CN111686690A

CN111686690A - Supported activated carbon and preparation method and device thereof

Info

Publication number: CN111686690A
Application number: CN202010719663.4A
Authority: CN
Inventors: 李清恩; 张冰剑; 漆志文; 张琪; 胡健; 钟耀武; 曾尚军; 邓维; 蒋小平
Original assignee: Foshan Shunde Apollo Air Cleaner Co Ltd; Sun Yat Sen University
Current assignee: Sun Yat Sen University; Freudenberg Apollo Filtration Technologies Co Ltd
Priority date: 2019-07-26
Filing date: 2020-07-23
Publication date: 2020-09-22
Also published as: CN213699906U; CN213699905U; CN213699904U; CN213699903U; CN111686689A; CN111686691A

Abstract

The invention relates to the technical field of activated carbon loading, in particular to loaded activated carbon and a preparation method and a device thereof. The preparation method of the supported activated carbon provided by the invention comprises the following steps: and vacuumizing the reaction kettle filled with the activated carbon, and introducing the impregnation liquid into the reaction kettle for impregnation to obtain the supported activated carbon. According to the invention, the reaction kettle filled with the activated carbon is vacuumized, so that the air pressure in the active carbon pore canal is reduced, a negative pressure environment is formed in the active carbon pore canal, the mass transfer process of the active carbon impregnation is enhanced through the pressure difference, the active components in the impregnation liquid can be promoted to be uniformly adsorbed on the adsorption sites on the surface of the active carbon, the loading capacity of the active components in the active carbon is improved, and the obtained loaded active carbon has good performance; the method provided by the invention is simple to operate and high in production efficiency, the whole preparation process is carried out in a sealed environment, no active carbon dust and chemical medicine escape exist, and the requirement of clean production is met.

Description

Supported activated carbon and preparation method and device thereof

Technical Field

The invention relates to the technical field of activated carbon loading, in particular to loaded activated carbon and a preparation method and a device thereof.

Background

With the rapid development of economy and improvement of living standard in China, the requirement of people on indoor environment is higher and higher. With the use of decoration and a large number of furniture decorations, a large number of chemical pollutants fill indoor environments such as offices, meeting rooms, home furnishings and the like, and serious harm is caused to human bodies. Indoor air pollution has become one of the problems of high concern to human beings, and especially, formaldehyde pollution is the most representative.

Formaldehyde, also known as formil, is a colorless irritant gas that has irritant effects on the eyes and nose of a human. Formaldehyde is the most common poison for indoor air pollution. At present, formaldehyde is determined as carcinogenic and teratogenic substances by the world health organization, and the indoor concentration reaches 0.5mg/m³Can cause the human body to generate lacrimation and the symptoms of abnormal sensitivity of eyes. Chronic respiratory diseases, nasopharyngeal carcinoma, colon cancer, brain tumor, cell nucleus gene mutation and the like can be caused by long-term exposure to low-dose formaldehyde.

Adsorption technology is one of the main methods for indoor air purification. The active carbon is a kind of adsorbent commonly used in adsorption method, and is a porous hydrophobic adsorbent prepared by taking carbon-containing substances (charcoal, wood chips, fruit shells, coal, coconut shells and the like) as raw materials through high-temperature dehydration, carbonization and activation, and has stable chemical properties, acid resistance, alkali resistance and heat resistance. Most of the formaldehyde-removing air purifiers produced at home and abroad currently use active carbon as a main adsorption material of a filter element, and remove pollutants such as formaldehyde in the air by an adsorption method. However, the air purifier with the common activated carbon as the filter element has low purification efficiency, and in the air purification process, the adsorbent needs to selectively adsorb target pollutants, but for different pollutant molecules with similar sizes, the adsorption effect of the activated carbon is not selective, and the pollutant molecules cannot be adsorbed directionally. Therefore, the activated carbon needs to be modified to improve the adsorption capacity of the activated carbon to target pollutants. Currently, a commonly used modification method is to impregnate activated carbon with a solution having a specific property or function, so that the activated carbon can selectively adsorb a target substance, thereby improving the air purification capability. However, the traditional activated carbon impregnation modification production process has the disadvantages of complex operation, low process efficiency, long production period, large material loss and poor activated carbon loading effect. Meanwhile, the problems of large occupied area, large noise and environmental pollution, high emission and the like caused by the lack of scientific process connection and equipment layout among different processes are solved.

Disclosure of Invention

The invention aims to provide a load type activated carbon and a preparation method and a device thereof, the method provided by the invention has high production efficiency, adopts automatic equipment integrating vacuum impregnation, filtration and vacuum drying to simplify equipment, simplifies a modification process, improves the load efficiency and effect of the activated carbon, obviously improves the production efficiency, reduces the material consumption and the human resource cost, and promotes clean production; in order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a preparation method of supported activated carbon, which comprises the following steps:

and vacuumizing the reaction kettle filled with the activated carbon, and introducing the impregnation liquid into the reaction kettle for impregnation to obtain the supported activated carbon.

Preferably, the operation method of the vacuum pumping treatment comprises the following steps: sealing the reaction kettle filled with the activated carbon, and vacuumizing the sealed reaction kettle by using a vacuum pump until the vacuum degree is selected from any one of the following numerical value ranges: 0.04 to 0.06MPa, 0.059 to 0.061MPa and 0.01 to 0.03 MPa. Further, the vacuum degree in the reaction kettle was maintained for 20min or more. Preferably, the vacuum degree in the reaction kettle is maintained for 25-30 min.

Preferably, the active component in the impregnation liquid comprises diethylenetriamine or tetraethylenepentamine, and the mass content of the active component is 10-15%.

Preferably, the mass ratio of the activated carbon to the impregnating solution is 1: (2.5-3).

Preferably, the mass ratio of the activated carbon to the impregnating solution is 1: (3.9 to 4.1)

Preferably, the time of the dipping treatment is 50-60 min.

Preferably, in the dipping treatment process, stirring for 30-60 s every 8-10 min; the stirring is realized by the integral rotation of the reaction kettle.

Preferably, the impregnation treatment further comprises the following heating and drying treatment steps: carrying out solid-liquid separation on the obtained system, and heating and drying the obtained activated carbon loaded with the impregnation liquid: controlling the temperature in the reaction kettle to rise to 90-100 ℃ for a preset time, then pumping out the water vapor in the reaction kettle, simultaneously ventilating the reaction kettle with the outside, and controlling the temperature in the reaction kettle to be kept at 75-85 ℃ for the preset time; and (4) reducing the temperature in the reaction kettle after drying, and discharging after the temperature reaches 40-45 ℃ to obtain the finished product of the activated carbon.

Preferably, in the step of dipping treatment, the rotation mode of the reaction kettle is set as follows: the rotation speed is 10-12rpm, and the rotation time is 45-47 seconds every 15-17 minutes.

Preferably, in the heating and drying treatment step, the rotation mode of the reaction kettle is set as follows: after stopping for 3-5 seconds every 45-47 seconds of forward rotation, reversely rotating for the same time.

Preferably, the initial concentration of the impregnation liquid is 10% to 15%.

Preferably, the temperature of the dipping treatment is 50-70 ℃.

The invention provides the supported activated carbon prepared by the method in the technical scheme.

The invention provides a device for preparing the load type active carbon in the technical scheme, which comprises a vacuum pump, a reaction kettle and a dosing box, wherein the reaction kettle is connected with the vacuum pump and/or the dosing box through a valve; the reaction kettle 3 is connected with a pressure gauge.

Preferably, when the reaction kettle is connected with the vacuum pump and the dosing tank through valves, the reaction kettle, the vacuum pump and the dosing tank are connected through a three-way valve.

The invention provides a preparation method of supported activated carbon, which comprises the following steps: and vacuumizing the reaction kettle filled with the activated carbon, and introducing the impregnation liquid into the reaction kettle for impregnation to obtain the supported activated carbon. According to the invention, the reaction kettle filled with the activated carbon is vacuumized, so that the air pressure in the active carbon pore canal is reduced, a negative pressure environment is formed in the active carbon pore canal, the mass transfer process of the active carbon impregnation is enhanced through the pressure difference, the active components in the impregnation liquid can be promoted to be uniformly adsorbed on the adsorption sites on the surface of the active carbon, the loading capacity of the active components in the active carbon is improved, and the obtained loaded active carbon has good performance; the method provided by the invention is simple to operate and high in production efficiency, the whole preparation process is carried out in a sealed environment, no active carbon dust and chemical medicine escape exist, and the requirement of clean production is met. The experimental results of the examples show that,the load type activated carbon prepared by the method is prepared into the filter element, and the formaldehyde clean air quantity (FCADR) of the filter element is 69.54-86.79 m³/h。

An apparatus for preparing a supported activated carbon, comprising: reactor and evacuating device, the reactor includes: the reactor comprises a base and a reactor shell, wherein the reactor shell is rotatably connected with the base, an accommodating cavity and a circulation cavity are arranged in the reactor shell, the accommodating cavity is used for storing materials, the circulation cavity is used for accommodating a heat exchange medium, and the circulation cavity is arranged at the outer side of the accommodating cavity and separated from the accommodating cavity; the vacuumizing device is connected with the containing cavity so as to vacuumize the containing cavity.

Therefore, the vacuum pumping device is arranged, so that negative pressure is generated in the containing cavity of the reactor shell, the negative pressure provides driving force for the dipping formula solution, solute in the solution can be favorably diffused in the active carbon pore canal, the solute can be easily combined with adsorption sites on the active carbon, and the purpose of strengthening adsorption is achieved.

In some embodiments, the vacuum pumping device comprises a vacuum unit and a buffer tank, the buffer tank is connected between the vacuum unit and the reactor, and an air outlet of the buffer tank is provided with a filtering structure.

In some embodiments, the vacuum assembly comprises a pressure sensor for emitting a hold pressure signal when detecting that the air inlet pressure of the vacuum assembly reaches a preset value.

In some embodiments, the vacuum pumping device is communicated with the accommodating cavity through a vacuum pumping pipeline, the reactor shell is pivotally connected with the base through a rotary connecting piece positioned on one side, the rotary connecting piece comprises a rotary shaft and a rotary shaft seat which are fixed with each other, the rotary shaft seat is fixed with the reactor shell, the rotary shaft and the rotary shaft seat are both of hollow structures, and the vacuum pumping pipeline axially penetrates through an inner hole of the rotary shaft and an inner hole of the rotary shaft seat, which are positioned on one side of the reactor shell.

In some embodiments, still include the adapter, the adapter is in the one end that deviates from the reactor casing of pivot with the pivot is connected, the pivot is fixed in the base and can rotate for the adapter, the evacuation pipeline pass the hole of adapter and with the adapter is fixed.

In some embodiments, the outer wall of the rotating shaft is provided with a first connecting flange which is matched with the rotating shaft in a rotating mode, the outer wall of the adapter is provided with a second connecting flange, the first connecting flange is connected with the second connecting flange through a fastener, the rotating shaft is provided with a positioning groove, the adapter is inserted into the positioning groove, and the rotating shaft can rotate relative to the adapter.

In some embodiments, the evacuation pipeline includes first pipeline and second pipeline and connects the cross joint between them, first pipeline locate the pivot in the adapter, the one end and the cross joint of second pipeline are connected and the other end with evacuating device connects, two interfaces of cross joint are equipped with manometer and thermometer respectively.

In some embodiments, the reactor housing comprises: the shell body, interior casing is in the inboard of shell body with shell body coupling, inject the chamber that holds that is used for holding the active carbon in the interior casing, interior casing with the shell body is injectd jointly and is used for holding heat transfer medium's circulation chamber, the circulation chamber is including being close to the feed liquor chamber that interior casing set up and the outside in feed liquor chamber with the liquid return chamber of feed liquor chamber intercommunication.

In some embodiments, the reactor shell has a double-cone shape, the liquid inlet cavity includes a cylindrical cavity and two truncated cone-shaped cavities connected to two ends of the cylindrical cavity, the shape of the liquid inlet cavity is identical to that of the inner shell, the liquid inlet cavity is disposed around the inner shell, the liquid return cavity extends linearly, and the liquid return cavity is opposite to a portion of the liquid inlet cavity on the outer side of the liquid inlet cavity.

In some embodiments, a side of the reactor shell is provided with a rotary connector connected to at least one of the outer shell and the inner shell, the rotary connector being adapted to be inserted into the liquid inlet chamber and the liquid return chamber to independently communicate with both.

In some embodiments, the rotational connection comprises at least: install the pivot seat at the lateral wall middle part of reactor housing, the center of pivot seat forms to rotation center, the pivot seat passes the shell body and stretches into in proper order return the liquid chamber in the feed liquor chamber, the pivot seat have with the inlet that the feed liquor chamber is linked together, with return the liquid mouth that the liquid chamber is linked together.

In some embodiments, the rotating shaft seat has a liquid returning inner hole communicated with the liquid returning port, and a liquid inlet inner hole connected with the liquid inlet, the liquid returning inner hole is used for being connected with an external liquid passing pipeline, the liquid inlet inner hole and the liquid returning inner hole are separated by a separating piece, and the liquid inlet cavity is used for being connected with an external liquid inlet pipeline through the separating piece.

In some embodiments, the inlet chamber has an inlet and an outlet, and a plurality of baffles are disposed in the inlet chamber between the inlet and the outlet.

Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.

Drawings

The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:

FIG. 1 is a schematic view showing the connection between a vacuum pump and a reaction vessel in an apparatus for producing a supported activated carbon (first connection mode);

FIG. 2 is a schematic view showing the connection between a dosing tank and a reaction vessel in an apparatus for preparing supported activated carbon (first connection means);

FIG. 3 is a schematic structural view of an apparatus for preparing a supported activated carbon (second connection means);

fig. 4 is a graph comparing the performance of the supported activated carbons prepared in the examples and comparative examples.

FIG. 5 is a schematic view of a simple apparatus for manufacturing a supported activated carbon in an actual test process.

FIG. 6 is a schematic view of an apparatus for preparing a supported activated carbon according to an embodiment of the present invention;

FIG. 7 is an enlarged partial schematic view of region B of FIG. 6;

FIG. 8 is a schematic sectional front view of a reactor shell according to an embodiment of the invention;

FIG. 9 is an enlarged partial schematic view of the reactor shell of FIG. 8;

fig. 10 is a partially enlarged schematic view of the region a in fig. 8.

Reference numerals:

in the figures 1-3, 1-a vacuum pump, 2-a valve, 3-a reaction kettle, 4-a pressure gauge, 5-a dosing tank, 6-a three-way valve, 7-a valve, 8-a valve, 9-a valve; 10-a suction filter flask, 11-a rubber tube, 12-a rubber plug, 13-a plastic tube, 14-a beaker, 15-a formula solution, 16-activated carbon and 17-a valve.

The reaction kettle comprises a reaction kettle 300, a reaction kettle shell 301, a base 302, a bearing seat 3021, a power mechanism 303, a driving motor 3031, a worm gear reducer 3032, a belt wheel mechanism 3033, a chain wheel mechanism 3034,

the outer shell 310, the liquid return chamber 311,

an inner shell 320, a liquid inlet cavity 321, an inlet 321a, an outlet 321b, a feed inlet 322, a discharge outlet 323, a baffle 324,

a second rotary connector 330, a second rotary shaft seat 331, a liquid inlet 331a, a liquid return port 331b, a liquid return inner hole 331c, a liquid inlet inner hole 331d, a partition 331e, a second rotary shaft 332,

a first rotary connector 340, a first rotary shaft seat 341, a first rotary shaft 342, a first connecting flange 344, a second connecting flange 343,

the first adapter part 350 is provided with a first connector,

an accommodating cavity a, a circulating cavity b, a central axis e and a rotating center f;

the vacuum-pumping device 400 is provided with a vacuum-pumping device,

the vacuum unit 410, the buffer tank 420, the filter structure 421, the first pipeline 431, the second pipeline 432, the four-way joint 433, the pressure gauge 434 and the thermometer 435.

Detailed Description

Embodiments of the present invention will be described in detail below, the embodiments described with reference to the drawings being illustrative, and the embodiments of the present invention will be described in detail below.

The invention carries out vacuum-pumping treatment on the reaction kettle filled with the activated carbon. The activated carbon is not particularly limited in the present invention, and may be one known to those skilled in the art; in the invention, the activated carbon preferably comprises DDT-046 formula activated carbon or DDT-030 formula activated carbon, wherein the index parameters of the DDT-046 formula activated carbon and the DDT-030 formula activated carbon are shown in a table 1 at the temperature of 25 ℃ and the air pressure of 101.325 KPa; the measurement method of each index is specifically as follows:

pH: uniformly mixing 10g of activated carbon and 40g of water, standing for 20min at room temperature, and measuring the pH value of the water in the obtained system by using an acidimeter;

water content: putting 1.5g of activated carbon into a moisture tester to measure the moisture content of the activated carbon;

filling density: the active carbon falls into a 100mL measuring cylinder through vibration, the active carbon is vibrated for many times until the volume of the active carbon is not changed, and the mass of the 100mL active carbon is weighed to calculate the filling density;

strength: the determination is carried out according to the strength test method of GB/T20451 and 2006 activated carbon ball disk method;

carbon tetrachloride adsorption efficiency (CTC): the carbon tetrachloride adsorption rate (activity) was measured by the method specified in "GB/T12496.5-1999 test method for woody activated carbon".

TABLE 1 index parameters for DDT-046 and DDT-030 formulations of activated carbon

Activated carbon	pH value	Water content (%)	Packing density (g/L)	Strength (%)	CTC(％)
						DDT-046 formula activated carbon	9.26	1.38	382	97.5	100
DDT-030 formula active carbon	1.74	1.49	580	98.5	100

In the present invention, the operation method of the vacuum treatment preferably includes the steps of: and (3) sealing the reaction kettle filled with the activated carbon (specifically, the reaction kettle can be sealed by using a sealing plug), vacuumizing the sealed reaction kettle by using a vacuum pump until the vacuum degree is 0.04-0.06 MPa, and closing the vacuum pump to keep the vacuum degree in the reaction kettle unchanged for 25-30 min. According to the invention, the reaction kettle filled with the activated carbon is vacuumized, so that the air pressure in the active carbon pore canal is reduced, a negative pressure environment is formed in the active carbon pore canal, the subsequent mass transfer process of activated carbon impregnation is enhanced through pressure difference, the active components in the impregnation liquid are promoted to be uniformly adsorbed on the adsorption sites on the surface of the activated carbon, the loading capacity of the active components in the activated carbon is improved, and the obtained loaded activated carbon has good performance. The method is favorable for fully and uniformly combining active components in the impregnation liquid with the adsorption sites on the surface of the active carbon by controlling the vacuum degree condition and the time for maintaining the vacuum degree; if the vacuum degree is too low, the pressure in the pores of the activated carbon cannot be effectively reduced, the impregnation mass transfer process is not enhanced by enough pressure difference, and the corresponding effect cannot be achieved; the vacuum degree is maintained for a period of time, so that the gas in the active carbon holes can be fully escaped, if the impregnation liquid is directly introduced without being maintained for a period of time after the vacuum pumping, the gas in the deep parts of the holes can not be discharged out of the holes, and the load of the active components is not obviously improved.

After the vacuum pumping treatment is finished, the impregnation liquid is introduced into a reaction kettle for impregnation treatment, and the load type activated carbon is obtained by drying after the impregnation treatment is finished. In the present invention, the impregnation liquid preferably includes an active component that facilitates selective adsorption of a target substance by the activated carbon, and a solvent. In the invention, the active component preferably comprises diethylenetriamine or tetraethylenepentamine, more preferably diethylenetriamine, and the mass content of the active component is preferably 10-15%; the solvent is preferably water. In the present invention, the mass ratio of the activated carbon to the impregnation liquid is preferably 1: (2.5-3).

In the present invention, the impregnation solution is introduced into the reaction vessel to perform the impregnation treatment, specifically, the impregnation solution is introduced into the reaction vessel under a normal pressure condition by using a pressure difference, and then the reaction vessel is returned to the normal pressure to perform the impregnation treatment. In the invention, the time of the dipping treatment is preferably 50-60 min, and the time of the dipping treatment is counted after the dipping solution is completely introduced into the reaction kettle; the dipping treatment is preferably carried out at room temperature and normal pressure (i.e. no additional heating, cooling or pressurizing or vacuumizing is needed), and more preferably carried out at 24-26 ℃ and normal pressure; in the invention, in the dipping treatment process, stirring is preferably carried out for 30-60 s every 8-10 min; the stirring is preferably realized through the whole rotation of reation kettle, specifically is whole along clockwise, rotate with 15 ~ 20rpm rotational speed with reation kettle, is favorable to realizing the even flooding of flooding liquid like this, guarantees that flooding liquid evenly supports on active carbon, and sets up the stirring rake in reation kettle among the conventional process, stirs through the stirring rake and has the dead angle easily, is difficult for realizing the even flooding of flooding liquid, and product quality homogeneity is poor. According to the invention, through a mass transfer process of pressure difference reinforced activated carbon impregnation, the active components in the impregnation liquid can be promoted to be uniformly adsorbed on the adsorption sites on the surface of the activated carbon, the loading capacity of the active components in the activated carbon is improved, and the obtained loaded activated carbon has good performance.

After the impregnation treatment is completed, the invention preferably performs solid-liquid separation on the obtained system, and dries the obtained activated carbon loaded with the impregnation liquid to obtain the loaded activated carbon. The solid-liquid separation method of the present invention is not particularly limited, and a solid-liquid separation method known to those skilled in the art, specifically, filtration, may be employed. In the invention, the drying temperature is preferably 100-110 ℃; the invention removes the solvent of the impregnation liquid in the activated carbon by drying, which is beneficial to improving the performance of the supported activated carbon.

The invention provides the supported activated carbon prepared by the preparation method in the technical scheme, which comprises activated carbon and active components loaded on the surface of the activated carbon. In the supported activated carbon provided by the invention, the active component is uniformly adsorbed on the surface of the activated carbon, the loading capacity of the active component (specifically, the mass of the active component loaded on each gram of activated carbon, and the unit is recorded as g/g of activated carbon) is high, and in the supported activated carbon, the loading capacity of the active component is preferably 0.13-0.21 g/g of activated carbon, and more preferably 0.17-0.19 g/g of activated carbon.

The invention provides a device for preparing load type active carbon by using the method of the technical scheme, which comprises a vacuum pump 1, a reaction kettle 3 and a dosing box 5, wherein the reaction kettle 3 is connected with the vacuum pump 1 and/or the dosing box 5 through a valve; the reaction kettle 3 is connected with a pressure gauge 4.

In an embodiment of the present invention, the apparatus specifically includes the following two connection modes:

the first connection is shown in fig. 1 and 2, and the reaction vessel 3 is connected to a vacuum pump 1 or a dosing tank 5 via a valve 2. Specifically, when the device is used for preparing the load-type activated carbon, firstly, a reaction kettle 3 is connected with a vacuum pump 1 through a conduit with a valve 2, the activated carbon is put into the reaction kettle 3, and the reaction kettle 3 is sealed by a sealing plug; then, starting the vacuum pump 1 until the vacuum degree in the reaction kettle 3 is increased to 0.04-0.06 MPa (the vacuum degree is calculated through the pressure indicated by the pressure gauge 4), closing the valve 2, then closing the vacuum pump 1, and maintaining the vacuum degree in the reaction kettle 3 for 25-30 min; putting the impregnation liquid into a dosing tank 5, taking down a vacuum pump 1, connecting a reaction kettle 3 with the dosing tank 5, opening a valve 2, introducing the impregnation liquid into the reaction kettle 3 by using pressure difference, recovering normal pressure in the reaction kettle 3 after the impregnation liquid is completely introduced into the reaction kettle 3, then carrying out impregnation treatment for 50-60 min at room temperature and normal pressure, and stirring for 30-60 s every 8-10 min in the impregnation treatment process (specifically, rotating the whole reaction kettle at a rotating speed of 15-20 rpm in a clockwise direction); and after the impregnation treatment is finished, carrying out solid-liquid separation on the obtained system (comprising impregnation residual liquid and the activated carbon loaded with the impregnation liquid), drying the obtained activated carbon loaded with the impregnation liquid at the temperature of 100-110 ℃ to obtain the loaded activated carbon, and recycling the impregnation residual liquid after further treatment (for example, when the activated carbon dust cannot be effectively removed under the solid-liquid separation precision, further filtration and other operations are needed).

The second connection mode is as shown in fig. 3, the reaction kettle 3 is connected with the vacuum pump 1 and the dosing tank 5 through a valve, at this time, the reaction kettle 3, the vacuum pump 1 and the dosing tank 5 are connected through a three-way valve 6, so that the vacuum pump 1 and the dosing tank 5 do not need to be exchanged in the using process, and the related operation can be realized by controlling the three-way valve 6, wherein a valve 7 is arranged between the vacuum pump 1 and the three-way valve 6, a valve 8 is arranged between the dosing tank 5 and the three-way valve 6, and a valve 9 is arranged between the reaction kettle 3 and the three-. Specifically, when the device is used for preparing load-type activated carbon, the activated carbon is placed in a reaction kettle 3, impregnation liquid is placed in a dosing tank 5, a vacuum pump 1, the dosing tank 5 and the reaction kettle 3 are respectively connected with a three-way valve 6 through a conduit with valves 7-9, the valve 8 is closed, the valves 7 and 9 are opened, and the reaction kettle 3 is sealed by a sealing plug; then, starting the vacuum pump 1 until the vacuum degree in the reaction kettle 3 is increased to 0.04-0.06 MPa (the vacuum degree is calculated by the pressure indicated by the pressure gauge 4), closing the valves 7 and 9, then closing the vacuum pump 1, and maintaining the vacuum degree in the reaction kettle 3 for 25-30 min; opening valves 8 and 9, introducing the impregnation liquid into the reaction kettle 3 by using pressure difference, recovering the normal pressure in the reaction kettle 3 after the impregnation liquid is completely introduced into the reaction kettle 3, then carrying out impregnation treatment for 50-60 min at room temperature and normal pressure, and stirring for 30-60 s every 8-10 min in the impregnation treatment process (specifically, rotating the whole reaction kettle in a clockwise direction at a rotating speed of 15-20 rpm); and after the impregnation treatment is finished, carrying out solid-liquid separation on the obtained system (comprising impregnation residual liquid and the activated carbon loaded with the impregnation liquid), drying the obtained activated carbon loaded with the impregnation liquid at the temperature of 100-110 ℃ to obtain the loaded activated carbon, and recycling the impregnation residual liquid after further treatment (for example, when the activated carbon dust cannot be effectively removed under the solid-liquid separation precision, further filtration and other operations are needed).

The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The apparatus of fig. 1 and 2 is used for preparing supported activated carbon, and comprises the following steps:

connecting a reaction kettle 3 with a vacuum pump 1 through a conduit with a valve 2, putting activated carbon (DDT-046 formula activated carbon, specific index parameters are shown in table 1) into the reaction kettle 3, and sealing the reaction kettle 3 by using a sealing plug; then, starting a vacuum pump 1 to vacuumize the reaction kettle 3 (the vacuum degree is calculated by the pressure indicated by a pressure gauge 4 and is 0.05MPa), closing a valve 2, then closing the vacuum pump 1, and maintaining the vacuum degree in the reaction kettle 3 for 30 min; putting an impregnation liquid (a diethylenetriamine aqueous solution, the mass fraction of diethylenetriamine is 13.3%, the mass ratio of active carbon to the impregnation liquid is 1: 3) into a medicine preparation tank 5, taking down a vacuum pump 1, connecting a reaction kettle 3 with the medicine preparation tank 5, opening a valve 2, introducing the impregnation liquid into the reaction kettle 3 by using pressure difference, recovering the normal pressure in the reaction kettle 3 after the impregnation liquid is completely introduced into the reaction kettle 3, carrying out impregnation treatment for 1h under the conditions of room temperature (24 ℃) and normal pressure, and stirring for 60s every 10min in the impregnation treatment process (specifically, rotating the whole reaction kettle in a clockwise direction at a rotating speed of 20 rpm); after the impregnation treatment is finished, filtering the obtained system (comprising impregnation residual liquid and activated carbon loaded with impregnation liquid), drying the obtained activated carbon loaded with the impregnation liquid at 100 ℃ to obtain loaded activated carbon (the loading amount of the active component is 0.16g/g of the activated carbon), and further treating the impregnation residual liquid for recycling.

Example 2

Supported activated carbon was produced in the same manner as in example 1, except that the degree of vacuum of the autoclave 3 was 0.04MPa when it was evacuated.

Example 3

Supported activated carbon was produced in the same manner as in example 1, except that the degree of vacuum of the reaction vessel 3 was 0.06MPa when the vacuum treatment was conducted.

Comparative example 1

Supported activated carbon was produced in the same manner as in example 1, except that the degree of vacuum of the reaction vessel 3 was 0MPa when the vacuum treatment was conducted.

Comparative example 2

Supported activated carbon was produced in the same manner as in example 1, except that the degree of vacuum of the reaction vessel 3 was 0.08MPa when the vacuum treatment was conducted.

Application example

Mixing the supported activated carbon prepared in examples 1-3 and comparative examples 1-2 with DDT-030 formula activated carbon (specific index parameters are shown in table 1) according to a mass ratio of 3:1 to obtain mixed activated carbon; and uniformly fixing the mixed activated carbon on a filter screen (488 +/-1 mm × 284 +/-1 mm) by using glue, and packaging to prepare the mesh-shaped air purifier filter element. The test is carried out in the detection center of Apollo environmental protection equipment Co., Ltd. of Sunshan district, Changshan, with reference to GB/T18801-2015 air purifier, GB/T18883-2002 indoor air quality standard, GB/T18204.2-2014 public place sanitation test method (part 2: chemical pollutants) and HJ/T167-2004 indoor environmental air quality monitoring technology, and the results are shown in figure 4 and table 2 (FCADR value of the product obtained under different vacuum degree conditions to formaldehyde is measured respectively, the arithmetic mean value is taken after the maximum value and the minimum value are removed and the measurement error is corrected, and the mean FCADR value of the product obtained under the vacuum degree condition to formaldehyde is obtained).

TABLE 2 Performance (FCADR) of Supported activated carbons prepared in examples 1 to 3 and comparative examples 1 to 2

As can be seen from fig. 4 and table 2, the product performance obtained under the vacuum degree of 0.04MPa, 0.05MPa and 0.06MPa is improved compared with the prior art (the vacuum degree is 0MPa), and the product performance may be reduced under the vacuum degree of 0.08MPa due to the blocking of the pores of the activated carbon by the adsorbed excessive diethylenetriamine; the product obtained under the condition that the vacuum degree is 0.05MPa has the optimal performance, and the average FCADR value of formaldehyde is up to 86.79m³And h, compared with the product obtained by the existing process (the vacuum degree is 0MPa), the performance is improved by 21.6 percent, which shows that the performance of the loaded activated carbon prepared by the method provided by the invention is greatly improved.

From the above, the present invention has the following advantages:

(1) according to the invention, the closed reaction kettle containing the activated carbon is vacuumized, so that the air pressure in the active carbon pore channel is reduced, the diffusion of active components in the impregnation liquid in the active carbon pore channel is facilitated, the adsorption of the active components by the activated carbon can be promoted, the loading capacity is improved, and the loaded activated carbon with better performance is obtained.

(2) The method of the invention accelerates the process of active carbon adsorption of active components compared with the process of normal pressure by vacuumizing and dipping to improve the product performance, shortens the working time and can obviously improve the production efficiency.

(3) The method is simple and convenient to operate, the connection between the devices is scientific and reasonable, multiple material turnover steps are omitted, material loss is reduced, and human resources are saved.

(4) The method is carried out in a sealed environment, no active carbon dust and chemical medicine escape, and the requirement of clean production is met.

Example 4

In order to improve the product performance, the closed container with the activated carbon 16 is vacuumized, the air pressure in the pore canal of the activated carbon 16 is reduced, then the solution is put in, and the pressure difference provides a driving force for mass transfer, so that solute in the solution can be favorably diffused in the pore canal of the activated carbon 16, the solute can be more easily combined with the adsorption site on the activated carbon 16, and the purpose of enhancing adsorption is achieved. Aiming at the normal-pressure impregnation process of the activated carbon 16, the influence trend of parameters such as the operation pressure, the mass ratio (liquid-solid ratio) of the impregnation solution to the activated carbon 16, the initial concentration of the solution, the impregnation temperature and the like on the product quality is researched, and the optimized parameters of the impregnation process are obtained.

A series of experiments were carried out, as shown in connection with figure 5, with the following experimental procedure:

1) putting a certain amount of activated carbon 16 into a suction filtration bottle 10, plugging the rubber stopper 12, closing a valve 17 on a connecting conduit between the rubber stopper 12 and a beaker 14, vacuumizing the interior of the bottle to a specified pressure by using a vacuum pump, maintaining for 25-30min, and then closing the vacuum pump;

2) opening a valve 17 on the conduit, guiding the formula solution 15 into the filtration bottle 10 through a plastic pipe 13 by using pressure difference, and further soaking the activated carbon 16;

3) filtering and separating the solution and the activated carbon 16 after the impregnation is finished, mixing 0.25-0.3g of the separated and filtered solution with 25-30ml of water, and titrating by using 0.1-0.12mol/L hydrochloric acid. Recording titration data, calculating the adsorption capacity of the activated carbon 16 according to the consumption of the hydrochloric acid, and judging whether the loading requirement of the activated carbon 16 is met;

4) and (4) putting the separated activated carbon 16 into an oven for drying, and recording the filling density and the pH value of the adsorbed activated carbon 16. Ensuring that the filling density of the activated carbon 16 is not more than 520g/L and the pH value is between 9.5 and 10.6;

5) mixing dried 230-250g of activated carbon and 030-16 activated carbon according to the mass ratio of 3:1 to remove amine odor, preparing a mesh filter element, and detecting FCADR (formaldehyde clean air quantity).

The experimental results are as follows:

five experiments are respectively carried out under the pressure of 0.09MPa to 0.11MPa and 0.059MPa to 0.061MPa in the bottle, fifteen groups of samples are obtained, and FCADR (formaldehyde clean air quantity) is respectively measured. Certain fluctuations in results can occur due to glue plugging during the process of manufacturing the reticulated filter element from different batches of activated

carbon

16 and 10% operational errors during the sample testing process. FCADR (formaldehyde clean air) was averaged for both process samples after removing the outlier minima results, as shown in table 3 below:

table 3 properties (FCADR) of the supported activated carbon prepared in example 4

Example 5

It can be seen that the FCADR (formaldehyde clean air content) product obtained by adopting the vacuum process is effectively improved compared with the original process (normal pressure), the improvement rate is 11.4%, and the product performance is obviously improved.

In order to explore the influence of factors such as the mass ratio (liquid-solid ratio) of the impregnation solution to the activated carbon 16 under normal pressure, the initial concentration of the solution, the impregnation temperature and the like on the adsorption quantity of the activated carbon 16 or the product quality, in the experimental process, the influence factors are changed one by one under the condition that other conditions are not changed under normal pressure. The specific experimental steps are as follows:

1) putting a certain amount of activated carbon 16 into the filtration bottle 10, opening the rubber stopper 12 on the filtration bottle 10, pouring the solution into the filtration bottle 10, then plugging the rubber stopper 12, and dipping the activated carbon 16 for a certain time;

2) the mass ratio of the active carbon to the diethylenetriamine solution, the initial concentration of the diethylenetriamine solution and the dipping temperature are respectively changed one by one. Only one parameter is changed at a time to keep the other parameters constant;

4) and drying the separated activated carbon 16, and recording the filling density and the pH value of the adsorbed activated carbon 16. Ensuring that the filling density of the activated carbon 16 is not more than 520g/L and the pH value is between 9.5 and 10.6;

The experimental results are as follows:

1) liquid-solid ratio

The performance results of the samples tested at liquid-to-solid ratios of 1.9-2.1,2.4-2.6,3.4-3.6, and 3.9-4.1 are shown in Table 4 below:

TABLE 4

Liquid-solid ratio	1.9-2.1	2.4-2.6	3.4-3.6	3.9-4.1
					FCADR (Formaldehyde clean air amount)/m³/h	66.24	70.02	70.74	74.16

It can be seen that the FCADR value increases with increasing liquid-solid ratio, the variation is not obvious between 2.4 and 3.6, the performance is optimal when the liquid-solid ratio is 3.9 to 4.1, and the FCADR (formaldehyde clean air quantity) is increased from 70.74 to 74.16.

2) Initial concentration of solution

Four sets of experiments were conducted at initial concentrations of 4.5% to 5.5%, 9.5% to 10.5%, 14.5% to 15.5%, 19.5% to 20.5% of the solution, and the results obtained are shown in table 5 below:

TABLE 5

Concentration (%)	4.5-5.5	9.5-10.5	14.5-15.5	19.5-20.5
					FCADR (Formaldehyde clean air amount)/m³/h	66.24	65.88	78.66	75.42

It can be seen that at low concentration, the influence of the increase of the initial concentration of the solution on the performance of the product is not obvious, the product performance increases with the increase of the initial concentration of the solution after the concentration is higher than 10%, the product performance reaches the optimum at the concentration of 14.5-15.5%, and the product performance is not changed after the concentration is continuously increased.

3) Temperature of

The experiments were carried out at 24-26 deg.C, 44-46 deg.C, 64-66 deg.C, and 84-86 deg.C, respectively, and the adsorption efficiency of the activated carbon 16 to the solute in the solution was measured by titration, and the results are shown in Table 6 below:

TABLE 6

Temperature (. degree.C.)	24-26	44-46	64-66	84-86
					Adsorption efficiency (%)	39.8	40.3	44.6	45.6

It can be seen that in the temperature range of 24-86 ℃, the adsorption efficiency of the activated carbon 16 on the aldehyde removing agent is gradually improved along with the temperature rise, the loading effect is best at 84-86 ℃, the adsorption efficiency reaches 45.6%, and is improved by 14.6% compared with the room temperature (24-26 ℃). However, considering industrial application, the temperature of 84-86 ℃ is not favorable for the safety of equipment, so that the adoption of the temperature of 50-70 ℃ can simultaneously achieve the safety of the equipment and the adsorption efficiency of the activated carbon.

Example 6

In the actual manufacturing process, the device for manufacturing the supported activated carbon 16 may include a vacuum generating device, a heating and cooling device and a double-cone reactor, all the parts are connected by a pipeline, the vacuum generating device may be a vacuum pump, and the double-cone reactor is a device for containing the activated carbon 16 and impregnating the activated carbon 16, and may also adopt a reaction kettle.

The specific manufacturing method of the supported activated carbon 16 is as follows:

1) adding a certain amount of original activated carbon 16 into the double-cone reactor, vacuumizing, and maintaining the pressure in the double-cone reactor to be stable for 30-60 min after reaching the preset pressure;

2) the valve 17 on the cover of the double-cone reactor is connected with the dosing box by a conduit, the valve 17 is opened, the solution is led into the double-cone reactor by pressure difference, then the valve 17 is closed, and the vacuum generating device and the heating and cooling device can be used for adjusting the temperature and pressure in the reactor during dipping. Setting a double-cone reactor rotation mode, wherein the rotation speed is 10-12rpm, and the rotation time is 45-47 seconds every 15-17 minutes;

3) after the impregnation is completed, the reactor is adjusted to the proper position and the valve 17 in the lid is opened to allow the effluent to flow out. After the waste liquid is discharged, the double-cone reactor is rotated, and the moisture accumulated between the gaps of the accumulated active carbon 16 is further discharged by centrifugal force drying. The valve 17 is closed after the waste liquid is exhausted;

4) the heating temperature is set, and the interior of the reactor is heated by a heating and cooling device to evaporate the residual water. Meanwhile, the rotation mode of the double-cone reactor is set to be rotation at the rotating speed of 10-12rpm, so that all parts in the reactor are heated uniformly. After the temperature in the double-cone reactor rises to 90-100 ℃, the vacuum pump is started to pump out water vapor in the reactor, and meanwhile, the valve 17 communicated with the outside is opened for ventilation, so that the boiling point of water is reduced because the pressure in the reactor is lower than the atmospheric pressure, the temperature in the reactor is constant at 75-85 ℃, and the reactor is safer. After drying, reducing the temperature in the reactor by using a heating/cooling device, and discharging after the temperature reaches 40-45 ℃ to obtain a finished product of the activated carbon 16;

5) the lid of the double cone reactor was opened and a small amount of the finished activated carbon 16 was taken to measure its packing density and its mass was calculated. The 030 active carbon 16 is taken according to a fixed mass ratio and put into a reactor, the rotating mode of the double-cone reactor is set after the cover is closed and the device is sealed, the rotating mode is that the double-cone reactor rotates in the reverse direction for the same time after the double-cone reactor stops rotating for 3 to 5 seconds every 45 to 47 seconds, and the total time is 10 to 15 minutes. And discharging after mixing.

In practice, the average FCADR (formaldehyde clean air) value of the finished activated carbon 16 made using the integrated equipment was 75.3. Compared with the finished product produced from a workshop in the same time period, the performance is improved by 12.2 percent.

Example 7

An apparatus for preparing a supported activated carbon according to an embodiment of the present invention is described below with reference to fig. 6 to 10.

As shown in fig. 6, an apparatus for preparing a supported activated carbon according to an embodiment of the first aspect of the present invention includes: a reactor 300 and a vacuum pumping device 400.

The reactor 300 includes: the reactor comprises a base 302, a reactor shell 301 and a power mechanism 303, wherein the reactor shell 301 is connected with the base 302, the power mechanism 303 is connected with the reactor shell 301 to drive the reactor shell 301 to rotate, an accommodating cavity and a circulation cavity are arranged in the reactor shell 301, the accommodating cavity is used for storing materials, the circulation cavity is used for accommodating a heat exchange medium, and the circulation cavity is arranged outside the accommodating cavity and separated from the accommodating cavity; the vacuum-pumping device 400 is connected to the receiving chamber to evacuate the receiving chamber.

From this, through setting up evacuating device 400 to make reactor shell 301 hold the intracavity and produce the negative pressure, the negative pressure provides the motive force for dipping prescription solution, is favorable to the solute in the solution to diffuse in the active carbon pore, makes the solute more combine with adsorption site on the active carbon, reaches the purpose of strengthening the absorption.

As shown in fig. 6, the vacuum pumping apparatus 400 includes a vacuum unit 410 and a buffer tank 420, the buffer tank 420 is connected between the vacuum unit 410 and the reactor 300, and a filter structure 421 is disposed at an air outlet of the buffer tank 420. In other words, the integrated equipment is composed of two parts, i.e., the vacuum pumping device 400 and the reactor 300, which are connected by a metal pipeline, the buffer tank 420 enables the vacuum mechanism to pump vacuum more stably on the reactor 300, and is favorable for maintaining the pressure of the evacuated cavity, and the filter structure 421 can be a filter screen, which can prevent the activated carbon dust from entering the vacuum pumping device 400.

Further, the vacuum unit 410 comprises a pressure sensor (not shown in the figure), and the pressure sensor is used for sending a pressure maintaining signal when detecting that the pressure of the air inlet of the vacuum unit 410 reaches a preset value. In the process of modified production of the activated carbon, after the activated carbon is placed in the reactor 300 and before the activated carbon is supplied with a formula solution, the containing cavity of the reactor shell 301 needs to be vacuumized and pressure-maintained for a preset time, so that automatic control of vacuumizing can be realized by the arrangement of the pressure sensor, when the pressure in the containing cavity reaches the vacuum degree of a preset value, the pressure sensor sends a pressure-maintaining signal, the vacuum unit 410 monitors the vacuum degree in the containing cavity in real time and keeps the vacuum degree in a preset range, and therefore real-time stable pressure maintaining is realized.

As shown in fig. 7, the evacuation device 400 is communicated with the receiving chamber through an evacuation pipe, the reactor shell 301 is pivotally connected to the base 302 through a first rotary connector 340 located at one side, the first rotary connector 340 includes a first rotary shaft 342 and a first rotary shaft 342 base 341 fixed to each other, the first rotary shaft 342 base 341 is fixed to the reactor shell 301, the first rotary shaft 342 and the first rotary shaft 342 base 341 are both hollow, and the evacuation pipe axially passes through an inner hole of the first rotary shaft 342 and an inner hole of the first rotary shaft 342 base 341 located at one side of the reactor shell 301. Specifically, the reactor 300 is connected to the base 302 by a first rotating shaft 342 capable of bearing weight and suspends the reactor shell 301 so that the reactor shell 301 rotates. Thus, the evacuated tube passes through a first rotary connection 340, such as a first shaft 342, to evacuate the receiving cavity. The rotation of the first rotating shaft 342 and the reactor shell 301 does not drive the vacuum-pumping pipeline to rotate together, so that the vacuum pumping and the rotation of the reactor shell 301 can be considered and do not interfere with each other.

Further, a first adapter 350 is further included, the first adapter 350 is connected to the first rotating shaft 342 at an end of the first rotating shaft 342 facing away from the reactor shell 301, the first rotating shaft 342 is fixed to the base 302 and can rotate relative to the first adapter 350, and the vacuum pipe passes through an inner hole of the first adapter 350 and is fixed to the first adapter 350.

Thus, the vacuum line is connected to the receiving cavity through the inner hole of the first adapter 350 and the inner hole of the first rotating shaft 342 in sequence, the first adapter 350 and the vacuum line are fixed relative to the base 302, the first rotating shaft 342 and the first adapter 350 are axially positioned, but the first rotating shaft 342 can rotate relative to the first adapter 350.

In some embodiments, the outer wall of the first rotating shaft 342 is provided with a first connecting flange 344 rotatably engaged with the first rotating shaft 342, the outer wall of the first rotating joint 350 is provided with a second connecting flange 343, the first connecting flange 344 and the second connecting flange 343 are connected by a fastener, the first rotating shaft 342 is provided with a positioning groove, the first rotating joint 350 is inserted into the positioning groove, and the first rotating shaft 342 is rotatable relative to the first rotating joint 350.

Specifically, the first connecting flange 344 is fitted in an annular groove formed in the outer wall of the first rotating shaft 342 so as to be axially positioned, while allowing the first rotating shaft 342 to rotate in an inner hole of the first connecting flange 344, the first connecting flange 344 is bolted to a second connecting flange 343 welded to the outer wall of the first rotating joint 350, and a seal ring may be provided between the end surface of the first rotating joint 350 and the end surface of the first rotating shaft 342.

Therefore, the first rotating shaft 342 and the first rotating joint 350 are axially positioned without restricting the rotation of the reactor shell 301, and the structure is compact and the arrangement is reasonable.

As shown in fig. 6, the vacuum-pumping pipe includes a first pipe 431, a second pipe 432 and a four-way joint 433 connecting the first pipe 431 and the second pipe 432, the first pipe 431 is disposed in the first rotating shaft 342 and the first rotating joint 350, one end of the second pipe 432 is connected to the four-way joint 433, the other end of the second pipe 432 is connected to the vacuum-pumping device 400, and two interfaces of the four-way joint 433 are respectively provided with a pressure gauge 434 and a temperature gauge 435. Through setting up manometer 434 and thermometer 435 directly on the evacuation pipeline to the temperature of holding the intracavity is surveyed indirectly through pressure and the temperature detection to the evacuation pipeline, has avoided additionally to set up the pipeline, has improved the life of manometer 434 and thermometer 435 moreover.

Of course, the temperature meter 435 and the pressure meter 434 may be disposed on the evacuation pipeline, or may be separately led out from the accommodating cavity to monitor the temperature and the vacuum degree in the accommodating cavity.

In addition, a control valve is arranged on the vacuum-pumping pipeline between the four-way joint 433 and the vacuum-pumping device 400. Therefore, the opening and closing state of the control valve is reasonably changed according to whether vacuum pumping is needed or not and pressure maintaining is needed or not, so that the vacuum pumping device 400 can pump vacuum.

The reactor housing 301 is described below with reference to fig. 8-10, the reactor housing 301 comprising: an outer housing 310, an inner housing 320.

As shown in fig. 8, the inner housing 320 is connected to the outer housing 310 at the inner side of the outer housing 310, a containing cavity a for containing activated carbon is defined in the inner housing 320, the inner housing 320 and the outer housing 310 together define a circulating cavity b for containing a heat exchange medium, and the circulating cavity b includes a liquid inlet cavity 321 disposed adjacent to the inner housing 320 and a liquid return cavity 311 communicated with the liquid inlet cavity 321 at the outer side of the liquid inlet cavity 321.

That is to say, hold and to hold the active carbon that can hold in the chamber a, the active carbon holds chamber a inner shell and is easily impregnated by the prescription and then modified processing to make the active carbon can adhere to the impregnating solution, and then have better adsorption performance. The heat exchange medium (such as oil) flows from the external drying device to the liquid inlet cavity 321, fully exchanges heat with the inner shell 320, flows to the liquid return cavity 311, and flows back to the external drying device from the liquid return cavity 311, so that the heat exchange medium circularly flows to realize continuous heat exchange. Certainly, when the heat exchange medium in the circulation cavity b is the liquid with higher temperature, the heat exchange medium can be used for heating the accommodating cavity a, and conversely, when the heat exchange medium in the circulation cavity b is the liquid with lower temperature, the heat exchange medium can be used for cooling the accommodating cavity a.

It should be noted that the flow-through chamber b may be partially defined by the outer housing and partially defined by the inner housing 320, or the flow-through chamber b may be located between the inner housing 320 and the outer housing 310. The liquid inlet cavity 321 and the liquid return cavity 311 may be distributed in sequence in a radial direction away from the receiving cavity a.

Therefore, the circulation cavity b is directly formed in the outer shell 310 and/or the inner shell 320, and the liquid inlet cavity 321 is arranged close to the inner shell 320, so that the heat exchange medium can be directly contacted with the inner shell 320, the problem of large energy loss of the coil type heat exchanger is avoided, and the full utilization of heat or cold is realized.

In some embodiments, the shape of the liquid inlet chamber 321 corresponds to the shape of the inner casing 320, and the liquid inlet chamber 321 is disposed around the inner casing 320. Specifically, the reactor shell 301 has a double-cone shape, and the liquid inlet cavity 321 includes a cylindrical cavity and two truncated cone cavities respectively connected to two ends of the cylindrical cavity. From this, feed liquor chamber 321 forms annular heating structure, and heat loss is less, and can be more even to holding the active carbon heating in the chamber a.

In some embodiments, the liquid return chamber 311 extends linearly, and the liquid return chamber 311 is opposite to a portion of the liquid inlet chamber 321 on the outer side of the liquid inlet chamber 321. Therefore, the space occupied by the liquid return cavity 311 is small, the space is saved, the heat exchange between the liquid return cavity and the liquid inlet cavity 321 is reduced, and heat or cold can be intensively used for heating or cooling the accommodating cavity a.

As shown in fig. 9, the inner shell 320 and the outer shell 310 are both a solid of revolution disposed around the central axis e, the two ends of the inner shell 320 disposed opposite to each other in the direction of the central axis e are respectively formed with a feed port 322 and a discharge port 323, the middle portion of the reactor shell 301 along the direction of the central axis e is formed as a rotation center f, the rotation center f is perpendicular to the central axis e, and the feed liquid chamber 321 is configured to feed liquid from a position close to the rotation center f and discharge liquid from a position close to the feed port 322 and the discharge port 323 to the return liquid chamber 311.

From this, under the more abundant prerequisite of guaranteeing that reactor shell 301 is rotatory so that hold the active carbon in the chamber a and be impregnated, make feed liquor chamber 321 can be closer to rotation center f to can make the feed liquor structure not influenced by reactor 300 rotation, compromise circulation and the rotation of reactor shell 301 of the heat transfer medium of circulation chamber b.

As shown in fig. 10, a second rotary connector 330 is further included, the second rotary connector 330 being connected to at least one of the outer housing 310 and the inner housing 320, the second rotary connector 330 being adapted to be inserted into the liquid inlet chamber 321 and the liquid return chamber 311 to independently communicate with both.

Specifically, the second rotary joint 330 includes at least: and a second rotating shaft seat 331 installed in the middle of the sidewall of the reactor shell 301, the center of the second rotating shaft seat 331 forming a rotation center f, the second rotating shaft seat 331 penetrating through the outer shell 310 and sequentially extending into the liquid returning cavity 311 and the liquid inlet cavity 321, the second rotating shaft seat 331 having a liquid inlet 331a communicated with the liquid inlet cavity 321 and a liquid returning port 331b communicated with the liquid returning cavity 311.

Thus, the heat exchange medium enters the liquid inlet chamber 321 through the second rotary connector 330 or flows from the liquid return chamber 311 to the second rotary shaft base 331. The problem of complex arrangement caused by complex pipelines is avoided, and heat exchange media are directly introduced and discharged by means of the second rotary connecting piece 330, so that the whole arrangement of the reactor shell 301 is more compact and reasonable, and the cost is lower.

Further, the second rotating shaft base 331 has a liquid returning inner hole 331c communicating with the liquid returning port 331b, and a liquid inlet inner hole 331d connecting with the liquid inlet 331a, the liquid returning inner hole 331c is used for connecting with an external liquid passing pipeline, the liquid inlet inner hole 331d is separated from the liquid returning inner hole 331c by a separating member 331e, and the liquid inlet cavity 321 is used for connecting with an external liquid inlet pipeline through the separating member 331 e. Wherein, an external liquid passing pipe and an external liquid passing pipe may be formed in the second rotating shaft 332 for connecting the reactor shell 301 and the base 302, and the second rotating shaft 332 is fixedly connected with the second rotating shaft seat 331 so as to drive the reactor shell 301 to turn over together when the second rotating shaft 332 is driven to rotate. Thus, the external liquid passing pipe enters the liquid inlet cavity 321 from the middle through the liquid inlet inner hole 331d and the liquid inlet 331a of the second rotating shaft seat 331, flows along the circumferential direction and the two ends, enters the liquid returning cavity 311 through the outlet 321b of the liquid inlet cavity 321, finally flows to the liquid returning inner hole 331c through the liquid returning port 331b, and is finally discharged through the external liquid passing pipe.

As shown in fig. 9, the liquid inlet chamber 321 is integrally formed by the inner housing 320, and the liquid return chamber 311 is integrally formed by the outer housing 310. That is, the liquid inlet cavity 321 is directly processed in the inner casing 320, and the liquid return cavity 311 is directly processed in the liquid return cavity 311, so that the liquid inlet cavity 321 can be communicated with the liquid return cavity 311 only by arranging a communication port at a corresponding position of the inner casing 320 and the outer casing 310. Thereby being more convenient for processing and production.

Optionally, the liquid inlet chamber 321 has an inlet 321a and an outlet 321b, and a plurality of partitions 324 are disposed in the liquid inlet chamber 321 between the inlet 321a and the outlet 321b, as shown in fig. 3. Specifically, the partition 324 may be provided with a through hole to allow the liquid in the liquid inlet cavity 321 to flow from the inlet 321a to the outlet 321b and further to the liquid return cavity 311, of course, the partition 324 may be a non-annular plate, the number of the partitions 324 may be more than one, and the heat exchange medium flows through the gap between the partitions 324 to flow from the inlet 321a to the outlet 321 b. Therefore, the baffle 324 is arranged to prevent liquid entering from the inlet 321a from directly flowing to the outlet 321b in the overturning process of the reactor shell 301, so that heat exchange media can fully exchange heat with the inner shell 320 in the liquid inlet cavity 321, and the activated carbon is heated or cooled more uniformly.

In the actual manufacturing process, the device for manufacturing the activated carbon may include a vacuum pumping device, a drying device and a reactor, the parts are connected by a pipeline, the vacuum pumping device may include a vacuum pump, the reactor may be a double-cone reactor, and the double-cone reactor is a device for containing the activated carbon and impregnating the activated carbon.

In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example.

While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.

Claims

1. A preparation method of supported activated carbon is characterized by comprising the following steps:

2. The method for preparing according to claim 1, wherein the operation method of the vacuuming treatment comprises the following steps: sealing the reaction kettle filled with the activated carbon, and vacuumizing the sealed reaction kettle until the vacuum degree is selected from any one of the following numerical value ranges: 0.04-0.06 MPa, 0.059-0.061 MPa, 0.01-0.03 MPa.

3. The preparation method according to claim 2, wherein the vacuum degree in the reaction kettle is maintained for more than 20min after the vacuum pumping is carried out to the corresponding numerical value range.

4. The method according to claim 1, wherein the vacuum degree in the reaction vessel is maintained for 25 to 30 minutes.

5. The preparation method according to claim 1, wherein the active component in the impregnation liquid comprises diethylenetriamine or tetraethylenepentamine, and the mass content of the active component is 10-15%.

6. The preparation method according to claim 2, wherein the mass ratio of the activated carbon to the impregnation liquid is 1: (2.5-3); or the mass ratio of the activated carbon to the impregnating solution is 1: (3.9-4.1).

7. The method according to any one of claims 1 to 4, wherein the time for the dipping treatment is 50 to 60 min.

8. The preparation method according to claim 7, wherein in the dipping treatment process, the stirring is carried out for 30-60 s every 8-10 min; the stirring is realized by the integral rotation of the reaction kettle.

9. The method according to claim 1, further comprising the following steps of heating and drying after the dipping treatment:

carrying out solid-liquid separation on the obtained system, and heating and drying the obtained activated carbon loaded with the impregnation liquid: controlling the temperature in the reaction kettle to rise to 90-100 ℃ for a preset time, then pumping out the water vapor in the reaction kettle, simultaneously ventilating the reaction kettle with the outside, and controlling the temperature in the reaction kettle to be kept at 75-85 ℃ for the preset time;

and (4) reducing the temperature in the reaction kettle after drying, and discharging after the temperature reaches 40-45 ℃ to obtain the finished product of the activated carbon.

10. The production method according to claim 9,

in the step of dipping treatment, the rotation mode of a reaction kettle is set as follows: the rotating speed is 10-12rpm, and the rotating time is 45-47 seconds every 15-17 minutes; and/or

In the heating, stoving treatment step, set up reation kettle's rotation mode: after stopping for 3-5 seconds every 45-47 seconds of forward rotation, reversely rotating for the same time.

11. The method according to claim 1, wherein the initial concentration of the impregnation fluid is 10% to 15%.

12. The method according to claim 1, wherein the temperature of the dipping treatment is 50 to 70 ℃.

13. The supported activated carbon prepared by the preparation method of any one of claims 1 to 12.

14. The device for preparing the loaded activated carbon according to claim 13, which comprises a vacuum pump, a reaction kettle and a dosing box, wherein the reaction kettle is connected with the vacuum pump and/or the dosing box through a valve; the reaction kettle is connected with a pressure gauge.

15. The apparatus of claim 14, wherein the reaction vessel, vacuum pump and dosing tank are connected by a three-way valve when the reaction vessel is connected to the vacuum pump and dosing tank via valves.

16. An apparatus for preparing the supported activated carbon of claim 13, comprising:

a reactor, the reactor comprising: the reactor comprises a base and a reactor shell, wherein the reactor shell is rotatably connected with the base, an accommodating cavity and a circulation cavity are arranged in the reactor shell, the accommodating cavity is used for storing materials, the circulation cavity is used for accommodating a heat exchange medium, and the circulation cavity is arranged at the outer side of the accommodating cavity and separated from the accommodating cavity; and

and the vacuumizing device is connected with the accommodating cavity so as to vacuumize the accommodating cavity.

17. The apparatus of claim 16, wherein the evacuation device is in communication with the receiving cavity via an evacuation conduit, the reactor shell is pivotally connected to the base via a first rotary connection on one side, the first rotary connection comprises a first rotary shaft and a first rotary shaft seat fixed to each other, the first rotary shaft seat is fixed to the reactor shell, the first rotary shaft and the first rotary shaft seat are both hollow, and the evacuation conduit axially passes through an inner hole of the first rotary shaft and an inner hole of the first rotary shaft seat on one side of the reactor shell.

18. The apparatus of claim 17, further comprising a first swivel connected to the first shaft at an end of the first shaft facing away from the reactor shell, the first shaft being fixed to the base and rotatable relative to the first swivel, the evacuation tube passing through an inner bore of the first swivel and being fixed to the first swivel.

19. The apparatus of claim 18, wherein the outer wall of the first shaft is provided with a first coupling flange for rotatably engaging the first shaft, the outer wall of the adapter is provided with a second coupling flange, the first coupling flange and the second coupling flange are coupled by a fastener, the first shaft has a positioning slot, the first adapter is inserted into the positioning slot, and the first shaft is rotatable relative to the adapter.

20. The apparatus of claim 16, wherein the reactor housing comprises:

an outer housing;

interior casing, interior casing is in the inboard of shell body with shell body coupling, inject the chamber that holds that is used for holding the active carbon in the interior casing, interior casing with the shell body is injectd jointly and is used for holding heat transfer medium's circulation chamber, the circulation chamber is including being close to the feed liquor chamber that interior casing set up and in the outside of feed liquor chamber with the liquid return chamber of feed liquor chamber intercommunication.

21. The apparatus of claim 20, wherein a side of the reactor housing is provided with a second rotary connection to at least one of the outer housing and the inner housing, the second rotary connection adapted to be inserted into the liquid inlet chamber and the liquid return chamber to independently communicate therewith.

22. The apparatus of claim 21, wherein the second rotational coupling comprises at least:

the second rotating shaft seat is arranged in the middle of the side wall of the reactor shell, the center of the second rotating shaft seat forms a rotating center, the second rotating shaft seat penetrates through the outer shell and sequentially extends into the liquid returning cavity and the liquid inlet cavity, and the second rotating shaft seat is provided with a liquid inlet communicated with the liquid inlet cavity and a liquid returning port communicated with the liquid returning cavity;

the second pivot seat have with return the liquid hole of liquid mouth intercommunication, with the feed liquor hole that the inlet is connected, return the liquid hole be used for with outside cross liquid pipe connection, the feed liquor hole with return the liquid hole and separated by the partition piece, just the feed liquor chamber passes through the partition piece is used for connecting outside liquid inlet pipe way.

23. The apparatus of claim 20, wherein the inlet chamber has an inlet and an outlet, and wherein a plurality of baffles are disposed in the inlet chamber between the inlet and the outlet.