CN115505169A - Preparation method of modified nano material/ethylene glycol dispersion liquid - Google Patents
Preparation method of modified nano material/ethylene glycol dispersion liquid Download PDFInfo
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- 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
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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Abstract
The invention discloses a preparation method of a modified nano material/ethylene glycol dispersion liquid, which comprises the following steps: s1, placing an inorganic nucleating agent in ethylene glycol, and shearing and dispersing to obtain a nano material/EG suspension; step S2, carrying out wet grinding on the suspension obtained in the step S1 by using a sand mill to obtain a preactivated nano material/EG; step S3, mixing a coupling agent, water and a solvent according to a mass ratio of 1: (1-8): (0-8) mixing and reacting to obtain a coupling agent hydrolysis dispersion liquid; step S4, adding the hydrolysis dispersion liquid prepared in the step S3 into the dispersion liquid prepared in the step S2, and stirring to obtain a surface modification inorganic nano nucleating agent-ethylene glycol dispersion liquid; and S5, carrying out rotary evaporation on the nano material/EG at 90 ℃, and carrying out post-treatment after the rotary evaporation to obtain a modified nano material/EG dispersion liquid. The preparation method of the modified nano material/EG dispersion liquid provided by the invention has excellent modification effect on nano materials, and can prepare the nano modified material/EG dispersion liquid with small particle size and stable dispersion performance.
Description
Technical Field
The invention belongs to the technical field of chemical material preparation, relates to a preparation method of a dispersion liquid, and particularly relates to a preparation method of a modified nano material/ethylene glycol dispersion liquid.
Background
The inorganic nano particles can improve the thermal stability, the crystallization property, the mechanical property and the like of the polymer, so that the polymer can be better applied to more fields. However, the inorganic nanoparticles have large surface area and high surface energy, and are difficult to be uniformly dispersed in the PET matrix, and a conglomerate structure is easily formed in the PET matrix, which restricts the industrial development and application fields of the composite material.
In the past research, the melt blending technology is mainly adopted to synthesize the PET/inorganic nano composite material; however, this technique has the following disadvantages: the dispersed phase can not be uniformly dispersed into the bulk phase, so that the product performance is seriously reduced; melt blending techniques involve secondary heating of the polymer, which can cause thermal decomposition of the polymer macromolecules into smaller molecules, affecting product quality. One of the main methods to solve these problems is to prepare polyester-based inorganic nanocomposite by in-situ polymerization; the method can eliminate or minimize the phase separation phenomenon, so that the inorganic nano particles are uniformly dispersed in the PET matrix to obtain the nano material modified PET composite material with excellent performance.
The process for preparing PET by in-situ polymerization of the nano material is to modify inorganic powder of the nano material, and then disperse the inorganic powder in slurry of PTA and EG for polymerization, so that the prepared process material has poor compatibility with organic phase, and the agglomeration phenomenon occurs in the polymerization process. In order to overcome the agglomeration phenomenon, the material and ethylene glycol are mixed to prepare a material/EG suspension, and the suspension is mixed with PTA and then subjected to in-situ polymerization; therefore, the preparation of the material/EG with excellent dispersion performance becomes the key work of in-situ polymerization.
The preparation process of the nano material/EG suspension on the market at present mainly comprises the following steps:
(1) The nano material glycol sol is prepared by utilizing the technical processes of solvation treatment, sol reaction, fractionation, water removal and the like, the sol has stable dispersity and smaller particle size, but the process is complicated, the cost is higher, and the nano material glycol sol is not suitable for large-scale industrial production;
(2) Modifying the nano material, and then preparing a modified material/suspension; the process has low cost, but the traditional modification process has poor modification effect on the nano material, so that the compatibility of the modified material and glycol is poor, the particle size of the material in dispersion liquid is large, and the material is easy to settle.
In view of the above, there is an urgent need to design a new way for preparing nanomaterial/EG suspension so as to overcome at least some of the above-mentioned disadvantages of the existing preparation ways.
Disclosure of Invention
The invention provides a preparation method of a modified nano material/glycol dispersion liquid, which has excellent modification effect on nano materials and can prepare the nano modified material/glycol dispersion liquid with smaller particle size and stable dispersion performance.
In order to solve the technical problem, according to one aspect of the present invention, the following technical solutions are adopted:
a method of preparing a modified nanomaterial/ethylene glycol dispersion, the method comprising:
s1, placing an inorganic nucleating agent in ethylene glycol, and shearing and dispersing to obtain a nano material/Ethylene Glycol (EG) suspension;
step S2, carrying out wet grinding on the suspension obtained in the step S1 by using a sand mill to obtain a nano material/ethylene glycol with excellent pre-activation and dispersion performances;
step S3, mixing a coupling agent, water and a solvent according to a mass ratio of 1: (1-8): (0-8), mixing, adjusting the pH value to 2-8, and reacting at the temperature of 20-40 ℃ for 1-8h to obtain a coupling agent hydrolysis dispersion liquid;
step S4, adding the hydrolysis dispersion liquid prepared in the step S3 into the dispersion liquid prepared in the step S2, and stirring for 2-6 hours at 50-100 ℃ to obtain a surface modified inorganic nano nucleating agent-glycol dispersion liquid;
and S5, carrying out rotary evaporation on the nano material/ethylene glycol at the temperature of 50-100 ℃, and carrying out post-treatment after the rotary evaporation to obtain the modified nano material/ethylene glycol dispersion liquid.
As an embodiment of the present invention, the inorganic nucleating agent in step S1 is an inorganic nano nucleating agent, which includes at least one of nano montmorillonite, barium sulfate, calcium carbonate, and hydrotalcite; the inorganic nano nucleating agent accounts for 5 to 25 percent of the dispersion liquid by mass.
In one embodiment of the present invention, the particle size of the zirconium beads used for grinding in step S2 is 0.05 to 0.2mm.
In step S3, the coupling agent includes at least one of amino triethoxysilane, amino trimethoxysilane, gamma- (2, 3 epoxypropoxy) propyl trimethoxysilane, dodecyl trimethoxysilane, and hexadecyl trimethoxysilane; the solvent comprises at least one of methanol, ethanol, acetone and glycol.
In step S3, the mass ratio of the coupling agent to the inorganic nano nucleating agent is 5% to 25%.
The invention has the beneficial effects that: the preparation method of the modified nano material/glycol dispersion liquid provided by the invention utilizes glycol as a solvent, and pre-activates the unmodified material/glycol dispersion liquid by a grinding dispersion means to expose more active groups; meanwhile, the modifier is pretreated to enhance the reactivity of the modifier, so that the nano modified material/glycol dispersion liquid with small particle size and stable dispersion performance is prepared.
Drawings
FIG. 1 is a flow chart of a method for preparing a modified nanomaterial/EG dispersion in accordance with one embodiment of the present invention.
FIG. 2 is a schematic diagram showing the particle size results of the conventional modified nanomaterial/EG.
FIG. 3 is a graph showing the results of particle size modification of the nanomaterial/EG in accordance with one embodiment of the present invention.
FIG. 4 is a graph showing the results of particle size modification of the nanomaterial/EG in another embodiment of the present invention.
FIG. 5 is a graph showing the results of particle size modification of nanomaterial/EG in another embodiment of the present invention.
FIG. 6 is a graph showing the results of particle size modification of nanomaterial/EG in another embodiment of the present invention.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
The description in this section is for several exemplary embodiments only and the invention is not to be limited in scope by the embodiments described. It is within the scope of the present disclosure and protection that the same or similar prior art means and some features of the embodiments may be interchanged.
The steps in the embodiments in the specification are only expressed for convenience of description, and the implementation manner of the present application is not limited by the order of implementation of the steps.
The invention discloses a preparation method of a modified nano material/ethylene glycol dispersion liquid, and fig. 1 is a flow chart of the preparation method of the modified nano material/ethylene glycol dispersion liquid in one embodiment of the invention; referring to fig. 1, the preparation method includes:
step S1, an inorganic nano nucleating agent is placed in ethylene glycol, and a nano material/Ethylene Glycol (EG) suspension is obtained through shear dispersion. In one embodiment, the nanomaterial/ethylene glycol suspension is obtained by shear dispersion with an emulsifying machine.
In an embodiment, in step S1, the inorganic nano nucleating agent includes at least one of nano montmorillonite, barium sulfate, hydrotalcite, and calcium carbonate; the inorganic nano nucleating agent accounts for 5 to 25 percent (such as 5 percent or 10 percent or 15 percent or 25 percent) of the mass fraction of the dispersion.
And (S2) carrying out wet grinding on the suspension obtained in the step (S1) by using a sand mill to obtain the nano material/glycol with excellent pre-activation and dispersion performance.
In one embodiment, in step S2, the milled zirconium beads used have a particle size of 0.05-0.2mm. And (3) performing pre-activation treatment on the nano material by adopting a grinding process to expose more active groups capable of reacting with the modifier.
Step S3, mixing a coupling agent, water, and a solvent in a mass ratio of 1: (1-8): (0-8), mixing, adjusting the pH value to 2-8 (such as optionally adjusting the pH value to 2 or 5 or 6 or 7 or 8, and the like), and reacting at the temperature of 20-40 ℃ for 1-8h (such as 1h, 3h, 5h and 8 h) to obtain the coupling agent hydrolysis dispersion liquid.
In one embodiment, in step S3, the coupling agent comprises at least one of amino triethoxysilane, amino trimethoxysilane, γ - (2, 3 glycidoxy) propyl trimethoxysilane, dodecyl trimethoxysilane, and hexadecyl trimethoxysilane; the solvent comprises at least one of methanol, ethanol, acetone and glycol. The mass ratio of the coupling agent to the inorganic nano nucleating agent can be 5-25%.
And (S4) adding the hydrolysis dispersion liquid prepared in the step S3 into the dispersion liquid prepared in the step S2, and stirring for 2-6 hours at 50-100 ℃ to obtain the surface-modified inorganic nano nucleating agent-ethylene glycol dispersion liquid.
And (S5) carrying out rotary evaporation on the nano material/EG at 50-100 ℃ (for example, 90 ℃), and carrying out post-treatment after the rotary evaporation to obtain the modified nano material/EG dispersion liquid with small particle size and excellent dispersion performance.
And (3) carrying out post-treatment on the modified nano dispersion liquid to remove redundant modifier and solvent, thereby avoiding the influence on post esterification and polycondensation reaction.
The invention can solve the technical problem of the dispersion of the nano material in EG, and prepare the nano material/EG dispersion liquid for PET in-situ polymerization with smaller dispersion particle size and excellent dispersion performance.
Hydrolysis pretreatment is carried out on the coupling agent, so that reactive groups reacting with the nano material are increased, and the modification effect is improved; meanwhile, a coupling agent capable of reacting with PET is adopted, one end of the coupling agent is used for modifying the nano material, and the other end of the coupling agent is chemically bonded with the PET in the polymerization process, so that the compatibility of the nano material and the PET is improved.
In one embodiment of the present invention, the preparation method of the modified nanomaterial/EG dispersion of the present invention comprises the following steps:
(1) Preparing 5% of nano material/EG dispersion liquid by using emulsification dispersion equipment, and grinding and dispersing by using sanding equipment to prepare pre-activated nano material/EG dispersion liquid with higher activity;
(2) Weighing a modifier which accounts for 15% of the mass of the nano material, dissolving the modifier in a solvent according to the ratio of m (modifier: solvent) = 1;
(3) Adding the modifier hydrolysate into the ground and dispersed material/EG dispersion liquid, and reacting for 4h at the temperature of 60 ℃ to prepare the surface modified nano material-ethylene glycol dispersion liquid.
(4) Performing rotary evaporation on the surface-modified nano material-glycol dispersion liquid to remove redundant solvent in the dispersion liquid; and grinding the dispersion liquid after rotary evaporation to obtain the modified nano material/EG dispersion liquid.
FIG. 3 is a graph showing the results of particle size modification of the nanomaterial/EG in accordance with one embodiment of the present invention.
In another embodiment of the present invention, the preparation method of the modified nanomaterial/EG dispersion of the present invention comprises the following steps:
(1) Preparing 5% of nano material/EG dispersion liquid by using emulsification dispersion equipment, and grinding and dispersing by using sanding equipment to prepare pre-activated nano material/EG dispersion liquid with higher activity;
(2) Weighing a modifier which accounts for 15% of the mass of the nano material, dissolving the modifier in a solvent according to the ratio of m (modifier: solvent) = 1;
(3) Adding the modifier hydrolysate into the ground and dispersed material/EG dispersion solution, and reacting for 4h at 100 ℃ to prepare the surface modified nano material-ethylene glycol dispersion solution.
(4) Performing rotary evaporation on the surface modified nano material-glycol dispersion liquid to remove redundant solvent in the dispersion liquid; and grinding the dispersion liquid after rotary evaporation to obtain the modified nano material/EG dispersion liquid.
FIG. 4 is a graph showing the results of particle size modification of the nanomaterial/EG in another embodiment of the present invention.
In another embodiment of the present invention, the preparation method of the modified nanomaterial/EG dispersion of the present invention comprises the following steps:
(1) Preparing 5% of nano material/EG dispersion liquid by using emulsification dispersion equipment, and grinding and dispersing by using sanding equipment to prepare pre-activated nano material/EG dispersion liquid with higher activity;
(2) Weighing 15% of modifier relative to the mass of the nano material, dissolving the modifier in the solvent according to the ratio of m (modifier: solvent) = 1.
(3) Adding the modifier hydrolysate into the ground and dispersed material/EG dispersion liquid, and reacting for 4h at the temperature of 60 ℃ to prepare the surface modified nano material-ethylene glycol dispersion liquid.
(4) Performing rotary evaporation on the surface-modified nano material-glycol dispersion liquid to remove redundant solvent in the dispersion liquid; and grinding the dispersion liquid after rotary evaporation to obtain the modified nano material/EG dispersion liquid.
FIG. 5 is a graph showing the results of particle size modification of nanomaterial/EG in accordance with still another embodiment of the present invention.
In another embodiment of the present invention, the preparation method of the modified nanomaterial/EG dispersion of the present invention comprises the following steps:
(1) Preparing 5% of nano material/EG dispersion liquid by using emulsification dispersion equipment, and grinding and dispersing by using sanding equipment to prepare pre-activated nano material/EG dispersion liquid with higher activity;
(2) Weighing a modifier which accounts for 15 percent of the mass of the nano material, dissolving the modifier in a solvent according to the ratio of m (modifier: solvent) = 1;
(3) Adding the modifier hydrolysate into the ground and dispersed material/EG dispersion solution, and reacting for 4h at 100 ℃ to prepare the surface modified nano material-ethylene glycol dispersion solution.
(4) Performing rotary evaporation on the surface-modified nano material-glycol dispersion liquid to remove redundant solvent in the dispersion liquid; and grinding the dispersion liquid after rotary evaporation to obtain the modified nano material/EG dispersion liquid.
FIG. 6 is a graph showing the results of particle size modification of nanomaterial/EG in accordance with still another embodiment of the present invention.
In summary, in the preparation method of the modified nanomaterial/EG dispersion provided by the invention, EG is used as a solvent, and the unmodified nanomaterial/EG dispersion is pre-activated by a grinding dispersion means, so that more active groups are exposed; meanwhile, the modifier is pretreated to enhance the reactivity of the modifier, so that the nano modified material/EG dispersion liquid has excellent modification effect on the nano material and is prepared to have small particle size and stable dispersion performance.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The description and applications of the invention herein are illustrative and are not intended to limit the scope of the invention to the embodiments described above. Effects or advantages referred to in the embodiments may not be reflected in the embodiments due to interference of various factors, and the description of the effects or advantages is not intended to limit the embodiments. Variations and modifications of the embodiments disclosed herein are possible, and alternative and equivalent various components of the embodiments will be apparent to those skilled in the art. It will be clear to those skilled in the art that the present invention may be embodied in other forms, structures, arrangements, proportions, and with other components, materials, and parts, without departing from the spirit or essential characteristics thereof. Other variations and modifications of the embodiments disclosed herein may be made without departing from the scope and spirit of the invention.
Claims (5)
1. A preparation method of a modified nano material/ethylene glycol dispersion liquid is characterized by comprising the following steps:
s1, placing an inorganic nucleating agent in ethylene glycol, and shearing and dispersing to obtain a nano material/ethylene glycol suspension;
step S2, carrying out wet grinding on the suspension obtained in the step S1 by using a sand mill to obtain a nano material/ethylene glycol with excellent pre-activation and dispersion performances;
step S3, mixing a coupling agent, water and a solvent according to a mass ratio of 1: (1-8): (0-8), mixing, adjusting the pH value to 2-8, and reacting at the temperature of 20-40 ℃ for 1-8h to obtain a coupling agent hydrolysis dispersion liquid;
step S4, adding the hydrolysis dispersion liquid prepared in the step S3 into the dispersion liquid prepared in the step S2, and stirring for 2-6 hours at 50-100 ℃ to obtain a surface modification inorganic nucleating agent-ethylene glycol dispersion liquid;
and S5, carrying out rotary evaporation on the nano material/ethylene glycol at the temperature of 50-100 ℃, and carrying out post-treatment after the rotary evaporation to obtain the modified nano material/ethylene glycol dispersion liquid.
2. The method of claim 1, wherein the modified nanomaterial/ethylene glycol dispersion is prepared by:
in the step S1, the inorganic nucleating agent is an inorganic nano nucleating agent and comprises at least one of nano montmorillonite, barium sulfate, calcium carbonate and hydrotalcite; the inorganic nano nucleating agent accounts for 5 to 25 percent of the dispersion liquid by mass.
3. The method of claim 1, wherein the modified nanomaterial/ethylene glycol dispersion is prepared by:
in step S2, the particle size of the grinding zirconium beads used is 0.05-0.2mm.
4. The method of claim 1, wherein the modified nanomaterial/ethylene glycol dispersion is prepared by:
in step S3, the coupling agent comprises at least one of amino triethoxysilane, amino trimethoxysilane, gamma- (2, 3-glycidoxy) propyl trimethoxysilane, dodecyl trimethoxysilane and hexadecyl trimethoxysilane; the solvent comprises at least one of methanol, ethanol, acetone and glycol.
5. The method of claim 1, wherein the modified nanomaterial/ethylene glycol dispersion is prepared by:
in the step S3, the mass ratio of the coupling agent to the inorganic nano nucleating agent is 5-25%.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1516712A (en) * | 2001-08-14 | 2004-07-28 | ��Ļ���Ű˾ | Proces for producing polyester with coated titanium dioxide |
| CN1616518A (en) * | 2004-09-23 | 2005-05-18 | 上海交通大学 | Process for in-situ quiclely preparing crystalline polyester using nano silicon dioxide |
| CN114409962A (en) * | 2022-01-07 | 2022-04-29 | 北京吉海川科技发展有限公司 | Treatment method and application of nucleating agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1516712A (en) * | 2001-08-14 | 2004-07-28 | ��Ļ���Ű˾ | Proces for producing polyester with coated titanium dioxide |
| CN1616518A (en) * | 2004-09-23 | 2005-05-18 | 上海交通大学 | Process for in-situ quiclely preparing crystalline polyester using nano silicon dioxide |
| CN114409962A (en) * | 2022-01-07 | 2022-04-29 | 北京吉海川科技发展有限公司 | Treatment method and application of nucleating agent |
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