent is 110 ml, magnetically stirring the mixture at 300 r/min until the mixture is completely dissolved, dropwise adding an ammonia water solution into the dissolved solution under stirring until no precipitate is generated, and then ultrasonically dispersing the precipitated mixture for 30 minutes to obtain a suspension mixture;
(2) preparing 95 ml of dilute nitric acid solution with the mass concentration of 7.0%, weighing 8.5 g of europium oxide powder, adding the europium oxide powder into a beaker, adding the prepared dilute nitric acid solution into the beaker, heating the beaker to 40 ℃ in a water bath, stirring the mixture clockwise by using a glass rod until all solids are dissolved, placing the beaker into a magnetic stirring device, stirring the beaker at 300 r/min, dropwise adding urea aqueous solution into the beaker until a large amount of precipitate is generated, finally, changing the solution into milky precipitate mixed solution, measuring the pH value of the precipitate mixed solution to be between 8.8 and 9.0, stopping dropwise adding the urea solution, adding the suspended mixture prepared in the step (1), and stirring and mixing the mixture uniformly;
(3) covering a double-layer preservative film on a beaker filled with the mixture, standing and refrigerating for 6 hours at 0 ℃, filtering the precipitate obtained by standing and refrigerating, repeatedly washing the precipitate to be neutral by deionized water, collecting the precipitate, putting the precipitate into a vacuum drying oven, drying the precipitate for 4 hours at 90 ℃, putting the dried precipitate into a crucible, putting the crucible into a preheated muffle furnace, and calcining the preheated muffle furnace for 6 hours at the calcining temperature of 580 ℃ to obtain the nanoscale flame retardant.
As a further description of the above aspect, the flame retardant is added in an amount of 0.21% by mass based on the polyurethane foam.
As a further description of the above scheme, the pH value of the aqueous ammonia solution in the step (1) is between 10.2 and 10.4.
As a further description of the above scheme, the mass concentration of the urea aqueous solution in the step (2) is 35%.
As a further description of the above scheme, the muffle preheating temperature in step (3) is 260 ℃.
As a further description of the scheme, the particle size of the nanoscale flame retardant prepared in the step (3) is 10-30 nanometers.
Example 2
A flame retardant for preparing polyurethane foam plastics is prepared by the following steps:
(1) weighing 11.1 g of zinc nitrate powder, adding the zinc nitrate powder into a flask, mixing deionized water and absolute ethyl alcohol according to a mass ratio of 1:4.2 to serve as a solvent, wherein the using amount of the solvent is 115 ml, magnetically stirring the mixture at 330 revolutions per minute until the mixture is completely dissolved, dropwise adding an ammonia water solution into the dissolved solution under stirring until no precipitate is generated, and then ultrasonically dispersing the precipitated mixture for 35 minutes to obtain a suspension mixture;
(2) preparing 98 ml of dilute nitric acid solution with the mass concentration of 7.5%, weighing 8.6 g of europium oxide powder, adding the europium oxide powder into a beaker, adding the prepared dilute nitric acid solution into the beaker, heating the beaker to 42 ℃ in a water bath, stirring the mixture clockwise by using a glass rod until all solids are dissolved, placing the beaker into a magnetic stirring device, stirring the beaker at 330 revolutions per minute, dropwise adding urea aqueous solution into the beaker until a large amount of precipitate is generated, finally, changing the solution into milky precipitate mixed solution, measuring the pH value of the precipitate mixed solution to be between 8.8 and 9.0, stopping dropwise adding the urea solution, adding the suspended mixture prepared in the step (1), and stirring and mixing the mixture uniformly;
(3) covering a double-layer preservative film on a beaker filled with the mixture, standing and refrigerating for 7 hours at the temperature of 2 ℃, filtering the precipitate obtained by standing and refrigerating, repeatedly washing the precipitate to be neutral by using deionized water, collecting the precipitate, putting the precipitate into a vacuum drying box, drying the precipitate for 4.5 hours at the temperature of 92 ℃, putting the dried precipitate into a crucible, putting the crucible into a preheated muffle furnace, and calcining the preheated muffle furnace for 6.5 hours at the calcining temperature of 590 ℃ to obtain the nanoscale flame retardant.
As a further description of the above-mentioned aspect, the flame retardant is added in an amount of 0.22% by mass based on the polyurethane foam.
As a further description of the above scheme, the pH value of the aqueous ammonia solution in the step (1) is between 10.2 and 10.4.
As a further description of the above scheme, the mass concentration of the urea aqueous solution in the step (2) is 38%.
As a further description of the above scheme, the muffle preheating temperature in the step (3) is 270 ℃.
As a further description of the scheme, the particle size of the nanoscale flame retardant prepared in the step (3) is 10-30 nanometers.
Example 3
A flame retardant for preparing polyurethane foam plastics is prepared by the following steps:
(1) weighing 11.2 g of zinc nitrate powder, adding the zinc nitrate powder into a flask, mixing deionized water and absolute ethyl alcohol according to a mass ratio of 1:4.5 to serve as a solvent, wherein the using amount of the solvent is 120 ml, magnetically stirring the mixture at 350 r/min until the mixture is completely dissolved, dropwise adding an ammonia water solution into the dissolved solution under stirring until no precipitate is generated, and then ultrasonically dispersing the precipitated mixture for 40 minutes to obtain a suspension mixture;
(2) preparing 100 ml of dilute nitric acid solution with the mass concentration of 8.0%, weighing 8.8 g of europium oxide powder, adding the europium oxide powder into a beaker, adding the prepared dilute nitric acid solution into the beaker, heating the beaker to 45 ℃ in a water bath, stirring the mixture clockwise by using a glass rod until all solids are dissolved, placing the beaker into a magnetic stirring device, stirring the beaker at 350 r/min, dropwise adding urea aqueous solution into the beaker until a large amount of precipitate is generated, finally, changing the solution into milky precipitate mixed solution, measuring the pH value of the precipitate mixed solution to be between 8.8 and 9.0, stopping dropwise adding the urea solution, adding the turbid mixture prepared in the step (1), and stirring and uniformly mixing the mixture;
(3) covering a double-layer preservative film on a beaker filled with the mixture, standing and refrigerating for 8 hours at the temperature of 5 ℃, filtering the precipitate obtained by standing and refrigerating, repeatedly washing the precipitate to be neutral by using deionized water, collecting the precipitate, putting the precipitate into a vacuum drying oven, drying the precipitate for 5 hours at the temperature of 95 ℃, putting the dried precipitate into a crucible, putting the crucible into a preheated muffle furnace, and calcining the preheated muffle furnace for 7 hours at the calcining temperature of 600 ℃ to obtain the nanoscale flame retardant.
As a further description of the above aspect, the flame retardant is added in an amount of 0.23% by mass based on the polyurethane foam.
As a further description of the above scheme, the pH value of the aqueous ammonia solution in the step (1) is between 10.2 and 10.4.
As a further description of the above scheme, the mass concentration of the urea aqueous solution in the step (2) is 40%.
As a further description of the above scheme, the muffle preheating temperature in step (3) is 280 ℃.
As a further description of the scheme, the particle size of the nanoscale flame retardant prepared in the step (3) is 10-30 nanometers.
Comparative example 1
The only difference from example 1 is that in the preparation of the flame retardant, the addition of the suspension mixture obtained in step (1) is omitted and the rest remains the same.
Comparative example 2
The only difference from example 2 is that in the preparation of the flame retardant, the preparation addition of the milky precipitation mixed liquid in the step (2) is omitted, and the rest is kept consistent.
Comparative example 3
The difference from example 3 is only that, in step (1), the same amount of absolute ethyl alcohol is used instead of the specific gravity of the deionized water in the mixed solvent of the deionized water and the absolute ethyl alcohol, and the rest is consistent.
Comparative example 4
The only difference from example 3 is that, in step (2), an aqueous solution of sodium hydroxide having a mass concentration of 18% was used instead of the aqueous urea solution, and the rest was kept the same.
Comparative example 5
The only difference from example 3 is that the calcination temperature in step (3) was 650 ℃ and the calcination time was 4 hours, and the rest remained the same.
Comparative experiment
The method for preparing the flame retardant for preparing the polyurethane foam plastics comprises the steps of respectively using the methods of examples 1-3 and comparative examples 1-5 to prepare the flame retardant for preparing the polyurethane foam plastics, taking a method (the adding amount is 1.4 percent of the mass of the polyurethane foam plastics) of taking melamine as the flame retardant as a control group, weighing 100 parts of polyether polyol and 100 parts of isocyanate according to parts by weight, adding 2 parts of initiator, 3 parts of cross-linking agent and 4 parts of foaming agent, and preparing the prepared flame retardant according to the methods of all the groups, carrying out prepolymerization reaction, processing and preparing the polyurethane foam plastics, wherein the materials for preparing all the groups are the same, then carrying out flame retardant performance and mechanical performance tests, comparing the results, keeping the independent variables in the test consistent:
| item | Tensile Strength (MPa) at 30 ℃ | Elongation (%) | Limiting oxygen index (%) | Heat-resistant temperature increase (. degree. C.) |
| Example 1 | 68.9 | 88 | 45.5 | 60 |
| Example 2 | 69.2 | 89 | 45.7 | 65 |
| Example 3 | 69.0 | 88 | 45.6 | 63 |
| Comparative example 1 | 48.2 | 72 | 25.2 | 26 |
| Comparative example 2 | 51.0 | 75 | 26.4 | 29 |
| Comparative example 3 | 55.8 | 78 | 31.5 | 36 |
| Comparative example 4 | 58.6 | 82 | 33.8 | 41 |
| Comparative example 5 | 62.5 | 85 | 37.0 | 50 |
| Control group | 42.3 | 66 | 22.6 | Control |
The flame retardant prepared by the invention solves the problem of poor flame retardant effect in the existing polyurethane foam plastic preparation, keeps higher mechanical stability, gives consideration to the improvement of flame retardant effect and strength performance of the polyurethane foam plastic, improves the development and utilization of the polyurethane foam plastic, can realize the practical significance of prolonging the service life of the polyurethane foam plastic and expanding the application field of the polyurethane foam plastic, and is a technical scheme which is extremely worthy of popularization and use.
Claims (6)
1. The flame retardant for preparing the polyurethane foam is characterized by comprising the following steps:
(1) weighing 11.0-11.2 g of zinc nitrate powder, adding the zinc nitrate powder into a flask, mixing deionized water and absolute ethyl alcohol according to the mass ratio of 1:4.0-4.5 to serve as a solvent, wherein the using amount of the solvent is 110-120 ml, magnetically stirring the mixture at 300-350 r/min until the solvent is completely dissolved, dropwise adding an ammonia water solution into the dissolved solution under stirring until no precipitate is generated, and then ultrasonically dispersing the precipitated mixture for 30-40 min to obtain a suspension mixture;
(2) preparing 95-100 ml of dilute nitric acid solution with the mass concentration of 7.0-8.0%, weighing 8.5-8.8 g of europium oxide powder, adding the europium oxide powder into a beaker, adding the prepared dilute nitric acid solution into the beaker, heating the beaker to 40-45 ℃ in a water bath, stirring the solution clockwise by using a glass rod until the solid is completely dissolved, placing the beaker into a magnetic stirring device, stirring the beaker at the speed of 300 revolutions per minute, dropwise adding urea aqueous solution into the beaker until a large amount of precipitate is generated, finally changing the solution into milky precipitate mixed solution, measuring the pH value of the precipitate mixed solution to be 8.8-9.0, stopping dropwise adding the urea solution, adding the suspended mixture prepared in the step (1), and stirring and mixing uniformly;
(3) covering a double-layer preservative film on the beaker filled with the mixture, standing and refrigerating for 6-8 hours at 0-5 ℃, filtering the precipitate obtained by standing and refrigerating, repeatedly washing the precipitate to be neutral by deionized water, collecting the precipitate, putting the precipitate into a vacuum drying box, drying the precipitate for 4-5 hours at 90-95 ℃, putting the precipitate into a crucible, and putting the crucible into a preheated muffle furnace for calcining for 6-7 hours at the calcining temperature of 580-600 ℃ to obtain the nanoscale flame retardant.
2. The flame retardant for polyurethane foam production according to claim 1, wherein the amount of the flame retardant added is 0.21 to 0.23% by mass based on the polyurethane foam.
3. The flame retardant for polyurethane foam production according to claim 1, wherein the pH of the aqueous ammonia solution in the step (1) is 10.2 to 10.4.
4. The flame retardant for polyurethane foam production according to claim 1, wherein the mass concentration of the aqueous urea solution in the step (2) is 35 to 40%.
5. The flame retardant for polyurethane foam production according to claim 1, wherein the muffle preheating temperature in step (3) is 260-280 ℃.
6. The flame retardant for polyurethane foam production according to claim 1, wherein the nanoscale flame retardant prepared in step (3) has a particle size of 10 to 30 nm.
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| CN101591468A (en) * | 2008-05-28 | 2009-12-02 | 上海仲真材料科技有限公司 | A kind of low-smoke halogen-free flame retardant PC/ABS Alloy And Preparation Method |
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