CN111662561B - Preparation method of flame-retardant and repeatedly-processable wood-plastic composite material - Google Patents
Preparation method of flame-retardant and repeatedly-processable wood-plastic composite material Download PDFInfo
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- CN111662561B CN111662561B CN202010671749.4A CN202010671749A CN111662561B CN 111662561 B CN111662561 B CN 111662561B CN 202010671749 A CN202010671749 A CN 202010671749A CN 111662561 B CN111662561 B CN 111662561B
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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
- C08L101/00—Compositions of unspecified macromolecular compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
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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
- C08L97/00—Compositions of lignin-containing materials
- C08L97/02—Lignocellulosic material, e.g. wood, straw or bagasse
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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
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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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Abstract
The invention discloses a preparation method of a flame-retardant and repeatedly-processable wood-plastic composite material, and relates to the field of wood-plastic composite materials. The preparation method of the flame-retardant and repeatedly-processable wood-plastic composite material comprises the steps of firstly dispersing organic aldehyde substances into ethyl acetate, then adding a certain amount of ammonium polyphosphate, then adding ethyl acetate dispersed with amine substances to prepare yellow suspension, and drying to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds; and then carrying out primary mixing, drying, plasticating, molding and cooling on ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics to prepare the flame-retardant and repeatedly-processable wood-plastic composite material. By introducing an imine dynamic covalent bond, the wood-plastic composite material is synchronously endowed with flame retardance, toughness and easy processability. The performance test shows that the limited oxygen index is 26.5-31.2%, and the impact strength is 6.4-8.0 kJ/m2And the melt viscosity is reduced by 72-77%.
Description
Technical Field
The invention discloses a preparation method of a flame-retardant and repeatedly-processable wood-plastic composite material, and particularly relates to a wood-plastic composite material crosslinked by an imine dynamic covalent bond, belonging to the field of composite materials.
Background
Wood Plastic Composites (WPC) are ecological and environment-friendly materials prepared by using wood and plastic as main raw materials and adopting molding processes such as extrusion, injection or mould pressing and the like through melt compounding. At present, the main products of domestic wood-plastic composite materials are various wallboards, planks, railings and the like. The function is single, the added value is low, and the high-performance wood-plastic composite material is still in the initial development stage. The wood-plastic composite material with high strength, good durability and flame retardant function is developed, so that the performance requirements of application fields such as buildings, decorations, doors, windows, electronic devices and the like are met, and the development and industrial transformation upgrading of the wood-plastic composite material in the high-end application field in China are facilitated.
Wood-plastic composite materials used for building materials must satisfy both flame retardant properties and mechanical properties. The wood-plastic composite material is flammable, the limited oxygen index is only 19.5-20.2%, and the wood-plastic composite material needs to be subjected to flame retardant treatment. The ammonium polyphosphate is a commonly used flame retardant in the wood-plastic composite material, can effectively improve the flame retardant property of the wood-plastic composite material, but when the ammonium polyphosphate is used alone, the mechanical properties (including strength and toughness) of the wood-plastic composite material are obviously reduced, and meanwhile, the melt viscosity of the system is rapidly increased in the extrusion process, so that the extrusion is difficult. The compatibility of the ammonium polyphosphate and the matrix material can be effectively improved through the compounding with the nano material or the surface modification technology, and the flame retardant property and the strength of the wood-plastic composite material are improved. However, the problems of toughness and difficulty in extrusion cannot be solved well. The patent CN 110229539A reports a preparation method of a composite polyelectrolyte synchronous flame-retardant toughened wood-plastic composite material, however, the method still cannot solve the limitation of difficult extrusion of the flame-retardant wood-plastic composite material.
A polymer material (also called a vitromer or a glass-like polymer) crosslinked by Dynamic covalent bonds is a type of polymer containing Dynamic covalent bonds. The dynamic covalent bond has the high strength of the covalent bond and the reversible property of the non-covalent bond, perfectly combines the advantages of thermosetting polymers and thermoplastic polymers, and makes remarkable progress in the aspects of epoxy resin and polyurethane at present. Among them, imine bond (C ═ N) is a dynamic reversible covalent bond generated by the reaction of a carbonyl group (aldehyde or ketone) -containing compound with an amine group-containing compound (primary amine, hydrazine and hydroxylamine), and has the characteristics of mild reaction conditions and high reaction rate. The patent CN 108530590A discloses that a Vitrimer containing a quasi-conjugated, rigid structure is prepared by introducing a monomer containing an aromatic structure, however, the patent does not indicate the applicable field of the Vitrimer with the structure and limits the development. By regulating and controlling the molecular groups at the two ends of the imine, the function of the system can be further improved, the performance of engineering materials and the preparation process are met, and the development of the application of Vistimer is facilitated.
The invention takes the preparation of the high-performance flame-retardant wood-plastic composite material as a starting point, and synchronously endows the wood-plastic composite material with flame retardance, toughness and easy processability by introducing an imine dynamic covalent bond.
Disclosure of Invention
The purpose of the invention is as follows: provides a preparation method of a flame-retardant and repeatedly-processable wood-plastic composite material.
The technical solution of the invention is as follows:
(1) weighing organic aldehyde substances, dispersing the organic aldehyde substances in ethyl acetate, and stirring to obtain yellow suspension;
(2) weighing amine substances, dispersing the amine substances in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, dispersing in the yellow suspension in the step (1), and enabling the mass ratio of the organic aldehyde substance to the ammonium polyphosphate to be (0.27-0.67) to 1;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing at 100-110 ℃ for 8-10 h, grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds, and enabling the mass ratio of amine substances to ammonium polyphosphate to be (0.12-0.3) to 1;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics in the step (4) according to the mass ratio of (20-30) to (25-45) to (25-50), primarily mixing, and drying at 50-60 ℃ for 2-4 hours to obtain a premix;
(6) and (5) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare the flame-retardant and repeatedly-processable wood-plastic composite material.
The invention has the advantages that:
(1) the introduction of the covalent bond enables the plant fiber, the flame retardant and the thermoplastic plastic in the wood-plastic composite material to form good interface compatibility, so that the material can transmit stress and absorb energy through the interface when bearing load, and the effect of strengthening and toughening is achieved. The wood-plastic composite material containing imine dynamic covalent bond modified ammonium polyphosphate has the limiting oxygen index of 26.5-31.2%, the tensile strength of 23.4-25.8 MPa and the impact strength of 6.4-8.0 kJ/m2Compared with the unmodified ammonium polyphosphate with the same addition amount, the modified ammonium polyphosphate is respectively improved by 18-35%, 16-24% and 28-53%.
(2) In the extrusion molding process, the plant fiber releases certain water vapor due to the heat effect to cause imine bond to be broken to generate aldehyde and amine substances, so that the viscosity is reduced, and the extrusion speed is increased. At 170 ℃ and 0.01Hz, the melt viscosity of the imine-containing dynamic covalent bond modified ammonium polyphosphate composite material is reduced to (1.37-1.67) × 105Pa s is reduced by 72-77% compared with unmodified ammonium polyphosphate in the same addition amount.
(3) The imine dynamic crosslinking endows the wood-plastic composite material with repeatable processing performance. When the circular processing is carried out for 3 times, the limit oxygen index is kept unchanged, the tensile strength is reduced by 14 percent, and the impact strength is reduced by 10 percent.
(4) The imine-containing dynamic covalent bond ammonium polyphosphate has simple synthesis process and reduces the production cost.
Drawings
FIG. 1 shows ammonium polyphosphate solid powder containing imine dynamic covalent bonds obtained in example 1.
FIG. 2 is a sample of the wood-plastic composite obtained in example 3, which was processed in 3 cycles.
Detailed Description
In the case of the example 1, the following examples are given,
(1) weighing terephthalaldehyde, dispersing in ethyl acetate, and stirring to obtain a yellow suspension;
(2) weighing ethylenediamine, dispersing in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, dispersing in the yellow suspension in the step (1), and enabling the mass ratio of terephthalaldehyde to ammonium polyphosphate to be 0.27: 1;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing air at 100-110 ℃ for 8-10 h, grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds, and enabling the mass ratio of ethylenediamine to ammonium polyphosphate to be 0.12: 1;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics in the step (4) according to the mass ratio of 25: 35: 40, primarily mixing, and drying at 50-60 ℃ for 2-4 h to obtain a premix;
(6) and (5) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare the flame-retardant and repeatedly-processable wood-plastic composite material.
The performance test shows that: the imine-containing dynamic covalent bond ammonium polyphosphate is used for treating the wood-plastic composite material, and has the limiting oxygen index of 26.5 percent, the tensile strength of 23.5MPa and the impact strength of 6.5kJ/m2At 170 ℃ and 0.01Hz, the viscosity of the wood-plastic composite material is reduced to 1.67 multiplied by 105Pa·s。
In the case of the example 2, the following examples are given,
(1) weighing terephthalaldehyde, dispersing in ethyl acetate, and stirring to obtain a yellow suspension;
(2) weighing ethylenediamine, dispersing in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, dispersing in the yellow suspension in the step (1), and enabling the mass ratio of terephthalaldehyde to ammonium polyphosphate to be 0.67: 1;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing air at 100-110 ℃ for 8-10 h, grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds, and enabling the mass ratio of ethylenediamine to ammonium polyphosphate to be 0.25: 1;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics in the step (4) according to the mass ratio of 20: 30: 50, primarily mixing, and drying at 50-60 ℃ for 2-4 h to obtain a premix;
(6) and (5) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare the flame-retardant and repeatedly-processable wood-plastic composite material.
The performance test shows that: the imine-containing dynamic covalent bond ammonium polyphosphate is used for treating the wood-plastic composite material, and has the limiting oxygen index of 28.2 percent, the tensile strength of 24.3MPa and the impact strength of 6.4kJ/m2At 170 ℃ and 0.01Hz, the viscosity of the wood-plastic composite material is reduced to 1.37 multiplied by 105Pa·s。
In the case of the example 3, the following examples are given,
(1) weighing terephthalaldehyde, dispersing in ethyl acetate, and stirring to obtain a yellow suspension;
(2) weighing polyethyleneimine, dispersing in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, dispersing in the yellow suspension in the step (1), and enabling the mass ratio of terephthalaldehyde to ammonium polyphosphate to be 0.6: 1;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing air at 100-110 ℃ for 8-10 h, grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds, and enabling the mass ratio of polyethyleneimine to ammonium polyphosphate to be 0.2: 1;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics in the step (4) according to the mass ratio of 20: 40, primarily mixing, and drying at 50-60 ℃ for 2-4 h to obtain a premix;
(6) and (5) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare the flame-retardant and repeatedly-processable wood-plastic composite material.
The performance test shows that: the imine-containing dynamic covalent bond ammonium polyphosphate is used for treating the wood-plastic composite material, and has the limiting oxygen index of 29.1 percent, the tensile strength of 24.6MPa and the impact strength of 8.0kJ/m2At 170 ℃ and 0.01Hz, the viscosity of the wood-plastic composite material is reduced to 1.5 multiplied by 105Pa.s。
In the case of the example 4, the following examples are given,
(1) weighing terephthalaldehyde, dispersing in ethyl acetate, and stirring to obtain a yellow suspension;
(2) weighing polyethyleneimine, dispersing in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, dispersing in the yellow suspension in the step (1), and enabling the mass ratio of terephthalaldehyde to ammonium polyphosphate to be 0.5: 1;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing air at 100-110 ℃ for 8-10 h, grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds, and enabling the mass ratio of polyethyleneimine to ammonium polyphosphate to be 0.3: 1;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds, plant fibers and plastics in the step (4) according to the mass ratio of 30: 25: 45, primarily mixing, and drying at 50-60 ℃ for 2-4 h to obtain a premix;
(6) and (5) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare the flame-retardant and repeatedly-processable wood-plastic composite material.
The performance test shows that: the imine-containing dynamic covalent bond ammonium polyphosphate is used for treating the wood-plastic composite material, and has the limiting oxygen index of 31.2 percent, the tensile strength of 25.8MPa and the impact strength of 7.2kJ/m2At 170 ℃ and 0.01Hz, the viscosity of the wood-plastic composite material is reduced to 1.45 multiplied by 105Pa·s。
Claims (4)
1. A preparation method of a flame-retardant and repeatedly-processable wood-plastic composite material is characterized by comprising the following steps:
(1) weighing organic aldehyde substances, dispersing the organic aldehyde substances in ethyl acetate, and stirring to obtain yellow suspension;
(2) weighing amine substances, dispersing the amine substances in ethyl acetate, and stirring to obtain colorless transparent liquid;
(3) weighing ammonium polyphosphate, adding the ammonium polyphosphate into the yellow suspension in the step (1), and stirring to obtain a yellow suspension;
(4) adding the colorless transparent liquid obtained in the step (2) into the yellow suspension obtained in the step (3), reacting at 60-70 ℃ until the solvent is completely volatilized, drying by blowing at 100-110 ℃ for 8-10 h, and grinding to obtain ammonium polyphosphate solid powder containing imine dynamic covalent bonds;
(5) weighing ammonium polyphosphate solid powder containing imine dynamic covalent bonds in the step (4), plant fibers and plastics, primarily mixing, and drying at 50-60 ℃ for 2-4 h to obtain a premix;
(6) performing extrusion molding and cooling on the premix obtained in the step (5) to prepare a flame-retardant and repeatedly-processable wood-plastic composite material;
the organic aldehyde substance is terephthalaldehyde, and the amine substance is one or a mixture of ethylene diamine, polyethyleneimine and polydopamine.
2. The preparation method of the flame-retardant and repeatedly processable wood-plastic composite material as claimed in claim 1, wherein the mass ratio of the organic aldehyde substance to the ammonium polyphosphate is (0.27-0.67) to 1.
3. The preparation method of the flame-retardant and repeatedly processable wood-plastic composite material as claimed in claim 1, wherein the mass ratio of the amine substance to the ammonium polyphosphate is (0.12-0.3) to 1.
4. The preparation method of the flame-retardant and repeatedly processable wood-plastic composite material as claimed in claim 1, wherein the mass ratio of the ammonium polyphosphate solid powder containing the imine dynamic covalent bond, the plant fiber and the plastic is (20-30): (25-45): (25-50).
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