CN117627305A - Degradable stone-plastic floor and preparation method thereof - Google Patents
Degradable stone-plastic floor and preparation method thereof Download PDFInfo
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- CN117627305A CN117627305A CN202311601400.3A CN202311601400A CN117627305A CN 117627305 A CN117627305 A CN 117627305A CN 202311601400 A CN202311601400 A CN 202311601400A CN 117627305 A CN117627305 A CN 117627305A
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- 239000003242 anti bacterial agent Substances 0.000 claims abstract description 17
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- LMQORFSQFKHATF-UHFFFAOYSA-N dimethoxy-methyl-[4-(oxiran-2-yl)butyl]silane Chemical compound CO[Si](C)(OC)CCCCC1CO1 LMQORFSQFKHATF-UHFFFAOYSA-N 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims 2
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 claims 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a degradable stone-plastic floor and a preparation method thereof. The degradable Dan Su floor comprises a TPU layer, a modified PBAT stone plastic substrate and a TPU layer from top to bottom. The antibacterial agent with good antibacterial effect is prepared; preparing the antibacterial agent, TPU, PBAT resin, an initiator, cobblestone powder, a colorant and a stabilizer into a modified PBAT stone plastic substrate; and finally, compounding the TPU layer, the modified PBAT stone plastic base material and the TPU layer. Compared with the prior art, the degradable stone plastic floor prepared by the invention has the advantages of degradability, antibacterial property and the like.
Description
Technical Field
The invention relates to the technical field of stone-plastic floors, in particular to a degradable stone-plastic floor and a preparation method thereof.
Background
The stone plastic floor is also called as stone plastic floor tile, and the normal name is PVC sheet floor, which is a novel floor decoration material developed by high quality and high technology research, adopts cobblestone powder to form a solid base layer with high density and high fiber net structure, and is coated with a super wear-resistant polymer PVC wear-resistant layer on the surface, and is processed by hundreds of procedures.
The stone plastic floor is generally composed of four layers, namely a wear-resistant layer, a decorative layer, a base layer and a bottom layer from top to bottom. The wear-resistant layer has the main function of resisting abrasion to ensure the durability of the floor, and mainly consists of transparent polyvinyl chloride (PVC) resin and special wear-resistant particles. The decorative layer is responsible for presenting the color and pattern of the stone plastic floor and mainly consists of a printed PVC film, and can simulate various natural or artificial patterns, such as wood grains and the like. The base layer is a bearing structure of the stone plastic floor and mainly plays a role in stabilizing and supporting, and is generally prepared by mixing raw materials such as PVC resin powder, plasticizer, calcium carbonate and the like. The main function of the bottom layer is to protect the floor from abrasion and scratch, increase the texture and stability of the floor, and is formed by laminating PVC materials and stone powder, and part of high-end products can be provided with a PVC stabilizing layer on the bottom layer for increasing the upper and lower quality stability of the structure.
Although PVC has the advantages of high strength, wear resistance, corrosion resistance, heat insulation, sound insulation, flame retardance and the like, is often used for manufacturing floor materials, PVC materials have some disadvantages, such as release of harmful gases such as hydrogen chloride and the like in the production process, and a large amount of solid waste is produced to influence the physical health of people, however PVC materials are non-degradable materials, so that the waste after use cannot be completely degraded and can affect the environment, and in addition, PVC materials are easy to deform and embrittle in high-temperature and high-humidity environments and can affect the service life and performance of the PVC materials.
Disclosure of Invention
In view of the fact that the materials adopted by the stone plastic floor can influence the health of people and are not easy to degrade, the technical problem to be solved by the invention is to provide the degradable stone plastic floor without halogen elements.
In order to achieve the aim, the invention provides a degradable stone plastic floor which sequentially comprises a TPU layer, a modified PBAT stone plastic substrate and a TPU layer from top to bottom.
Preferably, the modified PBAT stone plastic substrate comprises the following components: 10-25wt% of PBAT resin, 0.01-5wt% of antibacterial agent, 0.01-1wt% of initiator, 55-85wt% of cobble powder, 0.001-1wt% of colorant, 0.01-9wt% of stabilizer and the balance of TPU.
Preferably, the production method of the antibacterial agent comprises the following steps:
step 1: dissolving 2-25g of silane coupling agent in 20-70mL of formaldehyde aqueous solution, then regulating the pH to 2-5 by using 0.1-1wt% acetic acid aqueous solution, stirring for 1-6h, adding 1-6g of toughening agent, homogenizing for 1-10min at the rotating speed of 10000-15000r/min, stirring for 20-35h at the temperature of 50-85 ℃, and centrifuging; the supernatant was retained by filtration.
Step 2: weighing 1-12 parts of hexamethylene guanidine hydrochloride, dissolving in 5-50mL of water, and carrying out ultrasonic treatment for 2-15min;
step 3: transferring the polyhexamethylene guanidine hydrochloride aqueous solution obtained in the step 2 into the supernatant obtained in the step 1, and stirring the mixed solution at 50-85 ℃ for 8-12h;
step 4: weighing 2-10 parts of chitosan powder, adding into 3-25 parts of 0.01-10wt% acetic acid aqueous solution, and stirring until the chitosan is completely dissolved to obtain chitosan-acetic acid aqueous solution;
step 5: stirring the chitosan-acetic acid aqueous solution obtained in the step 4, the mixed solution obtained in the step 3 and 2-15 parts of plasticizer at 50-85 ℃ for 6-10h, and drying to obtain the antibacterial agent.
Preferably, the silane coupling agent is any one of 2-ethyl acrylate, 1, 2-ethylenediamine, trimethoxy [2- [ 7-oxabicyclo [4.1.0] heptane-3-yl ] ethyl ] silane, a polymer of N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine and trimethoxy [3- (epoxyethylmethoxy) propyl ] silane, 3-glycidylpropyl (dimethoxy) methylsilane, and [8- (epoxypropyloxy) -N-octyl ] trimethoxysilane.
Preferably, the toughening agent is any one of 4- (1, 2-dihydroxy-1-methylethyl) -1-methylcyclohexane-1,2-diol, cis- (1S, 4S) -4- ((tert-butyldimethylsilyl) oxy) cyclohexan-1-ol, p-menthane-1, 2, 8-triol, 9 ci) -1- (3-hydroxy-1, 1-dimethylpropyl) -4-methyl-1, 2-cyclohexanediol.
Preferably, the concentration of the formaldehyde aqueous solution is 0.91mol/L.
The plasticizer is one of tri-n-butyl 2-acetyl-3-citrate, tri (octyl dodecanol) citrate and acetyl trioctyl citrate.
The stabilizer is any one of zinc oxide, diphenyl ketone, hydroquinone and thiobisphenol
The invention also discloses a preparation method of the degradable stone-plastic floor, which comprises the following steps:
s1: weighing the raw materials according to the formula, and preparing a modified PBTA stone plastic substrate through the procedures of high mixing, cold mixing, double screw extrusion, calendaring, traction and cutting;
s2: respectively stacking the TPU layer, the modified PBTA stone plastic substrate and the TPU layer from top to bottom in sequence, placing the materials in a press, and integrally forming and unloading;
s3: UV heat treatment: placing the product obtained in the step S2 into UV heating equipment for ultraviolet irradiation, and then passing through a hot water area at a temperature of 75-95 ℃ and a speed of 13.5-15.5m/min; the temperature of the cold water area is 15-40 ℃ and the speed is 16-20m/min;
s4: slotting by a multi-blade saw: the floors are orderly stacked on a tray, multi-blade sawing slotting is carried out according to specification requirements, and the temperature is controlled to be 10-25 ℃;
s5: standing: ensuring that the standing time is not less than 80 hours.
TPU layer: the uppermost TPU layer of the stone plastic floor needs to have the functions of skid resistance, water resistance, moisture resistance, oil resistance, wear resistance, impact resistance, extrusion resistance, aging resistance and the like. The TPU is a high polymer material and has the characteristics of wear resistance, oil resistance, aging resistance and the like; in the preparation of the stone-plastic floor, TPU is used as one of main raw materials of the stone-plastic floor, and can provide good wear resistance, so that the service life of the floor is prolonged. And does not contain halogen elements, and is beneficial to the health of human bodies; while the chemical structure of the TPU material is made up of a plurality of units, which can be connected to each other by chemical bonds. When the chemical bonds are destroyed, the material is degraded, thereby being beneficial to reducing the pollution to the environment of the stone-plastic floor.
The TPU layer after the PBAT stone plastic substrate is modified mainly plays a role in balancing and buffering, and simultaneously provides dampproof, mildew-proof and other performances. The quality of the TPU layer determines the flatness and stability of the stone-plastic floor, and in general, the smoother the bottom layer, the less likely the stone-plastic floor is deformed. Thus, a degradable TPU material with wear resistance, oil resistance and aging resistance is adopted as one of the raw materials of the stone-plastic floor. Meanwhile, the modified PBTA stone plastic substrate can be synthesized with PBAT resin and other raw materials.
Modified PBTA stone molded substrate: the stone-plastic substrate is an important component of the stone-plastic floor, provides good bearing performance and stability, and also needs to have the advantages of higher hardness, wear resistance and the like. The PBAT is biodegradable plastic, has good ductility and elongation at break, can be decomposed rapidly at normal temperature and normal pressure, and has good biodegradability, so that the modified PBAT stone plastic substrate can be used as one of stone plastic floor raw materials, and not only provides bearing function, but also can be degraded. Is an excellent raw material.
PBAT resin: the PBAT molecular chain contains aromatic rings and aliphatic chain segments, and has good mechanical strength, heat resistance and chemical corrosion resistance. As one of the raw materials for the modified PBTA stone-molded substrate.
And (3) an initiator: the initiator may decompose at high temperature to generate free radicals, thereby initiating a polymerization reaction or a crosslinking reaction. In the production process of the stone plastic floor, the initiator initiates the polymerization reaction or the crosslinking reaction of the PBAT resin and the TPU material, so that the fusion performance of the modified PBTA stone plastic base material is improved, the hardness and the wear resistance of the stone plastic floor are further improved, and the service life of the stone plastic floor is prolonged.
Cobble powder: the cobble powder is used as one of the components of the modified PBTA stone plastic base material. The cobblestone powder mainly contains calcium carbonate, is a natural inorganic material, and can provide the hardness and stability required by the stone-plastic floor, and also increase the abrasion resistance of the stone-plastic floor, so that the stone-plastic floor is more durable; the second cobblestone powder has higher density, can increase the weight of the stone plastic floor, so that the second cobblestone powder is more attached to the ground and is not easy to deform; the third cobblestone powder is not easy to burn, so that the fireproof performance of the stone-plastic floor can be improved.
Coloring agent: the colorant is used as one of the components of the modified PBTA stone-molded substrate. On one hand, the addition of the coloring agent can make the stone-plastic floor exhibit various colors and textures, so that the decorative performance of the stone-plastic floor is enhanced; on the other hand, the addition of the coloring agent can form a layer of protective film on the surface of the stone plastic floor, prevent external pollution and abrasion and prolong the service life of the floor.
Stabilizing agent: the stabilizer is used as one of the components of the modified PBTA stone plastic substrate and can react with the PBTA resin and the TPU, so that the oxidation process of the PBTA resin is slowed down, and the heat resistance and the ageing resistance of the PBTA resin are improved; in addition, the stabilizer can also improve the antibacterial and mildew-proof capacities of the stone plastic floor and prolong the service life of the stone plastic floor.
Silane coupling agent: the silane coupling agent can play a bridge role in the reaction of the toughening agent and the polyhexamethylene guanidine hydrochloride, so that the polyhexamethylene guanidine hydrochloride modified toughening agent can be obtained. The silane coupling agent may promote the dispersibility of the toughening agent in the PBAT material.
Aqueous formaldehyde solution: the aqueous methanol solution can provide a certain solubility, so that the silane coupling agent is uniformly dispersed in the aqueous methanol solution, thereby enhancing the dissolution effect and facilitating the subsequent use.
Aqueous acetic acid: silane coupling agents may hydrolyze or react with other materials in a strongly acidic or strongly basic environment, resulting in their failure. Therefore, in order to maintain the stability of the silane coupling agent, it is necessary to dissolve it in an environment having a certain acidity. The pH of the solution can be reduced after the aqueous acetic acid solution is added to maintain the pH within a suitable range, thereby avoiding the failure of the silane coupling agent. The purpose of adjusting the pH to 4 by adding an aqueous acetic acid solution is to maintain the stability and solubility of the silane coupling agent and to improve the service performance thereof.
In glacial acetic acid for dissolving chitosan, the chitosan is a multipolymer, and the molecular structure of the multipolymer contains a plurality of amino groups, hydroxyl groups and other polar groups, so that the aqueous solution of acetic acid can provide enough hydrogen ions, the stereoregularity among chitosan molecules is broken, and the chitosan molecules are expanded and are easy to dissolve, namely the multipolymer is taken as a dissolution solvent of chitosan.
Toughening agent: the silane coupling agent can react with the toughening agent, and the toughening agent modified by the silane coupling agent reacts with polyhexamethylene guanidine hydrochloride, so that the polyhexamethylene guanidine hydrochloride modified toughening agent can be obtained. Thereby increasing the performance of the toughening agent.
Polyhexamethylene guanidine hydrochloride: the polyhexamethylene guanidine hydrochloride has strong bacteriostasis, and after the polyhexamethylene guanidine hydrochloride is modified and toughened, the polyhexamethylene guanidine hydrochloride is added into the PBAT material, so that the mechanical property of the PBAT material can be improved, and the antibacterial property of the stone plastic floor can be endowed.
Water: water is used as a dissolution medium for dissolving polyhexamethylene guanidine hydrochloride.
Chitosan: the chitosan has the advantages of wide source, good film forming effect, good biocompatibility, biodegradability, bioactivity, bacteriostasis, antioxidation and the like. The chitosan and the polyhexamethylene guanidine hydrochloride modified toughening agent are blended to form the antibacterial agent together, so that the aging of the stone-plastic floor caused by oxidization can be reduced, and the service life of the floor is prolonged.
And (3) a plasticizer: the plasticizer can cut the interaction force between chitosan and polyhexamethylene guanidine hydrochloride modified toughening agent molecules, so that the melting temperature and melt viscosity of the polymer are reduced, and the performance of the antibacterial agent is improved. So that the stone-plastic floor is softer and more comfortable, and the impact resistance and crack resistance of the stone-plastic floor can be improved.
The antibacterial agent is prepared by grafting chitosan into the polyhexamethylene guanidine hydrochloride modified toughening agent, so that the antibacterial agent is endowed with antibacterial, antioxidation and other performances. And then preparing TPU, PBAT resin, an antibacterial agent, cobblestone powder, a colorant and a stabilizer into a modified PBAT stone plastic substrate by using an initiator, so that the stone plastic substrate can be endowed with various performances such as antibacterial, antioxidant, oil resistance, impact resistance, wear resistance and the like. Finally, the TPU layer, the modified PBAT stone plastic substrate and the TPU layer are sequentially produced and prepared through an SPC substrate production line from top to bottom.
The invention has the beneficial effects that:
1. compared with the prior art, the PVC material is not contained, and can be degraded, so that the health and environmental protection concepts of people are compounded.
2. Compared with the prior art, the composite floor is not prepared by using glue in the production process, but the stone plastic base material is modified, and the performances of the stone plastic floor, such as antibiosis, antioxidation, oil resistance, impact resistance, wear resistance, degradability and the like, are further improved by utilizing the antioxidation and antibiosis performances of chitosan and polyhexamethylene guanidine hydrochloride.
Detailed Description
Using parameters of specific chemicals, sources:
4- (1, 2-dihydroxy-1-methylethyl) -1-methylcyclohexane-1,2-diol, CAS:5581-31-7.
Cis- (1S, 4S) -4- ((tert-butyldimethylsilyl) oxy) cyclohex-1-ol, CAS:103202-62-6.
For menthane-1, 2, 8-triol, CAS:62014-81-7.
9 ci) -1- (3-hydroxy-1, 1-dimethylpropyl) -4-methyl-1, 2-cyclohexanediol, CAS:748142-70-3.
Ethyl 2-acrylate with 1, 2-ethylenediamine and trimethoxy [2- [ 7-oxabicyclo [4.1.0] heptan-3-yl ] ethyl ] silane, CAS:67674-62-8.
Polymer of N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine with trimethoxy [3- (epoxyethylmethoxy) propyl ] silane, CAS:51729-43-2.
3-glycidoxypropyl (dimethoxy) methylsilane, CAS:65799-47-5.
[8- (epoxypropyloxy) -n-octyl ] trimethoxysilane, CAS:1239602-38-0.
Cobble powder: particle size: 800 mesh.
Zinc oxide: model: LA-8Q, shandong Liang New Material technologies Co., ltd.
Polyhexamethylene guanidine hydrochloride, cat No.: s66524 Shanghai Source leaf Biotechnology Co., ltd.
2wt% of an aluminum oxide UV paint, CAS:1344-28-1, available from Hangzhou Jikang New Material Co., ltd.
PBAT resin, cat: HY-CM-6, a company of modern precision machinery, inc. of Wuhan.
TPU layer with thickness of 1mm and TPU layer with thickness of 0.2mm are obtained by conventional melting and die forming of TPU granules.
TPU particles, model: desmopan 3059D, manufacturer: covestro scientific (primordial Bayer).
Example 1:
a preparation method of a degradable stone-plastic floor comprises the following steps:
step 1, weighing according to the formula of the modified PBAT stone plastic base material: 10 kg of TPU, 90 kg of PBAT resin, 20 kg of antibacterial agent, 1 kg of initiator, 300 kg of cobble powder, 0.5 kg of colorant and 2 kg of stabilizer;
step 2, firstly, carrying out heat stirring on the raw materials in the weighing step 1 at 45rpm for 2min by a high-speed stirrer, and then stirring at 120rpm for 3min to ensure that the raw materials are stable to 120 ℃;
step 3: the raw materials after hot mixing in the step 2 are put into a horizontal stirrer to be stirred and dispersed at 45rpm, so that the temperature of the materials is cooled to 30 ℃;
step 4: pushing the raw materials subjected to cooling and stirring in the step 3 into a transition bin, then sending the raw materials into a double-screw extruder to be extruded through a blanking hopper, extruding the raw materials into a continuous sheet-shaped plate through a die, further calendering the plate through a three-roller calender, and finally pulling and cutting the plate to prepare the modified PBAT stone plastic base material;
step 5: respectively weighing a modified PBTA stone plastic substrate with the thickness of 1.2mm prepared in the TPU layer with the thickness of 1mm in the step 4, and sequentially stacking TPU layers with the thickness of 0.2mm from top to bottom, placing the TPU layers in a press, hot-pressing for 30min at the hot-pressing temperature of 135 ℃, and then controlling the cold-pressing temperature of 25 ℃ for 30min; finally, discharging;
step 6: UV heat treatment: spraying the product obtained in the step 5 to 30g/m 2 UV paint containing 2wt% alumina, then passed through a 700mJ/cm 2 Curing by an energy UV lamp to form a protective layer with the thickness of 0.2mm on the surface of the product; carrying out heat preservation treatment on the plate subjected to surface treatment by using warm water with the temperature of 90 ℃ and the speed of 13.5m/min and 40 ℃ through a hot water tank, wherein the speed is 12m/min, and finally controlling the temperature of the cooled material to 18 ℃ and the speed to 16m/min;
step 7: slotting by a multi-blade saw: the stone plastic floors are orderly stacked on a tray, multi-piece sawing slotting is carried out according to specification requirements, and the temperature is controlled at 15 ℃;
step 8: standing: the standing time is ensured to be 80h.
The production steps of the antibacterial agent are as follows:
a1: dissolving 10g of silane coupling agent in 50mL of formaldehyde aqueous solution with the concentration of 0.91mol/L, then adjusting the pH to 4 by using acetic acid aqueous solution with the concentration of 0.1mol/L, stirring for 5 hours, adding 4g of toughening agent, homogenizing for 2 minutes by using a high-shear dispersing emulsifier at the rotating speed of 15000r/min, stirring for 28 hours at the temperature of 75 ℃, centrifuging, filtering and retaining supernatant;
a2: 1g of polyhexamethylene guanidine hydrochloride is weighed and dissolved in 8mL of water, and ultrasonic treatment is carried out for 8min at 30 ℃ and 25 KHz;
a3: transferring the polyhexamethylene guanidine hydrochloride aqueous solution obtained in the step A2 into the supernatant obtained in the step 1, and stirring for 9 hours at 75 ℃ to obtain a mixed solution;
a4: weighing 3g of chitosan, adding the chitosan into 14mL of acetic acid aqueous solution with the mass fraction of 0.1, and stirring until the chitosan is completely dissolved to obtain chitosan-acetic acid aqueous solution;
a5: and (3) adding the solution obtained in the step (A4) into the mixed solution obtained in the step (A3), adding 2g of plasticizer, stirring for 7h at 55 ℃, and drying to obtain the antibacterial agent.
The initiator is dicumyl peroxide.
The colorant is titanium dioxide.
The stabilizer is zinc oxide.
The silane coupling agent is a polymer of N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine and trimethoxy [3- (epoxyethylmethoxy) propyl ] silane.
The toughening agent is 4- (1, 2-dihydroxyl-1-methylethyl) -1-methylcyclohexane-1, 2-diol.
The plasticizer is acetyl trioctyl citrate.
Example 2
This embodiment 2 is different from embodiment 1 in that: the silane coupling agent is 2-ethyl acrylate, 1, 2-ethylenediamine and trimethoxy [2- [ 7-oxabicyclo [4.1.0] heptane-3-yl ] ethyl ] silane.
Example 3
This embodiment 3 is different from embodiment 1 in that: the silane coupling agent is 3-glycidoxypropyl (dimethoxy) methylsilane.
Example 4
This embodiment 4 is different from embodiment 1 in that: the silane coupling agent is [8- (epoxypropyloxy) -n-octyl ] trimethoxy silane.
Example 5
This embodiment 5 is different from embodiment 1 in that: the toughening agent is menthane-1, 2, 8-triol.
Example 6
This embodiment 5 is different from embodiment 1 in that: the toughening agent is cis- (1S, 4S) -4- ((tert-butyldimethylsilyl) oxy) cyclohex-1-ol.
Example 7
This embodiment 5 is different from embodiment 1 in that: the toughening agent is 9 ci) -1- (3-hydroxy-1, 1-dimethylpropyl) -4-methyl-1, 2-cyclohexanediol.
Comparative example 1
This comparative example 1 is different from example 1 in that: the silane coupling agent in A1 is 7g, and the toughening agent is 7g.
Comparative example 2
This comparative example 2 is different from example 1 in that: no toughening agent is added in A1.
Comparative example 3
This comparative example 3 is different from example 1 in that: a1 is not added with a silane coupling agent.
Comparative example 4
This comparative example 4 is different from example 1 in that: a1 is not added with a silane coupling agent and a toughening agent.
Test example 1
Performance test:
warping after heating: the stone-plastic panels produced in examples 1 to 7 and comparative examples 1 to 4 were taken, respectively, and then the panels were cut into 240mm by 240mm panel samples, and then placed in a thermostatic oven, the temperature in the thermostatic oven was adjusted to 80 ℃, and the panels were placed under conditions of 25 ℃ and 50% rt for 24 hours, and the warp of the panel samples after heating was measured by calipers in mm.
Coefficient of thermal expansion (24 h): MD refers to the direction along the color film; CD means the direction perpendicular to the color film; the coefficient of thermal expansion is the ratio of the dimensional change of the floor as the temperature increases. The test temperature was 0-40 ℃.
Flexural strength: reference is made to GB/T9341-2008 in psi.
Smoke density: the dimensions were 25.4X25.4X4 mm, according to GB/T8627-2007 standard. The Smoke Density Rating (SDR) and Maximum Smoke Density (MSD) of the samples were tested by a construction smoke density tester. After the instrument is calibrated, a sample to be tested is placed in the center of a steel wire mesh, the sample is burnt by liquefied petroleum gas with a pressure value of 276KPa, three experiments are carried out for 4min each time, and SDR and MSD values of the sample after the three experiments can be calculated according to the curve of the light absorptivity and time of the sample. The smoke density grade SDR is lower than 26.9, meets the requirements of GB/T8627-2007 'method for testing the smoke density of combustion or decomposition of building materials' (SDR is less than or equal to 75), and has excellent flame retardance.
Table 1 shows the degradable stone-plastic flooring performance tests of examples 1-7 and comparative examples 1-4.
TABLE 1
Test example 2
Waterproof test: soaking a sample with the specification of 20 multiplied by 5mm in a water bath with room temperature (25 ℃) for 24 hours, and directly taking out and wiping to obtain the product from A= (M-M) 0 )/M 0 Calculating the water absorption rate by using a x 100, wherein A is the water absorption rate,%; m is the mass of the sample after wiping water, g; m is M 0 G is the initial mass of the sample.
Ultraviolet rapid aging test: the floor was placed in an aging test chamber and rotated at 60 c for 20 days to test the mass loss rate.
The composting method test can degrade: at 60 ℃, the prepared sample is buried in soil mixed with farmyard manure, waste vegetables, fallen leaves, excrement and the like for composting degradation experiment, and the experiment time is 90 days.
Antibacterial test: the antibacterial property test method and the antibacterial effect of the QB/T2591-2003 antibacterial plastic are adopted. Antibacterial test: the stone-plastic floors prepared in examples 1 to 7 and comparative examples 1 to 4 were each cut out into 50 mm. Times.50 mm. Times.4 mm samples, and subjected to an antibacterial test using Escherichia coli (Escherichia coli) ATCC25922 and Staphylococcus aureus (Staphylococcus) ATCC 6538.
Table 2 shows other performance tests of the degradable stone-plastic flooring of examples 1-7 and comparative examples 1-4.
TABLE 2
From the performance test data of tables 1 and 2, it can be seen that the products of example 1 are superior in performance to examples 2-7 and comparative examples 1-4 in all respects. Only different silane coupling agents were used in examples 1-4. It is possible that the properties of the degradable stone-plastic flooring are different in all respects due to the difference of the silane coupling agents, and the silane coupling agents in example 1 and example 2 are all block polymers, which have the characteristics of polymers such as larger molecular weight, solubility, reactivity, etc., and the silane coupling agents in examples 3 and 4 are small molecular weight silane coupling agents as compared with those in examples 1 and 2. And the silane coupling agent is a bridge capable of effectively combining the toughening agent and the polyhexamethylene guanidine hydrochloride. When the silane coupling agent with the block polymer is selected, the silane coupling agent of the high-molecular polymer can effectively improve the physical properties of the polymer and provide more sites due to longer molecular chains and more active groups, so that the toughening agent and the polyhexamethylene guanidine hydrochloride can be tightly combined, and the bonding effect can be improved. Thus, the degradable stone-plastic flooring prepared in example 1 and example 2 has better performance. The silane coupling agents of examples 1 and 2 were further compared to find that N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine and trimethoxy [3- (ethoxymethoxy) propyl ] silane had a greater number of substituents than ethyl 2-acrylate and 1, 2-ethylenediamine and trimethoxy [2- [ 7-oxabicyclo [4.1.0] heptan-3-yl ] ethyl ] silane, and thus N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine and trimethoxy [3- (ethoxymethoxy) propyl ] silane provided more active sites, i.e., the degradable stone plastic flooring prepared in example 1 was better in mechanical properties, degradability and antibacterial properties.
From the performance test data in tables 1 and 2, it can be seen that the product of example 1 is superior in performance to examples 5-7 in all respects. Examples 1 and 5-7 used only different toughening agents. It is possible that the different toughening agents can cause the different performances of the degradable stone-plastic floor in all aspects. First, the silane coupling agent is required to react with the hydroxyl groups contained in the toughening agent, and observing the number of hydroxyl groups contained in the different toughening agents used in examples 5-7 shows that the number of hydroxyl groups contained in the menthane-1, 2, 8-triol is smaller than four, and 4- (1, 2-dihydroxy-1-methylethyl) -1-methylcyclohexane-1,2-diol contains 4 hydroxyl groups, and cis- (1S, 4S) -4- ((tert-butyldimethylsilyl) oxy) cyclohex-1-ol contains one hydroxyl group, (9 ci) -1- (3-hydroxy-1, 1-dimethylpropyl) -4-methyl-1, 2-cyclohexanediol contains three hydroxyl groups, so that the number of hydroxyl groups contained in other toughening agents is smaller than four, and the 4- (1, 2-dihydroxy-1-methylethyl) -1-methylcyclohexane-1,2-diol can react with the silane coupling agent to form a stronger bond. Thus, the mechanical properties, degradability and antibacterial properties of example 1 are better.
From the performance test data in tables 1 and 2, it can be seen that the product of example 1 is superior in all respects to comparative examples 1-4. The possible reasons are that the silane coupling agent, the toughening agent or part of the antibacterial agent is not completely added, so that the silane coupling agent, the toughening agent, the polyhexamethylene guanidine hydrochloride and the chitosan are unreacted or the various factors such as incomplete reaction affect the various performances of the degradable stone-plastic floor.
Claims (9)
1. The utility model provides a degradable stone plastic floor which characterized in that: the modified PBAT plastic substrate comprises a TPU layer, a modified PBAT stone plastic substrate and a TPU layer from top to bottom.
2. The degradable stone-plastic floor of claim 1, wherein the modified PBAT stone-plastic substrate comprises the following components: 10-25wt% of PBAT resin, 0.01-5wt% of antibacterial agent, 0.01-1wt% of initiator, 55-85wt% of cobble powder, 0.001-1wt% of colorant, 0.01-9wt% of stabilizer and the balance of TPU.
3. The degradable stone-plastic floor according to claim 2, wherein the production method of the antibacterial agent comprises the following steps:
step 1: dissolving 2-25g of silane coupling agent in 20-70mL of formaldehyde aqueous solution; then adjusting the pH to 2-5 with 0.1-1wt% acetic acid aqueous solution, stirring for 1-6h, adding 1-6g of toughening agent, homogenizing for 1-10min at the rotation speed of 10000-15000 r/min; stirring at 50-85deg.C for 20-35 hr, and centrifuging; filtering to retain supernatant;
step 2: weighing 1-12 parts of hexamethylene guanidine hydrochloride, dissolving in 5-50mL of water, and carrying out ultrasonic treatment for 2-15min;
step 3: transferring the polyhexamethylene guanidine hydrochloride aqueous solution obtained in the step 2 into the supernatant obtained in the step 1, and stirring for 8-12 hours at 50-85 ℃ to obtain a mixed solution;
step 4: weighing 2-10 parts of chitosan, adding into 3-25 parts of 0.01-10wt% acetic acid aqueous solution, and stirring until the chitosan is completely dissolved to obtain chitosan-acetic acid aqueous solution;
step 5: stirring the chitosan-acetic acid aqueous solution obtained in the step 4, the mixed solution obtained in the step 3 and 2-15 parts of plasticizer at 50-85 ℃ for 6-10h, and drying to obtain the antibacterial agent.
4. A degradable stone-plastic floor as claimed in claim 3, characterized in that: the silane coupling agent is any one of polymer of 2-ethyl acrylate, 1, 2-ethylenediamine, trimethoxy [2- [ 7-oxabicyclo [4.1.0] heptane-3-yl ] ethyl ] silane, N- [3- (trimethoxysilyl) propyl ] -1, 2-ethylenediamine and trimethoxy [3- (epoxy ethylmethoxy) propyl ] silane, 3-glycidylpropyl (dimethoxy) methylsilane and [8- (epoxy propyloxy) -N-octyl ] trimethoxysilane.
5. A degradable stone-plastic floor as claimed in claim 3, characterized in that: the toughening agent is any one of 4- (1, 2-dihydroxyl-1-methylethyl) -1-methylcyclohexane-1,2-diol, cis- (1S, 4S) -4- ((tert-butyldimethylsilyl) oxy) cyclohexan-1-ol, menthane-1, 2, 8-triol and 9 ci) -1- (3-hydroxy-1, 1-dimethylpropyl) -4-methyl-1, 2-cyclohexanediol.
6. A degradable stone-plastic floor as claimed in claim 3, characterized in that: the concentration of the formaldehyde aqueous solution is 0.91mol/L.
7. A degradable stone-plastic floor as claimed in claim 3, characterized in that: the plasticizer is 2-acetyl-3-tri-n-butyl citrate, tri (octyl dodecanol) citrate and acetyl trioctyl citrate.
8. The degradable stone-plastic flooring of claim 2, wherein: the stabilizer is any one of zinc oxide, diphenyl ketone, hydroquinone and thiobisphenol.
9. A method for preparing a degradable stone-plastic floor according to any one of claims 1-8, comprising the steps of:
s1: weighing the raw materials according to the formula, and preparing a modified PBTA stone plastic substrate through the procedures of high mixing, cold mixing, double screw extrusion, calendaring, traction and cutting;
s2: respectively stacking the TPU layer, the modified PBTA stone plastic substrate and the TPU layer from top to bottom in sequence, placing the materials in a press, and integrally forming and unloading;
s3: UV heat treatment: placing the product obtained in the step S2 into UV heating equipment for ultraviolet irradiation, and then placing the product in a hot water area at a temperature of 75-95 ℃ and a speed of 13.5-15.5m/min; the temperature of the cold water area is 15-40 ℃ and the speed is 16-20m/min;
s4: slotting by a multi-blade saw: the floors are orderly stacked on a tray, multi-blade sawing slotting is carried out according to specification requirements, and the temperature is controlled to be 10-25 ℃;
s5: standing: ensuring that the standing time is not less than 80 hours.
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