CN108219190B - Method for preparing aramid pulp by using scrapped bulletproof helmet - Google Patents
Method for preparing aramid pulp by using scrapped bulletproof helmet Download PDFInfo
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- CN108219190B CN108219190B CN201711370279.2A CN201711370279A CN108219190B CN 108219190 B CN108219190 B CN 108219190B CN 201711370279 A CN201711370279 A CN 201711370279A CN 108219190 B CN108219190 B CN 108219190B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
- C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/02—Recovery or working-up of waste materials of solvents, plasticisers or unreacted monomers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
Abstract
The invention relates to a method for preparing aramid pulp by utilizing a scrapped bulletproof helmet, belonging to the technical field of high polymer materials. Firstly, disassembling the helmet, cutting and crushing the helmet into strips, then soaking the strips in a solvent, peeling off resin attached to the fiber surface by using a ball mill, then removing the resin by a centrifugal separation mode, and finally defibering and disc-grinding the aramid fiber to obtain the aramid pulp. Compared with the prior art, the method almost completely recycles the aramid fiber in the helmet, and achieves the most efficient utilization of resources; the method for stripping the resin and the fiber by combining solvent swelling and physical shearing has the advantages of high efficiency, mild conditions, simple equipment and convenience for large-scale production.
Description
Technical Field
The invention relates to a method for preparing aramid pulp by utilizing a scrapped bulletproof helmet, belonging to the technical field of high polymer materials.
Background
The para-aramid fiber is a high-performance polymer material, has a series of excellent performances such as high strength, high modulus, high temperature resistance, corrosion resistance, flame retardance and the like, and is widely applied to the fields of military affairs, aerospace, electromechanics, buildings and the like. The helmet prepared from the para-aramid fiber is provided with various military and police systems in a large quantity, and plays a very important role in ensuring the fighting capacity and life safety of military and police personnel. However, since the para-aramid fiber and the cured material thereof are both high molecular polymers, the service life of the para-aramid fiber and the cured material thereof is long, and the para-aramid fiber must be discarded when the para-aramid fiber is expired.
There is currently no universal and mature method of disposing of spent bulletproof helmets. From public reports, the retired helmet is mainly treated by the disposal methods such as open-air incineration, underground landfill and stacking, but the methods have the problems of pollution, waste, high cost and the like. CN201710052354.4 provides a new method for processing police bulletproof helmets, which adopts a high-temperature degradation gasification method to carry out harmless treatment on high-molecular helmets. This method still has a problem of waste. Because the aramid fiber used by the aramid helmet has important recycling value, the aramid fiber in the aramid helmet can not have obvious performance reduction due to the protection of the cured resin and the shading protection of the outer layer in the whole service period, and therefore if only the aramid fiber is subjected to pyrolysis treatment, huge waste can be caused to resources.
The use of pulp from discarded helmet fibers is a viable recycling method, but it is technically challenging. The aramid bulletproof helmet is generally formed by curing and compounding aramid fiber and phenolic aldehyde or epoxy resin and the like. To recover the aramid fiber, the aramid fiber and the resin must be efficiently separated. Phenolic and epoxy resins used in helmets are crosslinked and are difficult to remove by dissolution and by physical crushing, which poses a serious obstacle to the further use of resin-bearing aramid pulp.
Disclosure of Invention
The invention aims to provide a method for preparing aramid pulp by utilizing a scrapped bulletproof helmet, which aims to overcome the defects of the prior art so that the scrapped bulletproof helmet can be effectively treated and aramid fibers can be recycled.
The invention provides a method for preparing aramid pulp by utilizing a scrapped bulletproof helmet, which comprises the following steps:
(1) disassembling the scrapped bulletproof helmet:
removing the protective cloth and the head supporting structure on the surface of the scrapped bulletproof helmet, and cutting and crushing the main body part of the scrapped bulletproof helmet into strip-shaped aramid fiber/resin composites of 1-5 cm;
(2) stripping fibers and resin:
soaking the strip-shaped aramid fiber/resin compound obtained in the step (1) in an amide solvent, wherein the addition amount of the solvent is based on the immersion of the strip-shaped aramid fiber/resin compound, the soaking time is 1-2 hours, then the compound is added into a ball mill, the ball milling is carried out for 5-10 hours, discharging is carried out, the length of the aramid fiber subjected to the ball milling is controlled within 5cm, and the amide solvent is N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide;
(3) separating fibers and resins:
pouring the ball-milled material obtained in the step (2) into 2-5 times of water, uniformly stirring, adding the mixture into a centrifuge with a screen mesh of 50-100 meshes for centrifugal treatment, adding water again for dispersing and washing the fiber material after the centrifugal treatment, then performing centrifugal treatment again, and performing centrifugal treatment for multiple times to obtain pure aramid fiber, wherein the solvent content in the aramid fiber is lower than 500ppm, and the resin content is lower than 3%;
(4) preparing pulp:
dispersing the para-aramid fiber separated and purified in the step (3) into 2-5 times of water again, stirring uniformly, defibering into dispersed short fibers by using a defibering machine, beating and decomposing into aramid pulp aqueous dispersion by using a double-disc refiner, controlling the beating degree to be 30-50 degrees SR (Shore degree), dehydrating aramid pulp water, drying, controlling the drying temperature to be 60-120 ℃, controlling the water content of the dried aramid pulp to be 3-7 wt%, drying the aramid pulp, and performing opening mechanical treatment to obtain fluffy and dried aramid pulp;
(5) and (3) solvent recovery:
and (3) filtering the mixture obtained in the step (3) by multiple times of centrifugation to remove solid impurities in the mixture, and recovering the filtered liquid by a vacuum rectification mode to be used as the solvent of the step (2).
The method for preparing the aramid pulp by utilizing the scrapped bulletproof helmet has the following advantages:
1. the method almost completely recycles the aramid fiber in the helmet, can effectively recycle the aramid fiber short fiber with higher purity, and further prepares the aramid fiber short fiber into pulp, thereby realizing the most efficient utilization of resources.
2. The method of the invention utilizes the mode of combining solvent swelling and physical shearing to strip the resin and the fiber, thereby not only having high efficiency, but also having mild condition, simple equipment and being convenient for large-scale production.
Detailed Description
The invention provides a method for preparing aramid pulp by utilizing a scrapped bulletproof helmet, which comprises the following steps:
(1) disassembling the scrapped bulletproof helmet:
removing the protective cloth and the head supporting structure on the surface of the scrapped bulletproof helmet, and cutting and crushing the main body part of the scrapped bulletproof helmet into strip-shaped aramid fiber/resin composites of 1-5 cm;
(2) stripping fibers and resin:
soaking the strip-shaped aramid fiber/resin compound obtained in the step (1) in an amide solvent, wherein the addition amount of the solvent is based on the immersion of the strip-shaped aramid fiber/resin compound, the soaking time is 1-2 hours, then the compound is added into a ball mill, the ball milling is carried out for 5-10 hours, discharging is carried out, the length of the aramid fiber subjected to the ball milling is controlled within 5cm, and the amide solvent is N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide;
(3) separating fibers and resins:
pouring the ball-milled material obtained in the step (2) into 2-5 times of water, uniformly stirring, adding the mixture into a centrifuge with a screen mesh of 50-100 meshes for centrifugal treatment, adding water again for dispersing and washing the fiber material after the centrifugal treatment, then performing centrifugal treatment again, and performing centrifugal treatment for multiple times to obtain pure aramid fiber, wherein the solvent content in the aramid fiber is lower than 500ppm, and the resin content is lower than 3%;
(4) preparing pulp:
dispersing the para-aramid fiber separated and purified in the step (3) into 2-5 times of water again, stirring uniformly, defibering into dispersed short fibers by using a defibering machine, beating and decomposing into aramid pulp aqueous dispersion by using a double-disc refiner, controlling the beating degree to be 30-50 degrees SR (Shore degree), dehydrating aramid pulp water, drying, controlling the drying temperature to be 60-120 ℃, controlling the water content of the dried aramid pulp to be 3-7 wt%, drying the aramid pulp, and performing opening mechanical treatment to obtain fluffy and dried aramid pulp;
(5) and (3) solvent recovery:
and (3) centrifuging the mixture obtained in the step (3) for many times, wherein the mixture contains resin, solvent, water and trace aramid fiber, filtering to remove solid impurities in the mixture, and recovering the filtered liquid in a vacuum rectification mode to be used as the solvent in the step (2).
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
Example 1:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and phenolic resin) are removed, the main body part of the helmet is cut and crushed into strips of 1 cm. And then soaking the strip aramid fiber/phenolic resin compound into N-methyl pyrrolidone for 2 hours, adding into a ball mill, carrying out ball milling for 5 hours, and discharging. The average length of the aramid fiber after ball milling is about 5 cm. Then pouring the ball-milled materials into 2 times of water, stirring uniformly, and adding into a 50-mesh centrifuge for centrifugal treatment. And obtaining pure aramid fiber after 3 times of circulating treatment. The final fiber had a solvent content of about 300ppm and a phenolic resin content of about 0.5%. Then dispersing the separated and purified aramid fiber into 2 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 40 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 5 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And filtering the centrifuged mixture (containing phenolic resin, N-methyl pyrrolidone, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Example 2:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and phenolic resin) are removed, the main body part of the helmet is cut and crushed into strips of 5 cm. And then soaking the strip aramid fiber/phenolic resin compound in N, N-dimethylformamide for 2h, adding the compound into a ball mill, carrying out ball milling for 10h, and discharging. The average length of the aramid fiber after ball milling is about 3 cm. Then pouring the ball-milled materials into 5 times of water, stirring uniformly, and adding into a centrifuge with a 80-mesh filter screen for centrifugal treatment. And obtaining pure aramid fiber after 5 times of circulating treatment. The final fiber had a solvent content of about 400ppm and a phenolic resin content of about 1.5%. Then dispersing the separated and purified aramid fiber into 2 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 30 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 7 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And (3) filtering the centrifuged mixture (containing phenolic resin, N-dimethylformamide, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Example 3:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and phenolic resin) are removed, the main body part of the helmet is cut and crushed into strips of 3 cm. And then soaking the strip aramid fiber/phenolic resin compound in N, N-dimethylacetamide for 1h, adding into a ball mill, ball-milling for 6h, and discharging. The average length of the aramid fiber after ball milling is about 4 cm. Then pouring the ball-milled materials into 3 times of water, stirring uniformly, and adding into a centrifuge with a 80-mesh filter screen for centrifugal treatment. And obtaining pure aramid fiber after 5 times of circulating treatment. The final fiber had a solvent content of about 200ppm and a phenolic resin content of about 1%. Then dispersing the separated and purified aramid fiber into 5 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 50 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 7 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And filtering the centrifuged mixture (containing phenolic resin, N-dimethylacetamide, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Example 4:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and epoxy resin) are removed, the main body part of the helmet is cut and crushed into 4cm strips. And then soaking the strip aramid fiber/epoxy resin composite into N-methyl pyrrolidone for 2 hours, adding into a ball mill, carrying out ball milling for 5 hours, and discharging. The average length of the aramid fiber after ball milling is about 4 cm. Then pouring the ball-milled materials into 5 times of water, stirring uniformly, and adding into a 50-mesh centrifuge for centrifugal treatment. And obtaining pure aramid fiber after 3 times of circulating treatment. The solvent content in the final fiber was about 400ppm and the epoxy resin content was about 0.5%. Then dispersing the separated and purified aramid fiber into 3 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 35 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 4 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And filtering the centrifuged mixture (containing epoxy resin, N-methyl pyrrolidone, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Example 5:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and epoxy resin) are removed, the main body part of the helmet is cut and crushed into strips of 3 cm. And then soaking the strip aramid fiber/epoxy resin composite into N, N-dimethylformamide for 1h, adding into a ball mill, carrying out ball milling for 6h, and discharging. The average length of the aramid fiber after ball milling is about 3 cm. Then pouring the ball-milled materials into 3 times of water, stirring uniformly, and adding into a centrifuge with a 80-mesh filter screen for centrifugal treatment. And obtaining pure aramid fiber after 5 times of circulating treatment. The solvent content in the final fiber was about 200ppm and the epoxy resin content was about 0.5%. Then dispersing the separated and purified aramid fiber into 2 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 45 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 6 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And filtering the centrifuged mixture (containing epoxy resin, N-dimethylformamide, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Example 6:
after the surface protective cloth and the head supporting structure of a certain retired bulletproof helmet (cured by para-aramid fiber and epoxy resin) are removed, the main body part of the helmet is cut and crushed into 1cm strips. And then soaking the strip aramid fiber/epoxy resin composite into N, N-dimethylacetamide for 1h, adding into a ball mill, ball-milling for 5h, and discharging. The average length of the aramid fiber after ball milling is about 2 cm. Then pouring the ball-milled materials into 2 times of water, stirring uniformly, and adding into a centrifuge with a 80-mesh filter screen for centrifugal treatment. And obtaining pure aramid fiber after 3 times of circulating treatment. The solvent content in the final fiber was about 200ppm and the epoxy resin content was about 0.5%. Then dispersing the separated and purified aramid fiber into 5 times of water again, uniformly stirring, then using a fluffer to fluff the aramid fiber into dispersed short fibers, and then using a double-disc refiner to beat the aramid fiber pulp into the aramid fiber pulp aqueous dispersion, wherein the beating degree is controlled to be about 40 DEG SR. Dehydrating and drying the aramid pulp, controlling the drying temperature to be between 60 and 120 ℃, and controlling the water content of the pulp after drying to be about 6 wt%. And drying the pulp, and then performing opening mechanical treatment to obtain the fluffy and dry aramid pulp. And filtering the centrifuged mixture (containing epoxy resin, N-dimethylacetamide, water and trace aramid fiber) to remove solid impurities, and recovering the solvent from the liquid by means of reduced pressure rectification.
Claims (1)
1. A method for preparing aramid pulp by using a scrapped bulletproof helmet is characterized by comprising the following steps:
(1) disassembling the scrapped bulletproof helmet:
removing the protective cloth and the head supporting structure on the surface of the scrapped bulletproof helmet, and cutting and crushing the main body part of the scrapped bulletproof helmet into strip aramid fiber/phenolic resin or epoxy resin compounds with the length of 1-5 cm;
(2) release fibers and phenolic or epoxy resins:
soaking the strip aramid fiber/phenolic resin or epoxy resin compound obtained in the step (1) into an amide solvent, wherein the addition amount of the solvent is based on the immersion of the strip aramid fiber/phenolic resin or epoxy resin compound, the soaking time is 1-2 hours, then adding the mixture into a ball mill, performing ball milling for 5-10 hours, discharging, controlling the length of the aramid fiber subjected to ball milling within 5cm, and the amide solvent is N-methylpyrrolidone, N-dimethylformamide or N, N-dimethylacetamide;
(3) separation fiber and phenolic or epoxy resin:
pouring the ball-milled material obtained in the step (2) into 2-5 times of water, uniformly stirring, adding the mixture into a centrifuge with a screen mesh of 50-100 meshes for centrifugal treatment, adding water again for dispersing and washing the fiber material after the centrifugal treatment, then performing centrifugal treatment again, and performing centrifugal treatment for multiple times to obtain pure aramid fiber, wherein the solvent content in the aramid fiber is lower than 500ppm, and the resin content is lower than 3%;
(4) preparing pulp:
dispersing the para-aramid fiber separated and purified in the step (3) into 2-5 times of water again, uniformly stirring, fluffing into dispersed short fibers by using a fluffer, beating and fluffing into an aramid pulp water dispersion liquid by using a double-disc refiner, controlling the beating degree to be 30-50 DEG SR, dehydrating and drying aramid pulp water, controlling the drying temperature to be 60-120 ℃, enabling the water content of the dried aramid pulp to be 3-7 wt%, drying the aramid pulp, and then performing opening mechanical treatment to obtain fluffy and dried aramid pulp;
(5) and (3) solvent recovery:
and (3) filtering the mixture obtained in the step (3) by multiple times of centrifugation to remove solid impurities in the mixture, and recovering the filtered liquid by a vacuum rectification mode to be used as the solvent of the step (2).
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| CN110760096A (en) * | 2019-10-29 | 2020-02-07 | 中国科学院山西煤炭化学研究所 | Method for dissolving para-aramid in waste bulletproof clothes |
| CN114226409A (en) * | 2021-12-08 | 2022-03-25 | 江苏安卡新材料科技有限公司 | Fiber recovery process |
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| CN1456719A (en) * | 2003-06-05 | 2003-11-19 | 上海依极科技有限公司 | Production of aromatic copolymide fiber dissolving pulp |
| CN101250771A (en) * | 2008-04-01 | 2008-08-27 | 上海依极科技有限公司 | Method for producing aramid fiber pulp by aramid fiber waste material |
| CN102391543A (en) * | 2011-09-02 | 2012-03-28 | 中国科学院宁波材料技术与工程研究所 | Method for recovering carbon-fiber enhanced epoxy resin composite material |
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