CN109593359B - Preparation method of high-filling polyimide pulp masterbatch - Google Patents
Preparation method of high-filling polyimide pulp masterbatch Download PDFInfo
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- CN109593359B CN109593359B CN201811490960.5A CN201811490960A CN109593359B CN 109593359 B CN109593359 B CN 109593359B CN 201811490960 A CN201811490960 A CN 201811490960A CN 109593359 B CN109593359 B CN 109593359B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Abstract
The invention relates to a preparation method of high-filling polyimide pulp masterbatch, which mainly comprises the following steps: stirring the polyimide pulp and a dispersing agent in a high-speed stirrer to obtain pre-dispersed polyimide pulp; adding a small amount of liquid rubber into the pre-dispersed polyimide pulp, and stirring at high speed again to ensure that the liquid rubber is uniformly attached to the surface of the polyimide pulp; and (3) mixing the polyimide pulp with the liquid rubber attached to the surface and the solid rubber on an open mill to obtain the polyimide pulp master batch. The filling amount of the polyimide pulp in the masterbatch prepared by the invention can reach 40%, and the polyimide pulp in the masterbatch has no entanglement phenomenon under a digital optical microscope, thereby solving the problem of poor dispersibility of the polyimide pulp in rubber at present.
Description
Technical Field
The invention relates to a preparation method of a high-filling polyimide pulp masterbatch, which prepares the high-filling polyimide pulp masterbatch by methods of polyimide pulp pretreatment, material adding sequence change during mixing and the like, and belongs to the field of polymer material processing modification.
Background
The polyimide material has a unique aromatic heterocyclic rigid structure, and has the characteristics of excellent high-temperature resistance, mechanical property, insulating property, corrosion resistance, irradiation resistance and the like. Films, fibers, composite materials and the like produced by taking the fibers as raw materials are widely applied to various fields of electronics and electricians, mechanical manufacturing, aerospace and the like. Although our country has made great progress in the development and production of polyimide fibers in recent years, the development and development of polyimide pulp is still in the beginning. Polyimide pulp has a large specific surface area, and is more likely to be entangled relative to polyimide fibers, resulting in poor dispersibility in rubber, thereby limiting the application of polyimide pulp filled rubber composites. The invention patent CN 107573601A discloses an ablation-resistant ethylene propylene diene monomer thermal insulation material filled with polyimide fibers, and even if the polyimide fibers are adopted, the filling amount of the polyimide fibers is only 7 percent to the maximum; the invention patents CN 106751797A and CN106750390A disclose an aromatic polyamide fiber premix master batch, which can obtain a highly filled premix master batch by pulping aromatic polyamide fiber in water at a high speed, buckling and grinding to prepare aromatic polyamide pulp, but the dispersion solvent of the master batch contains volatile toxic physical properties such as tetrahydrofuran, acetone and the like, thereby bringing adverse effects to the production safety and the environment. The invention patent CN 104231348A discloses a preparation method of a high-damping polyimide fiber reinforced composite material, which comprises the steps of firstly mixing rubber and a processing aid uniformly through an open mill, extruding and granulating through a double-screw extruder in a rubber main feeding mode and a polyimide fiber side feeding mode after vulcanization to obtain the high-damping composite material with the polyimide fiber content of 5 percent.
Disclosure of Invention
The invention aims to overcome the defects of volatile toxic solvent, complex preparation process, low filling amount and the like in the invention, and provides a preparation method of a high-filling polyimide pulp masterbatch, so as to solve the problem of poor dispersibility of polyimide pulp in rubber.
In order to realize the purpose, the invention relates to a preparation method of high-filling polyimide pulp masterbatch, which comprises the following steps:
stirring 30-60 parts of polyimide pulp and 0.1-5.0 parts of dispersant in a high-speed stirrer for pre-dispersion, preferably for about 5min, until the bulk polyimide pulp is dispersed; the dispersant is inorganic filler with the particle size of 1-100nm, and comprises but is not limited to one or more of white carbon black, glass beads, montmorillonite, kaolin and calcium carbonate;
adding 5-20 parts of liquid rubber into the pre-dispersed polyimide pulp, and stirring at a high speed to ensure that the liquid rubber is uniformly attached to the surface of the polyimide pulp, preferably for about 3 min;
and (2) putting the polyimide pulp with the surface attached with the liquid rubber on an open mill for mixing, adding 20-60 parts of solid rubber into the open mill, and uniformly mixing to obtain the polyimide pulp master batch.
Wherein the diameter of the polyimide pulp is 5-20 μm, preferably 5-10 μm; the length of the polyimide pulp is 3-10 mm, and preferably 3-6 mm.
The dispersant is an inorganic filler with the particle size of preferably 20-50nm, and the inorganic filler comprises one or more of but not limited to white carbon black, glass beads, montmorillonite, kaolin and calcium carbonate, and is preferably white carbon black or glass beads.
The liquid rubber is ethylene propylene rubber, and is heated to 70 ℃ to reduce the viscosity, so that the liquid rubber is more easily dispersed and attached to the surface of the polyimide pulp.
Wherein, the solid rubber comprises but is not limited to one or more of ethylene propylene rubber, natural rubber, butadiene rubber, styrene butadiene rubber and nitrile butadiene rubber.
The feeding sequence in the mixing process of the open mill is that solid rubber is used as an additive and added into a polyimide pulp matrix with liquid rubber attached to the surface, so that the dispersibility of the polyimide pulp is ensured.
Compared with the prior art, the invention has the following advantages:
(1) the preparation process is simple, volatile toxic solvent is not used, the dispersant and the polyimide pulp are pre-dispersed in a closed high-speed mixer, the energy consumption and the environmental pollution are reduced, and the field working environment is improved;
(2) the viscosity of the liquid rubber is reduced by heating, so that the liquid rubber is more easily dispersed and attached to the surface of the polyimide pulp;
(3) in the mixing process of the open mill, the polyimide pulp with the surface attached with the liquid rubber is used as a matrix, the solid rubber is used as an additive, the dispersibility of the polyimide pulp in the rubber is effectively improved, and the content of the polyimide pulp in the prepared master batch reaches 40 percent.
Description of the drawings:
FIG. 1 is a process flow diagram of a method for preparing a highly filled polyimide pulp masterbatch according to the present invention.
FIG. 2 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 1.
FIG. 3 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 2.
FIG. 4 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 3.
FIG. 5 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 4.
FIG. 6 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 5.
FIG. 7 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 6.
FIG. 8 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in example 7.
FIG. 9 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in comparative example 1.
FIG. 10 is a digital optical micrograph of the dispersibility of the polyimide pulp in rubber in comparative example 2.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Example 1:
step one, stirring 30 parts of polyimide pulp and 2 parts of nano white carbon black in a high-speed stirrer at the rotating speed of 500r/min for about 5min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 2:
step one, stirring 40 parts of polyimide pulp and 3 parts of nano white carbon black in a high-speed stirrer at the rotating speed of 500r/min for about 7min to obtain pre-dispersed polyimide pulp;
heating 15 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 5 minutes at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 2min, adding 42 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 5min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 40%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 3:
step one, stirring 40 parts of polyimide pulp and 3 parts of nano white carbon black in a high-speed stirrer at the rotating speed of 500r/min for about 7min to obtain pre-dispersed polyimide pulp;
heating 15 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 5 minutes at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer attached to the surface on an open mill, mixing for 2min, adding 42 parts of solid nitrile rubber into the matrix, and mixing for 5min to obtain the nitrile rubber master batch with the polyimide pulp filling amount of 40%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 4:
step one, stirring 40 parts of polyimide pulp and 5 parts of glass beads in a high-speed stirrer at the rotating speed of 300r/min for about 7min to obtain pre-dispersed polyimide pulp;
heating 20 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 5 minutes at the rotating speed of 300r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 2min, adding 35 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 5min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 40%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 5
Step one, stirring 30 parts of polyimide pulp and 2 parts of montmorillonite in a high-speed stirrer at the rotating speed of 500r/min for about 5min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 6
Step one, stirring 30 parts of polyimide pulp and 2 parts of kaolin for about 5min in a high-speed stirrer with the rotating speed of 500r/min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Example 7
Step one, stirring 30 parts of polyimide pulp and 2 parts of calcium carbonate in a high-speed stirrer at the rotating speed of 500r/min for about 5min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Comparative example 1
Step one, stirring 30 parts of polyimide pulp and 2 parts of acetone in a high-speed stirrer at the rotating speed of 500r/min for about 5min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
Comparative example 2
Step one, stirring 30 parts of polyimide pulp and 60 parts of acetone in a high-speed stirrer at the rotating speed of 500r/min for about 5min to obtain pre-dispersed polyimide pulp;
heating 10 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring the mixture for about 3min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer rubber attached to the surface on an open mill, mixing for 1min, adding 58 parts of solid ethylene propylene diene monomer rubber into the matrix, and mixing for 3min to obtain the ethylene propylene diene monomer rubber master batch with the polyimide pulp filling amount of 30%.
Step four: and (3) taking a small amount of prepared masterbatch to pass through the open mill with the minimum roll spacing to ensure that the masterbatch has light transmittance, and observing the dispersion condition of the polyimide pulp in the masterbatch under the same magnification of a DM-BA200-C digital optical microscope. Cutting the rest rubber materials into the size of a mold, molding for 10min at the vulcanization temperature of 160 ℃, and preparing the obtained vulcanized rubber into a standard tensile sample, a tearing sample and a roller abrasion sample for testing.
The mechanical property test results of the examples and the comparative examples are as follows:
from the dispersion condition of the polyimide pulp in the masterbatch and the mechanical property test results of the polyimide pulp in the examples and the comparative examples, the polyimide pulp masterbatch prepared by the invention still has better dispersion in rubber under the condition of high filling. Compared with the existing preparation method, the preparation method has better tensile strength and tearing strength and excellent wear resistance.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (1)
1. A preparation method of high-filling polyimide pulp masterbatch comprises the following steps:
step one, stirring 40 parts of polyimide pulp and 3 parts of nano white carbon black for 7min in a high-speed stirrer with the rotating speed of 500r/min to obtain pre-dispersed polyimide pulp;
heating 15 parts of liquid ethylene propylene diene monomer to 70 ℃, adding the heated liquid ethylene propylene diene monomer into the pre-dispersed polyimide pulp, stirring for 5min at the rotating speed of 500r/min, and enabling the liquid ethylene propylene diene monomer to be uniformly attached to the surface of the polyimide pulp;
step three: and (3) putting the polyimide pulp with the liquid ethylene propylene diene monomer attached to the surface on an open mill, mixing for 2min, adding 42 parts of solid nitrile rubber into the matrix, and mixing for 5min to obtain the nitrile rubber master batch with the polyimide pulp filling amount of 40%.
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| CN105418988A (en) * | 2015-11-24 | 2016-03-23 | 黑龙江弘宇短纤维新材料股份有限公司 | Formula and preparation method of pre-dispersion aramid short fiber masterbatch |
| CN107034541B (en) * | 2017-04-13 | 2019-04-26 | 江苏先诺新材料科技有限公司 | A kind of halogen-free flameproof fibrous material of resistance to ablation and its preparation method and application |
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