CN109401060B - Preparation method of aramid polyacrylamide β nucleating agent - Google Patents
Preparation method of aramid polyacrylamide β nucleating agent Download PDFInfo
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Abstract
The invention relates to a preparation method of an aramid polypropylene β nucleating agent, belonging to the field of modification of polymer additives and providing a preparation method of an aramid polypropylene β nucleating agent, which comprises the steps of firstly dissolving the existing aramid polypropylene β nucleating agent by adopting a solvent sulfuric acid at room temperature or at 60-200 ℃ to obtain a nucleating agent solution, then precipitating the nucleating agent in the nucleating agent solution by utilizing an anti-solvent to obtain a suspension or emulsion, and finally drying the solid obtained by filtering the suspension or the emulsion to obtain the modified aramid polypropylene β nucleating agent.
Description
Technical Field
The invention relates to a preparation method of an aramid polypropylene β nucleating agent, belonging to the field of modification of polymer additives.
Background
The polypropylene material mainly comprising β crystal (including PP-based composite material) has higher impact strength and ductility than α type PP material, and has higher heat deformation temperature and larger rigidity than rubber modified PP composite material, therefore, α 0 type polypropylene is a polypropylene variety with wider application range, the method for obtaining α type polypropylene mainly comprises quenching method, temperature gradient method, shearing or stretching deformation method and β nucleating agent adding method, wherein β nucleating agent adding method is the most effective and best implemented method for obtaining PP with high content of β crystal, the polypropylene β nucleating agent widely used in industry mainly comprises dicyclohexyl terephthalamide (TMB-5 or DCHT), N' -dicyclohexyl-1, 6-naphthamide (NJS or NU100) and rare earth β nucleating agent (WBG and II), wherein the former two are better nucleating agents, aromatic amides β (including TMB series, such as TMB-5 series, NJS or NU100) and rare earth β nucleating agent (WBG and II), the former two are better nucleating agents, the aromatic amides β nucleating agent is better, the white polyamide nucleating agent is better (including TMB-5 series, the white polyamide nucleating agent) and the white polyamide nucleating agent is better than the polypropylene nucleating agent which is a high-white polyamide nucleating agent, the white polyamide nucleating agent which is better, the polypropylene nucleating agent is suitable for forming, the polypropylene film, the high-white polyamide nucleating agent is suitable for forming, the high-white polyamide film forming method is a high-white polyamide film forming method, the high-white polyamide nucleating agent is good for the high-white polyamide film forming method, the high-resistant polypropylene film is good for the high-resistant polypropylene film forming method of the high-resistant polypropylene film forming method, the high-resistant polypropylene film is.
Disclosure of Invention
The invention aims to provide a preparation method of an aramid polypropylene β nucleating agent, which can be used for preparing polypropylene β nucleating agents with various shapes and sizes, namely the shape and the size of the aramid polypropylene β nucleating agent can be regulated and controlled by the method.
The technical scheme of the invention is as follows:
the first technical problem to be solved by the invention is to provide a preparation method of an aramid polypropylene β nucleating agent, which comprises the steps of firstly dissolving the existing aramid polypropylene β nucleating agent by using solvent sulfuric acid at room temperature or at 60-200 ℃ to obtain a nucleating agent solution, then precipitating the nucleating agent in the nucleating agent solution by using an anti-solvent to obtain a suspension or emulsion, and finally drying the solid obtained by filtering the suspension or emulsion to obtain the modified aramid polypropylene β nucleating agent.
Further, the solvent sulfuric acid is sulfuric acid with mass concentration of more than 37%.
Further, the anti-solvent is deionized water (H)2O), ethanol (C)2H5OH), dimethyl sulfoxide (DMSO), N' -Dimethylformamide (DMF), dichloromethane, chloroform, methanol, benzene or xylene, and the like. In the invention, the non-solvent is other than concentrated sulfuric acid, and the chemical structure of the aramid nucleating agent is not changedThe solvent of (1).
In the invention, the dosage of the solvent sulfuric acid ensures that the nucleating agent of the aramid polypropylene β is completely dissolved, and the dosage of the anti-solvent ensures that the nucleating agent of the aramid polypropylene β is almost completely separated out or most of the nucleating agent is separated out.
Further, the mass ratio of the sulfuric acid to the existing aramid polypropylene β nucleating agent is 50-1000 parts by weight of sulfuric acid and 1-50 parts by weight of existing aramid polypropylene β nucleating agent, and preferably 200-350 parts by weight of sulfuric acid and 10-20 parts by weight of existing aramid polypropylene β nucleating agent.
Further, the mass ratio of the anti-solvent to the existing aromatic amide-based polypropylene β nucleating agent is 200-5000 parts by weight of the anti-solvent and 1 part by weight of the existing aromatic amide-based polypropylene β nucleating agent.
In the invention, the anti-solvent is utilized to immediately separate out the nucleating agent in the nucleating agent solution to obtain suspension or emulsion; that is, the nucleating agent precipitates while the anti-solvent is added.
Further, the method for separating out the nucleating agent in the nucleating agent solution by using the anti-solvent to obtain the suspension or the emulsion comprises the following steps: the nucleator solution was slowly poured into the anti-solvent and rapidly stirred to dissipate heat. In the invention, the rapid stirring speed is only required to prevent bumping caused by uneven heat dissipation when the solution is mixed, and the stirring can be generally carried out for 8-20 min, so that the stirring is carried out for uniform heat dissipation and convenient for subsequent filtration.
Further, in the above method, the suspension or emulsion may be filtered, washed with the same anti-solvent until neutral, and then dried.
Further, the sulfuric acid is selected from one of fuming sulfuric acid, concentrated sulfuric acid (mass concentration is more than 70 percent) and medium-concentration sulfuric acid. In the present invention, sulfuric acid having a mass concentration of more than 37% can be used.
The invention firstly indicates that the sulfuric acid with the mass concentration of more than 37 percent is used as the solvent of the aramid PP β nucleating agent, so that the high-concentration dissolution at room temperature is realized, and simultaneously, the chemical structure of the aramid PP β can be ensured not to be changed or the nucleating performance is not changed or improved.
Further, in the preparation method of the aramid polypropylene β nucleating agent, different anti-solvents are selected to regulate and control the crystal form and/or shape of the obtained modified aramid polypropylene β nucleating agent, and the specific regulation and control mode is as follows:
when the anti-solvent is deionized water, the obtained modified aramid-based polypropylene β nucleating agent is a microcrystalline nucleating agent;
when the anti-solvent is ethanol, the obtained modified aramid-based polypropylene β nucleating agent is a square single crystal nucleating agent;
when the anti-solvent is dimethyl sulfoxide, the obtained modified aramid-based polypropylene β nucleating agent is a long-strip-shaped single-crystal nucleating agent;
when the anti-solvent is N, N' -dimethylformamide, the obtained aramid-based polypropylene β nucleating agent is a long-strip-shaped single-crystal nucleating agent.
In the invention, the size of the obtained modified aramid-based polypropylene β nucleating agent can be regulated by selecting different anti-solvents, for example, the nucleating agent obtained by using water as the anti-solvent is smallest (nanometer), the nucleating agent obtained by using ethanol as the anti-solvent is largest (micrometer), and the nucleating agent obtained by using DMF and DMSO as the anti-solvent is medium (micrometer).
The second technical problem to be solved by the invention is to provide an aramid-based polypropylene β nucleating agent, which is obtained by adopting the preparation method.
The invention has the beneficial effects that:
the invention provides a novel preparation method of an aramid polypropylene β nucleating agent, which can be used for not only obtaining polypropylene β nucleating agents with different shapes, crystal forms and sizes, but also effectively regulating and controlling the crystal forms, the shapes and the sizes of the aramid polypropylene β nucleating agent in a larger range, because the shape and the size of the nucleating agent can influence the content of PP β crystals and the morphology of β crystals, the content and the morphology of PP β crystals can influence the mechanical (impact resistance) and the thermal (thermal deformation) properties of PP materials, and the β crystal content or the PP with special crystal morphology is high, so that the nucleating agent is suitable for preparing PP-R pipes, automobiles and other products requiring high impact resistance and high thermal deformation, and can also be used for processing high porosity, high-porosity and high-thermal deformation products of PP artificial paper and other printable thin film products, and has industrial application value.
Drawings
FIG. 1 is a graph showing the morphology of a nucleating agent obtained in example 1 of the present invention.
FIG. 2 is a topographic map of the nucleating agent obtained in example 2 of the present invention.
FIG. 3 is a graph showing the morphology of the nucleating agent obtained in example 3 of the present invention.
FIG. 4 is a graph showing the morphology of the nucleating agent obtained in example 4 of the present invention.
FIG. 5 is a graph showing the morphology of the nucleating agent obtained in example 5 of the present invention.
FIG. 6 is a topographic map of the nucleating agent obtained in example 6 of the present invention.
FIG. 7 is an NMR chart of a commercial TMB-5 used in the examples.
FIG. 8 is an NMR chart of the modified nucleating agent obtained in example 1.
FIG. 9 is an NMR chart of the modified nucleating agent obtained in example 2.
FIG. 10 is an NMR chart of the modified nucleating agent obtained in example 3.
FIG. 11 is an NMR chart of a modified nucleating agent obtained in example 4; as can be seen from FIGS. 7 to 11, the chemical structure of the nucleating agent was not changed by the method of the present invention.
Detailed Description
The invention provides a method for dissolving an aramid PP β nucleating agent by using concentrated sulfuric acid and precipitating and modifying the size and the shape of the nucleating agent by an anti-solvent.
The invention discloses a method for preparing aromatic amide nucleating agent, which comprises the steps of preparing aromatic amide nucleating agent β, dissolving aromatic amide nucleating agent in a solvent, and controlling the size and the shape of the aromatic amide nucleating agent by using a concentrated sulfuric acid.
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
10g of commercial TMB-5 was added to 200ml of concentrated sulfuric acid and stirred until the solution was clear and transparent, yielding a homogeneous nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of deionized water, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM), the morphology observation result of the prepared nucleating agent is shown in figure 1, and as can be seen from figure 1, if deionized water is used as an anti-solvent, microcrystals can be obtained, the shape of the microcrystals is shown in figure 1, and the size of the microcrystals is 30-500 nanometers.
Example 2
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
Adding 10g of TMB-5 into 200ml of concentrated sulfuric acid, and stirring until the solution is clear and transparent to obtain a uniform nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of ethanol, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM), the morphology observation result of the prepared nucleating agent is shown in figure 2, and it can be known that if ethanol is used as an anti-solvent, square single crystals can be obtained, the shape is shown in figure 2, and the size is 5-90 micrometers.
Example 3
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
Adding 10g of TMB-5 into 200ml of concentrated sulfuric acid, and stirring until the solution is clear and transparent to obtain a uniform nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of dimethyl sulfoxide, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM). The morphology observation result of the prepared nucleating agent is shown in figure 3, and it can be known that if dimethyl sulfoxide is used as an anti-solvent, a long-strip-shaped single crystal can be obtained, the shape is shown in figure 3, and the size is 1-40 micrometers.
Example 4
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
Adding 10g of TMB-5 into 200ml of concentrated sulfuric acid, and stirring until the solution is clear and transparent to obtain a uniform nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of N, N' -dimethylformamide, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM), the morphology observation result of the prepared nucleating agent is shown in figure 4, and the figure shows that if N, N' -dimethylformamide is used as an anti-solvent, a long-strip-shaped single crystal can be obtained, the shape is shown in figure 4, and the size is 1-40 micrometers.
Example 5
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
Adding 10g of NJS into 200ml of concentrated sulfuric acid, and stirring until the solution is clear and transparent to obtain a uniform nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of deionized water, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM), the morphology observation result of the prepared nucleating agent is shown in figure 5, and it can be known that if deionized water is used as an anti-solvent, microcrystals can be obtained, the shape is shown in figure 5, and the size is 30-500 nanometers.
Example 6
A method for dissolving an aramid PP β nucleating agent by adopting concentrated sulfuric acid at room temperature and then separating out and controlling the size and the shape of the nucleating agent by an anti-solvent comprises the following specific steps:
nucleating agent for dissolving aromatic amide PP β
Adding 10g of NJS into 200ml of concentrated sulfuric acid, and stirring until the solution is clear and transparent to obtain a uniform nucleating agent concentrated sulfuric acid solution.
Secondly, the nucleating agent in the solution in the first anti-solvent precipitation step
Slowly adding 50ml of the solution prepared in the first step into 1000ml of ethanol, stirring for 10min, filtering, and drying the obtained sample in an oven at 70 ℃ for 24 h;
the morphology of the prepared nucleating agent is observed by adopting a JSM-5900L V Scanning Electron Microscope (SEM), the morphology observation result of the prepared nucleating agent is shown in figure 6, and it can be known that if ethanol is used as an anti-solvent, square single crystals can be obtained, the shape is shown in figure 6, and the size is 5-90 micrometers.
Claims (8)
1. A preparation method of an aramid polypropylene β nucleating agent is characterized by comprising the steps of firstly dissolving the existing aramid polypropylene β nucleating agent by adopting concentrated sulfuric acid as a solvent at room temperature to obtain a nucleating agent solution, then separating out the nucleating agent in the nucleating agent solution by utilizing an anti-solvent to obtain a suspension or emulsion, and finally drying the solid obtained by filtering the suspension or the emulsion to obtain the modified aramid polypropylene β nucleating agent, wherein the anti-solvent is ethanol, dimethyl sulfoxide or N, N '-dimethylformamide, the aramid polypropylene β nucleating agent is dicyclohexyl terephthalamide or N, N' -dicyclohexyl-2, 6-naphthamide, and the concentrated sulfuric acid is sulfuric acid with the mass concentration of more than 70%.
2. The preparation method of the aramid polypropylene β nucleating agent as claimed in claim 1, wherein the mass ratio of the concentrated sulfuric acid to the existing aramid polypropylene β nucleating agent is 50-1000 parts by weight of the concentrated sulfuric acid and 1-50 parts by weight of the existing aramid polypropylene β nucleating agent.
3. The preparation method of the aramid polypropylene β nucleating agent as claimed in claim 2, wherein the mass ratio of the concentrated sulfuric acid to the existing aramid polypropylene β nucleating agent is 200-350 parts by weight of the concentrated sulfuric acid and 10-20 parts by weight of the existing aramid polypropylene β nucleating agent.
4. The preparation method of the aramid polypropylene β nucleating agent as claimed in claim 1 or 2, wherein the mass ratio of the anti-solvent to the existing aramid polypropylene β nucleating agent is 200-5000 parts by weight of the anti-solvent and 1 part by weight of the existing aramid polypropylene β nucleating agent.
5. The preparation method of the aramid polypropylene β nucleating agent as claimed in claim 1 or 2, wherein the method for precipitating the nucleating agent from the nucleating agent solution by using the anti-solvent to obtain a suspension or emulsion comprises slowly pouring the nucleating agent solution into the anti-solvent, and rapidly stirring for heat dissipation.
6. The method for preparing the nucleating agent of the aramid polypropylene β as defined in claim 1 or 2, wherein the suspension or emulsion is filtered, washed with the same anti-solvent until neutral and then dried.
7. The preparation method of the aramid polypropylene β nucleating agent as claimed in claim 1 or 2, wherein in the preparation method of the aramid polypropylene β nucleating agent, the crystal form and/or shape of the obtained modified aramid polypropylene β nucleating agent is controlled by selecting different anti-solvents in a manner that:
when the anti-solvent is ethanol, the obtained modified aramid-based polypropylene β nucleating agent is a square single crystal nucleating agent;
when the anti-solvent is dimethyl sulfoxide, the obtained modified aramid-based polypropylene β nucleating agent is a long-strip-shaped single-crystal nucleating agent;
when the anti-solvent is N, N' -dimethylformamide, the obtained aramid-based polypropylene β nucleating agent is a long-strip-shaped single-crystal nucleating agent.
8. An aramid polypropylene β nucleating agent, characterized in that the aramid polypropylene β nucleating agent is prepared by the preparation method of any one of claims 1 to 7.
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