CN114196109B - Polypropylene odor adsorption master batch and preparation method thereof - Google Patents
Polypropylene odor adsorption master batch and preparation method thereof Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/10—Homopolymers or copolymers of propene
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Abstract
The invention discloses a polypropylene odor adsorption master batch and a preparation method thereof, and belongs to the technical field of plastic materials. According to the invention, the modified diatomite is introduced into the components to serve as an odor adsorption effect component, meanwhile, the fluidity of the matrix polypropylene resin and the types of compatilizers are optimized, so that the odor adsorption effect component is uniformly dispersed in the master batch, and the obtained product can effectively adsorb various organic molecular substances, and has obvious odor removal effect when being used in automobile parts. The invention also discloses a preparation method of the polypropylene odor adsorption master batch and application of the polypropylene odor adsorption master batch in preparation of automobile parts.
Description
Technical Field
The invention relates to the technical field of plastic materials, in particular to a polypropylene odor adsorption master batch and a preparation method thereof.
Background
In recent years, pollution events in various automobile rooms are frequent, and consumers have strong demands on the health links in the automobiles. The problem of air pollution in vehicles has become an indoor environment pollution problem which is the third greatest hazard to human health after decoration and furniture pollution in China and PM2.5 pollution in indoor environments. In general, in-car air quality problems are mainly toxic substances released from automotive interior materials, and unpleasant odors are emitted, which have a direct relation with vehicle manufacturing processes and parts, and affect relatively large automobile instrument panel assemblies, door trim panels, carpets, ceilings, automobile harnesses, seat assemblies, and the like. The parts are generally made of the color-mixed polypropylene plastic, and although the emission characteristics of the polypropylene are greatly improved through formula adjustment and process adjustment in the prior art, no related research exists in the aspect of related processing raw material master batches, and most of products which are directly mixed with the polypropylene and injection molded by master batches have high odor and have adverse effects on the overall vehicle emission.
Diatomite is a biogenic siliceous sedimentary rock, has the characteristics of light weight, porosity and large specific surface area, has high melting point and chemical stability, has certain surface charge, and can be used for adsorbing various metal ions, organic compounds, high-molecular polymers and the like; on the other hand, the diatomite has rich resources, the price of the raw materials is only half of that of the activated carbon, and the cost performance is high. However, the natural diatomite mineral raw material has poor adsorption performance of odor molecules, and is difficult to adsorb organic small molecules containing odor in various materials, meanwhile, the adsorption efficiency of macromolecular substances compounded with resin is often reduced by more than 50% because the organic small molecules are easy to agglomerate in a resin matrix, and the organic small molecules cannot be temporarily applied to preparing polyolefin (especially polypropylene) odor adsorption master batches.
Disclosure of Invention
Based on the defects existing in the prior art, the invention aims to provide the polypropylene odor adsorption master batch, modified diatomite is introduced into components to serve as an odor adsorption effect component, meanwhile, the fluidity of the matrix polypropylene resin and the types of compatilizers are optimized, so that the odor adsorption effect component is uniformly dispersed in the master batch, and the obtained product can effectively adsorb various organic molecular substances and has obvious odor removal effect when being used in automobile parts.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the polypropylene odor adsorption master batch comprises the following components in parts by weight:
35-55 parts of polypropylene resin, 40-60 parts of polyacrylamide modified diatomite, 3-5 parts of compatilizer, 0.5-5 parts of heat stabilizer and 0.5-5 parts of processing aid;
the melt flow rate of the polypropylene resin at 230 ℃ under the condition that 2.16kg accords with 20-50 g/10min, and the melt flow rate is tested according to ASTMD 1238-2011;
the compatilizer is hyperbranched epoxy polyester.
In the polypropylene odor adsorption master batch, the diatomite modified by the polyacrylamide not only maintains the original surface charge property of the diatomite, but also can effectively adsorb various organic high molecular substances and other impurities, and can further adsorb odor small molecular organic substances, so that the adsorption effect is obviously improved; meanwhile, through the polypropylene resin with specific melt flow rate (the melt flow rate of the polypropylene resin has larger influence on the performance of the product, if the melt flow rate is too small, the fluidity is insufficient, the processability is low, the compatibility with the components is very poor, the uniform distribution of other components is difficult to realize, and if the melt flow rate is too large, the mechanical property of the prepared product is obviously reduced, the application range is also reduced, and the modified diatomite can be obviously improved, and the adsorption efficiency is ensured, if the modified diatomite is particularly difficult to be applied to automobile parts with certain requirements on the mechanical property) as a matrix, and is matched with the preferable hyperbranched epoxy polyester as the compatibility, so that the compatibility between the components is obviously improved, and the modified diatomite can be uniformly dispersed in the preparation and application processes of the product.
Preferably, the particle size of the polyacrylamide modified diatomite is 250-500 meshes.
Preferably, the preparation method of the polyacrylamide modified diatomite comprises the following steps:
(1) Preparing polyacrylamide solution from polyacrylamide by deionized water, and adding sodium hydroxide to carry out hydrolysis reaction to obtain hydrolyzed solution;
(2) Adding baked and dried diatomite into the hydrolyzed solution, fully soaking, filtering and drying to obtain the polyacrylamide modified diatomite;
more preferably, the mass percentage of the polyacrylamide in the polyacrylamide solution is 1-10%, and the mass ratio of the polyacrylamide to the sodium hydroxide is (0.9-1.1): (0.9-1.1), wherein the temperature of the hydrolysis reaction is 40-60 ℃ and the time is 4-5 h.
Under the conditions, the polyacrylamide can be effectively hydrolyzed, meanwhile, the consistency of the hydrolyzed solution is improved, the hydrolyzed solution is more favorable for uniformly modifying and adhering to diatomite, the sodium hydroxide content is too high, the reaction conditions are too severe, the hydrolysis degree of the polyacrylamide can not be continuously improved, and the raw material waste and the safety problem are caused.
More preferably, the mass ratio of the hydrolyzed solution to diatomaceous earth is 1 (0.002-0.012).
On the one hand, if the proportion of the diatomite is too small in the reaction, the unit surface modification degree of the diatomite is too high, the porosity of the diatomite is reduced, the specific surface area is reduced, and the physical adsorption capability of the diatomite on some macromolecular organic substances is weakened; on the other hand, if the diatomite proportion is too high, accumulation is likely to occur during soaking modification, surface modification is uneven, and the adsorption efficiency of the product is lowered. Through experimental screening of the inventor, the polyacrylamide modified diatomite prepared by the above proportion has the best effect.
More preferably, the diatomaceous earth has a particle size of 300 to 500 mesh.
The inventors have found after the experiment that although the difference between the particle size of the diatomaceous earth before and after the modification and the particle size of the final product is not large, the particle size of the diatomaceous earth before the modification has an influence on the odor adsorption effect of the polyacrylamide modified diatomaceous earth obtained after the modification and the final product prepared, and in the above range, the odor adsorption effect of the product is optimal.
Preferably, the hyperbranched epoxy polyester is obtained by catalytic polymerization reaction of an AB2 monomer and trimellitic anhydride, and the molecular weight of the hyperbranched epoxy polyester is 3000-6000;
more preferably, the preparation method of the hyperbranched epoxy polyester comprises the following steps:
(1) Uniformly mixing trimellitic anhydride and ethylene glycol, adding phosphoric acid as a catalyst, and reacting for 8-10 hours at 130-160 ℃ to obtain an AB2 type monomer; the mole ratio of the trimellitic anhydride to the glycol is (0.9-1.1): (0.9 to 1.1);
(2) Adding trimellitic anhydride into the AB2 type monomer, keeping the temperature for reaction for 1-3 hours, and finally adding epoxy chloropropane for keeping the temperature for reaction for 1-3 hours to obtain the hyperbranched epoxy polyester;
more preferably, the molar ratio of the AB2 type monomer to the trimellitic anhydride in the step (2) is (6-12): 1, wherein the molar ratio of the AB2 type monomer to the epichlorohydrin is (0.9-1.1): (0.9-1.1).
The inventor tries for many times, the macromolecular hyperbranched epoxy polyester prepared by the preparation method can effectively improve the compatibility of the polyacrylamide modified diatomite in the product components after being matched with a specific polypropylene resin matrix and uniformly disperse the macromolecular hyperbranched epoxy polyester in the obtained polypropylene odor adsorption master batch, the existing common macromolecular compatilizer is difficult to achieve the same effect, and the obtained product has higher yield by adopting the preferable technical parameters.
Preferably, the heat stabilizer is at least one of a phenolic heat stabilizer, an amine heat stabilizer, a phosphite heat stabilizer, a complex heat stabilizer of an acryl functional group and a thioester, and a calixarene heat stabilizer.
Preferably, the processing aid is at least one of a lubricant and a weather-resistant agent.
The invention also aims to provide a preparation method of the polypropylene odor adsorption master batch, which comprises the following steps: and mixing the polypropylene resin, the polyacrylamide modified diatomite, the compatilizer, the heat stabilizer and the processing aid, and then carrying out melt extrusion granulation to obtain the polypropylene odor adsorption master batch.
The preparation method of the polypropylene odor adsorption master batch has simple operation steps and can realize industrial mass production.
Preferably, the temperature at the time of melt extrusion is 190 to 240 ℃.
It is still another object of the present invention to provide the use of the polypropylene odor adsorbing masterbatch in the preparation of automotive parts.
The polypropylene odor adsorption master batch disclosed by the invention has extremely high odor adsorption performance, can realize a good adsorption effect under the condition that the addition amount is 1-5wt% when being applied to the preparation of various polypropylene matrix automobile parts with different properties, and obviously reduces the odor of the obtained product.
The invention has the beneficial effects that the invention provides the polypropylene odor adsorption master batch, the modified diatomite is introduced into the components to serve as the odor adsorption effect component, meanwhile, the fluidity of the matrix polypropylene resin and the types of the compatilizer are optimized, so that the odor adsorption effect component is uniformly dispersed in the master batch, and the obtained product can effectively adsorb various organic molecular substances, and has obvious odor removal effect when being used in automobile parts. The invention also provides a preparation method of the polypropylene odor adsorption master batch and application of the polypropylene odor adsorption master batch in preparation of automobile parts.
Detailed Description
The present invention will be further described with reference to specific examples and comparative examples for better illustrating the objects, technical solutions and advantages of the present invention, and the object of the present invention is to be understood in detail, not to limit the present invention. All other embodiments, which can be made by those skilled in the art without the inventive effort, are intended to be within the scope of the present invention. The experimental reagents and instruments designed for the implementation of the invention are common reagents and instruments unless otherwise specified.
Examples 1 to 8
In the embodiment of the polypropylene odor adsorption master batch and the preparation method thereof, the components of the polypropylene odor adsorption master batch are shown in table 1.
TABLE 1
The preparation method of the polypropylene odor adsorption master batch comprises the following steps: and mixing the polypropylene resin, the polyacrylamide modified diatomite, the compatilizer, the heat stabilizer and the processing aid, and then carrying out melt extrusion granulation to obtain the polypropylene odor adsorption master batch.
The polypropylene resin 1 is a PP EP548R product produced by medium petrochemical production, and the melt flow rate of the polypropylene resin at 230 ℃ under the condition that 2.16kg is consistent is 20g/10min;
the polypropylene resin 2 is a PP K7760H product produced by medium petrochemical industry, and the melt flow rate of the polypropylene resin at 230 ℃ under the condition that 2.16kg is consistent is 50g/10min;
the polyacrylamide modified diatomite 1 is self-made, and the preparation steps are as follows:
(1) Preparing a polyacrylamide solution with the weight percent of 5% from commercially available polyacrylamide by deionized water, adding sodium hydroxide, and reacting for 5 hours at 50 ℃ to carry out hydrolysis reaction to obtain a hydrolyzed solution; the mass ratio of the polyacrylamide to the sodium hydroxide is 1:1;
(2) Adding commercial diatomite (with the average grain size of 400 meshes) subjected to baking and drying (baking and drying at 550 ℃ for 2 hours) into the hydrolyzed solution, soaking for more than 10 hours, filtering and drying at 40 ℃ to obtain the polyacrylamide modified diatomite with the grain size of 350 meshes; the mass ratio of the hydrolyzed solution to the diatomite is 1:0.008.
The polyacrylamide modified diatomite 2 is self-made, and the preparation steps are different from those of the polyacrylamide modified diatomite 1 only in that the average particle size of the commercially available diatomite is 200 meshes, and the particle size of the polyacrylamide modified diatomite 2 is 170 meshes;
the polyacrylamide modified diatomite 3 is self-made, and the preparation steps are different from those of the polyacrylamide modified diatomite 1 only in that the average particle size of the commercially available diatomite is 800 meshes, and the particle size of the polyacrylamide modified diatomite 3 is 600 meshes;
the compatilizer 1 is self-made hyperbranched epoxy polyester with the molecular weight of 5500, and the preparation method of the hyperbranched epoxy polyester comprises the following steps:
(1) Uniformly mixing trimellitic anhydride and ethylene glycol according to a molar ratio of 1:1, adding a small amount of phosphoric acid as a catalyst, and reacting for 10 hours at 150 ℃ to obtain an AB2 type monomer; the molar ratio of the trimellitic anhydride to the ethylene glycol is 1:1;
(2) Adding trimellitic anhydride into the AB2 type monomer, keeping the temperature for reaction for 2 hours, and finally adding epoxy chloropropane for keeping the temperature for reaction for 2 hours to obtain the hyperbranched epoxy polyester; the molar ratio of AB2 type monomer to trimellitic anhydride is 8:1, wherein the molar ratio of the AB2 type monomer to the epichlorohydrin is 1:1, and the yield of the obtained product is 78%.
The heat stabilizer is a phosphite ester heat stabilizer sold in the market;
the processing aid is magnesium stearate, a commercially available lubricant.
Comparative examples 1 to 5
The comparative examples differ from example 3 only in the raw materials used and the proportions shown in table 2, the specific raw materials used comprising the following:
the polypropylene resin 3 is a polypropylene product produced by medium petrochemical production, and the melt flow rate of the polypropylene resin at 230 ℃ under the condition that 2.16kg is consistent is 15g/10min;
the compatilizer 2 is 1001CN product produced by Strukol;
the compatilizer 3 is Bynel5000 product produced by Strukol;
the organic silica gel powder is a silica gel powder product produced by Daqingbao seal character company, and the average aperture is 1000A degrees;
the diatomite is a commercial product, and the grain size is 300-500 meshes;
except for the above specific description, other raw materials used and raw materials used in each example are the same commercial products or homemade products.
TABLE 2
Effect example 1
The products obtained in examples 1 to 8 and comparative examples 1 to 5 were subjected to performance testing, and each product was applied to the preparation of polypropylene base products, comprising the steps of:
in order to simulate the production of actual polypropylene automobile parts, 100 parts of polypropylene resin is taken, the polypropylene resin is placed into a double screw extruder at 190-240 ℃ for melt extrusion granulation, 3wt% of master batch products obtained in each example or comparative example are respectively added during melt extrusion, and the obtained products are subjected to project test; the polypropylene resin is a polypropylene EP548R product produced by medium petrochemical industry;
the project toilet was a smell grade test, which was performed according to the standard of the public standard PV 3900 smell grade-2000, and the test results are shown in table 3.
TABLE 3 Table 3
As can be seen from Table 3, when the product of each embodiment of the invention is applied to the preparation of polypropylene automobile parts, the odor grade of the obtained product can be effectively reduced, the odor grade of each product is less than or equal to 3.5, and as the content of the polyacrylamide modified diatomite in the polypropylene odor adsorption master batch is gradually increased, the odor grade is reduced to the grade 3 described in embodiment 3, but the inventor experiment shows that the master batch product is difficult to be finally molded due to the continuous increase of the content of the polyacrylamide modified diatomite, so that the addition part of the polyacrylamide modified diatomite is most suitable for 40-60 parts; from examples 4 and 5, it can be seen that the hyperbranched epoxy polyester is used as the compatilizer to effectively improve the component compatibility of the product, and the ideal effect can be achieved only by adding a small amount, while the performance of the product is not obviously improved by excessively increasing the addition amount of the compatilizer; as can be seen from the products obtained in examples 7 and 8, the particle size of the starting material diatomaceous earth selected from the polyacrylamide-modified diatomaceous earth in the composition also has an effect on the odor adsorption properties of the product. According to the comparison of the performances of the three products of the example 3 and the comparative examples 1-2, the effect of selecting unmodified diatomite or the conventional commercially available common adsorption filler is not as good as that of the polyacrylamide modified diatomite, but according to the comparative examples 3-5, besides the effective odor adsorption effect components, the types of the polypropylene resin and the compatilizer directly influence the compatibility and the dispersion condition of each component in the product, and further influence the odor adsorption performance of the product.
In order to further verify the practical application diversity of the polypropylene odor adsorption master batch according to the invention, the product of example 3 with the best odor grade was used for injection molding polypropylene products:
in order to simulate the production of actual polypropylene automobile parts, 100 parts of modified polypropylene resin is respectively added with 1wt percent, 3wt percent and 5wt percent of the polypropylene odor adsorption master batch product obtained in the example 3 to be melted and injection molded at 210 ℃ to obtain a product, and meanwhile, a control group without addition is arranged, and the obtained product is subjected to the same odor grade test; the modified polypropylene resin is a polypropylene EP548R product produced by medium petrochemical industry; the results are shown in Table 4.
TABLE 4 Table 4
| Polypropylene odor adsorption masterbatch addition (wt%) | 1 | 3 | 5 | 0 |
| Odor grade (grade) | 3.8 | 3.5 | 3 | 4.5 |
As can be seen from table 4, the polypropylene odor adsorption master batch of the present invention also has significant odor adsorption performance when applied to injection molded polypropylene products.
Furthermore, the product of example 3, with the best odor rating, was used for spinning polypropylene products:
in order to simulate the production of actual polypropylene automobile parts, 100 parts of modified polypropylene resin is respectively added with 1wt percent, 2wt percent and 4wt percent of the polypropylene odor adsorption master batch product obtained in the example 3 to be melted and spun at 200 ℃ to obtain a product, and meanwhile, a control group without addition is arranged, and the obtained product is subjected to the same odor grade test; the modified polypropylene resin is a polypropylene T30S product produced by medium petrochemical industry; the results are shown in Table 5.
TABLE 5
| Polypropylene odor adsorption masterbatch addition (wt%) | 1 | 2 | 4 | 0 |
| Odor grade (grade) | 4 | 3.8 | 3.5 | 4.5 |
As can be seen from Table 5, the polypropylene odor adsorbing master batch of the present invention is equally applicable to spun polypropylene products.
Example 9
To verify the effect of the addition ratio of the polyacrylamide solution and the diatomite after hydrolysis in the preparation process of the polyacrylamide modified diatomite in the invention on the performance of the final product, a control system with different diatomite addition amounts is provided, the parameters are shown in table 6, the parameters are different from those in table 6, the other parameters are the same as those in example 3, the obtained product is subjected to odor grade test by using the same application (polypropylene odor adsorption master batch obtained by adding in the melt extrusion process) and the test method in effect example 1, and the results are shown in table 6.
TABLE 6
As can be seen from Table 6, the amount of diatomite added during the surface modification of diatomite is not as high as possible, and if the diatomite content is too low or too high, the odor level of the final product in application is reduced, and the product effect is optimal when the mass ratio of the hydrolyzed solution to diatomite is 1 (0.002-0.012) after screening.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. The polypropylene odor adsorption master batch is characterized by comprising the following components in parts by weight:
35-55 parts of polypropylene resin, 40-60 parts of polyacrylamide modified diatomite, 3-5 parts of compatilizer, 0.5-5 parts of heat stabilizer and 0.5-5 parts of processing aid;
the melt flow rate of the polypropylene resin at 230 ℃ under the condition of 2.16kg is 20-50 g/10min;
the compatilizer is hyperbranched epoxy polyester, and the molecular weight is 3000-6000; the hyperbranched epoxy polyester is prepared by the catalytic polymerization reaction of AB2 type monomer and trimellitic anhydride through epichlorohydrin, and the preparation method of the hyperbranched epoxy polyester comprises the following steps:
(1) Uniformly mixing trimellitic anhydride and ethylene glycol, adding phosphoric acid as a catalyst, and reacting at 130-160 ℃ for 8-10 hours to obtain an AB2 type monomer; the mole ratio of the trimellitic anhydride to the glycol is (0.9-1.1): (0.9 to 1.1):
(2) Adding trimellitic anhydride into the AB2 type monomer, continuously preserving heat for reaction for 1-3 hours, and finally adding epoxy chloropropane for continuously preserving heat for reaction for 1-3 hours to obtain hyperbranched epoxy polyester; the molar ratio of the AB2 type monomer to the trimellitic anhydride is (6-12): 1, wherein the molar ratio of the AB2 type monomer to the epichlorohydrin is (0.9-1.1): (0.9 to 1.1);
the preparation method of the polyacrylamide modified diatomite comprises the following steps:
(1) Preparing polyacrylamide solution from polyacrylamide by deionized water, and adding sodium hydroxide to carry out hydrolysis reaction to obtain hydrolyzed solution;
(2) Adding baked and dried diatomite into the hydrolyzed solution, fully soaking, filtering and drying to obtain the polyacrylamide modified diatomite;
the mass percentage of polyacrylamide in the polyacrylamide solution is 1-10%, and the mass ratio of the polyacrylamide to the sodium hydroxide is (0.9-1.1): (0.9-1.1), wherein the temperature of the hydrolysis reaction is 40-60 ℃ and the time is 4-5 h; the mass ratio of the hydrolyzed solution to the diatomite is 1 (0.002-0.012).
2. The polypropylene odor adsorption master batch of claim 1, wherein the particle size of the polyacrylamide modified diatomaceous earth is 250-500 mesh.
3. The polypropylene odor absorbing masterbatch of claim 1 wherein said heat stabilizer is at least one of a phenolic heat stabilizer, an aminic heat stabilizer, a phosphite heat stabilizer, a complex of an acryl functional group and a thioester, a calixarene heat stabilizer; the processing aid is at least one of a lubricant and a weather-proof agent.
4. A method for preparing a polypropylene odor adsorption master batch according to any one of claims 1 to 3, comprising the steps of: and mixing the polypropylene resin, the polyacrylamide modified diatomite, the compatilizer, the heat stabilizer and the processing aid, and then carrying out melt extrusion granulation to obtain the polypropylene odor adsorption master batch.
5. Use of the polypropylene odor adsorption master batch according to any one of claims 1 to 3 for the preparation of automotive parts.
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