CN110586022A - Method for removing fatty acid from textile industrial wastewater by using acid-base modified porous boron nitride - Google Patents
Method for removing fatty acid from textile industrial wastewater by using acid-base modified porous boron nitride Download PDFInfo
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- CN110586022A CN110586022A CN201910880018.8A CN201910880018A CN110586022A CN 110586022 A CN110586022 A CN 110586022A CN 201910880018 A CN201910880018 A CN 201910880018A CN 110586022 A CN110586022 A CN 110586022A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
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Abstract
The invention relates to a method for removing fatty acid from textile industrial wastewater by using porous boron nitride, which uses acid-base modified porous boron nitride to adsorb fatty acid in textile wastewater. Wherein the acid modification is carried out by using 2% nitric acid, 2% citric acid or mixed acid, and the alkali is modified by using 2% sodium hydroxide, 2% calcium hydroxide or 2% ammonia water. The method has wide application range, can adsorb the textile wastewater fatty acid with the concentration of 0.15-0.2mg/L, the pH value of 2-7 and the temperature of 25-55 ℃, and the adsorption rate can reach more than 79 percent. The operation is simple, and the reproducibility is high. Is very feasible in the aspect of textile wastewater treatment.
Description
Technical Field
The invention belongs to the technical field of environmental chemistry, and particularly relates to a method for removing fatty acid from textile industrial wastewater by using acid-base modified porous boron nitride.
Background
The textile industry of China is a major part of the global textile trade. The textile industry wastewater contains a large amount of fatty acid, glycerol, surface active substances, grease and the like, the content of the fatty acid, the glycerol, the surface active substances, the grease and the like is between 0.15mg/L and 0.20mg/L, the fatty acid, the glycerol, the surface active substances, the grease and the like have good emulsibility and affinity, and the COD and the BOD of a water body can be rapidly increased by a small amount of the fatty acid. Oily medium-chain fatty acid and solid long-chain fatty acid block the grating in a wastewater treatment plant, and slag is accumulated in a sludge pump to influence the normal operation of equipment. And in the aerobic treatment unit and the final sedimentation tank, the mixture containing fatty acid can be formed into 'fat globules' and is in a suspension state together with the adhered sludge, and the fat globules are discharged along with final effluent. On one hand, the sludge loss is caused, and the effluent quality is also influenced.
At present, the textile industry mainly uses a biodegradation method, a sedimentation method, a chemical oxidation method, an adsorption method and the like. Because of large processing capacity and high efficiency, the biological method is widely used in various enterprises at present; but its secondary product is in large quantity, difficult to handle and its reproducibility is poor. Sedimentation is inefficient and is commonly used for pretreatment. The chemical oxidation method can change the chemical property of the wastewater to a certain extent, and is not favorable for the stability of the wastewater. The adsorption method is widely concerned due to its simplicity, easy availability of adsorbent, economy, and various kinds of adsorbents, and the commonly used adsorbent mainly comprises activated carbon, but its adsorption efficiency is low, and adsorption has no selectivity. The reproducibility is poor. At present, new adsorbents are gradually synthesized, including kaolin, adsorbent made of tetrabutyl urea (CN 109626724a), nutshell activated carbon (CN 107651715 a), boron nitride, and the like.
Boron nitride is a porous adsorbent material and is called white graphite because its chemical structure is similar to that of graphite. Due to the chemical stability, thermal stability, strong conductivity, selective adsorption and other properties of boron nitride, boron nitride is currently used in the fields of electrical conductivity, adsorbents, aerospace materials and the like. According to different preparation methods, boron nitride materials with different morphological characteristics can be prepared, and the preparation method is applicable to different fields. BN is exposed in fluid and applied with electric field to produce active boron nitride which can be applied in accumulator, fuel cell and electrolytic bath (CN 101715611A). Calcining urea and boron nitride at 600 ℃ to prepare mesoporous boron nitride (CN 107265415A) with high dye removal rate. The ammonia and boric acid are reacted at high temperature in an inert gas to prepare spherical boron nitride particles which are suitable for high-thermal-conductivity fillers (CN 105980298A). The porous boron nitride is prepared at high temperature by mixing melamine with boric acid. Currently, boron nitride modification is mainly focused on adding a catalyst to increase functional groups, changing contact angles, or changing the pore structure of boron nitride by using bubble generation. The research on acid-base modification is less. The acid contains a large number of H + ions and is easily replaced by exchange. Moreover, most acids have certain oxidation performance, such as nitric acid, which can corrode the surface structure of the adsorbent and increase the pore volume, thereby increasing the specific surface area and enhancing the adsorption. The alkaline solution can increase the-OH structure on the surface of the adsorbent. Therefore, the acid-base modified porous boron nitride has practical significance in the application of the fatty wastewater.
Disclosure of Invention
In order to solve the problems, the invention provides a method for efficiently removing fatty acid in water, which utilizes porous boron nitride as an adsorbent and adopts a reflux adsorption method to effectively and efficiently remove fatty acid in a textile mill. The boron nitride has a large number of mesopores, has strong adsorption capacity to fatty acid, has no secondary pollution, and can be recycled.
The method comprises the following steps:
(1) mixing melamine and boric acid in a nitrogen protective atmosphere, and activating at high temperature to obtain porous boron nitride; (2) boiling 100g of boron nitride for 30min, rinsing with deionized water to neutrality, drying for 24h, dissolving 10g of boron nitride in 100ml of 2% nitric acid or 2% citric acid or mixed acid of nitric acid and sulfuric acid (15ml of HNO)3And 14ml of H2SO4Dissolving in deionized water, fixing the volume to 1L), and standing for 4h at 40 ℃; or mixing boron nitride with 2% sodium hydroxide, 2% calcium hydroxide or 2% ammonia water solution at a solid-to-liquid ratio of 1:5-1: 10.
And (3) putting the boron nitride prepared in the step (2) into a circular quartz device, wherein the content of the boron nitride is kept in a range of 1-4 mg/L, introducing the boron nitride into textile industry wastewater with the concentration range of 0.15-0.2mg/L and the pH value of 2-7, keeping the temperature at 25-55 ℃, performing centrifugal filtration, taking supernatant, testing the content of fatty acid, and marking the content as C. Using formulas
Wherein: q is boron nitride adsorption amount mg/g
C0The initial concentration of fatty acid is mg/L
C is the concentration mg/L of fatty acid after adsorption
V is the volume ml of the solution
m is boron nitride mass mg
The invention has the beneficial effects that:
the boron nitride modified by acid greatly increases the specific surface area of the boron nitride, and is mainly based on physical adsorption and assisted by chemical adsorption. The alkali modified boron nitride mainly changes the functional group on the surface of the boron nitride, so the adsorption principle of the application takes chemical adsorption as the main part and physical adsorption as the auxiliary part. The adsorbent has high preparation success rate and stable preparation process; the modified boron nitride has more mesopores and regular structure; has selectivity to the adsorption of fatty acid, high adsorption rate and reproducibility. The adsorbent is fully contacted with the adsorbate and completely reacted, and the adsorption rate of the adsorbent to fatty acid in textile industry wastewater is higher than 79%.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a diagram of an inventive operating device arrangement;
1. 2 is a water inlet and a water outlet of the water temperature control part respectively, 3 and 4 are filter membranes of the reaction device, 5 and 6 are a textile wastewater inlet and a textile wastewater outlet respectively, and 7 is a pressurizing device air pump;
FIG. 2 is a scanning electron micrograph of porous boron nitride obtained in example 1 of the present invention;
FIG. 3 is an XRD pattern of porous boron nitride obtained in example 1 of the present invention;
FIG. 4 is the isotherm of adsorption and desorption of porous boron nitride low-temperature nitrogen obtained in example 1 of the present invention;
FIG. 5 is a TEM image of porous boron nitride obtained in example 1 of the present invention;
fig. 6 is an XRD pattern of boron nitride obtained in example 2 of the present invention.
Detailed Description
The invention is illustrated in detail by the following examples in connection with fig. 1-6:
example 1:
method for removing fatty acid from textile industry wastewater
(1) Mixing 3.18g of boric acid and 1.59g of melamine, fully dissolving in enough deionized water, sealing with a preservative film, and oscillating for 2 hours in a constant temperature shaking table at 85 ℃.
(2) Stopping oscillation, carrying out vacuum filtration at room temperature after cooling, drying for 12h in an oven at 105 ℃ after the filtration is finished, cooling, and grinding to obtain white powder.
(3) 0.2g of the white powder obtained in step (2) was weighed and spread on a corundum boat (Al)2O3) The medicine spoon is used for keeping the medicine loose.
(4) And (3) putting the corundum boat containing the white powder into a tube furnace, and activating at a high temperature of 1350 ℃ for 4 hours, wherein the activation reaction is carried out under the protection atmosphere of nitrogen, the gas flow is 100ml/min, and the heating rate is set to be 5 ℃/min. Soaking 10g of the boron nitride in 100ml of 2% NaOH solution for 4h to obtain 515m of specific surface area2(iv) a white powdery substance in g, noted BN.
(5) BN in the step (4) is weighed and put between two filter membranes at 4mg/L, and warm water with the temperature of 35 ℃ is introduced into a water bath area. 0.2mg/L short chain fatty acid was refluxed 50 times.
(6) Placing the solution in the step (5) in a centrifuge, centrifuging for 15min at 1000r/min, taking supernatant, and utilizing a formula
Calculated adsorption capacity was 55 mg/g.
Example 2
(1) Mixing 3.18g of boric acid and 1.59g of melamine, fully dissolving in enough deionized water, sealing with a preservative film, and oscillating for 2 hours in a constant temperature shaking table at 85 ℃.
(2) Stopping oscillation, carrying out vacuum filtration at room temperature after cooling, drying for 12h in an oven at 105 ℃ after the filtration is finished, cooling, and grinding to obtain white powder.
(3) 0.2g of the white powder obtained in step (2) was weighed and spread on a corundum boat (Al)2O3) The medicine spoon is used for keeping the medicine loose.
(4) And (3) putting the corundum boat containing the white powder into a tube furnace, and activating at a high temperature of 1350 ℃ for 4 hours, wherein the activation reaction is carried out under the protection atmosphere of nitrogen, the gas flow is 100ml/min, and the heating rate is set to be 5 ℃/min. A white powdery substance was obtained, and 10g of the above boron nitride was immersed in 50ml of a 2% NaOH solution for 4 hours to record BN.
(5) BN in the step (4) is weighed and put between two filter membranes at the concentration of 1mg/L, and warm water with the temperature of 35 ℃ is introduced into a water bath area. Short-chain fatty acid (0.15 mg/L) was added and refluxed 50 times.
(6) And (5) placing the solution in the step (5) in a centrifuge, centrifuging for 15min at 1000r/min, and taking supernatant.
Example 3
(1) Mixing 3.18g of boric acid and 1.59g of melamine, fully dissolving in enough deionized water, sealing with a preservative film, and oscillating for 2 hours in a constant temperature shaking table at 85 ℃.
(2) Stopping oscillation, carrying out vacuum filtration at room temperature after cooling, drying for 12h in an oven at 105 ℃ after the filtration is finished, cooling, and grinding to obtain white powder.
(3) 0.2g of the white powder obtained in step (2) was weighed and spread on a corundum boat (Al)2O3) The medicine spoon is used for keeping the medicine loose.
(4) And (3) putting the corundum boat containing the white powder into a tube furnace, activating at the high temperature of 1350 ℃ for 4 hours, wherein the activation reaction is carried out under the protection atmosphere of nitrogen, the air flow is 100ml/min, the heating rate is set to be 5 ℃/min, and a white powdery substance is prepared and is marked as BN. Weighing 100g of boron nitride, boiling for 30min, rinsing with deionized water, drying for 24h, soaking in 2% dilute nitric acid, and stirring at 40 ℃ for 4h to obtain modified porous boron nitride;
(5) weighing the modified porous boron nitride in the step (4) at a concentration of 4mg/L, placing the modified porous boron nitride between two filter membranes, and introducing warm water at 35 ℃ into a water bath area. The textile wastewater with the concentration of 0.1mg/L fatty acid is led in for 50 times of reflux.
(6) Placing the solution in step (5) in a centrifuge, centrifuging at 1000r/min for 15min, collecting supernatant, and testing by liquid chromatography to obtain 30mg/g solution.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (4)
1. A method for removing fatty acid in textile wastewater by using acid-base modified porous boron nitride.
2. The method for removing fatty acid in textile wastewater by using acid-base modified porous boron nitride as claimed in claim 1, wherein the boron nitride is modified boron nitride, and the preparation method comprises two methods:
(1) acid-modified boron nitride: the acid is 2% nitric acid or 2% citric acid or mixed acid of nitric acid and sulfuric acid, and is 15ml HNO3And 14ml of H2SO4Dissolving in deionized water, diluting to a constant volume of 1L, dissolving 10g of boron nitride in 100ml of the acid solution respectively, and standing for 4h at 40 ℃;
(2) alkali-modified boron nitride: the alkali liquor is 2% sodium hydroxide, 2% calcium hydroxide or 2% ammonia water, wherein the solid-to-liquid ratio of the boron nitride to the alkali liquor is 1:5-1: 10.
3. The method for removing fatty acid in textile wastewater by using porous boron nitride as claimed in claim 1, wherein the adsorbate is fatty acid in textile wastewater, and the concentration of the removed fatty acid is 0.15mg/L-0.2 mg/L.
4. The method for removing fatty acid in textile wastewater by using porous boron nitride as claimed in claim 1, wherein the addition amount of boron nitride is 1mg/L-4mg/L, and the removal environment is as follows: the adsorption temperature is 25-55 ℃, the pH is 2-7, and the removal rate of fatty acid in the textile wastewater is 79-96%.
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Cited By (3)
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| CN112108104A (en) * | 2020-09-23 | 2020-12-22 | 沈阳航空航天大学 | Method for removing proteins in slaughter wastewater by using modified porous boron nitride |
| CN112133888A (en) * | 2020-10-20 | 2020-12-25 | 天津市捷威动力工业有限公司 | Power battery composite positive electrode with excellent performance and preparation method of power battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111151287A (en) * | 2020-01-17 | 2020-05-15 | 厦门大学 | Alkaline oxide modified boron nitride catalyst and preparation method and application thereof |
| CN111151287B (en) * | 2020-01-17 | 2021-12-03 | 厦门大学 | Alkaline oxide modified boron nitride catalyst and preparation method and application thereof |
| CN112108104A (en) * | 2020-09-23 | 2020-12-22 | 沈阳航空航天大学 | Method for removing proteins in slaughter wastewater by using modified porous boron nitride |
| CN112133888A (en) * | 2020-10-20 | 2020-12-25 | 天津市捷威动力工业有限公司 | Power battery composite positive electrode with excellent performance and preparation method of power battery |
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Application publication date: 20191220 |