CN111841505A - Preparation method of collagen fiber aerogel material for efficiently capturing iodine vapor - Google Patents

Preparation method of collagen fiber aerogel material for efficiently capturing iodine vapor Download PDF

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CN111841505A
CN111841505A CN202010723453.2A CN202010723453A CN111841505A CN 111841505 A CN111841505 A CN 111841505A CN 202010723453 A CN202010723453 A CN 202010723453A CN 111841505 A CN111841505 A CN 111841505A
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collagen fiber
iodine vapor
deionized water
collagen
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CN111841505B (en
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周建
朱辉
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Southwest University of Science and Technology
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Abstract

The invention discloses a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor, which comprises the following steps: adding collagen fibers into water, ultrasonically cleaning, washing to be neutral, filtering and drying; crushing the cleaned collagen fibers in a crusher, adding the collagen fibers into water, adding an alkali modifier solution, and mixing to obtain a suspension; transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, carrying out hydrothermal reaction, cooling, washing to be neutral, filtering, and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3-5 times by using deionized water and absolute ethyl alcohol; and (3) washing the product in deionized water to be neutral, freezing the product in a low-temperature refrigerator, and drying the product in a vacuum low-temperature freeze dryer to obtain the collagen fiber aerogel high-efficiency iodine vapor capturing material. The preparation method disclosed by the invention is simple in preparation process, low in cost, green and environment-friendly, and avoids secondary pollution to the environment in the preparation process.

Description

Preparation method of collagen fiber aerogel material for efficiently capturing iodine vapor
Technical Field
The invention belongs to the environmental protection field of biomass waste resources used for radioactive iodine vapor adsorption in the environment, and particularly relates to a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor.
Background
With the rise of the leather-making industry, the market demand of leather is large, but the utilization rate of raw material animal skin in the leather-making process is not high, so that a large amount of leather raw materials are wasted, particularly, waste materials with small particle sizes are difficult to reuse, and meanwhile, the environment is also seriously polluted. How to reuse the leather waste resources is always a hot issue of attention of researchers. Research shows that the leather waste can be converted into collagen fibers with strong hydrophilicity after being washed, subjected to alkali treatment, dehydrated and the like by a conventional method. As natural high molecular substance, the collagen fiber has a spiral structure composed of three polypeptide chains, has a unique molecular structure and excellent physical properties, and contains various functional groups including-OH, -COOH and-NH2and-CONH2Etc., containing numerous intramolecular hydrogen bonds. Although the collagen fiber has strong hydrophilic performance and is insoluble in water, the collagen fiber is in a dispersed state after swelling in water, shows excellent specific surface area and has good biocompatibility, and is easy to biodegrade in the later period without polluting the environment.
With the rapid development of the nuclear energy industry in China, the safe treatment of nuclear radioactive waste becomes the focus of increasing attention, especially the leakage of the nuclear power station in Fudao of Japan causes the existence of a large amount of radioactive gas iodine and inorganic iodine in the environment of the surrounding area, wherein129The longest I half-life (1.6X 10)7Year), radiation damage such as thyroid gland pathological changes can be caused, and radioactive iodine existing in nature can be finally enriched in a human body through a food chain path. Therefore, the removal of radioactive gaseous iodine from ambient gases is a very important task. At present, the adsorption material for radioactive gaseous iodine mainly comprises zeolites and activated carbon, but the wide application is limited by factors such as difficult later-stage treatment, low recycling rate, high practical application cost and the like. Recently, adsorbent materials such as COFS, MOFS, POPs, CMPs and aerogelThe preparation method has the advantages of good performance, large specific surface area, abundant microporous structures and strong adsorption effect on gaseous iodine, but practical application is limited due to the problems of complex preparation process, high preparation cost, low stability, difficult later-stage treatment and the like.
Disclosure of Invention
Aiming at the technical defects, the invention provides the collagen fiber aerogel material which has the advantages of low preparation cost, simple preparation process, no secondary pollution to the environment, high iodine vapor adsorption capacity, high stability and natural biodegradation. The invention combines the characteristics of collagen fiber, firstly carries out alkali treatment on the collagen fiber, breaks the hydrogen bonds in molecules, exposes more hydroxyl and amino, and enhances the affinity ability to iodine vapor. Then treated by a hydrothermal reaction kettle to ensure that the internal cross-linking bond is irreversibly broken and the structure and the property are stabilized. And then preparing the flocculent collagen fiber aerogel material which is light in weight, large in specific surface area, porous and stable by a freeze-drying technology. The aerogel material enhances the adsorption capacity to iodine vapor, and has the technical characteristics that the adsorption effect is mainly physical adsorption and is auxiliary chemical adsorption.
An object of the present invention is to solve at least the above problems and/or disadvantages and to provide at least the advantages described hereinafter.
To achieve these objects and other advantages in accordance with the present invention, there is provided a method for preparing a collagen fiber aerogel material with high efficiency for capturing iodine vapor, comprising the steps of:
adding collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaning machine, cleaning to be neutral, filtering, and drying in an oven;
step two, crushing the cleaned collagen fibers in a crusher, adding the collagen fibers into deionized water, and then adding an alkali modifier solution for mixing to obtain a suspension;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, carrying out hydrothermal reaction, and then cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3-5 times by using deionized water and absolute ethyl alcohol;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator, and drying the reaction product in a vacuum low-temperature freeze dryer to obtain the collagen fiber aerogel high-efficiency iodine vapor capturing material.
Preferably, the collagen fiber in the first step is animal skin without tanning treatment, and is washed, alkali treated, dehydrated and the like by a conventional method, and then is crushed by a crusher to obtain granular substances with the grain diameter of 10-80 meshes.
Preferably, the ultrasonic cleaning temperature and the oven temperature in the first step are in the range of room temperature to 70 ℃.
Preferably, the particle size of the collagen fiber crushed in the second step is controlled to be 30-100 meshes.
Preferably, in the second step, the mass ratio of the collagen fibers to the deionized water is 1: 80-120; the alkali modifier in the alkali modifier solution accounts for 5-20% of the mass of the collagen fibers; the alkali modifier solution is one or more of potassium hydroxide solution, sodium hydroxide solution, ammonium hydroxide solution and sodium carbonate solution; the mass fraction of the alkali modifier solution is 5-10%.
Preferably, in the second step, the collagen fibers are taken and added into deionized water, and then an alkali modifier solution is added for mixing in the following manner: adding collagen fibers, deionized water and an alkali modifier solution into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 38-45 ℃ and the pressure at 15-25 MPa for 30-45 min, and releasing pressure within 30-60 s; after pressure release, the reaction mass was added to an ultrasonic reactor and treated with ultrasound.
Preferably, the ultrasonic treatment frequency is 45-90 kHz, the power is 100-450W, the temperature is 40-50 ℃, and the time is 30-45 min.
Preferably, in the third step, the temperature range of the hydrothermal reaction is 90-180 ℃, and the reaction time is 0.5-24 h; the volume concentration of the glutaraldehyde solution is 0.1-10% (glutaraldehyde: water, v/v), the curing temperature is 10-60 ℃, and the curing time is 0.5-8 h.
Preferably, in the fourth step, the freezing temperature in the low-temperature refrigerator is-20 ℃; the temperature for drying in the vacuum low temperature freeze dryer is-50 ℃.
The invention at least comprises the following beneficial effects:
(1) the flocculent collagen fiber aerogel is light and soft in texture, large in pores, large in specific surface area, not easy to absorb water and agglomerate, stable in property, high in iodine vapor adsorption capacity which is far higher than that of other types of biomass materials, and high in cyclic utilization rate.
(2) The raw materials used in the invention are waste materials generated by processing the leather scraps, the resources are recycled, the problem of environmental pollution is avoided, the sources are wide, the price is low, and the later natural organisms are more easily degraded.
(3) The preparation method disclosed by the invention is simple in preparation process, low in cost, green and environment-friendly, and avoids secondary pollution to the environment in the preparation process.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Description of the drawings:
FIG. 1 is a schematic diagram of a collagen fiber aerogel material for capturing iodine vapor with high efficiency, which is prepared in example 5 of the present invention;
FIG. 2 is a diagram of a collagen fiber aerogel prepared in example 5 of the present invention after iodine vapor is adsorbed by the iodine vapor-capturing material;
FIG. 3 is a graph showing the result of adsorption of iodine vapor by the collagen fiber aerogel efficient capturing iodine vapor material prepared in embodiments 1 to 5 of the present invention at different time intervals;
FIG. 4 is a graph showing the result of adsorbing iodine vapor at different intervals by the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 1 and 6 of the present invention;
FIG. 5 is a graph showing the results of adsorbing iodine vapor at different intervals by the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 4 and 7 of the present invention;
FIG. 6 is a graph showing the result of adsorbing iodine vapor at different intervals by the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 5 and 8 of the present invention;
FIG. 7 is a graph showing the results of adsorbing iodine vapor at different intervals by the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 2 and 9 of the present invention;
FIG. 8 is a graph showing the results of adsorbing iodine vapor at different intervals by the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 3 and 10 of the present invention;
FIG. 9 is a graph showing the result of iodine vapor cyclic adsorption of the collagen fiber aerogel efficient iodine vapor capturing material prepared in embodiments 1 to 5 of the present invention;
FIG. 10 is a graph showing the result of iodine vapor adsorption in cycles of the collagen fiber aerogel high-efficiency iodine vapor capturing materials prepared in examples 1 and 6 of the present invention;
fig. 11 is a graph showing the result of iodine vapor adsorption in cycles of the collagen fiber aerogel high-efficiency iodine vapor capturing material prepared in example 2 and example 9 of the present invention;
FIG. 12 is a graph showing the results of iodine vapor adsorption in cycles of the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 3 and 10 of the present invention;
FIG. 13 is a graph showing the results of iodine vapor adsorption in cycles of the collagen fiber aerogel high efficiency iodine vapor capturing materials prepared in examples 4 and 7 of the present invention;
fig. 14 is a graph showing the result of iodine vapor cyclic adsorption of the collagen fiber aerogel high-efficiency iodine vapor trapping material prepared in example 5 and example 8 of the present invention.
The specific implementation mode is as follows:
the present invention is further described in detail below with reference to the attached drawings so that those skilled in the art can implement the invention by referring to the description text.
It will be understood that terms such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 40 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber into 500mL of deionized water, then adding 5g of potassium hydroxide solution with the mass fraction of 5%, mixing, and stirring to obtain a suspension;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 100 ℃ for 5 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 2:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 50 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber into 500mL of deionized water, then adding 10g of ammonium hydroxide solution with the mass fraction of 5%, mixing, and stirring to obtain a suspension;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 120 ℃ for 5 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 3:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 55 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber into 500mL of deionized water, then adding 20g of mixed solution of 5% by mass of ammonium hydroxide and sodium hydroxide, mixing, and stirring to obtain suspension; the mass ratio of the ammonium hydroxide to the sodium hydroxide is 1: 1;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 150 ℃ for 8 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 4:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 60 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 60 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 80-mesh particles; adding 5g of collagen fiber into 500mL of deionized water, then adding 15g of mixed solution of 5% by mass of ammonium hydroxide, sodium hydroxide and sodium carbonate, mixing, and stirring to obtain suspension; the mass ratio of the ammonium hydroxide to the sodium hydroxide to the ammonium carbonate is 1:1: 1;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 150 ℃ for 12 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 5:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 60 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 60 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 80-mesh particles; adding 5g of collagen fiber into 500mL of deionized water, then adding 15g of mixed solution of 5% by mass of ammonium hydroxide, potassium hydroxide and sodium carbonate, mixing, and stirring to obtain suspension; the mass ratio of the ammonium hydroxide to the potassium hydroxide to the ammonium carbonate is 1:1: 1;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 180 ℃ for 18h, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 6:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 40 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber, 500mL of deionized water and 5g of 5% by mass potassium hydroxide solution into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 45 ℃ and the pressure at 25MPa for 45min, and releasing pressure within 60 s; after pressure relief, adding the reaction materials into an ultrasonic reactor, and carrying out ultrasonic treatment to obtain a suspension; the ultrasonic treatment frequency is 45kHz, the power is 350W, the temperature is 50 ℃, and the time is 45 min;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 100 ℃ for 5 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 7:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 60 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 60 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 80-mesh particles; adding 5g of collagen fiber, 500mL of deionized water and 15g of a mixed solution of 5% by mass of ammonium hydroxide, sodium hydroxide and sodium carbonate into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 45 ℃ and the pressure at 25MPa for 45min, and releasing the pressure within 60 s; after pressure relief, adding the reaction materials into an ultrasonic reactor, and carrying out ultrasonic treatment to obtain a suspension; the ultrasonic treatment frequency is 45kHz, the power is 350W, the temperature is 50 ℃, and the time is 45 min;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 150 ℃ for 12 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 8:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 60 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 60 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 80-mesh particles; adding 5g of collagen fiber, 500mL of deionized water and 15g of a mixed solution of 5% by mass of ammonium hydroxide, potassium hydroxide and sodium carbonate into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 45 ℃ and the pressure at 20MPa for 45min, and releasing the pressure within 60 s; after pressure relief, adding the reaction materials into an ultrasonic reactor, and carrying out ultrasonic treatment to obtain a suspension; the ultrasonic treatment frequency is 45kHz, the power is 350W, the temperature is 50 ℃, and the time is 45 min;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 180 ℃ for 18h, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 9:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 50 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber, 500mL of deionized water and 10g of ammonium hydroxide solution with the mass fraction of 5% into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 45 ℃ and the pressure at 20MPa for 45min, and releasing the pressure within 60 s; after pressure relief, adding the reaction materials into an ultrasonic reactor, and carrying out ultrasonic treatment to obtain a suspension; the ultrasonic treatment frequency is 55kHz, the power is 350W, the temperature is 50 ℃, and the time is 45 min;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 120 ℃ for 5 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Example 10:
a preparation method of a collagen fiber aerogel material for efficiently capturing iodine vapor comprises the following steps:
step one, washing animal skins which are not tanned, carrying out alkali treatment, dehydration and other treatments according to a conventional method, crushing the animal skins by a crusher to obtain granular collagen fibers with the grain diameter of 40 meshes, adding the granular collagen fibers into deionized water, carrying out ultrasonic washing for 5 hours in an ultrasonic washing machine, washing the collagen fibers to be neutral, filtering the collagen fibers, and drying the collagen fibers in an oven; wherein the ultrasonic cleaning temperature and the oven temperature are controlled to be 55 ℃;
step two, crushing the cleaned collagen fibers in a crusher to obtain 60-mesh particles; adding 5g of collagen fiber, 500mL of deionized water and 20g of a mixed solution of 5% by mass of ammonium hydroxide and sodium hydroxide into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 45 ℃ and the pressure at 20MPa for 45min, and releasing the pressure within 60 s; after pressure relief, adding the reaction materials into an ultrasonic reactor, and carrying out ultrasonic treatment to obtain a suspension; the ultrasonic treatment frequency is 55kHz, the power is 350W, the temperature is 50 ℃, and the time is 45 min; the mass ratio of the ammonium hydroxide to the sodium hydroxide is 1: 1;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, reacting at the temperature of 150 ℃ for 8 hours, and cooling to room temperature; washing the reaction product in deionized water to be neutral, filtering and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3 times by using deionized water and absolute ethyl alcohol; the volume concentration of the glutaraldehyde solution is 1%, the curing temperature is 35 ℃, and the curing time is 4 hours;
and step four, washing the reaction product obtained in the step three in deionized water to be neutral, freezing the reaction product in a low-temperature refrigerator at the temperature of 20 ℃ below zero, and drying the reaction product in a vacuum low-temperature freeze dryer at the temperature of 50 ℃ below zero to obtain the yellow flocculent collagen fiber aerogel material for efficiently capturing iodine vapor.
Wherein the BET specific surface area of the untreated collagen fibers in the first step is 18.57m2/g。
The collagen fiber aerogel high-efficiency iodine vapor capturing material prepared in the examples 1 to 10 is subjected to specific surface area test and total pore volume test, and the results are shown in table 1;
TABLE 1
Figure BDA0002600848670000111
Figure BDA0002600848670000121
FIG. 1 is a photograph of a physical representation of the collagen fiber aerogel material prepared in example 5; the prepared collagen fiber aerogel material is light, loose and cotton-shaped dark yellow substance; FIG. 2 is a photograph of the collagen fiber aerogel material prepared in example 5 after adsorbing iodine vapor; when the iodine vapor is adsorbed, the color is changed into purple black, the appearance shape is in a certain degree of contraction state, and the quality is far higher than that before the adsorption.
Carrying out an iodine vapor adsorption experiment on the collagen fiber aerogel high-efficiency iodine vapor capturing material prepared in the embodiment 1-10; the method comprises the following steps: the invention adopts non-radioactive iodine simple substance to replace radioactive iodine simple substance; firstly, placing excessive iodine elementary substance at the bottom of a 250mL serum bottle, placing 100mg of collagen fiber aerogel high-efficiency iodine vapor capturing material (examples 1-10) in filter paper folded into a funnel shape, placing the filter paper in a serum bottle mouth, screwing down a bottle cap, sealing the bottle cap with a sealing film, placing the serum bottle in a 75 ℃ oven at different time intervals, and most preferably placing the serum bottle in the ovenAnd taking out the collagen fiber aerogel after long adsorption for 24 hours from the oven, cooling to room temperature, and measuring the content of the iodine vapor adsorbed by the collagen fiber aerogel high-efficiency capture iodine vapor material according to a gravimetric method. The calculation formula is as follows: q ═ m2-m1)/m1X 100 wt%, wherein Q (wt%) is the adsorption amount of iodine, m1(mg) and m2(mg) the weights of the collagen fiber aerogel before and after the iodine vapor material is efficiently captured to adsorb iodine are respectively, three adsorption experiments are performed on each adsorption material in parallel, and the average value is obtained, and the result is shown in fig. 3-8; the adsorption amount of iodine gradually increases with the increase of the contact time.
After the iodine vapor material is efficiently captured by the collagen fiber aerogel and adsorbs iodine vapor, desorbing the collagen fiber aerogel in absolute ethyl alcohol, circularly adsorbing the iodine vapor again after drying (the process is consistent as the first adsorption experiment), wherein the circular adsorption result is shown in fig. 9-14, and the result shows that the adsorption quantity is reduced along with the increase of the number of circulation times, but the reduction amplitude is smaller; and after five times of circulation, the material with high initial adsorption capacity continuously keeps high adsorption capacity in the same circulation batch, which shows that the material has excellent recycling performance.
While embodiments of the invention have been described above, it is not limited to the applications set forth in the description and the embodiments, which are fully applicable in various fields of endeavor to which the invention pertains, and further modifications may readily be made by those skilled in the art, it being understood that the invention is not limited to the details shown and described herein without departing from the general concept defined by the appended claims and their equivalents.

Claims (9)

1. A preparation method of a collagen fiber aerogel material capable of efficiently capturing iodine vapor is characterized by comprising the following steps:
adding collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaning machine, cleaning to be neutral, filtering, and drying in an oven;
step two, crushing the cleaned collagen fibers in a crusher, adding the collagen fibers into deionized water, and then adding an alkali modifier solution for mixing to obtain a suspension;
step three, transferring the suspension into a polytetrafluoroethylene hydrothermal reaction kettle, carrying out hydrothermal reaction, cooling to room temperature, washing the reaction product in deionized water to be neutral, filtering, and drying in an oven; soaking the dried product in glutaraldehyde solution, curing for a certain time in a constant-temperature oscillation box, and repeatedly washing for 3-5 times by using deionized water and absolute ethyl alcohol;
and step four, washing the product obtained in the step three in deionized water to be neutral, freezing the product in a low-temperature refrigerator, and drying the product in a vacuum low-temperature freeze dryer to obtain the collagen fiber aerogel high-efficiency iodine vapor capturing material.
2. The method for preparing a collagen fiber aerogel material capable of capturing iodine vapor with high efficiency as claimed in claim 1, wherein the collagen fiber in the first step is animal skin without tanning treatment, and after washing, alkali treatment, dehydration and other treatments according to a conventional method, the collagen fiber is pulverized by a pulverizer to obtain granular substances with a particle size of 10-80 meshes.
3. The method for preparing a collagen fiber aerogel material with high efficiency capturing iodine vapor according to claim 1, wherein the ultrasonic cleaning temperature and the oven temperature in the first step are in the range of room temperature to 70 ℃.
4. The method for preparing a collagen fiber aerogel material capable of capturing iodine vapor with high efficiency as claimed in claim 1, wherein the particle size of the collagen fiber pulverized in the second step is controlled to 30-100 mesh.
5. The preparation method of the collagen fiber aerogel material for efficiently capturing iodine vapor according to claim 1, wherein in the second step, the mass ratio of the collagen fibers to the deionized water is 1: 80-120; the alkali modifier in the alkali modifier solution accounts for 5-20% of the mass of the collagen fibers; the alkali modifier solution is one or more of potassium hydroxide solution, sodium hydroxide solution, ammonium hydroxide solution and sodium carbonate solution; the mass fraction of the alkali modifier solution is 5-10%.
6. The method for preparing the collagen fiber aerogel material capable of efficiently capturing iodine vapor according to claim 1, wherein in the second step, the collagen fibers are taken and added into deionized water, and then the alkali modifier solution is added for mixing in a manner that: adding collagen fibers, deionized water and an alkali modifier solution into a high-pressure reactor, injecting high-pressure carbon dioxide into the reactor, keeping the temperature at 38-45 ℃ and the pressure at 15-25 MPa for 30-45 min, and releasing pressure within 30-60 s; after pressure release, the reaction mass was added to an ultrasonic reactor and treated with ultrasound.
7. The preparation method of the collagen fiber aerogel material for efficiently capturing iodine vapor as claimed in claim 6, wherein the ultrasonic treatment frequency is 45-90 kHz, the power is 100-450W, the temperature is 40-50 ℃, and the time is 30-45 min.
8. The preparation method of the collagen fiber aerogel material for efficiently capturing iodine vapor according to claim 1, wherein in the third step, the temperature of the hydrothermal reaction ranges from 90 ℃ to 180 ℃, and the reaction time is 0.5-24 h; the volume concentration of the glutaraldehyde solution is 0.1-10%, the curing temperature is 10-60 ℃, and the curing time is 0.5-8 h.
9. The method for preparing collagen fiber aerogel material with high efficiency capturing iodine vapor as claimed in claim 1, wherein in the fourth step, the temperature for freezing in the low temperature refrigerator is-20 ℃; the temperature for drying in the vacuum low temperature freeze dryer is-50 ℃.
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