Preparation method of leakage-proof adsorption material

Abstract

The invention discloses a preparation method of a leakproof adsorption material, which comprises the following steps: S1, respectively crushing metallocene polypropylene, styrene and an organic peroxide degradation agent, uniformly mixing, extruding a melt through a single screw extruder, and carrying out water cooling, traction, pelletizing and drying to obtain molten particles; s2, processing the melt-blown grafted material particles through a melt-blown unit to prepare melt-blown non-woven fabric; s3, cutting the melt-blown non-woven fabric into a required size, soaking the melt-blown non-woven fabric in ethanol, and drying the melt-blown non-woven fabric in a drying oven after surface impurities are removed; s4, dipping the dried melt-blown non-woven fabric in a grafting reaction solution, placing the melt-blown non-woven fabric in a nitrogen environment, and then placing the melt-blown non-woven fabric in an ultraviolet environment for irradiation to initiate a grafting reaction; and S5, washing the melt-blown non-woven fabric subjected to the grafting reaction, placing the melt-blown non-woven fabric in dimethyl sulfoxide, removing impurities, and placing the melt-blown non-woven fabric in a drying oven to obtain the leakage-proof adsorption material. The oil stain leakage-proof adsorption device has the advantages that oil stain leakage-proof adsorption can be effectively achieved, and the adsorption capacity is high.

Description

Technical Field

[0001] The invention relates to the technical field of adsorption materials, and in particular to a method for preparing a leakage-proof adsorption material. Background Art

[0002] The phenomenon of a substance transferring from one phase to another is called adsorption. At present, anti-spill materials are necessary in factory workshops, cruise ships, oil wells and oil depots and other working environments. The principle of using anti-spill materials is to use their own hydrophobic and oleophilic properties and the gaps between polymer molecules to absorb oil stains.

[0003] Lightweight polypropylene (PP) is uniform in quality, not easy to loosen, reusable, and has a large adsorption area. It is often used to clean up and recover spilled oil. Existing materials used to contain spills are usually ordinary PP materials, which have weak adsorption capacity, are easily deformed after absorbing liquid, and have poor oil retention performance. Oil easily overflows from PP non-woven fabrics, causing environmental pollution. In addition, since PP materials cannot intuitively show the adsorption situation, it is difficult for users to deal with the spill in time, which is inconvenient in use. Summary of the invention

[0004] The purpose of the present invention is to provide a method for preparing a leakproof adsorption material, which can effectively realize the leakproof adsorption of oil pollution and has a strong adsorption capacity.

[0005] The above technical objectives of the present invention are achieved through the following technical solutions:

[0006] A method for preparing a leakproof adsorbent material, characterized in that it comprises the following steps:

[0007] S1, taking metallocene polypropylene, styrene and an organic peroxide degradation agent and crushing them respectively and mixing them evenly, extruding the melt through a single screw extruder, and then cooling with water, pulling, pelletizing and drying to obtain molten pellets;

[0008] S2, processing the melt-grafted pellets through a melt-blown unit to prepare a melt-blown nonwoven fabric;

[0009] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven;

[0010] S4, immersing the dried melt-blown nonwoven fabric in a grafting reaction solution, placing it in a nitrogen environment, and then irradiating it in an ultraviolet environment to induce a grafting reaction;

[0011] S5, washing the melt-blown nonwoven fabric after the grafting reaction is completed, placing it in dimethyl sulfoxide, removing impurities and placing it in an oven to obtain a leak-proof adsorption material.

[0012] Preferably, the mass ratio of the metallocene polypropylene, styrene and organic peroxide degradation agent in S1 is 91:9:1.

[0013] Preferably, the organic peroxide degradation agent in S1 is selected from one of di-tert-butyl peroxide, diisopropylbenzene peroxide, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane or 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane.

[0014] Preferably, the extrusion parameters of the single screw extruder in S1 are: temperature of zone 1 is 180° C., temperature of zone 2 is 190° C., and screw speed is 60 r / min.

[0015] Preferably, the melt-blowing parameters of the melt-blowing unit in S2 are: extruder temperature is 160-230°C, metering pump temperature is 270-300°C, flow channel temperature is 270-290°C, hot air temperature is 300-310°C, receiving distance is 15-20cm, metering pump speed is 10-12r / min, and the gram weight of the melt-blown non-woven fabric is 25-30g / m 2 .

[0016] Preferably, the oven temperature in S3 is 70-85°C.

[0017] Preferably, the preparation method of the grafting reaction solution in S4 is: first dissolve benzophenone in acetone to obtain an acetone solution with a mass fraction of 4-6% benzophenone, then dissolve N-vinyl pyrrolidone in deionized water to obtain an N-vinyl pyrrolidone solution with a mass fraction of 20-25%, and mix the acetone solution of benzophenone and the N-vinyl pyrrolidone solution in a mass ratio of 1:2 to obtain a grafting reaction solution.

[0018] Preferably, the wavelength of the ultraviolet light in S4 is 365nm and the irradiance is 45mW / cm 2 .

[0019] Preferably, S5 is specifically as follows: washing the meltblown nonwoven fabric that has completed the grafting reaction in deionized water, ethanol, and acetone for multiple times in sequence, then soaking the meltblown nonwoven fabric that has completed the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours, rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0020] In summary, the present invention has the following beneficial effects:

[0021] 1. The present invention adopts a modification method of melt-grafting styrene onto metallocene polypropylene to introduce a styrene functional unit with low crystallinity and a solubility parameter similar to that of benzene series, thereby breaking free from the restraint of water on the fiber surface, greatly enhancing the mass transfer effect between oil and fiber, and adsorbing benzene series through the principle of like dissolves like, thereby significantly improving the saturated adsorption capacity of benzene series, and preparing the corresponding oil-absorbing fiber using melt-blown spinning technology.

[0022] 2. The present invention subsequently introduces lipophilic groups on the surface of polypropylene non-woven fabric by using ultraviolet grafting technology through a graft polymerization method to prepare a new type of oil-absorbing material with strong adsorption capacity, not easy to deform after absorbing liquid, and excellent oil retention performance. DETAILED DESCRIPTION

[0023] The specific implementation modes of the present invention are further described below, and these embodiments do not constitute a limitation of the present invention.

[0024] A method for preparing a leak-proof adsorbent material comprises the following steps:

[0025] S1, taking metallocene polypropylene, styrene and an organic peroxide degradation agent in a mass ratio of 91:9:1, respectively crushing and mixing them evenly, and then extruding the melt through a single screw extruder, and then obtaining molten pellets after water cooling, pulling, pelletizing and drying. The extrusion parameters of the single screw extruder are: a zone 1 temperature of 180° C., a zone 2 temperature of 190° C., and a screw speed of 60 r / min. The organic peroxide degradation agent is selected from one of di-tert-butyl peroxide, diisopropylbenzene peroxide, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane or 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane.

[0026] S2, the molten grafted pellets are processed by a melt-blown unit to prepare a melt-blown non-woven fabric. The melt-blown parameters of the melt-blown unit are: extruder temperature is 160-230°C, metering pump temperature is 270-300°C, flow channel temperature is 270-290°C, hot air temperature is 300-310°C, receiving distance is 15-20cm, metering pump speed is 10-12r / min, and the gram weight of the melt-blown non-woven fabric is 25-30g / m 2 .

[0027] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven at 70-85°C.

[0028] S4, the dried melt-blown nonwoven fabric is immersed in the grafting reaction solution and placed in a nitrogen environment, and then placed in a wavelength of 365nm and an irradiance of 45mW / cm 2 The grafting reaction was initiated by irradiation under ultraviolet light.

[0029] S5, washing the melt-blown non-woven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in turn, then soaking the melt-blown non-woven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours to remove excess solvent and impurities such as unreacted initiator and monomer, and rinsing with a large amount of deionized water after soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0030] The preparation method of the grafting reaction solution is as follows: firstly dissolving benzophenone in acetone to obtain an acetone solution with a mass fraction of 4-6% benzophenone, then dissolving N-vinyl pyrrolidone in deionized water to obtain an N-vinyl pyrrolidone solution with a mass fraction of 20-25%, and mixing the acetone solution of benzophenone and the N-vinyl pyrrolidone solution in a mass ratio of 1:2 to obtain a grafting reaction solution.

[0031] Example 1

[0032] A method for preparing a leak-proof adsorbent material comprises the following steps:

[0033] S1, taking metallocene polypropylene, styrene and organic peroxide degradation agent diisopropylbenzene peroxide in a mass ratio of 91:9:1, respectively crushing and mixing evenly, and then extruding the melt through a single screw extruder, and then obtaining molten pellets after water cooling, pulling, pelletizing and drying. The extrusion parameters of the single screw extruder are: zone 1 temperature 180°C, zone 2 temperature 190°C, and screw speed 60r / min.

[0034] S2, the molten grafted pellets are processed by a melt-blown unit to prepare a melt-blown non-woven fabric. The melt-blown parameters of the melt-blown unit are: extruder temperature is 160°C, metering pump temperature is 270°C, flow channel temperature is 270°C, hot air temperature is 300°C, receiving distance is 15cm, metering pump speed is 12r / min, and the gram weight of the melt-blown non-woven fabric is 30g / m 2 .

[0035] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven at 70°C.

[0036] S4, the dried melt-blown nonwoven fabric is immersed in the grafting reaction solution and placed in a nitrogen environment, and then placed in a wavelength of 365nm and an irradiance of 45mW / cm 2 The grafting reaction was initiated by irradiation under ultraviolet light.

[0037] S5, washing the melt-blown non-woven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in turn, then soaking the melt-blown non-woven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours to remove excess solvent and impurities such as unreacted initiator and monomer, and rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0038] Example 2

[0039] A method for preparing a leak-proof adsorbent material comprises the following steps:

[0040] S1, take metallocene polypropylene, styrene and organic peroxide degradation agent 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane in a mass ratio of 91:9:1, grind them respectively and mix them evenly, then extrude the melt through a single screw extruder, and then obtain molten pellets after water cooling, pulling, pelletizing and drying. The extrusion parameters of the single screw extruder are: zone 1 temperature 180°C, zone 2 temperature 190°C, and screw speed 60r / min.

[0041] S2, the molten grafted pellets are processed by a melt-blown unit to prepare a melt-blown non-woven fabric. The melt-blown parameters of the melt-blown unit are: extruder temperature is 170°C, metering pump temperature is 280°C, flow channel temperature is 280°C, hot air temperature is 300°C, receiving distance is 17cm, metering pump speed is 11r / min, and the gram weight of the melt-blown non-woven fabric is 27g / m 2 .

[0042] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven at 75°C.

[0043] S4, the dried melt-blown nonwoven fabric is immersed in the grafting reaction solution and placed in a nitrogen environment, and then placed in a wavelength of 365nm and an irradiance of 45mW / cm 2 The grafting reaction was initiated by irradiation under ultraviolet light.

[0044] S5, washing the melt-blown non-woven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in turn, then soaking the melt-blown non-woven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours to remove excess solvent and impurities such as unreacted initiator and monomer, and rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0045] Example 3

[0046] A method for preparing a leak-proof adsorbent material comprises the following steps:

[0047] S1, taking metallocene polypropylene, styrene and organic peroxide degradation agent 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane in a mass ratio of 91:9:1, respectively crushing and mixing evenly, and then extruding the melt through a single screw extruder, and then obtaining molten pellets after water cooling, pulling, pelletizing and drying. The extrusion parameters of the single screw extruder are: zone 1 temperature 180°C, zone 2 temperature 190°C, and screw speed 60r / min.

[0048] S2, the molten grafted pellets are processed by a melt-blown unit to prepare a melt-blown non-woven fabric. The melt-blown parameters of the melt-blown unit are: extruder temperature is 210°C, metering pump temperature is 290°C, flow channel temperature is 280°C, hot air temperature is 310°C, receiving distance is 18cm, metering pump speed is 12r / min, and the gram weight of the melt-blown non-woven fabric is 30g / m 2 .

[0049] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven at 80°C.

[0050] S4, the dried melt-blown nonwoven fabric is immersed in the grafting reaction solution and placed in a nitrogen environment, and then placed in a wavelength of 365nm and an irradiance of 45mW / cm 2 The grafting reaction was initiated by irradiation under ultraviolet light.

[0051] S5, washing the melt-blown non-woven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in turn, then soaking the melt-blown non-woven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours to remove excess solvent and impurities such as unreacted initiator and monomer, and rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0052] Example 4

[0053] A method for preparing a leak-proof adsorbent material comprises the following steps:

[0054] S1, taking metallocene polypropylene, styrene and organic peroxide degradation agent diisopropylbenzene peroxide in a mass ratio of 91:9:1, respectively crushing and mixing evenly, and then extruding the melt through a single screw extruder, and then obtaining molten pellets after water cooling, pulling, pelletizing and drying. The extrusion parameters of the single screw extruder are: zone 1 temperature 180°C, zone 2 temperature 190°C, and screw speed 60r / min.

[0055] S2, the molten grafted pellets are processed by a melt-blown unit to prepare a melt-blown non-woven fabric. The melt-blown parameters of the melt-blown unit are: extruder temperature is 230°C, metering pump temperature is 300°C, flow channel temperature is 290°C, hot air temperature is 310°C, receiving distance is 20cm, metering pump speed is 12r / min, and the gram weight of the melt-blown non-woven fabric is 30g / m 2 .

[0056] S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven at 85°C.

[0057] S4, the dried melt-blown nonwoven fabric is immersed in the grafting reaction solution and placed in a nitrogen environment, and then placed in a wavelength of 365nm and an irradiance of 45mW / cm 2 The grafting reaction was initiated by irradiation under ultraviolet light.

[0058] S5, washing the melt-blown non-woven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in turn, then soaking the melt-blown non-woven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours to remove excess solvent and impurities such as unreacted initiator and monomer, and rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.

[0059] Taking the oil-absorbing felt with a polypropylene content of ≥99% available on the market as a comparative example, the adsorption performance of the leak-proof adsorbent materials obtained in Examples 1-4 and the comparative example were tested at room temperature and pressure. The test conditions and results are shown in the following table.

[0060] size Benzene adsorption Crude oil adsorption Crude oil retention rate Example 1 1cm×5cm 40.1wt.% 8.0 times its own weight 92.3％ Example 2 1cm×5cm 41.2wt.% 8.2 times its own weight 92.5％ Example 3 1cm×5cm 39.2wt.% 7.8 times its own weight 91.6％ Example 4 1cm×5cm 39.8wt.% 7.9 times its own weight 90.7％ Comparative Example 1 1cm×5cm 30.9wt.% 5.9 times its own weight 79.2％

[0061] The present invention adopts a modification method of melt-grafting styrene onto metallocene polypropylene to introduce a styrene functional unit with low crystallinity and a solubility parameter similar to that of benzene series, thereby breaking free from the restraint of water on the fiber surface, greatly enhancing the mass transfer effect between oil and fiber, and adsorbing benzene series through the principle of like dissolves like, thereby significantly improving the saturated adsorption capacity of benzene series, and preparing corresponding oil-absorbing fibers using melt-blowing spinning technology.

[0062] The present invention subsequently introduces lipophilic groups on the surface of the polypropylene non-woven fabric by using a graft polymerization method and ultraviolet grafting technology to prepare a new type of oil-absorbing material with strong adsorption capacity, not easy to deform after absorbing liquid, and excellent oil retention performance.

[0063] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Those skilled in the art may make various modifications or equivalent substitutions to the present invention within the essence and protection scope of the present invention, and such modifications or equivalent substitutions should also be deemed to fall within the protection scope of the technical solution of the present invention.

Claims

1. A method for preparing a leakproof adsorbent material, characterized in that: The steps include: S1, taking metallocene polypropylene, styrene and an organic peroxide degradation agent and crushing them respectively and mixing them evenly, extruding the melt through a single screw extruder, and then cooling with water, pulling, pelletizing and drying to obtain molten pellets; S2, processing the melt-grafted pellets through a melt-blown unit to prepare a melt-blown nonwoven fabric; S3, cutting the meltblown nonwoven fabric into required sizes, soaking it in ethanol, removing surface impurities and drying it in an oven; S4, immersing the dried melt-blown nonwoven fabric in a grafting reaction solution, placing it in a nitrogen environment, and then irradiating it in an ultraviolet environment to induce a grafting reaction; S5, washing the melt-blown nonwoven fabric after the grafting reaction is completed, placing it in dimethyl sulfoxide, removing impurities and placing it in an oven to obtain a leak-proof adsorption material.

2. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The mass ratio of the metallocene polypropylene, styrene and organic peroxide degradation agent in S1 is 91:9:

1.

3. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The organic peroxide degradation agent in S1 is selected from one of di-tert-butyl peroxide, diisopropylbenzene peroxide, 2,5-dimethyl-2,5-di(tert-butylperoxy)hexane or 3,6,9-triethyl-3,6,9-trimethyl-1,4,7-triperoxynonane.

4. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The extrusion parameters of the single screw extruder in S1 are: temperature of zone 1 is 180° C., temperature of zone 2 is 190° C., and screw speed is 60 r / min.

5. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The melt-blowing parameters of the melt-blowing unit in S2 are as follows: the extruder temperature is 160-230°C, the metering pump temperature is 270-300°C, the flow channel temperature is 270-290°C, the hot air temperature is 300-310°C, the receiving distance is 15-20cm, the metering pump speed is 10-12r / min, and the gram weight of the melt-blown non-woven fabric is 25-30g / m 2 .

6. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The oven temperature in S3 is 70-85°C.

7. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The preparation method of the grafting reaction solution in S4 is: first dissolve benzophenone in acetone to obtain an acetone solution with a mass fraction of 4-6% benzophenone, then dissolve N-vinyl pyrrolidone in deionized water to obtain an N-vinyl pyrrolidone solution with a mass fraction of 20-25%, and mix the acetone solution of benzophenone and the N-vinyl pyrrolidone solution in a mass ratio of 1:2 to obtain a grafting reaction solution.

8. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The wavelength of the ultraviolet light in S4 is 365nm and the irradiance is 45mW / cm 2 .

9. The method for preparing a leakproof adsorbent material according to claim 1, characterized in that: The S5 is specifically as follows: washing the meltblown nonwoven fabric after the grafting reaction in deionized water, ethanol and acetone for multiple times in sequence, then soaking the meltblown nonwoven fabric after the grafting reaction in excess dimethyl sulfoxide, standing at 60°C for 6 hours, rinsing with a large amount of deionized water after the soaking, and then drying in a 60°C oven to obtain a leak-proof adsorption material.