CN111138605A - Low-temperature-resistant chemical-resistant composite material and preparation method thereof - Google Patents
Low-temperature-resistant chemical-resistant composite material and preparation method thereof Download PDFInfo
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- CN111138605A CN111138605A CN202010029461.7A CN202010029461A CN111138605A CN 111138605 A CN111138605 A CN 111138605A CN 202010029461 A CN202010029461 A CN 202010029461A CN 111138605 A CN111138605 A CN 111138605A
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Abstract
The invention relates to the technical field of high polymer materials, in particular to a low-temperature-resistant chemical-resistant composite material and a preparation method thereof, wherein the composite material is prepared from the following raw materials in parts by weight: 1-5 parts of carbon fiber; 20-25 parts of polyimide resin; 40-50 parts of dibasic acid anhydride; 20-25 parts of vinyl chloride. The invention takes carbon fiber as a substrate, firstly oxidizes the surface of the carbon fiber and enriches a large amount of carboxyl, then reacts with dicarboxylic anhydride to obtain carboxylic anhydride carbon fiber, then the carboxylic anhydride carbon fiber is mixed with polyimide resin and reacts with amino at the end position of the polyimide resin to obtain free carboxyl, the free carboxyl reacts with chloroethylene under the action of sodium hydroxide to graft the chloroethylene on the carbon fiber, and then the ethylene is polymerized to obtain the composite material with low temperature resistance and chemical resistance.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a low-temperature-resistant chemical-resistant composite material and a preparation method thereof.
Background
The composite material is a new material formed by two or more materials with different properties through a physical or chemical method; the various materials make up for each other in performance to generate synergistic effect, so that the comprehensive performance of the composite material is superior to that of the original composition material to meet various requirements, the development of modern high-tech technology cannot be separated from the composite material, and the composite material plays an important role in the development of modern scientific technology.
In the prior art, most of reaction kettles for organic synthesis are made of high-temperature-resistant and corrosion-resistant materials, and partial reaction in the organic synthesis needs to be carried out at low temperature, so that a low-temperature-resistant and chemical-resistant material needs to be embedded in the reaction kettle, and chemical reaction can be carried out at low temperature.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a composite material with low temperature resistance and chemical resistance and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
the composite material with low temperature resistance and chemical resistance comprises the following raw materials in parts by weight: 1-5 parts of carbon fiber; 20-25 parts of polyimide resin; 40-50 parts of dibasic acid anhydride; 20-25 parts of vinyl chloride.
Preferably, the composite material also comprises 5-10 parts of a reinforcing material, wherein the reinforcing material is one of glass fiber, boron fiber and silicon carbide fiber.
Preferably, the dibasic acid anhydride is one of acetic anhydride, propionic anhydride and succinic anhydride.
The invention also provides a preparation method of the composite material with low temperature resistance and chemical resistance, which comprises the following steps:
(1) weighing: weighing the following raw materials in parts by weight: 1-5 parts of carbon fiber; 20-25 parts of polyimide resin; 10-50 parts of dibasic acid anhydride; 20-25 parts of chloroethylene for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated acid solution, performing ultrasonic treatment at 40-60 ℃ for 2-3h, then washing with water to neutrality, and drying at 60-80 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the dibasic acid anhydride into the modified carbon fiber prepared in the step (2), heating to 140-165 ℃, refluxing for 5-8h, cooling to room temperature, filtering and washing with water to neutrality to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into an aprotic solvent, reacting at 10-25 ℃ for 2-3h to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 8-10h, filtering, washing with water, and anhydrous NaSO4Drying to obtain a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 10-12h at 55-65 ℃ and 15-30MPa under the action of a Ziegler-Natta catalyst, and then cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 1-2: 100.
preferably, the concentrated acid solution in the step (2) is selected from a concentrated sulfuric acid solution with a mass fraction of 98% or a concentrated nitric acid solution with a mass fraction of 68%, and the ratio of the volume of the concentrated acid solution to the mass of the carbon fibers is 4-6 mL: 1g of the total weight of the composition.
Preferably, the ultrasonic power of step (2) is 250W, and the ultrasonic frequency is 50 kHz.
Preferably, the aprotic solvent in step (4) is selected from one of diethyl ether, carbon tetrachloride, dimethyl sulfoxide, N-dimethylformamide or acetone.
Preferably, the raw materials weighed in the step (1) also comprise 5-10 parts of a reinforcing material, and the reinforcing material is added after the grafted polyimide compound is reacted for 10-12h at the temperature of 55-65 ℃ and under the pressure of 15-30MPa in the step (5), and the stirring is continued for 5-8h at the temperature of 55-65 ℃.
Preferably, the composite material with low temperature resistance and chemical resistance prepared in the step (5) is formed in a film pressing machine.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention takes carbon fiber as a substrate, firstly oxidizes the surface of the carbon fiber to enrich a large amount of carboxyl on the surface of the carbon fiber, then obtains higher-level carboxylic anhydride carbon fiber through the reaction of the carboxyl and dibasic acid anhydride, after the carboxylic anhydride carbon fiber is blended with polyimide resin, the amino at the end position of the polyimide resin is more active and can generate amidation reaction with one carboxyl after the carboxylic anhydride carbon fiber is broken, and the other carboxyl is in a free state, at the moment, the free carboxyl reacts with chloroethylene under the action of sodium hydroxide, so that the chloroethylene is grafted on the carbon fiber, and chlorine atoms are separated from chloroethylene molecules, at the moment, double bonds are polymerized, and the composite material with low temperature resistance and chemical resistance is prepared.
2. According to the invention, the carbon fiber is selected as the matrix, because the carbon fiber is a very excellent corrosion-resistant material, the carbon content of the carbon fiber is very high and exceeds 90%, and the fibrous carbon material can form a composite material with resin and is one of the most corrosion-resistant materials, so that the carbon fiber is used as the matrix in the application and is modified, and not only grafting of other organic macromolecules is realized, but also the carbon fiber has excellent corrosion resistance.
3. The composite material with low temperature resistance and chemical resistance prepared by the invention not only contains carbon fiber, but also contains polyethylene and polyimide resin, the polyimide resin is one of organic polymer materials with the best comprehensive performance, the high temperature resistance reaches 400 ℃ and above, the low temperature resistance reaches-300 ℃ and above, and the long-term use temperature range is-200-; the polyethylene is a high polymer material which is odorless, nontoxic, has wax-like hand feeling, has excellent low-temperature resistance, has the lowest use temperature of-100-70 ℃, has good chemical stability, can resist the corrosion of most acid and alkali, is insoluble in common solvents at normal temperature, has small water absorption and excellent electrical insulation property; according to the preparation method, polyimide resin and polyethylene are grafted on carbon fibers together, the carbon fibers are used as a matrix to form a large organic polymer, and the purpose of low-temperature resistance and chemical resistance corrosion resistance is achieved through the polyimide resin, the polyethylene and the carbon fibers together.
Drawings
FIG. 1 is a schematic diagram of the preparation of the composite material of example 1 of the present invention having low temperature and chemical resistance.
Detailed Description
The following description is provided to best mode embodiments of the present invention in conjunction with examples 1-4.
Example 1
(1) Weighing: weighing the following raw materials in parts by weight: 1 part of carbon fiber; 20 parts of polyimide resin; 40 parts of acetic anhydride; 20 parts of chloroethylene for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated sulfuric acid solution with the mass fraction of 98%, performing ultrasonic treatment for 3 hours at the temperature of 40 ℃ under the conditions of ultrasonic power of 250W and ultrasonic frequency of 50kHz, then washing the mixture to be neutral, and drying the mixture at the temperature of 60 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the acetic anhydride into the modified carbon fiber prepared in the step (2), heating to 140 ℃, refluxing for 8 hours, cooling to room temperature, filtering, and washing with water to be neutral to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into N, N-dimethylformamide, reacting at 10 ℃ for 3h to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 8h, filtering, washing with water, and anhydrous NaSO4Drying to obtain a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 10 hours at 55 ℃ and 30MPa under the action of a Ziegler-Natta catalyst, and then cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 1: 100.
the schematic diagram is shown in fig. 1.
Example 2
(1) Weighing: weighing the following raw materials in parts by weight: 3 parts of carbon fiber; 15 parts of polyimide resin; 30 parts of propionic anhydride; 15 parts of chloroethylene for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated nitric acid solution with the mass fraction of 68%, carrying out ultrasonic treatment for 2.5h at the temperature of 50 ℃ under the conditions that the ultrasonic power is 250W and the ultrasonic frequency is 50kHz, then washing the mixture to be neutral, and drying the mixture at the temperature of 70 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the propionic anhydride into the modified carbon fiber prepared in the step (2), heating to 155 ℃, refluxing for 6h, cooling to room temperature, filtering, and washing with water to be neutral to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into carbon tetrachloride, reacting at 20 ℃ for 2.5 hours to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 9 hours, filtering, washing with water, and anhydrous NaSO4Drying to obtainTo a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 11 hours at the temperature of 60 ℃ and under the pressure of 25MPa under the action of a Ziegler-Natta catalyst, and then cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 1.5: 100.
example 3
(1) Weighing: weighing the following raw materials in parts by weight: 5 parts of carbon fiber; 25 parts of polyimide resin; 50 parts of succinic anhydride; 25 parts of chloroethylene for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated sulfuric acid solution with the mass fraction of 98%, carrying out ultrasonic treatment for 2 hours at the temperature of 60 ℃ under the conditions that the ultrasonic power is 250W and the ultrasonic frequency is 50kHz, then washing the mixture to be neutral, and drying the mixture at the temperature of 80 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the succinic anhydride into the modified carbon fiber prepared in the step (2), heating to 165 ℃, refluxing for 5 hours, cooling to room temperature, filtering, and washing with water to be neutral to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into an aprotic solvent, reacting at 25 ℃ for 2h to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 10h, filtering, washing with water, and carrying out anhydrous NaSO4Drying to obtain a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 12 hours at 65 ℃ and 15MPa under the action of a Ziegler-Natta catalyst, and then cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 2: 100.
example 4
(1) Weighing: weighing the following raw materials in parts by weight: 1 part of carbon fiber; 20 parts of polyimide resin; 40 parts of acetic anhydride; 20 parts of chloroethylene and 8 parts of reinforcing materials for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated sulfuric acid solution with the mass fraction of 98%, performing ultrasonic treatment for 3 hours at the temperature of 40 ℃ under the conditions of ultrasonic power of 250W and ultrasonic frequency of 50kHz, then washing the mixture to be neutral, and drying the mixture at the temperature of 60 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the acetic anhydride into the modified carbon fiber prepared in the step (2), heating to 140 ℃, refluxing for 8 hours, cooling to room temperature, filtering, and washing with water to be neutral to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into N, N-dimethylformamide, reacting at 10 ℃ for 3h to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 8h, filtering, washing with water, and anhydrous NaSO4Drying to obtain a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 10 hours at 55 ℃ and 30MPa under the action of a Ziegler-Natta catalyst, then adding a reinforcing material, continuously stirring at 55-65 ℃ for 5-8 hours, and cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 1: 100.
comparative example 1
Example 2 the resulting grafted polyimide compound was prepared.
Comparative example 2
Polyimide resins of the prior art.
Comparative example 3
Polyethylene resins of the prior art.
The low-temperature-resistant and chemical-resistant composite materials prepared in the embodiments 1 to 4 of the present invention all have excellent low-temperature-resistant and chemical-resistant properties, and can be applied to synthesis of low-temperature chemical reactions in a reaction kettle, and the low-temperature-resistant and chemical-resistant composite materials prepared in the embodiments 1 to 4 of the present invention have similar properties, and the low-temperature-resistant and chemical-resistant composite materials prepared in the embodiments 1 to 4 of the present invention are studied, and the specific study contents are shown in the following table:
the high-low temperature circulation method comprises the following steps:
high-low temperature circulation: the composite material with low temperature resistance and chemical resistance prepared by the invention is observed after 9 cycles according to the following method:
storing for 4h under the environment of 50 +/-2 ℃ → storing for 30min under the environment of-50 +/-2 ℃ → storing for 3h under the environment of 100 +/-2 ℃ → storing for 30min under the environment of-100 +/-2 ℃ → storing for 2h under the environment of 150 +/-2 ℃ → storing for 30min under the environment of-150 +/-2 ℃ → storing for 1h under the environment of 200 +/-2 ℃ → storing for 30min under the environment of-196 +/-2 ℃ (liquid nitrogen) → storing for 0.5h under the environment of 300 +/-2 ℃.
Chemical resistance test: the composite material with low temperature resistance and chemical resistance is cut into samples of 80mm multiplied by 60mm multiplied by 3mm, and the samples are put into different solvents for soaking for 24 h.
According to a low-temperature test, the elongation at break of the low-temperature-resistant chemical-resistant composite material prepared by the invention is higher at-100 ℃ and-200 ℃, which shows that the low-temperature-resistant chemical-resistant composite material prepared by the invention has excellent performance at low temperature and does not have brittle fracture phenomenon.
As shown by a corrosion resistance test, the composite material with low temperature and chemical resistance prepared by the invention has excellent corrosion resistance in an organic reagent and a non-oxidizing acid, because the composite material with low temperature and chemical resistance contains polyethylene and polyimide, and the polyethylene and the polyimide can not stably exist in a concentrated acid and can be corroded by the concentrated acid, the surface of the composite material with low temperature and chemical resistance prepared by the invention can bulge after being soaked in the oxidizing acid, while the matrix of the composite material with low temperature and chemical resistance prepared by the invention is carbon fiber which can be stably kept in the concentrated acid and can not be corroded by the concentrated acid, so that the surfaces of the composite material prepared by the invention in the embodiments 1 to 4 and the grafted polyimide compound prepared by the comparative example 1 slightly bulge after being soaked in the concentrated acid, the inner layer has no change phenomenon, so the composite material with low temperature resistance and chemical resistance prepared by the method cannot be corroded by concentrated acid, but the surface is corroded.
From the high-low temperature cycle performance, the low-temperature-resistant chemical-resistant composite material prepared by the invention can be subjected to sexual cycle at-200-350 ℃, the composite material is subjected to cycle under the condition of-196 ℃, the-196 ℃ is an environment of liquid nitrogen, and the composite material is not deformed after the cycle, so that the composite material can be suitable for stably existing in the environment and the condition of the liquid nitrogen.
In conclusion, the composite material with low temperature resistance and chemical resistance prepared by the invention has excellent low temperature resistance and chemical corrosion resistance, and experiments prove that the structure of the composite material is still kept intact in liquid nitrogen, so that the composite material can be embedded in a reaction kettle to perform chemical reaction at low temperature, and the composite material with low temperature resistance and chemical resistance prepared by the invention cannot be applied to the reaction of oxidizing acid and oxidizing reagents.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (9)
1. The composite material with low temperature resistance and chemical resistance is characterized by comprising the following raw materials in parts by weight: 1-5 parts of carbon fiber; 20-25 parts of polyimide resin; 40-50 parts of dibasic acid anhydride; 20-25 parts of vinyl chloride.
2. The low temperature chemical resistant composite of claim 1, further comprising 5-10 parts of a reinforcing material, wherein the reinforcing material is one of glass fibers, boron fibers, and silicon carbide fibers.
3. The low temperature chemical resistant composite of claim 1, wherein the dibasic acid anhydride is one of acetic anhydride, propionic anhydride, succinic anhydride.
4. The method of preparing a composite of low temperature and chemical resistance according to claim 1, comprising the steps of:
(1) weighing: weighing the following raw materials in parts by weight: 1-5 parts of carbon fiber; 20-25 parts of polyimide resin; 10-50 parts of dibasic acid anhydride; 20-25 parts of chloroethylene for later use;
(2) modification of carbon fibers: mixing carbon fibers with a concentrated acid solution, performing ultrasonic treatment at 40-60 ℃ for 2-3h, then washing with water to neutrality, and drying at 60-80 ℃ until the weight of the carbon fibers is not changed any more, thereby obtaining modified carbon fibers;
(3) preparation of carboxylic anhydride carbon fiber: adding the dibasic acid anhydride into the modified carbon fiber prepared in the step (2), heating to 140-165 ℃, refluxing for 5-8h, cooling to room temperature, filtering and washing with water to neutrality to obtain carboxylic anhydride carbon fiber;
(4) grafting of polyimide: adding polyimide resin and the carboxylic anhydride carbon fiber prepared in the step (3) into an aprotic solvent, reacting at 10-25 ℃ for 2-3h to obtain polyamic acid, adding NaOH and chloroethylene into the polyamic acid, stirring at normal temperature for 8-10h, filtering, washing with water, and anhydrous NaSO4Drying to obtain a grafted polyimide compound;
(5) preparation of a composite material resistant to low temperature and chemicals: reacting the grafted polyimide compound prepared in the step (4) for 10-12h at 55-65 ℃ and 15-30MPa under the action of a Ziegler-Natta catalyst, and then cooling to room temperature to obtain a low-temperature-resistant chemical-resistant composite material;
wherein the mass ratio of the Ziegler-Natta catalyst to the grafted polyimide compound is 1-2: 100.
5. the method for preparing the composite material with low temperature and chemical resistance according to claim 4, wherein the concentrated acid solution in the step (2) is selected from a concentrated sulfuric acid solution with a mass fraction of 98% or a concentrated nitric acid solution with a mass fraction of 68%, and the ratio of the volume of the concentrated acid solution to the mass of the carbon fibers is 4-6 mL: 1g of the total weight of the composition.
6. The method for preparing the composite material with low temperature resistance and chemical resistance according to claim 4, wherein the ultrasonic power of the step (2) is 250W, and the ultrasonic frequency is 50 kHz.
7. The method for preparing the composite material with low temperature and chemical resistance according to claim 4, wherein the aprotic solvent in the step (4) is selected from one of diethyl ether, carbon tetrachloride, dimethyl sulfoxide, N-dimethylformamide or acetone.
8. The method for preparing the composite material with low temperature resistance and chemical resistance according to claim 4, wherein the raw materials weighed in the step (1) further comprise 5-10 parts of a reinforcing material, and the reinforcing material is added in the step (5) after the grafted polyimide compound is reacted for 10-12 hours at 55-65 ℃ and 15-30MPa, and the stirring is continued for 5-8 hours at 55-65 ℃.
9. The method for preparing the composite material with low temperature and chemical resistance according to claim 4, wherein the composite material with low temperature and chemical resistance prepared in the step (5) is formed in a laminator.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113529242A (en) * | 2021-07-29 | 2021-10-22 | 吉祥三宝高科纺织有限公司 | Method for preparing anti-cutting gloves by using carbon fiber composite material |
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| CN109021435A (en) * | 2018-06-28 | 2018-12-18 | 芜湖卓越线束系统有限公司 | A kind of anticorrosive heat-shrinkable T bush material and preparation method thereof that insulate |
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| US20060197246A1 (en) * | 2005-03-02 | 2006-09-07 | Hale Wesley R | Process for the preparation of transparent shaped articles |
| CN104212126A (en) * | 2014-09-09 | 2014-12-17 | 丹阳丹金汽车部件有限公司 | Carbon fiber/carbon nanotube/epoxy resin/polyimide multi-dimensional mixed composite material and preparation process thereof |
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| CN113529242A (en) * | 2021-07-29 | 2021-10-22 | 吉祥三宝高科纺织有限公司 | Method for preparing anti-cutting gloves by using carbon fiber composite material |
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Application publication date: 20200512 |