CN107829293B - Fiber material for degrading p-aminobenzoic acid and process flow - Google Patents
Fiber material for degrading p-aminobenzoic acid and process flow Download PDFInfo
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- CN107829293B CN107829293B CN201711090312.6A CN201711090312A CN107829293B CN 107829293 B CN107829293 B CN 107829293B CN 201711090312 A CN201711090312 A CN 201711090312A CN 107829293 B CN107829293 B CN 107829293B
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- aminobenzoic acid
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/58—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/38—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by oxidation; by combustion
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Abstract
The invention discloses a fiber material for degrading p-aminobenzoic acid and a process flow, and belongs to the field of wastewater treatment. The preparation method comprises the following steps: firstly, grinding and sieving chestnut shells, and then soaking in a sodium hydroxide solution under the stirring state; then washing with distilled water, soaking in nitric acid solution, washing again and drying to obtain chestnut shell fiber; and finally, soaking the chestnut shell fibers in a ferric nitrate solution, taking out and drying to obtain the fiber material for degrading the p-aminobenzoic acid. The technological process of degrading p-aminobenzoic acid with the fiber material includes adding the fiber material into solution containing p-aminobenzoic acid and introducing ozone into the solution. The fiber material for degrading the p-aminobenzoic acid prepared by the invention is insensitive to the pH value in the degradation process, and has wide application range of the pH value, so that the pH value of the solution does not need to be adjusted in the degradation process, the process cost is reduced, and secondary pollution is avoided.
Description
Technical Field
The invention belongs to the field of wastewater treatment, and particularly relates to a fiber material for degrading p-aminobenzoic acid and a process flow.
Background
The ultraviolet absorbent has increasingly obvious influence on the environment, such as influence on gene expression of fishes in water, high risk on shrimps and algae, and low natural degradation rate in the environment, so that the ultraviolet absorbent can be accumulated in large quantity in the nature, and at present, China does not pay much attention to treatment of the ultraviolet absorbent.
At present, the domestic degradation method of p-aminobenzoic acid only adopts photodegradation, but the direct photodegradation is very slow, and the direct photodegradation is in' Mengsui, Quyun, ever-super, Yanxi et al, the photolysis research [ J ] environmental science, 2011, 32(9) "of sunscreen p-aminobenzoic acid in nitrate solution, and the 4h direct photolysis rate of p-aminobenzoic acid of 10mg/L is only 40.8%. And the p-aminobenzoic acid can be converted into quinone substances in the degradation process, and the quinone substances have very strong toxicity and can cause serious harm to the ecological environment.
Therefore, it is necessary to design a new process flow for degrading p-aminobenzoic acid aiming at the defects of the p-aminobenzoic acid photodegradation process.
Disclosure of Invention
The invention aims to solve the problems of long degradation time and low degradation rate of the existing p-aminobenzoic acid degradation process, and provides a fiber material for degrading p-aminobenzoic acid and a process flow.
The invention adopts the following specific technical scheme:
the fiber material for degrading the p-aminobenzoic acid is characterized in that firstly chestnut shells are crushed and sieved, and then are soaked in a sodium hydroxide solution under the stirring state; then washing with distilled water, soaking in nitric acid solution, washing again and drying to obtain chestnut shell fiber; and finally, soaking the chestnut shell fibers in a ferric nitrate solution, taking out and drying to obtain the fiber material for degrading the p-aminobenzoic acid.
Preferably, the chestnut shell fiber is repeatedly soaked twice by using ferric nitrate solution, and after the first soaking is finished, the chestnut shell fiber is taken out, dried and washed. Then the impregnation is carried out again.
Another objective of the present invention is to provide a process for degrading p-aminobenzoic acid by using any one of the above fiber materials, which specifically comprises: and (2) adding the fiber material into a solution containing p-aminobenzoic acid, and then introducing ozone into the solution to degrade the p-aminobenzoic acid.
Preferably, the pH value of the solution containing p-aminobenzoic acid is 1-10.
Preferably, the temperature of the solution containing p-aminobenzoic acid is 20 ℃ to 50 ℃, preferably 40 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the fiber material for degrading the p-aminobenzoic acid prepared by the invention is insensitive to the pH value in the degradation process, and has wide application range of the pH value, so that the pH value of the solution does not need to be adjusted in the degradation process, and the process cost is reduced.
2. Compared with the photodegradation process of p-aminobenzoic acid, the degradation time is shorter, and the degradation rate is higher.
3. The invention can not generate poisonous quinone by-product after being completely degraded, does not cause secondary pollution, and has low process cost.
Drawings
FIG. 1 is a graph showing the effect of different pH on the degradation effect of aminobenzoic acid; the horizontal axis is pH, and the vertical axis is degradation rate of p-aminobenzoic acid;
FIG. 2 shows the effect of different fiber material dosage on the degradation effect of aminobenzoic acid; the horizontal axis is the adding amount (unit g) of the fiber material, and the vertical axis is the degradation rate of the para aminobenzoic acid;
FIG. 3 is a graph showing the effect of different initial concentrations of para-aminobenzoic acid on the degradation effect of para-aminobenzoic acid; the horizontal axis is the initial concentration (unit mg/L) of the p-aminobenzoic acid, and the vertical axis is the degradation rate of the p-aminobenzoic acid;
FIG. 4 is a graph showing the effect of different solution temperatures on the degradation effect of p-aminobenzoic acid; the horizontal axis represents the solution temperature (unit is ℃), and the vertical axis represents the degradation rate of the para aminobenzoic acid;
FIG. 5 shows the effect of different ozone introduction times on the degradation effect of p-aminobenzoic acid; the horizontal axis represents ozone introduction time (in min) and the vertical axis represents degradation rate of p-aminobenzoic acid.
Detailed Description
The invention will be further elucidated and described with reference to the drawings and specific embodiments.
Example 1
In this example, the preparation method of the fiber material is as follows:
1. a 10% sodium hydroxide solution, a 10% nitric acid solution, and a 10% ferric nitrate solution were prepared.
2. Preprocessing the chestnut shells: firstly grinding the chestnut shells, sieving with a 20-mesh sieve, soaking in 10% sodium hydroxide solution, stirring for 5min, washing with distilled water until the pH is 7, then immersing in 10% nitric acid solution for 1h, taking out, washing again and drying to obtain the chestnut shell fibers.
The chestnut shell fibers of this example were not impregnated with a solution of ferric nitrate.
Example 2
This example is mainly intended to prepare a fibrous material for degrading p-aminobenzoic acid.
The chestnut shells used in this example were obtained by removing the pulp of chestnuts and washing them.
The preparation method of the fiber material comprises the following steps:
1. a 10% sodium hydroxide solution, a 10% nitric acid solution, and a 10% ferric nitrate solution were prepared.
2. Preprocessing the chestnut shells: firstly grinding the chestnut shells, sieving with a 20-mesh sieve, soaking in 10% sodium hydroxide solution, stirring for 5min, washing with distilled water until the pH is 7, then immersing in 10% nitric acid solution for 1h, taking out, washing again and drying to obtain the chestnut shell fibers.
3. Modification of Chinese chestnut fibers: soaking the chestnut shell fiber obtained in the last step in a 10% ferric nitrate solution for 18h, taking out, drying the fiber in an oven to constant weight, and then putting the fiber in a drying dish for subsequent use. Thereby, the preparation of the fiber material is completed.
Example 3
This example differs from example 2 in that the impregnation of the chestnut shell fibres with a solution of ferric nitrate is repeated twice. The method is that after the impregnation is finished in the previous embodiment, the fiber is taken out, dried and cleaned. Then soaking the mixture again by using a 10% ferric nitrate solution, drying the mixture to constant weight, and finally putting the mixture into a drying dish for subsequent use. Thereby, the preparation of the fiber material is completed.
Example 4
15 250ml Erlenmeyer flasks were aliquoted into three groups. Each group of erlenmeyer flasks was charged with 0.5000g of each different fiber material, group a of erlenmeyer flasks was charged with the fiber material prepared in example 1, group b of erlenmeyer flasks was charged with the fiber material prepared in example 2, and group c of erlenmeyer flasks was charged with the fiber material prepared in example 3. 100ml of 50mg/L p-aminobenzoic acid solution is added into each conical flask, and the pH value of the p-aminobenzoic acid solution is adjusted to 1,3,5,7 and 10 by sodium hydroxide or nitric acid in 5 conical flasks in the same group. And (3) introducing ozone into the solution in each conical flask at the temperature of 20 ℃ to degrade the aminobenzoic acid, wherein the ozone introduction time is 30 min.
In addition, because the material may have iron ion dissolved out in water to cause the increase of absorbance, and may also have a small part of decomposition under the condition of illumination to aminobenzoic acid, a corresponding blank test is required. The above experiment was repeated in a blank test by replacing the 50mg/L concentration of p-aminobenzoic acid solution with an equal amount of distilled water.
The wavelength of p-aminobenzoic acid has an ultraviolet maximum absorption peak under 282 nm. The invention uses the ultraviolet absorption wave of the p-aminobenzoic acid to determine the degradation rate of the p-aminobenzoic acid. During measurement, a marked line equation of the concentration and the absorbance of aminobenzoic acid is firstly made, then the absorbance of an experimental group minus the absorbance of a blank group under the same pH and the same material is substituted into the marked line equation to calculate the concentration of the aminobenzoic acid, and then the degradation rate is calculated.
The degradation effect of the three materials on aminobenzoic acid at different pH is shown in figure 1 and table 1.
TABLE 1 Effect of different pH's on the degradation Effect of three materials
It can be seen from fig. 1 and table 1 that the change of pH has little effect on the degradation rate of the c-group material to aminobenzoic acid, and the p-aminobenzoic acid organic matter can be directly oxidized by ozone without adjusting pH. The materials of the group a and the group b are slightly improved when the pH is higher, but the improvement range is not obvious, the organic matters are mainly directly oxidized and degraded by ozone under the acidic state according to the mechanism, the ozone is accelerated to be converted into the oxidized organic matters generated by hydroxyl free radicals under the alkaline condition, and Fe3+Can catalyze the ozone to be converted into hydroxyl free radicals.
Therefore, the chestnut shell fiber is added, so that the ozone degradation system of the aminobenzoic acid is not very sensitive to pH change, and the degradation process flow can be obviously simplified. From the aspect of degradation rate, the secondary load of ferric nitrate can effectively improve the degradation rate of the ozone of the p-aminobenzoic acid when the ozone is introduced into the system from the aspect of example 3 to example 2 to example 1.
Comparative example 1
First, an Fe-loaded fibrous material was prepared according to the method of example 3 using bagasse as a raw material, and the specific steps and parameters were the same as in example 3, except that the raw material was changed from chestnut shells to bagasse.
4 250ml conical flasks were equally divided into two groups, the first group of conical flasks was charged with 0.5000g of the above Fe-loaded bagasse fibers as the loading material, and the second group was not charged with any fiber loading material. In each flask, 100ml of a 50mg/L strength p-aminobenzoic acid solution was added, and then the pH was adjusted to 2.5 and 6 with sodium hydroxide or nitric acid for each set of two flasks, respectively. And (3) introducing ozone into the solution of each conical flask at the temperature of 20 ℃ to degrade the aminobenzoic acid, wherein the ozone introduction time is 30 min. Meanwhile, another 4 flasks were taken and the p-aminobenzoic acid solution was replaced with distilled water, and the above test was repeated as a blank test.
The degradation rate of p-aminobenzoic acid was measured in the same manner as in example 4. The degradation rate of p-aminobenzoic acid in erlenmeyer flasks with different pH and addition materials is shown in Table 2.
TABLE 2 Effect of different pH's on the degradation Effect of two materials
As can be seen from Table 2, the degradation rate of p-aminobenzoic acid under acidic conditions was significantly lower than that of the treatment with higher pH, regardless of the treatment with bagasse as a supporting material or the treatment with direct ozone. Thus, in combination with the results of example 4, it can be shown that the addition of chestnut shell fibers enables the ozone degradation process of p-aminobenzoic acid to have a reduced pH requirement.
Example 5
This example is mainly used to show the effect of the amount of fiber material added on the degradation effect of p-aminobenzoic acid.
The fiber materials obtained in example 3 were added to 4 flasks at 0.2500 g, 0.5000g, 0.7500g, and 0.9000g, respectively. Adding 100ml of 50mg/L p-aminobenzoic acid solution into each conical flask, adjusting the pH value to 3 by using sodium hydroxide or nitric acid, introducing ozone into the solution in each conical flask at the temperature of 20 ℃ for degrading the p-aminobenzoic acid, wherein the ozone introduction time is 30min, and performing 3 groups of parallel tests.
In addition, 4 more 250ml Erlenmeyer flasks were taken to replace the p-aminobenzoic acid solution with distilled water, and the above test was repeated as a blank test.
The degradation rate of p-aminobenzoic acid was measured in the same manner as in example 4. The degradation rate of p-aminobenzoic acid in different amounts of the flask is shown in FIG. 2. As can be seen, the degradation rate of p-aminobenzoic acid is continuously increased along with the addition of the chestnut shell fibers.
Example 6
This example is mainly used to show the effect of the initial concentration of p-aminobenzoic acid on the degradation effect of the material.
The fiber materials prepared in example 3 were added to 4 flasks, respectively, at an amount of 0.5000 g. 100ml of p-aminobenzoic acid solution with the concentration of 25mg/L, 50mg/L, 100mg/L and 150mg/L was added into 5 Erlenmeyer flasks, respectively. Then, the pH was adjusted to 3 with sodium hydroxide or nitric acid, ozone was introduced at a temperature of 20 ℃ for 30min and 3 sets of parallel tests were carried out.
In addition, 4 more 250ml Erlenmeyer flasks were taken to replace the p-aminobenzoic acid solution with distilled water, and the above test was repeated as a blank test.
The degradation rate of p-aminobenzoic acid was measured in the same manner as in example 4.
The degradation rate of p-aminobenzoic acid in the conical flasks with different initial concentrations of p-aminobenzoic acid is shown in fig. 3. As can be seen from the graph, the degradation rate of p-aminobenzoic acid of the fiber material prepared in example 3 decreased as the initial concentration of p-aminobenzoic acid increased, more ozone or hydroxyl radicals were available for contact at the concentration of 25mg/L to 100mg/L of p-aminobenzoic acid as the concentration increased, and a significant decrease was observed at the initial concentration of 150 mg/L.
Example 7
This example is mainly used to show the effect of temperature on the degradation effect of a material.
The fiber material prepared in example 3 was added to 4 flasks, respectively, at an amount of 0.5000 g. 100ml of 50mg/L p-aminobenzoic acid solution is added into each conical flask, the pH value is adjusted to 3 by using sodium hydroxide or nitric acid, the ozone is introduced for 30min, the temperature of the solution in 4 conical flasks is respectively adjusted to 20 ℃,30 ℃,40 ℃ and 50 ℃, and 3 groups of parallel tests are carried out.
In addition, 4 more 250ml Erlenmeyer flasks were taken to replace the p-aminobenzoic acid solution with distilled water, and the above test was repeated as a blank test.
The degradation rate of p-aminobenzoic acid was measured in the same manner as in example 4.
The degradation rate of p-aminobenzoic acid in the conical flasks at different temperatures is shown in FIG. 4. It can be seen from the figure that the degradation rate of p-aminobenzoic acid in the fiber material prepared in example 3 is reduced as the temperature increases, the ozone molecules and hydroxyl radical ions in the solution and p-aminobenzoic acid molecules move in the solution at an accelerated speed at 20 ℃ to 40 ℃ along with the increase of the temperature to increase the collision, although the solubility of ozone in water is reduced along with the increase of the temperature, the degradation rate is increased because ozone is not dominant in the process, and the condition that the solubility of ozone in water is reduced along with the increase of the temperature at 50 ℃ becomes a main factor to reduce the degradation rate.
Example 8
This example is mainly used to show the effect of time on the degradation effect of a material.
5 conical flasks were each charged with 0.5000g of the fiber material prepared in example 3. Each flask was charged with 100ml of 50mg/L p-aminobenzoic acid solution, adjusted to pH 3 with sodium hydroxide or nitric acid, and subjected to ozone aeration at 20 ℃ for 10, 20, 30, 40, and 50min for 3 parallel tests.
In addition, 5 additional 250ml Erlenmeyer flasks were taken and the above test was repeated as a blank test with distilled water instead of the p-aminobenzoic acid solution.
The degradation rate of p-aminobenzoic acid was measured in the same manner as in example 4.
The degradation rate of p-aminobenzoic acid in erlenmeyer flasks with different ozone introduction times is shown in fig. 5. As can be seen in the figure, the degradation rate increases as the ozone passage time, i.e., the degradation time, increases. But reaches the maximum degradation rate basically when the time is 30-40 min.
In addition, quinone substances which cause light red or red solution are easily generated in the degradation process of the p-aminobenzoic acid, for example, the solution still presents light red after the photo-hydrolysis method is processed for 3-4 days. However, in this example, it can be seen that after ozone is introduced for 6-8 minutes, the red color in the solution is removed, and the solution is substantially colorless, indicating that the quinone substances are sufficiently degraded.
The above-described embodiments are merely preferred embodiments of the present invention, which should not be construed as limiting the invention. Various changes and modifications may be made by one of ordinary skill in the pertinent art without departing from the spirit and scope of the present invention. Therefore, the technical scheme obtained by adopting the mode of equivalent replacement or equivalent transformation is within the protection scope of the invention.
Claims (5)
1. A process method for degrading p-aminobenzoic acid by using a fiber material is characterized in that the preparation method of the fiber material comprises the following steps: firstly, grinding and sieving chestnut shells, and then soaking in a sodium hydroxide solution under the stirring state; then washing with distilled water, soaking in nitric acid solution, washing again and drying to obtain chestnut shell fiber; finally, soaking the chestnut shell fibers in a ferric nitrate solution, taking out and drying to obtain a fiber material for degrading p-aminobenzoic acid; the process flow comprises the following steps: and (2) adding the fiber material into a solution containing p-aminobenzoic acid, and then introducing ozone into the solution to degrade the p-aminobenzoic acid.
2. The process for degrading p-aminobenzoic acid with fiber material according to claim 1, wherein the chestnut shell fiber is repeatedly dipped with ferric nitrate solution twice, and after the first dipping, the chestnut shell fiber is taken out, dried and cleaned; then the impregnation is carried out again.
3. The process for degrading p-aminobenzoic acid with fibrous material according to claim 1, characterized in that the pH of the solution containing p-aminobenzoic acid is 1 ~ 10.
4. The process for degrading p-aminobenzoic acid with fibrous material according to claim 1, wherein the temperature of the solution containing p-aminobenzoic acid is 20 ℃ ~ 50 ℃.
5. The process for degrading p-aminobenzoic acid with fibrous material according to claim 4, wherein the temperature of the solution is 40 ℃.
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Citations (4)
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| JP2004131628A (en) * | 2002-10-11 | 2004-04-30 | Advics:Kk | Method for producing brake pad |
| CN101914466A (en) * | 2010-07-02 | 2010-12-15 | 郑州大学 | Achromobacter xylosoxidans and application thereof for degrading o-aminobenzoic acid |
| CN103923446A (en) * | 2014-04-01 | 2014-07-16 | 江苏科技大学 | Degradable biomass polylactic acid magnetic card material |
| CN106582526A (en) * | 2016-12-22 | 2017-04-26 | 重庆文理学院 | Chestnut shell, pistachio shell/tourmaline adsorbent and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004131628A (en) * | 2002-10-11 | 2004-04-30 | Advics:Kk | Method for producing brake pad |
| CN101914466A (en) * | 2010-07-02 | 2010-12-15 | 郑州大学 | Achromobacter xylosoxidans and application thereof for degrading o-aminobenzoic acid |
| CN103923446A (en) * | 2014-04-01 | 2014-07-16 | 江苏科技大学 | Degradable biomass polylactic acid magnetic card material |
| CN106582526A (en) * | 2016-12-22 | 2017-04-26 | 重庆文理学院 | Chestnut shell, pistachio shell/tourmaline adsorbent and preparation method thereof |
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