CN115155515A - High-performance adsorption material for typical hazardous chemical substances (PX) - Google Patents

High-performance adsorption material for typical hazardous chemical substances (PX) Download PDF

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Publication number
CN115155515A
CN115155515A CN202210639241.5A CN202210639241A CN115155515A CN 115155515 A CN115155515 A CN 115155515A CN 202210639241 A CN202210639241 A CN 202210639241A CN 115155515 A CN115155515 A CN 115155515A
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China
Prior art keywords
solution
bentonite
ethanol
high performance
hours
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CN202210639241.5A
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Chinese (zh)
Inventor
刘晨
陈荣昌
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China Waterborne Transport Research Institute
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China Waterborne Transport Research Institute
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Priority to CN202210639241.5A priority Critical patent/CN115155515A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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 physical properties
    • B01J20/28009Magnetic properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid 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 physical properties
    • B01J20/28011Other properties, e.g. density, crush strength
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054Solid 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
    • B01J20/28057Surface area, e.g. B.E.T specific surface area

Abstract

The invention discloses a high-performance adsorption material for typical hazardous chemical substances (PX), which is mainly prepared from a solution A, a solution B, bentonite, ferric trichloride, water and the like, wherein the solution A is prepared from ethanol, acetic acid and tetrabutyl titanate, and the solution B is prepared from ethanol, hydrochloric acid and water. The invention realizes the selective adsorption of different functional groups of pollutants and optimizes the adsorption performance of the adsorption material by regulating and controlling the microstructure in the adsorption material, the magnetic bentonite loaded iron oxide modified nano titanium dioxide has simple preparation process, reduces the calcination times, and generates the semiconductor alpha-Fe with smaller forbidden band width at one time 2 O 3 And gamma-Fe having magnetism 2 O 3, Magnetic gamma-Fe 2 O 3 The material can be recovered, the specific surface area and the dispersibility of the material are greatly improved after the bentonite is loaded, and the material has the advantages of large specific surface area, high visible light absorbance and no inhibitionNarrow width of belt, strong magnetism, recoverability and the like.

Description

High-performance adsorption material for typical hazardous chemical substances (PX)
Technical Field
The invention relates to the technical field of hazardous chemical substance adsorbing materials, in particular to a high-performance adsorbing material for typical hazardous chemical substances (PX).
Background
Statistically, over 80% of global trade is carried out by sea, while sea of chemicals is an important component of the shipping market. With the increasing variety and quantity of chemical water transportation, the corresponding risk of water leakage accidents is increased. In the process of transporting chemicals on water, once leakage accidents happen, a large amount of chemicals can overflow in a short time, and environmental pollution causes great danger. For a long time, the aquatic emergency treatment is difficult and complicated due to various types and properties of chemicals, and the serious problem to be solved is still urgent worldwide.
Para-xylene (PX), which is mainly used as a raw material for producing polyester fibers and resins, paints, dyes and pesticides, is a major water transport chemical in the world and is also classified by the international maritime organization as one of the 20 major chemicals that are most likely to pose a high risk. For the emergency treatment of water leakage accidents of paraxylene, the methods of containment, recovery, adsorption and the like are mainly adopted at present. Because the existing adsorbent products are generally of broad-spectrum type, the adsorption performance is different for different chemicals, and the adsorbent is difficult to recover.
Therefore, the invention provides a high-performance adsorption material for typical hazardous chemical substances (PX), which realizes the high-efficiency adsorption of the PX through the load bentonite and the microstructure regulation and control in the material, and endows the material with magnetism to realize the effective recovery of the adsorption material.
Disclosure of Invention
The invention aims to provide a high-performance adsorbing material for typical hazardous chemical substances (PX), wherein magnetic bentonite is loaded with ferric oxide modified nano titanium dioxide and then is loaded with bentonite, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a high-performance adsorption material for typical dangerous chemicals (PX) is mainly prepared from solution A, solution B, bentonite, ferric trichloride, water, etc.,
the solution A is prepared from ethanol, acetic acid and tetrabutyl titanate,
the solution B consists of ethanol, hydrochloric acid and water.
In a further embodiment, the material is prepared by the steps of;
the method comprises the following steps: putting ethanol and acetic acid into a three-neck flask, and then dripping tetrabutyl titanate into the three-neck flask and stirring the mixture to prepare a solution A;
step two: putting ethanol, hydrochloric acid and water into a beaker, and stirring to prepare a solution B;
step three: slowly dripping the solution A into the solution B, adding bentonite, and stirring for half an hour to form sol;
step four: placing the sol in the third step for 24 hours to form gel;
step five: drying the gel in the fourth step at high temperature for a plurality of hours to form dry gel of the bentonite loaded titanium dioxide;
step six: dissolving ferric trichloride in water to obtain a ferric trichloride solution;
step seven: and D, adding the bentonite-loaded titanium dioxide xerogel in the step five into the ferric trichloride solution in the step six, stirring for a plurality of hours, heating at high temperature for a plurality of hours, and fishing out the gel wrapped with the ferric trichloride solution.
Step eight: and putting the gel wrapped with the ferric trichloride solution fished out in the step seven into a quartz boat, calcining in an atmosphere furnace, stably heating, calcining for a plurality of hours, and grinding into powder.
In a further example, the ethanol in step one is 30 to 90ml, the acetic acid is 1 to 3ml, and the tetrabutyl titanate is 10 to 30ml.
In a further embodiment, the ethanol in the second step is 10 to 30ml, the hydrochloric acid is 0.3 to 0.9ml, and the water is 4 to 12ml.
In a further embodiment, the bentonite in step three is 0.5-1.5g.
In a further embodiment, the temperature of step five is 80 ℃ and the drying time is 12 hours.
In a further embodiment, the ferric trichloride in step six is 20-60g.
In a further embodiment, the temperature in step seven is 70 ℃ and the heating time is 4 hours.
In a further embodiment, the calcination temperature in the step eight is 600 ℃, and the temperature rise rate is 5 ℃/min.
Compared with the prior art, the invention has the beneficial effects that:
aiming at the typical dangerous chemical substance water leakage treatment, the efficient adsorption material with the micro-nano scale is designed and synthesized. By being absorbed in the adsorption materialThe microstructure of the part is regulated and controlled to realize the selective adsorption of different functional groups of pollutants and optimize the adsorption performance of an adsorption material, the magnetic bentonite loads ferric oxide to modify the nano titanium dioxide, the preparation process is simple, the calcination times are reduced, and the semiconductor alpha-Fe with smaller forbidden band width is generated at one time 2 O 3 And gamma-Fe having magnetic properties 2 O 3, Magnetic gamma-Fe 2 O 3 The material can be recycled, after the bentonite is loaded, the specific surface area and the dispersibility of the material are greatly improved, and the material has the advantages of large specific surface area, high visible light absorbance, narrow forbidden band width, strong magnetism, recyclability and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
A high-performance adsorption material for typical hazardous chemicals (PX) is mainly prepared from a solution A, a solution B, bentonite, ferric trichloride, water and the like, wherein the solution A is prepared from ethanol, acetic acid and tetrabutyl titanate, and the solution B is prepared from ethanol, hydrochloric acid and water.
Specifically, the method comprises the following steps: 60ml of ethanol and 2ml of acetic acid are put into a three-necked flask, 20ml of tetrabutyl titanate is dropped into the flask and stirred to form a solution A, and 20ml of ethanol, 8ml of water and 0.6ml of hydrochloric acid are added into the flask and stirred uniformly to form a solution B.
Slowly dripping the solution B into the solution A, quickly stirring, adding 1g of bentonite after dripping, and continuously stirring for half an hour to form sol. Gel is formed after the mixture is placed at room temperature for 24 hours, and the bentonite-loaded titanium dioxide xerogel is obtained after the mixture is dried at 80 ℃ for 12 hours.
Dissolving 40g of ferric trichloride in 50mL of water to obtain a ferric trichloride solution, then immersing the xerogel into the solution, stirring for 2 hours, heating at 70 ℃ for 4 hours, taking out the gel coated with the ferric trichloride solution, putting the gel into a quartz boat, calcining in an atmosphere furnace at 600 ℃, heating at 5 ℃/min, calcining for 2 hours and grinding into powder.
The method simplifies the preparation process, and bentonite-loaded magnetic Fe can be obtained by one-step calcination 2 O 3 The modified nano titanium dioxide saves energy.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.

Claims (9)

1. A high performance adsorbent material for typical hazardous chemicals (PX), characterized in that: the material is mainly prepared from solution A, solution B, bentonite, ferric trichloride, water and the like, wherein,
the solution A is prepared from ethanol, acetic acid and tetrabutyl titanate,
the solution B consists of ethanol, hydrochloric acid and water.
2. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 1, wherein:
the preparation steps of the material are as follows:
the method comprises the following steps: putting ethanol and acetic acid into a three-neck flask, and then dripping tetrabutyl titanate into the three-neck flask and stirring the mixture to prepare a solution A;
step two: putting ethanol, hydrochloric acid and water into a beaker and stirring to prepare a solution B;
step three: slowly dripping the solution A into the solution B, adding bentonite, and stirring for half an hour to form sol;
step four: standing the sol obtained in the third step for 24 hours to form gel;
step five: drying the gel in the fourth step at high temperature for a plurality of hours to form a bentonite-loaded titanium dioxide xerogel;
step six: dissolving ferric trichloride in water to obtain a ferric trichloride solution;
step seven: and D, adding the bentonite-loaded titanium dioxide xerogel in the step five into the ferric trichloride solution in the step six, stirring for a plurality of hours, heating at high temperature for a plurality of hours, and fishing out the gel wrapped with the ferric trichloride solution.
Step eight: putting the gel wrapped by the ferric trichloride solution fished out in the step seven into a quartz boat, calcining in an atmosphere furnace, stably heating, and grinding into powder after calcining for a plurality of hours.
3. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: in the first step, 30-90ml of ethanol, 1-3ml of acetic acid and 10-30ml of tetrabutyl titanate are used.
4. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: in the second step, 10 to 30ml of ethanol, 0.3 to 0.9ml of hydrochloric acid and 4 to 12ml of water are used.
5. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: the bentonite in the third step is 0.5-1.5g.
6. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: the temperature of the fifth step is 80 ℃, and the drying time is 12 hours.
7. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: and in the sixth step, the amount of ferric trichloride is 20-60g.
8. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 3, wherein: the temperature in the seventh step is 70 ℃, and the heating time is 4 hours.
9. A high performance sorbent material for typical hazardous chemicals (PX) according to claim 2, wherein: and the calcination temperature in the step eight is 600 ℃, and the temperature rise speed is 5 ℃/min.
CN202210639241.5A 2022-06-08 2022-06-08 High-performance adsorption material for typical hazardous chemical substances (PX) Pending CN115155515A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101322944A (en) * 2008-07-28 2008-12-17 吉林大学 Composite photocatalyst prepared from stephanoporate mineral and method thereof
CN107537437A (en) * 2017-09-29 2018-01-05 天津大学 A kind of support type bi-component nano-oxide adsorbent, its preparation method and its application
CN109174014A (en) * 2018-10-17 2019-01-11 内蒙古工业大学 Nano barium titanate iron-base magnetic adsorbent material and its preparation method and application

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101322944A (en) * 2008-07-28 2008-12-17 吉林大学 Composite photocatalyst prepared from stephanoporate mineral and method thereof
CN107537437A (en) * 2017-09-29 2018-01-05 天津大学 A kind of support type bi-component nano-oxide adsorbent, its preparation method and its application
CN109174014A (en) * 2018-10-17 2019-01-11 内蒙古工业大学 Nano barium titanate iron-base magnetic adsorbent material and its preparation method and application

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
YIYUN CAO ET AL.: "Green synthesis of reusable multifunctional γ-Fe2O3/bentonite modified by doped TiO2 hollow spherical nanocomposite for removal of BPA" *
曹茜: "纳米零价铁与光触媒原位修复水污 染作用机制及应用——以去除地下水六价铬和地表水苯系物为例" *

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Application publication date: 20221011